I N O R G AN I C

G E N E RALj M E D I CAL AN D PHA R M A C E U T I C A L

C H E M S TR Y
TH E O R ET I CA L AN D PR A C T I C A L

A TE XT BO O K -
AN D LA BO RA T O R Y M A N U A L

C O N T A I N I NG

T H E O R ETIC A L , D ES C R I PTIVE , T E C H N O L O G I C A L C H E M I S T R Y ; C L A S S E XE R C I S E S
AN D IN

C H E M I C A L E Q U ATIO N S A N D M ATH E M ATI C S ; A N D PR A CTI C AL M A N U F AC

TU RI N G PR O C E S S E S FO R FI VE H U N D R E D C H E M I C A L PR E P
A R A T I O N S WITH E X PL A N ATO R Y N OT E S
,

O S CA R O L D BE R G ,
Ph a r m . D .

P R OF E S OR O F H A R AC I RE C T OR O F T H E H A R A C E T I CA
S P M Y D P M U L A B OR A T OR I E S
L AND
E A N OF T H E FAC T O F T H E C H O O O F H A R A C
,

D U L Y S L P M Y OF N O R T H
W E S T ER N N I ER I T C H I CA G O U V S Y ,

I N T WO VOL UM E S

VO L U M E II .
—
I L L U S TR ATE D

1 900

C H I C A GO M ED I C A L BOO K C O M PA N Y
C H I C AG O
E N ERE
T D A CC OR D I NG TO A CT O E C O NG RE S S I N 1 900, A T TH E O FF I C E OE
E G I S T ER C O RIGH T I A RY O NG RE SS
,

R OF PY S, L B R OE C , BY

O S CA R OL D B E R G .

ALL R I G H T S R E SE R V E D .
 PR E F A C E TO T H E S E CO N D VO L U M E .

The laws and conditions w hi c h govern chemical reactions

and their d irection velocit y and relative approach to completi on
,

have been treat e d o f in the first volume including the necessary ,

conditions O f success in preparation work so far a s they may be

indicated by general principl es T h e materials an d methods
.

employed for t h e p r o d u c t i on o f inorganic pharmaceutical prepa

’

ration s were pointed out in a general w a y the subj ect o f oxidation ,

and reduction was full y discuss ed an d the us e o f chemical ,

equations an d stoechiometry explained and exemplified .

Part I o f the second volume discusses more fully the i nte l l i

'

gent choice o f method s materials and apparatus and the p ra c

, ,

tical manipulations o f actual laboratory operations in the produc

tion o f inorganic preparations and Part I I contains detailed
,

descriptions o f th e modes of preparation o f five hun dred inor

g a n i c chem icals These proces
. ses shoul d be o f practical val ue to
pharmacists and manu factu ring chemists as well as to teachers
and students Chemical laboratory work in the schools has in
.

the past been almost exclusively analytical work ; but the at l east
equal value and importance o f practical work in the production
o f chemical compounds i s now fully recognized .

O S C A R O L D B E R G;
S c h o ol ofP har m ac y of N ort h w e s tern U n i v e r s ity ,

Ch i c a g o 1 900
, .
 C O N TE N TS
O F T H E S E C O N D VO L U M E .

3PA R T I

GE N E RA L PR I N C I PL E S A N D M ET H O D S APP L I CA B L E
IN T H E P R O D U C T I O N O F I N O R GA N I C
C H E M I C A L P R E PARA T I O N S .

C H A PT E R I .

Ch o ice o f M e t h od s a nd M a t e ri a l s

C H AP T E R II .

Cr u s h i n g and P o w d e ri n g
C H AP T E R III .

D ry Che m ic a l P r oc e s s e s
C H AP T E R I V .

S o l u ti on I t s N at u r e C au s es a n d E ff e c ts
.
, 24 - 3 2

C H AP T E R V .

S ol v e nts S o l u bi lit y S o lu ti o n s
.
,

C H AP T E R V I .

T h e Cl ari fi c ati o n o f L i q u i d s S tr a i n e r s P r e s s e s
.
, , F iltrati on

C H AP T E R V I I .

E v a p or ati on

C H AP T E R V I I I .

C H AP T E R I X .

C H AP T E R X .

Cr y s t a lli z ti o
a n fr o m S ol u ti o n s

C H AP T E R X I .

0 0 0 0 0

CH AP T E R X I I .

P r e c i p it ati on 1 00 - 1 1 6

C H AP T E R X I I I .

Ch e m i c al S ol uti o n . W et O x i d a ti on W e t Ga s
. O p er ti ns
a o .
‘
1 1 7 - 1 27
 TA B L E O F C ONT E N T S .

C H AP T E R XIV
AG E S
.

U se s o f fi n i s h e d P r o d u c t s P u ri fi c a ti o n o f C ru de Ch e m i c als
U n . .

W h at t o do w ith D a m a g e d Pro d u cts P ro fi t ab l e Ch e m i c a l .

W or k
/

1 28 - 1 3 2

C H AP T E R X V .

T he P r e s e rv ati o n of M e di c i n al S u b s t a n ces : 1 3 3 - 1 40

C H A PT E R X V I .

S o l u b iliti e s of Ch e m i c a l Co m p oun d s in W a t e r a nd in A l c o h ol . 1 41 - 1 50

C H AP T E R X V I I .

T h e D e n s iti e s of S o li d s a nd L i q u i d s T h e M o h r W e s t p h a l B a l
.

ance H y dro m e te rs
. P y c n o m e t e r s et c
.
,
1 5 1 66
1 -

C H AP T E R X V I I I .

R u l es fo r M a k i n g S ol u ti o n s O I A n y Gi v e n S tr e n g th a nd fo r ,

D il u ti n g F o rti fy i n g a nd M i x i n g
, . 1 6 7 1 78
-

C H AP T E R x rx
’

L ab orat ory F u rn it ure a nd A pp aratu s . 1 7 9 — 1 96

L b r t ry R u l es a nd P r
a o a o e c au ti on s Wh a t t o do in
‘

A cc i d e nt s
H w t o Cl ea n A pp r t
o a a us A “ .

PA R T l l .

L A B O RA T O RY M A N U A L O F I N O R GA N I C CH E M I C A L
PRE PA RA TI O N S .

W i gh t a nd
e s M r
e asu e s

A cid s
O th e r P r e p ara ti on s _ . .

T ab l e s
I nd e x
 I LLUS T R ATI O N S .

P o rc e l a i n M orta rs
S p at u l a s
D ru m S i e v e
Cru c i b l e s
Cru c i b l e T on g s
P e r fo r ated P or c e l a i n B a s k e t fo r Cir c u l at o ry D i s p l ac e m e n t in
Ch e mical S ol"uti o n
W e i g h i n g B ottl e .

D r Ric e s L y s i met e r
’
.

B u c h n e f F u nn e l .

P e r fo rat ed D i s Cs for F u nn e ls
C r o p F unn e l
D e c a n t a ti o n O v e r a G r e a s e d R i m
U s e o f t h e Gu i d i n g Rod i n D e c a n t a ti o n
“ ”

C asser o l e

A ut o m ati c F il tr ati o n A rr a n g t
eme n s

S tra i n e r S ta n d
i

an d

T e n a cul um
U s e o f S iri al l S t ra i n i n g Cl o t h
~

W itt ’
s P re s s
Cy li n d ri cal Pr e s s
M o h r s Pf es s
’

C orru g ated F il te r F u n n e l
P e r for at e d P o r cel a i n F u n n e l s
P e rforated P l at i n u m C o n e fo r F il ters
P a p e r F ilt e r s .

A pp a ra t u s fOr H o t F iltra ti o n
F ilt e r P u m p .

F iltr ati o n w ith P r e s s ur e

E v a p o r a ti o n D ish e s
P o r c e l a i n S tirr e rs
D e s i c c a t or
L ab orat ory T h e rmo m e t e r
L i b i g s Cond e n ser
e
’
.

S q i bb U p ri gh t Cond e ns er
’
u s

M it h l i h
sc er C o nden se r
sc
’
s
 iii I LLU S T R AT I O N S .

Re t o r t; T u b u l a t ed .

G l a s s T u b e F itti n g s for Co nn e c ti o n s in D i s tilli n g A pp r t

a a us

a n d Ga s A pp a r a t u s

T his t l e T u b e a n d S a fe t y T u b es
C o r k B or e r
P e r forat e d R u bb e r S t o pp e r s
A pp ar at u s S t a n d s

Cry st alli zr e of Gl a s s
H ow S m a ll C r op s of Cry s t al s M ay B e D ra i n e d
Ce n t r i fu g a t or
D i al y s e r
T u b u lat e d Pr e c i p it ati o n a n d D e c a n t ati o n V ess el of P o rc e l ai n .

Pr e c i p it ati o n Ja r o f G l a s s
B e ak e rs
P r e c i p it ati on F las k s E rl e n m e y e r ,

S p rit z B ottl e s . .

K i pp s A pp a ra t u s
’
.

Gas E v o l u ti o n A pp a ra t u s
W a s h B ottl e s
W oul ff B ottl e s
M oh r W e s t p h a l B a l a n c e
-

Py c n o m e t e r s
D r S q ui b b s Py c n o m e t e r s
’
.

G ra d uat e d F l a s k s
H y d rom e t e rs
Gr a d u a t e d Cy li n d e rs
Gr a d u at e d G l a s s M e a s u r e
F l e t c h e r s L o w T e m p e r at u r e B u r n e r
’ “

F l e t c h e r s R a di a l B u r n e r
’

B u n s e n B u rn e r s
E rl e n m e y e r B u r n e r
Ga s F l a m e s
R o essl e r F u rn a c e .

B a rt h e l s S pi rit L a m p
’

W ir e Cl o t h fo r B ur n e rs
T ri p o d s
S a nd b at h D i s h e s
-

W a t e r b at h s
-

I n s t a n t a n e ou s W a t e r H e a t e r
D ry i n g O v ens C o p p e r ,
 CH E M I CA L PR E PA R AT I O N S .

C H AP TE R I .

TH E C H O I C E O F M E T H O D S A ND M A T E R I AL S .

1 . The method s o f preparation by which inorganic pharma

c e u t i ca l products are obtained may be physical process es not

resulting in any alteration o f the mol ecul es o f the material s

operated upon or they may include chem i cal as well as physical
,

ch anges .

M any processes of preparation are purely phys ical ch an ge s of

f orm such as comminution si fting drying fusion subl imation
, , , , , ,

solution crystallization t u rbi d at i on physical precipitation gran

, , , ,

u l a t i on etc
, .

O ther phys ica l processes o f preparation are me th ods of se para

t i on or extraction by which one or more o f the component i n
,

g e di e n t s o f mixtures are separated

r The m eans employed for .

this purpose include fus ion subl imation distillation solution

, , , ,

filtration c rystallization physical precipitation and other

, , ,

methods .

Pr oce s se s of p u ri fi cat i on are o f cours e also essentially

, ,

methods o f separation o f d i ff erent k inds o f matter from each

other ; but distinction may well be made between a m i x t u r e of
tw o or m or e s u bs ta n c es and a crude product or natural m a t e r i a l
,

c ons i s ti ng a l m os t w h ol ly of o n e s u bs t a n c e contaminated with

“
smal l proportions o f other substances which are regarded as i m
”
purities Proces ses o f purification are frequently pu rely phys i
.

c a l processes ; but they are much more frequently c h e m i c a l proc

esses .

Pr oce s se s of pr odu ct i on o f chemical substances are always

chemical processes resulting in the formation o f new molecules .

But all chemical proces ses inclu de physical operations .

2 . To recognize clearly how the processes employed in the

laboratory may or may not be accompanied by chemical reactions
the student i s invited to note th e d i ff erences between : I t he ,

3
4 TH E C H O I CE OF M E T H OD S AN D M AT E R I AL S .

purely phys i c al pr oc e s s of s u bl i m a ti on by which the volatile ben

zoic acid contained in benzoin is separ ated from the non volatile -

resin and other fixed substances with which it i s associated and ,

the c h e m i ca l s u bl i m a ti on by which m ercuric chloride i s produced

from a m ixture O f mercuric sulphate and sodium chloride ; 2 the ,

purely phys i ca l pr oc e s s of tr i tu r a ti on by which any single sub

stance may be reduced to powder and the tri tu r a ti on by mean s ,

o f which mercury an d iodine are brought into contact w ith each

other for the purpos e o f causing them t o u ni te ch e m i c ally to form
mercurou s iodide ; 3 the purely phys i ca l pr oc e s s of fus i on by
,

which metallic bismuth is l iquefied so that it may be run O ff

from accompanying in fus ibl e mineral s and the f us i on to i n d u c e ,

c h e m i c a l c om bi n a ti on by which iodine and arsen ic are melted

together to produce iodi de o f arsenic ; 4 the s i mpl e di s ti ll a ti on ,

by which the eth er contained in a m ixture o f alcohol and ether

may be to a great extent s eparated from the alcohol and the ,

c h e m i ca l di s ti l l a ti on by which ether is pr o d u c e d and separated

by d istilling it from a mixture o f alcohol and sulphuric aci d ; 5 ,

the s i mpl e s ol u ti on by which z inc chloride i s dissolved in water ,

and the c h e m i c a l s ol u ti on by which metallic z inc is d issolved in

hydrochloric acid to form zinc chloride ; and 6 the phys i c a l pr e ,

c i pi t a ti on by which alum is s e pa r a t e d from its water solution by -

the addition O f al cohol and the c h e m i ca l pr e c i pi ta ti on by wh ich

,

alum inum hyd roxide is pr od u c e d when an alum solution is mixed

with a solution o f sodium carbonate .

.3 A ll the var i ous processes o f preparation separation p u rifi , ,

cation or production o f chemical s may be conveniently clas sified

,

into : I d ry processes ; and 2 wet processes

, , .

D ry pr oce sse s are those in which the materials employed are

not l iquid at the ordinary room temperatures nor dissolved in or ,

m ixed with any l iquid .

T h e m a te r i a l s employed in dry processes are accord ingly either

sol ids or gases ; bu t th e s ol i ds m ay be l i q u e fie d by f us i on or th e
g a s e s l i q u e fi e d by c o n d e n s a t i on I n most dry process
. es the ma
t e r i a l s are exclusively solids .

The pr od u c ts Obtained by dry processes may be either sol ids ,

l iqu ids O I gases ; but they are in most cases sol ids s epa rable by
’ ‘

fusion or sublimation or solids a n d gases

, .

'

D r y processes include tritu ration fusion subl imation d e by , , ,

d ra t i on ignition calcination roasting d ry distil lation

, , , , .
 TH E C H OI CE OF M E T H OD S AN D M A T E R I AL S .
5

We t pr oce sse s are those in whic h the m a te r i a ls employed include

l iquids whether the l iqui d or l iquids employed constitute chemi
,

cal factors O r are used as simple solvents or other physical media

to promote the attainment o f the ends sought .

The pr od u cts o f w e t processes may be solids l iquids or gas es , ,

.

The w e t processes include solution cr y stall ization precipita , ,

tion distillation and var ious other methods

, ,
.

4. The ch oi ce of me th od must be determined by : I the nature ,

o f the product sought ; 2 the material s availabl e for its produc

,

tion 3 the nature of the bye products i f any ; and 4 the chemi
,
-
, ,

cal laws g overning the behavior o f factors and p roducts in all

ca ses where the results depen d upon chemical changes or re a c
tions .

A mong the most important facts to be considered are the state

o f cohesion relative water solubility an d relative vo latil ity o f the
,
-

products and material s ; then the various chemical reactions which

may be util ized to convert the diff erent availabl e material s into
the products desi red and the s eparability o f the s evera l products
,

f rom e a ch other when more than one product i s formed

r

5. M ost o f the chem ical p roducts are sol i d s For the pur .

pos es o f this treati s e we shall cl a ss i fy the sol id chemical products

into s ol u bl e s ol i ds and i ns ol u bl e s ol i ds ; into v ol a ti l e s oli d s and
n on vol a ti l e s ol i d s ; and into f u s i bl e s ol i d s and i n f u s i bl e s ol i d s
-
.

The wat e r sol u bl e me t a l l i c s a l t s are very generally produced

-

from the corresponding acids Thus th e water soluble metallic .

-

nitrates are generally made from nitric acid sulphates from sul ,

p u r i c acid chlorides from hydrochloric acid acetates from acetic

h , ,

acid a n d s o on The processes employed for this purpos e are

,
'
.

c h e m i c a l s ol u ti on s a t u r a ti on o r n e u tr al i z a ti on
,
followed by the
-

requisite method of separation o f th e products from the by e

products The material s required in addition to the acids are the
.

'

metals themselves or thei r oxides h y droxides o r carbonates or ,

other compounds yiel ding uno bj ectionabl e bye products water - —

or gases .

The water soluble metallic compounds may also be made by

-

d ou bl e d e c om pos i ti on between factors producing insolubl e bye

products .

I n s ol ubl e m e t a ll i c comp oun ds are most frequently made by pr e

ci pi t a ti on the materials emplo y ed being water solutions o f the
,
-

required factors and the bye products being water solubl e - -

.
6 TH E C H O I C E or M E T H OD S A N D M A T E R I A L S .

l i d s may be made by s u bl i m a ti on i f no volatile bye

V ol a t i l e so

product be formed .

N on vol at i l e sol i d s when not produced by chemical soluti on or

-
,

by precipitation may be made by variou s dry processes including

, ,

double decomposition between d ry materials i f the by e product -

be volatile so that it m a y be eliminated by sublimation or by d iss i

p a t i o n with the aid o f heat .

F u si bl e s ol i d s are frequently made by fusion when the bye

product i f any i s in fusible so that separation i s practic a ble
, ,
.

L i q u i d p r odu ct s are generall y produced by chemical distil

lation or by chem ical solution
,
.

6 . Gase s are generally produced by metathesis or by dissocia ,

tion at high temperatures

, .

7 . From the facts mentioned in the preceding paragraphs t h e

'
student will note that the se p ar abi l i ty of t h e pr odu ct s is an ex
t r e m e l y important factor in the selection o f methods for the pro
duction o f chemical s A ssum ing that t w o products are formed
.

( which is generally the case ) they may of course be readily

, , ,

separated and the process thus rendered practicabl e : I i f one ,

product be solubl e and th e other insoluble ; 2 i f one product be ,

non volatile and the other volatile ; 3 i f one is a fusible solid and
-
,

the other in fusible ; 4 i f one be a gas and the other a solid or

,

l iquid at the temperature o f the reaction ; an d 5 i f one product ,

be water or some other l iqu id which i s unobj ectionabl e or easily

separated from th e other product .

8 . But two or more soluble salts contained together in one

solution or mixture may frequentl y be separated from each other
( )
6 i f they di ff er materially in their respective ratios o f solubility
in the sam e solvent at any conveniently attainabl e temperature ;
or ( 7 ) i f one be soluble without alteration and the other insol uble , ,

in another l iquid m iscibl e without chemical reaction with the com

mon solvent for both .

Thus i f A and B be both contained in nearly equal proportions

in solution in the same water an d i f A be freel y soluble while B
is only sparingly solubl e it follows that when the solution is con
,

c e n t ra t e d by evaporation B must separate from the s olution before

A A nd i f A and B be both contained in solution in the same

.

water and i f A be insoluble in alcohol and in diluted alcohol while

B is soluble in either then A must be precipitated on the addition
,

o f alcohol whil e B remains in the l iqu id .

 TH E C H O I CE OF M E T H OD S AN D M A T E R I AL S .
7

9 . The prognosis o f the reactions which will probably take

place between the factors brought into contact w ith each other in
any chemical process is g enerally ren dered practicabl e by a good
knowl ed g e o f the conditions which are known to a ff ect their d i r e c
tion and relative completeness such as : I the qual ity quantity
, , ,

and intensity o f the chemical combining power o f the elements

composing the factors o f the reaction includin g the greater ,

energy o f radical s in the nascent state ; 2 the influ ence o f predis ,

posing a ffi nity ; 3 the freedom of contact between the factors in

, ,

clu ding the removal of one o f the products from the scene o f
action and the influence in that d irection o f the cohesion s olu ,

bili ty fusibility and volatility o f the products ; 4 the influence o f

, ,

temperature ; and 5 the relative masses o f the reacting sub

,

stances .

Thes e matters were discus sed i n Chapter XI X o f Vol I . .

10 T he di ff erent form s o f chemical reacti on were fully de

.

scribed in Chapter X V I I o f Vol I The most common reactions . .

by which inorganic chem ical products are formed are : D i s s oc i a

ti on or dec omposition ; S y n th e s i s or combination or composition ;
, ,

M e ta th e s i s or double decomposition includ ing S u bs ti tu ti on ; and

, ,

reactions o f O x i d a ti on a n d R e d u c ti on or reactions inv olving ,

chan g es o f atomic polarity value -

.

11 Th e ch oi ce of mat er i al s The factors or materials that can

. .

be used for the production o f chemical preparations may generally

be any substances contain ing or furnishing the elements composing
the product sought Thus any compound o f mercury can be made
.

out o f any other compound o f mercury and any io dide can b e ,

employed for the preparation o f any other iodine compound .

But the best material s are those that g ive satis factory results
with the l east expenditure o f tim e an d labor and at the least cost .

Hence w e would not make mercuric iodide out o f m ercuric sul

phate nor out o f aristol or any other expensive or compl ex iodine
,

compound .

Th e materials necessa ry are generally in any g iven case t w o ,

one o f the m to contribute the positive radical and the othe r t o

contribute th e negative radical o f the product sou ght .

There are usually s everal kinds o f inexpensive material s avail

abl e ; but the cheapest materials frequently demand the mos t
t edious and expensive processes whil e easy and inexpensive ,

method s are general ly appl icabl e when the materials are o f a

8 TH E C H O I C E O F M E T H OD S A N D M AT E R IAL S .

higher grade Cheap raw materials are therefore used only in

.
, ,

manu facturing on a lar g e scal e with al l the labor saving devices -

a n d s p e c i a l facilities requ isite to obtain satis factory results at the

'

least cost .

To prepare pharmaceutical chemicals and other pu r e ch e m i ca l

p r o d u c ts it is necessary to employ as far as practicable ,materials ,

of definite composition and free from any impurities that can not
be easily removed in the process adopted U nfit material s furnish .

unfit prod ucts .

12
. Th e most common mat er i al s employed for the production
o f pure inorganic chemical s are :
A cids and thei r solut ions .

A lkal ies and thei r solutions .

The metals .

M etallic Oxi des .

M etallic hydroxides .

M etallic carbonates .

S oluble metallic sulphates nitrates phosphates acetates and

, , ,

other solubl e metallic oxygen salts .

S oluble metall ic chlorides bromides and iodides

, .

The non metalli c elements chlorine bromine iodine sulphur

-
, , ,

and carbo n .

13
. Whenever solutions o f acids alkalies or salts or other , , ,

solutions are employed as material s it i s necessary that thei r ,

strength shall be exactly determined and that the relative pro

p ortions u sed be governed accordingly and the quantitie s pre ,

scribed i n stated formulas must be corrected in every instance as

required .

The a c t ua l s tr e ng th o f acids ammonia water and other sol u

, ,

tions frequently varies materially from the O ffi cial or commonly

recognized standards and from the stren gth specified on the label
or indicated by the title .

I f the material s be crystallized substances containing water o f

crystallization they must be in per fect condition either containing ,

the known full amount o f such water or dried until they ceas e ,

to lose weight or attain a definite compos ition in accordance with

which the proportion requi red for the reaction may be exactly
determined It is cl ear i f 1 0 0 Gm o f crystallized sodium car
. .

bonate is required that 1 0 0 Gm o f e ffl or e s c e d sodium carbonat e

,
.

must be too much ; an d that i f one kilogram of an anhydrous salt

 C H AP TE R I I .

CR U S H I N G AN D POWD E R I N G .

16 . It is frequently necessary to cru sh solid substances pre

paratory to their use as material s .

A large piece may be broken on the anvil with a hammer or ,

in an iron mortar by wel l di rected blows with the pestle To .

prevent the fragments from being scattered the piece may first
be wrapped in several thicknesses o f strong paper .

Cr u s h i ng m a c hi n e s or iron m i l l s are u se ful for coarse c om m i n u

tion when the substance to be c ru shed or coarsely ground does
not cons ist o f or conta i n p i eces too large to be put through the
machine .

Hard and tough minerals l ike manganes e di oxide in lumps ,

h aematite i ron sulphide ant i mony sulphide marble and other

, , , ,

materials used in con si derable quantities may be a dvantageously ,

broken crushed and even powdered in a deep iron mortar

, , , .

17 . S om e mineral s wh ich are too unyielding to be crushed and

powdered in the iron morta r without other aids may be h eated
t o dull redness or near it an d then while hot d ropped into cold
, , , ,

water Thi s treatment sometimes renders such substances much

.

more tractable H aematite can be reduced in that manner This

. .

plan is o f course not appl icable to substances which are d e com

, ,

posed or fused by the high temperature .

18 . The i r on mor t ar must be large and deep and the pestle ,

heavy enough t O d O a considerable portion o f the work o f con

'

tus ion by its own weight .

S mall mortars are practicall y u seless for such purposes as the

c r u s h i n g a n d pulverization o f hard and tough substances becaus e ,

the quantity operated upon at one time must not be greater than
that barely su fficient to cover the bottom o f the mortar to the
depth o f about I O to 5 0 millimeters accordin g to its size , .

A n i t on mortar a bout 0 5 0 meter deep and meter in

diameter i s perhaps most us eful in the average laboratory being ,

su fficient for the e ff ective contu s ion o f as large quantities as can

be conveniently treated all at once and not too large for much ,

10
 CR U S H I N G AND O W DE R I N G
P . I I

smaller q uantities When a very large quantit y o f any material

.

is to be crushed or powdered it is o f course n e c essary to divide , ,

it into portions not too large for e ff ective work .

A larger i ron mortar is probably too heavy for general labora

tory use but an a dditional mortar o f about one third the d i m e n
,
-

sions specified will be found use ful occasional ly .

B eing very h eavy the large iron mortar should be placed firmly
upon a sol id foundation preferably on a wooden block fixed in th e
,

ground and resting on a large stone

‘

Fi g . S ma ll i r on m or t a r .

Fi g . 1 . L g i
ar e r on m or t a r . Fi g . 3 . S h lla ow i r on m ort a r .

The iron mortar and pestle are more generally use ful and e f
f e c t i ve than any crushing machines or mill s for ordinary opera
tions Insoluble sol ids rarely attack iron and may be powdered
.

in the iron mortar without becoming contaminated with iron .

E ve n soluble chem icals may frequently be sa fely permitted to

come in contact w ith iron ; but the mortar and pestle must be at
all times kept bright and cl ean quite free from rust —
.

Perfectly dry chemical s can usually be sa fely pulverized in a

bright dry iron mortar ; but moist chemical s an d such as contain
,
12 CR U S H I N G A N D POW DE RI NG .

water o f crystal lization shoul d be powdered in porcelain mortars .

Very brittle or friable substances that can be eas ily crushed and
reduced to powder by trituration in a porcelain mortar S hould not
be powdered in the iron mortar ; nor should a n y acid or alkali ‘

Fi g 4 S te e l p S l
atu a use d wi t h sma ll
i i di h
. .

r on m or t a r s and r on s es .

o r other substance which may act chemically upon the iron be ,

placed in it ,
.

19 Por ce l ai n mor t ar s for crush ing an d powdering chemicals

.
,

and for mixing powdered material s should l ike the iron mortar , , ,

be very capaciou s in proportion to the quantities triturated a t

Fi g . 5 . T it r i
u r a t on m or t a r of p or c e a nli
one time in them bu t not so deep S everal S i zes o f porcelain
,
.

mortars are required varying from 1 0 0 to 4 0 0 millimeters in

,

diameter and o f a depth equal to about t w o thi rds o f the diameter -

.

I t i s very important that every morta r shall have a regular ,

“ ”
spherically concave smooth bottom free from nipples and
, ,

“
wrinkles or from el evations or irregular depressions o f any
,

kind and that its pestle shal l fit it perfectly T h e convex head

,
. .

o f the pestl e must be large and perfectl y spherical but o f a ,

sl ightl y smaller radius than that o f the cur ved bottom or grinding
surface o f the mortar The handle o f the pestle mu st be large
.

and strong so that it can be firml y gras ped with the whol e hand
 CR U S H I N G AN D P O W D E R I N G . I 3

in Order that su fficient pressure may be conveniently exercised in

the act o f tritu rating .

E ff ective trituration is impracticable when the quantity o f

material contained in th e mortar is too great and the best results ,

are attained when the layer o f powder is not greater than that r e
quired to well cover the bottom o f the mortar .

When large crystals are to be broken or

cru shed in the porcelain mortar su fficient care ,

shoul d be exercised to prevent the scattering

o f the fra gments and it is sometimes best to
,

w rap the large crystal or piece in muslin O r F i g 6 S l i

gggép
. . p rc e a n
a

paper .

O nly comparatively brittl e substances can be eas ily powdered

by trituration .

20. When d ry pois on ou s s u bs ta n c e s are triturated in a mortar ,

care must be taken to prevent the danger from dust ris ing out o f
the mortar It is sometimes advisable to moisten the contents
.

O f the mortar with water or alcohol i f admissible A rs enous oxide .

a n d mercuric oxi de are good examples o f substances that ought

not to be triturated or s i fted in a dry condition i f considerable

quantities are thu s treated so that the operations are too extensive
and extended to be sa fe .

21
. The s pa tu l a is indispensable in employing trituration as a
means o f reducing subst ances to fine powder and in mixing pow
dered materials for most substances have a tendency to adhere
,

Fi g . 7 . S te e l p
S l
atu a .

more or less to the surfaces of mortars and pestles when tritu rated
under pr essure and must be scraped off with the spatula
, .

22 L e vi g a ti on i s the trituration o f a powder to an extremely

.

fin e state o f d i v i s i on on a S lab with a muller adding a l iqu id a s

,
, ,

either water or oil to form a very so ft paste with the powder

, .

But the levigation m a y al so be very advantageousl y e ff ected in a

perfect morta r with a per fect pestle instead o f using a sla b and ,

mull er .

23 S ometimes levigation is followed by e l u tr i a ti on

. This .

process consists in agitating finely powdered insolubl e substances

with large quantities o f water then perm itting the coarser par ,
I 4 CR U S H I N G AN D P O W DE R I N G .

t i cle sto subs ide during a brief cessation o f the agitation af ter ,

which the l iquid hol din g the finest powder still in suspens ion is
, ,

decanted into another vessel By repeated alternate levigatio n .

“
and elutriation th e product may thus be reduced t o an i m p a l
”
p abl e or extremely fine powder Prepared chalk and purified .

antimony sulphide are thus treated .

24 D ry substances which have been powdered by grinding

.
,

contu sion or trituration require s i f ti ng i f it i s necessary to render

thei finen ess uni form or to remove any coarse particles the p ow
r

ders may contain The s i e ve s may be made o f hair cloth s ilk or

.
, ,

brass wire gauze The finest powders a re s i fted through boltin g

“
'

cloth o f silk Insoluble inorganic substances shoul d be reduced t o

.

the finest powder attainable and should in no case be coarser than ,

N O 80 . .

The numbers employed to designate the finenes s of powders

are al so applied to the sieves and they ,

refer to the meshes or openings to each

l inear inch Thu s a N O 8 0 s ieve i s . .

one havin g 8 0 meshes t o each l inear

inch o f the sieve cloth and a N O 8 0 ,
.

powder is on e that has been passed

through such a sieve It were better .

i f the diameter o f each mesh were

given for the meshes are not alwa y s
F i g 8 M t l i v w i t h ov se
quare
a
an d the
s e
wire
e
hair or thread
c e rs , , , ,

d m iv
. .

or ru s e e
not always o f the same calibre.

A s finely powdered inorganic substances are generally l ight

enough to rise into the ai r when s i fted in an op e n s i e ve makin g ,

the operation very troublesom e on account of the dust it is cus ,

t om a ry to us e d ru m s i e ve s or sieves provi ded with co ff ers above ,

and receptacles below Thes e covers are made o f d rum skin in .

wooden frames like thos e in which the s ieve cloth i s placed or _ ,

the s ieve frame an d covers are made of bras s or o f tinned iron .

For s i fting insolubl e inorganic substances the drum sieves made

wholly o f metal are gen erally most useful .

25 Ver y friabl e soft masses o f dried precipitates such a s

.
,

thos e o f magnesium carbonate bismuth subnitrate bismuth s u b , ,

carbonate etc can be powdered by g e n tly rubbin g them through

,
.
,
 CR U S H I N G A N D PO W D E RI N G . 1 5

the s ieve cloth with a comparatively soft brush or by rubbing ,

the pieces against the brass wire cloth in the s ieve .

Powders shoul d never be f or ce d through the s ieve i f a soft and

]

fine product is desired an d a fine soft powder shoul d be made in

,

every cas e where it is possible .

26 . Zinc tin and some other readily fusible metal s may be

, ,

“
reduced to smal l pieces or granulated by pouring the m elted
, .
fl
,

metal int o a p a n or bucket o f water .

27. Coarse powder or granular products may be Obtained by

precipitation granulation and t u r bid a t i on described elsewhere
, , ,
.
 C H AP TE R III .

D R Y C H E M I C AL P R O C E SS E S .

28 R e act i on s i n d u ce d by t ri t ur at i on
. . A few chemical com
pounds a nd pharmaceutical chem ical s o f indefinite compo sition
can be produced by triturating the dry materials together L ong
‘

continued trituration and strong pressure are nece s sary in such

c ases Chemical reactions brought about in t his way are generally
.

incomplete and the products accordingly impure and u n sa t i s fac

,

tory .

A nhydrous substances and many other per fectly dry chemical s

may somet i mes be intimately mixed with each other by light
trituration W ithout any chemical reaction ; this happens too in , ,

cases where at least partial reaction takes place between the same
material s i f tritu rated together under strong pressure or i f water
is added .

Crystallized hydrou s salts when triturated together may react .

upon each other and a wet mixture m ay be obtained without the

‘

addition o f any moistu re on account o f the libe ration o f the water

o f crystall ization .

When dry solids unite chemically under strong trituration the

synthes is may develop so high a temperature that means must be
tak en to control it Thus alcohol is added when mercury and
.

iodine are rubbed together to form iodide o f mercury ; the evap

oration o f the alcohol then lowers the temperature and prevents
the loss of iodine by vaporization .

29 F u si on is frequently resorted to in chemical operations

.
,

sometimes simply to separate fusible from in fusible substances ,

but in other cas es to induce chem i cal reactions between the mate
rials fused together .

Whenever the obj ect i s to induce chemical reaction the mate

rials shoul d i f practicable first be powdered and well m ixed
, ,
.

The temperature required to produce fus ion is obtained partl y

from the heat appl ied to start the reaction and partly from the
h eat generated by the reaction itsel f when once started .

The vessel s in which substances are fused di ff er widely accord ,

16
I 8 DR Y C H E M I C AL P R O C E SS E S .

granulated z i nc the iodides o f arsenic and sulphur potassium

, ,

cyanide an d sulphurated potassa .

D istinction is to be made between true fus ion ( sometimes called

”
igneous fus ion when accompl ished at a very high tempera
,

Fi g . 12 a nd 13 . Cr u c ibl e t on g s .

ture ) an d the s bl u t i on o f hydrous crystallized salts in thei r own

,

“
water o f crystallization when heated ( which i s called aqueou s
fu sion ) S e e par 3 3
. . .

30 I gni t i on without fus ion always h as for its obj ect a greater
.

or les s change in the compos ition o f the substance heated These .

changes include the expulsion o f volatile impurities the expulsion ,

o f water dissociation oxi dation and various intramolecula r rear

, , ,

rangements o f the atomic linking .

Ignition i s e ff ected in i ron pots clay crucibles and other ves , ,

s els and generally at very high temperatures The substances to

,
.

be subj ected to ignition are i f practicabl e first powdered and , , ,

when two or more substances are to be ignited together they are

first m ixed with each other as intimately as possible .

E xs iccation calcination and dry oxidation are examples o f

, ,

ignition .

31 D eh y dr at i on of s ol i d s
. The removal o f water held by .

chemical products i s called dehydration It is e ffected by various .

methods o f drying .

H yg r os c opi c m oi s tu r e may be expelled from solids by d e si cca

t i on The heat appl ied for this purpose must be su ffi cient to ac ;
.

compl ish th e Obj ect without unnecessar y loss o f time but not so ,

high that the product may be inj ured or lost by decomposition or

volatilization The sol id substance in coars e or fine powder or in
.

a gran ular or crystall ine condition according to its nature is , ,

spread out over the bottom o f a shallow dish an d care fully heated .

I t must be constantly or frequently stirred during the process o f

desiccation and when quite d ry the product should be a t on c e put
,
.
 DR Y C H E M I C AL P R O C E SS E S . 19

into prefectly dry warm containers which must be tightl y closed

, , .

S ome sol ids must be kept in fusion for some time in order to
render them anhydr ous .
'

U n stabl e or volatil e sol ids when moi st may o ften be success fully
dried over lime sulphu ric acid or other substances having a great
, ,

avidity for water This method o f des iccation will be described

.

later .

Wa te r of crys ta l li za ti on is eliminated by e ffl or e s ce n c e or by e x

s i c c a ti on .

32 . The partial or complete removal o f water o f c ry s ta l l i za

tion at common room temperatu res or its gradual expulsion by ,

moderate heat i s called e ffl or e sce n ce

,
.

S ubstances which crystalliz e with several molecul es o f water

do not hol d all o f that water w ith equal force Thus many salts .

lose a portion o f the water o f crystall ization at about 2 0 or 3 5 ° °

to 4 0 or °
but retain the remainder at higher temperatures .

( S e e also par .

S everal substances which give up a portion o f their water o f

crystallization at the common room temperatu res i n d ry a i r do
not e ffl or e s c e at the same temperatures i n m oi s t a i r .

When the gradual e fflore s c e n c e of a salt is desired the tempera

ture must be regulated according to the known results o f e x p e
r i e n c e with that pa rticular salt for no general rul e is appl icable to
,

di ff erent salts .

Large crystals shoul d be broken into small fragments be fore

being exposed to the ai r to e ffl ore s c e .

The e fflor e s c e n c e shoul d be effected in a current o f dry warm ,

-air and the substance subj ected to this treatment shoul d be sp read
,

out in a thin layer and occasionally stirred .

D ryi ng cl os e ts are necessary in all laboratories where chemical

products are made in considerabl e quantities .

33 . S ome readily water soluble su bstances in the form o f crys

-

tals containing much water o f crystallization dissolve in thei r

crystal water when heated They are t h e n s a i d to un dergo a q u e ou s
-

fus i on A lum sodium phosphate sodium carbonate ferrous sul

.
, , ,

phate sodium sulphate an d several other salts may be easily d is

, ,

solved i n their own water o f crystallization by heating the crystal s .

When the temperatu re is raised above that required to caus e

aqueous fusion the salt be g ins to give up its crystal water and
,
-
,
 DRY C H E M I C AL P R O C E SS E S .

final ly becomes dry although i t m a y still retain some molecul a rly

combined water i f the temperature is insu ffic ient to expel all .

34
. The amount o f water o f c rystallization expelled by heat
depends upon the temperature I f the substance contains two or
.

more molecules o f water it may give up one or more mol ec ules at

one given temperature and other molecules o f it at certain definite
,

higher temperatures .

S odium arsenate loses al l o f its s even molecul es o f water at

°
about 1 4 9 but five molecul es o f it are expelled by complete e f
fl or e s c e n c e at a gentl e heat .

35
. E xsi cca t i on i s a term u sed to signi fy the expul s ion o f
water o f cr y stallization by the aid o f heat .

D ried sodium carbonate sodium sulphate sodium phosphate

, , ,

alum ferrous sulphate magnesium sulphate and s everal other ex

, , ,

s iccated salts are common preparations .

S uch preparations are not always anhydrous but each e x s i c ,

c a t e d salt i f not anhydrous must contain a definite amount o f

water .

The d ried alum o f the Pharmacopoeia must be anhydrous ;

dried ferrous sulphate must consist o f two molecules o f
“
F e H S O 5 with not Over one molecule o f water ; dried sodium
,

carbonate o f the Pharmacopoeia contains two mol ecules o f water ;

and anhydrous sodium carbonate i s al so u sed .

In order to obtain products O f definite composition by e x s i c c a

tion it is necessar y that the crystallized or e ffl o r e sc e d sol ids shall
be subj ected to a fixed degree o f heat until they cease to lose
weight .

It is generall y ( but not always ) advantageou s to reduce crys

t a l li z e d salts to coars e powder before they a re subj ected to e x s i c
cation In some cases a so fter product is obtained when the
.

crystall ized salt is first e ffl or e s c e d at a tempera ture su fficiently l ow

to prevent aqueou s fus ion and th e exsiccation compl eted at the
,

lowest temperature su fficient to expel all o f the water which it i s

des ired to el iminate .

In all operations O f e fflor e s c e n c e and exsiccation it i s important

that the product be well protected against contamination by dust “

36
. D ry dissociation o f chem ical compounds yielding gaseous
decomposition products occurs in various laborator y processes
—
.

The production o f oxy g en by heating either potassium chlorat e

or mercuric oxide and other dry gas operations and th e conve r
,
-
,
 DR Y C H E M I C AL P R O C E S S E S . 21

S i on o f phosphates into illu strate the decomposi

pe p h o s p h a t e s ,

tion o f chemical compounds in a sol id state by heat .

B ut the most common exampl e o f dry dissociation by heat is

the p roduction o f metallic Oxides by strongly heating the h y
d r ox i d e s nitrates oxalate s sulphates or other salts a ff ording
, , ,

volatile bye products -

This i s called cal ci n at i on and it is so
.
,

nam ed becaus e l ime ( ca lr ) or calcium oxide i s obtained by

strongly heating calcium carbonate in l ime kilns .

A mong the metall ic oxides that may be prepared by calcination

are : m ag ne s i u m Oxide from the hydroxide or the carbonate ; the
,

oxides o f ca l ci u m s tr on ti u m and ba r i u m from the hydroxides

, ,

or the carbonates ; f e r r i c oxide from the hydroxide o r the oxalate ; ,

c u pr i c Oxide from t h e hydroxide or the n itrate ; z i n c oxide from

, ,

the hydro x ide or the carbonate ; m e r c u r i c oxide from the nitrate ; ,

l e a d oxide from the hydroxide or th e carbonate or nitrate ; and

,

bi s m u th oxide from the hydroxide

,
.

37. D ry oxi dat i on i s o ften e ff ected by the c om bu s ti on o f metals

in free access o f air or by the i g n i ti on o f reducing agents with
,

oxid izing agents or by r oas ti ng m etallic sulphides

,
.

A mong the metal lic oxides that can be produced by the oxida
tion o f the metals in air w e have magnesium oxide zinc oxide , ,

lead oxide an d mercuri c oxide .

The oxides o f z inc lead antimony and some other metal s can
, ,

“
be made by roasting their sulphides in the a ir .

A rsenites may be oxidized to arsenates by ignition with nitrates ,

and other analogous dry oxidations may be e ff ected with various

oxidizing agents such as manganese dioxi de potass ium d i ch ro ,

mate and l ead dioxide

, .

38. S u bl i mat i on Volatil e sol ids may be vaporized and the

.

vapor condensed to the sol id state again either in the upper and
cooler portions o f the same vessels in which the soli d substances
‘

are heated or in su itable receivers connected therewith

, .

The vessels employed are special flasks o r retorts o f glass earth ,

e n w a r e or metal and the condensing receptacles i f any a re r e

, ,

quired may be cones or chambers O f the same materials or o f

,

paper etc , .

Calomel mercuric chloride iodine mercuric sulphide arsenous

, , , ,

oxide ammonium chloride ammonium carbonate an d certain

, , ,

other substances may be prepared or purified by sublimation .

I n the separation o f volatile sol ids from fixed solids by means

22 DRY C H E M I C AL P R O C E SS E S .

oi heat the volatile substance may be an impurity which it may

,

or may not be worth while to c ollect by condensation or the vola ,

tile substance may be the chief product and the fixed subs tances
impurities .

The condensed volatile sol id i s called a s u bl i m a te .

In processes o f sublimation the con denser is usually closer to the

vessel in which the vapor i s produced than is the ca se in distilla
tion because the di fference between the temperatu re to which the
,

vapor l s heated and that at which it is condensed is not great .

The subl imate may be in the form o f fine powder as in the ,

case o f calomel or in large aggregated crystal s or crystalline

,

masses as in corrosive sublimate or in large amorphous masses

, , ,

as in arsenous acid when manu factured on a large scale .

When the subl imate must be i n a finely divided condition th e

vessel in which the vapor i s formed must be kept at a su fficiently
high temperature in every part to prevent any condensation o f
the vapor before it passes into th e condenser and the condenser ,

must be cooled considera bl y below that temperature .

But when large masses o f sublimate ( whether crystall ine o r

amorphous ) are desired the condensation must be e ff ected at a
,

temperature but l ittle l O Vv

e r than that o f the vaporization O f the

solid and in such cases the product is frequently collected in the

,

upper part o f the same vessel in which the vapor is produced ,

or the whol e apparatu s incl uding connecting tube and condenser

, ,

must be kept hot enough to insu re the desired result .

When a flask or retort i s emplo y ed for the vaporization it is

“ ”
necessary to guard against choking caused by the accumulation
o f subl imate in the neck whereby th i s may be nearly or qu ite
closed The neck must there fore in all processes o f sublima
.
, ,

tion be quite short and in some cases it must be occasionally

, ,

freed from sublimate by raking the latter out .

In some cases it i s the best plan when the quantities operated ,

upon are not too large to use tall enough cyl indrical vessel s o f
suitabl e m
,

aterial vaporiz ing the solid at the bottom o f the

,

cyl inders and l etting the vapor be condensed at the up per end
which is to be rather loosely closed with chalk stoppers paper ,

or clean cotton The c y linders tubes or cylindrical wide

.
, ,

mouthed bottles used for sublimation are generally placed in an

,

inclined position .

[ T h e student may make a few preliminary experiments in sub

 DR Y C H E M I C AL P R O C E SS E S . 23

l imation by operating upon very small quantities ( say about ,

Gm ) o f any o f the following named substances : camphor ben

.
,

zoic acid iodine calomel corrosive sublimate m ercuric iodide

, , , , ,

mercuric sulphide ammonium carbonate ammonium chloride

, , ,

arsenous oxide U se a l ong test tube ; place the substance to be

.
-

subl imed in the botto m o f the tube ; use a test tube hol der to pre -

vent burning the fingers heat the lower third o f the tube espe ,

c i a l l y at th e bottom by movin g it up an d down in the flame o f a

,

Bunsen burner or a spirit lamp and let the sublimate be con

,

d e n s e d in the c oOl e r upper end o f the tube I f arsenous oxi de

.
,

or any mercury compound or other poisonous substance is ex

,

p e r i m e n t e d w ith care must be taken not to permit the escape o f

,

the po i sonous vapor and its inhalation ] .

 C H AP TE R IV .

S OLUT I ON —
I TS NATU R E C AU S E S AND E FF E C T S
,
.

39 . umerou s striking phenomena o f s ol ut i on are familiar to

N
all S ugar salt washing soda and many other solids are com
.
, ,

p l e t e l y liquefied when put in a su fficient quan tity o f water an d ,

the result in each cas e is a perfectly homogeneous l iquid .

Pieces of camphor when put in alcohol d i s s ol ve in that l iq uid ,

yielding a uni form solution containing no visible pa rticles o f the

camphor .

M etal lic iron placed in hydrochloric acid disappears as i ron

and i f a su fficient quantity o f acid be u sed a liquid is obtained
, , ,

in which no solid particles o f matter are vis ible .

R osin is taken up in sol ution by oil o f turpentine ; g lycerin

dissolves crystall ized carbol ic acid ; hot ol ive oil makes a perfect
solution with wax ; and benzin forms with lard an entirely homo
g e n e o u s liqu id .

These phenom ena o f the s ol u ti on of s ol i ds i n l i q u i ds are more

striking than solutions o f liquids in each other sol utions o f gases ,

in liquids and other instances O f intimate molecular blending of

,

two or more substances because we see that the pieces or particles ,

o i sol ids gra dually dissolve and finally disappear in the l iquid or
-

solvent .

40 We know further that many sol ids a re una ff ected by

.

water and by var i ou s other l iqu ids .

M arble does not dissolve in water alcohol ether chloroform , , , ,

benzin oil s or glycerin ; but it does d issolve in h y drochloric

, ,

acid in nitric acid an d in vinega r Glass is insoluble in nearly

, , .

all l iquids except h y droflu oric acid and strong alkal i solutions .

D iamond is insoluble in all liquid

41 Zinc chloride dissolves in les s than one third o f its weight
.
-

o f water ; potassium hydroxide in about one hal f o f its weight -

p o t a s s i u m i o d i d e in three
O fourths o f its weight ; sodium
-
thi o

sulphate in t w o thirds ; R ochelle salt in one and one hal f times its
- -

weight o f water ; alum in nine times its weight ; baking soda ’

requires nearly twelve times its weight o f water to dissolve it ;

24
26 S OLUT I ON —
I TS NATU R E C AU S E S AND
,
E FFE CTS .

But any two liquids which dissolve each other in certain

definite proportions bu t not in all proportions can be combined
into perfect homogeneous solutions by th e addition o f a thi rd
l iqu id m iscibl e in all proportions with each o f the other t w o .

44. S ol u ti on s of g as e s i n l i q u i d s are also formed I n fact, al l

.

gases are solubl e to some extent in all liquids although it o ften ,

h appens that the gas dis solves in the l iqu id so sparingly a s to

be regarded as practically insoluble .

O ne volume o f water dissol ves about volumes o f carbon

dioxide ; volumes o f h y drogen sulphide ; volumes o f sul
phur dioxide ; 5 0 3 volumes o f hydrochloric acid ; 1 0 5 0 volumes o f
ammonia .

A ny given vol u rn e o f any given l iqu i d dis solves a given number

o f volumes o f any given gas at any giv en temperature without
regard to the pres sure Thus one volume o f water dis solves
.

volumes o f carbon dioxi de not only at the ordinary atmospheric

pressure but also under twice that pres sure o r three or any
, ,

other number o f times that pressure ; but volumes o f carbon

dioxide under the pres sure of two atmospheres weighs tw ice a s
much or is twice as large a quantity o f carbon dioxide as the
same number of volumes o f that gas under the pres sure of one
atmosphere .

45. F or the purposes o f this book w e shall adher e to the

generally recognized d e fi ni t i on of s ol u t i on : th e lique faction o f
a n y substance by the action upon it o f a n y liqu i d the product ,

being a homogeneous clear liqu id made up o f all o f the liquid

used as a solvent and all o f the substance dissolved in it .

This definition recognizes no solvent except a l iquid solvent ,

and no solution except a liquid solution .

But in a more general sense we have also solutions of gases

in other gases solutions o f gases and sol ids in each other and
, ,

products of the process o f solution which are not liqu id The .

evaporation o f a liqu id into the air may be looked upon as a

solution o f the liquid in the gases o f which the air consists .

46. A real or pe r f e ct s ol u ti on is accordingly for the purposes

, ,

o f practical pharmacy and pharmaceutical ch e m istry a perfectly ,

homogen eous and clear liquid consisting o f one substance

originally in liquid form recogn ized as the solvent and on e ,

or more other subst ances which may have been p re v i ou s l v to their

,
 S OLUT I O N —
I T S NATU R E C AU S E S , AN D E FF E C T S . 27

solution eithe r sol id liquid or gaseous but which are contained

, , , ,

in the solution in a li quid form .

47
. S ol utions can in man y cases be separated again into
, ,

their original constituents Thus a solution o f salt in water can .

be boil ed down to d rynes s the water being thus eliminated by ,

vaporization leaving the whol e quantity o f th e salt in its original

,

sol id state and w ith its characteristic properties unchanged .

Water can also be at least partially separated from solutions by

freezing for onl y the water enters into the formation o f the ice
, .

A solution made o f glycerin and alcohol can be s eparated into

its original components by distilling it the volatil e alcohol form , ,

ing the distillate while the non volatile glycerin remains in the -

still or fla sk A solution o f ammoni a in water can be more or

.

less completely separated into H 3 N an d H , O by heating it

whereby the ammon i a i s expelled .

But when iron is dissolved in h y d rochloric acid o r zinc in sul ,

p h u r i c acid the,
metal can not be recovered from the solution nor ,

th e acid separated from it by any such s imple means because , ,

these solutions do not cons ist o f the original material s put to

gether but o f d iff erent substances formed by chemical reaction
,

between the original substances .

48
. S i mp l e s ol u t i on i s to be distinguish ed from chemical
solution by the fact that in s imple solution the ori gi nal mol ecules
o f the solvent and dissolved matter remain unaltered and no new
molecules are formed whil e ,

Ch e mi cal s ol u t i on results in the formation o f new molecules

which take the place o f the original substances .

It is s el f evident however that chemical solution is a chemical

-
, ,

reaction in which one o f the factors i s a li quid and resulti ng in

p roducts which form together a homogeneous liqui d by solution .

In other w ords chemical solution i s simpl e solution preceded

,

by a chemical reaction between factors o f which one i s a l iquid .

E xamples o f simple solution are very numerou s for nearly all

solutions in which water alcohol a volatile oil or a hydrocarbon
, , ,

i s the solvent are s imple solutions

,
.

A mong th e most common examples o f chemical solution are

the solution o f metal s m etall ic Oxides and h y droxides an d other
, ,

m etallic compounds in acids the solution o f brom ine or iodine

, , ,

or sulphur in alkal i solutions ; the solution o f iron and brom ine

, ,

or o f iron and iodine together in water ; the o fficial proces ses

, ,
28 S OLUTION —
I T S NAT U R E C AU S E S A N D E FF E C T S
,
.

for the preparation of solution of potassium arsenite solution o f ,

subacetate o f lead etc , .

49. S i mp l e s ol v e n t s or neutral solvents are l iquids which dis

, ,

s olve solubl e substances without c h emical change .

Ch e mi cal sol ve n t s are l iquids wh ich dis solve substances by trans

forming them into new an d di fferent substances the original ,

molecu l es o f both solvent and dissolved matter disappearing .

50. S ol u ti on i s ca u s e d by som e form o f m ol e c u l a r a ttr a c ti on .

I t i s generally ascribed to adhes i on the attraction be tween unlike

—

mol ecul es .

'
51.
_
M e n d e l e e fi describes solution s as fluid unstabl e definite , ,

” “
chemical compounds in a state o f di ssociation He says the con
.

c e p t i on o f solutions a s liquid dissociated definite chemical com

pounds is based on the following considerations : ( 1 ) that there

exist certain undoubtedl y definite chemical crystall ine compounds
( such as or N a Cl I O H O or
.
2 ,
etc ) .

which melt on a certain rise o f temperature and then form real ,

solutions [ see Pa r .
( )
2 that metall ic alloys in a molten
condition are real sol utions but on cooling they o ften give entirely
,

distinct and d efinite crystall in e compounds which are recognized ,

by the properties o f alloys ; ( 3 ) that between the solvent and

the substance dis solved there are formed in a number o f cases , ,

many undoubtedl y definite compounds such as comp ounds with ,

water o f crystallization ; ( 4 ) that the phys ical properties o f sol u

tions and especiall y their specific gravities ( which are v e rv a c
,

c u ra t e l y observable ) var y with a change in composition an d in ,

such a manner as the formation o f one or several definite but

dis sociating compounds woul d require Thus for example on .
, ,

adding water to fuming sulphuric acid its density is observed

to decrease until it attains the definite composition H S O , o r , ,

S O 3 + H 20 [ see Par . when the specific gravity increas es ,

”
although on further dilutin g with water it again falls .

“
T h e two aspects o f solution above mentioned and t h e h y p o , ’

theses which have as y e t been appl ied to the examination o f solu

tion s although the y have partially di fferent s t a rt i n g p oi nt s yet
, l w ,

will doubtless in time l ead to a general theory o f solutio ns be ,

caus e the s ame common laws govern both ph y sical an d chemical

phenomena inasmuch as the properties and movements o f mole
,

cules which determine ph y sica l properties are dependent on the

, ,
 S OLUTIO N —
I T S N ATU RE C AU S E S , AN D E F FE CT S .

9
'

movements a n d p r op e r t i e s o f the atoms which determine chemi ,

”
cal mutual actions .

52
. The student is a dvised to hold fast to the distinction be
tween physical and chemical phenomena a s indicated in the fore
going statement and to the di ff erence between a molecule con
,

sisting o f atoms united to each other by one complete system o f

atomic l inking in harmony with the doctrines o f polarity and
valence an d a combination o f unl ike mol ecul es hel d together by
,

some form o f molecular attraction evidently independent o f the

laws o f polarity and valence E very molecule has its own ( and .

o n ly one ) unbroken s y stem o f atomic linking whereby all of its

atoms are hel d together as one united whole ; but in such a com
pound as Ca Cl 6 H O it is impos sibl e to discover a nv l ink or
,
.
z

l inks between any atom o r atoms o f the Ca Cl on the one hand 2

and any atom or atoms o f the 6 H O on the other so that the Q ,

Ca Cl and 6 H zO must be held to each other by a m ol e cu l ar force

2

quite di ff erent from the a tom i c attraction which makes the mole
cule o f Ca Cl 2 a d istinct system o f atomic linking an d each mole
cule of H O another and equally independent system
Z
.

'

M oreover th e student m u s t r e i n e m be r that a salt combined

“ ” “
with the water called water o f hydration and that call ed water
”
o f crystall ization does not di ff er essentially in its chem ical prop
e r t i e s from the anhydrou s salt and that a dilute water solution
,
-

o f any salt i s abs o l u t e l y i d e nt i c al with any other equally dilute

.

water solution o f the same salt wh ether the kind o f salt used to
-
,

make the sol ution be the anh y drous salt or the salt containing a
maximum or a minimum amount o f water o f c rystall ization .

Water solution s o f sodium carbo nate all o f them absolutely

-
,

i dentical as to strength composition and every property can be

, , ,

made out o f either N a CO or N a CO 3 H O or N a CO 3 5 H zO

2 z
.
z , z
.
,

or o r N a CO ao O or N a CO I 5 H , O g g , z 3 . .

53
. A ll water solutions contain water as water
—
.

54
. D eliquescence indicates a molecular attraction o f t h e
del iquescent bod y for water resulting in the formation o f that ,

kind o f a combination or union ( o f the water and the deliquescent

body ) which we call a solution .

55
. But when water is added to 5 0 the result i s not a simple 3

solution but a chemical solution for H zS O 4 i s formed which is

, , ,

not
3 0 S OLUTI ON —
I T S N AT U R E C AU S E S AND E F F E C T S
, .

with H —
O —
H ,
but

O
I
H —
o
—
s —
O —
H .

l
0

A nd when H zS O
is brought into contact with another mole
cule O f water the resulting product is not a solution o f H zS O 4
in water but the chem i cal compound
,

or H ,SO

which contains no water .

I f still another mol ecule o f water be added the compound ,

H GS O 6 i s formed This too i s a true chemical compound or

.
, , ,

complete system o f atomic l inking and not a sol ution S ince it ,

contains only one kind o f molecules .

56 . We know that some substances are soluble an d others

insoluble in the same solvent ; that different solubl e substances
di ff er wi dely in their respective ratios o f solubility in the sam e
solvent ; and that a substance may be freely solubl e in one solvent ,

moderately soluble in another sparingly soluble in a third an d

, ,

quite insolubl e in a fourth solvent We also know that any given .

solvent dis solves the sam e quantity o f any given substance under
the same conditions B ut the law which must specially govern
.

solution and solubilities is not yet understood .

57 . That mol ecular attraction o f some kind has to do w ith

solution m a y be seen from the phenomenon o f deliquescence ;
from the fact that a contraction o f volume takes place when mis
cible l iqui ds are united into solutions ; from the upward di f
fus ion o f a heav y salt in water solution through superincumbent
-

pure water ; from the fact that when a water solution of a gas -

is heated it sometimes happens that water alon e is first e vap or

ated until the s olution acquires a certain degree o f concentrat i on ,

a fter which this solution containin g a definite proportion o f t h e

,
 S OLUT I ON —
IT S N AT U R E C AU S E S
,
AN D E F F E CT S .
’

3 I

gaseous substance evaporates without further separation ; an d

,

from other facts .

The wel l known fact that H Cl can not be evaporated off from
its water solution proves that th e H Cl and H 0 are held to 2

gether strongly ; but it does not prove that they are chemically
combined ( by any atomic l inking ) .

58
. Ost w a l d supports the conclusi on that salts in water solu -

tion are separated into simpler constituents He calls attention .

to the fact that aqueou s solutions o f salts and aqueous solutions

o f the stronger acids and bases al l o f which he calls s a l t s ol u,
-

“
ti ons for the sake o f brevity behave as i f they contained a greater
,

n u m be r o f molecules than corresponds with the formul ae of the

~

”
dissolved salts From thes e considerations and from the facts
.
,

o f electrolysis he concludes that salt solutions contain parts o f

,
-

the molecul es o r the i on s o f the salts Thi s is in agreement

, , .

’
w ith M e n d e l e e ff s definition o f solutions [ S e e also Chap
ter V I Par 1 3 1 V ol I ]
.
, .
,
. .

59
. The velocity o f reactions occurring in solutions may be at
once unde stood upon the theor y that the reagents are in a state
r

o f dissociation into thei r respective ions or radicals .

60 The di visibility o f matter i s most strikingly illustrated by

'

the color reactions which m a y be produced in certain extremely

dilute solutions and O stwal d points out that e l e m e n ta l r a d i ca ls
,

or ions present in a solution behave quite di ff erently from the

c om pou n d r a d i c a ls or ions containing the same elements Thus .

the negative ion o f a chloride Cl behaves di ff erently from the , ,

negative ion Cl O , o f the perchlorates ; the negative ion S o f , ,

the sulphides p roduces reaction s quite di ff erent from those pro

'

d u c e d by and the pos itive ion Co o f c oba l t salts behaves di f

f e r e n t l y from the negative ion CO ( CN ) 6 .

61
. The colors o f salt solutions are es sentially the colors o f
-

the ions contained therein ( O stwal d )

”
.

V ery dilute solutions o f cupric chloride ( containing little o f the

und issociated compound but many free copper ions ) are blue ;
but concentrated solutions o f the same compound are green ( be
caus e they contain fewer copper ion s and much undissociated
cupric chloride ) This and other examples are mentioned to
.

show that the color o f a sol ution i s sometimes du e to free ions and
sometimes to the undecomposed compound A solution o f .

chromic anh y dride does not contain H 2Cr O , for i f it did the , , ,
3 2 S OLUT I ON —
I T S N ATU R E C AU S E S
,
AN D E FF E C T S .

ions o f Cr O , woul d make it yellow ; but it does contain H 2Cr Z O 7

and is therefore colored red by th e ion Cr zO 7
, , .

A n interesting example not m entioned in O stwald s bo ok i s ’

that presented by ferrous and ferric salts I f ferrous chloride .

and ferric chlori de are dissociated into thei r respective ions by

solution it must be admitted that the ions o f both chlorides are
Fe and Cl ; but the green solution o f ferrou s chloride contains
d iad ferrous ions while the reddish brown solution o f ferric -

chloride contains triad ferric ions I t is true that t he di ff erence .

between ferrous iron and ferric iron is known o nly from their
compounds and that ferrous iron can be oxidized to ferric and
,

ferric iron reduced to ferrous so that the distinction between

”

diad iron a n d triad iron must depend upon their respective units
o f combining value actually used ( their respective polarity
values ) but the dissociated ferrou s and ferric ions in solutions
must still be respectively bivalent and trivalent s ince the removal
o f a n y ion from the solution can not be admitted .

T he color may depend on either positive or negative ions .

I f it be admitted that iron salts are in a state o f partial d i ssociation

“
when in water solution and that the colors o f salt solutions are
-
,
”
essentially the colors o f the ions contained therein then the solu ,

tions o f ferrous salts are colored green by the ions o f diad o r

ferrous iron while the solutions o f ferric salts are colored red
,

dish brown by the ion s o f triad or ferric iron Y et ferrous iron

—
.
,

and ferric i ron are both commonly regarded a s s ingl e atoms .

[ Ferrou s and ferric salts in the dry state are generally n early
white or very pal e but they exhibit a decided color as soon as
,

dissolved in water O ther anhydrous salts also exhibit di ff erent

.

colors when dissolved in water ] .

62 . O nl y acids bases and salts are believed to undergo dis

,

sociation in thei r water solutions I f this be true there are

-
.

numerous substances which form solutions without dissociation .

M oreover the compounds which become separated into their ions

,

by solution in water may dis solve in other liquids without

dissociation strong solution s m a y contain no free ions while
, ,

weaker solutions o f the same salt give evi dence o f partial disso
c i a t i on ; an d complete dissociation is not believed to be e ff ected

except in infinitely dilute solutions .

34 S OLV E N T S —
S OL U B ILIT Y —
S OL U TIO N S .

di ff erent liqu ids and o f di fferent substances in the same l iquid

, ,

m a y range al l the way from absolute insolubility to unl imited

.

solubility Fl int is absolutely insoluble in water and all other

.

simp l e solvents ; but a solution of ferric citrate may be evaporated

to complete dryness without a n y separation o f the salt from it .

65
. The relation o f the solubility of a substance to its chemical
composition is not understood Hence the chemical compos ition
.

does not furnish a reliable or consistent guide to sol ubil it y for ,

there are man y apparent exceptions or inconsistencies .

Thus whil e the hal ides o f the three common alkal i metals are
,

al l readi l y water solubl e and thos e o f l ithium more solubl e than

-

thos e o f sodium and potas sium their h y droxides an d carbonates

,

stand in the opposite order O f the hal ides o f calcium strontium

.
,

'
and barium tho se O f calcium are most freely soluble an d those
, ~

o f barium least so which woul d seem to agree with the order in

,

which the hal ides o f the alkal i metals stand to each other the ,

metal having the smallest atom i c we i ght forming the most readily
solubl e hali de B ut on the other hand l ead iodide is far more
.
, ,

readily S oluble than m ercuric iodide whil e mercuric chloride is ,

far more soluble than lead chloride The nitrates o f copper s il .

,

ver and lead are all very readily solubl e ; but while copper sul
phate dissolves in parts o f water silver sulphate requires 2 00
,

parts o f water for its solution an d lead sulphate parts .

S od ium dichromate is mor e soluble than sodium chromate ; but

potassium dich romate is less solubl e than potass ium chromate .

Borax i s solubl e in 1 6 parts o f water and cream o f tartar in ,

20 1 parts ; but the two substances together dissolve in a very

“
small amount of water to form borax tartar or potas sium s o - -

d i u m boro tartrate which is soluble in water without a n y limit

-
,

being del iquescent .

66
. The ratio of solub i l ity of a substance may be materially
a ff ected by its condition A hydrou s substance is frequently
.

more soluble than the anhydrous ; the amorphous substance may

be more or les s readil y soluble than the cry stall ized ; a substance
containing more water o f crystall ization is usually more rea dily
soluble than the same substance with a l es s percentage o f water ;
a recen t ly prepared chemical compound m a y be more or less
readil y soluble than the same substance a fter it has been kept a
long time ; dry heat ( as for instance fusion ) may al so a ffect the
, ,
 S oL VE N T s — S OL U B ILIT Y —
S OL U TIO N S .
35

solubility o f a sol id ; and solubilit y may further be aff ected by

contact with other su bstances .

Cr y stall ized A l ( O H ) 3 is d i ffic u l t ly soluble in acids while a ,

freshly precipitated amorphou s A l ( O H ) 3 is easily solubl e in

acids but gradually los es its solubilit y when kept .

67 . The presence o f one substance in a solution may very

greatly a ffect the solubility o f another substance in the sam e
l iquid Thus water solubl e potass ium salts are frequently i n
.
-

soluble i n saturated solutions o f ammonium salts ; potassium sul

phate is insolubl e in a saturated solution o f ammonium sulphate ,

potas sium nitrate in a saturated solution o f ammon ium nitrate ,

and potass ium carbonate in strong ammonia water Potassium .

sulphate is insoluble in a saturated solution o f potass i um carbon

ate and potass ium hydroxide in a solution o f calcium hydroxide
, .

The total d isplacement o f one salt from its solution by the

addition o f another salt can sometimes be eff ected
'

68 . O rganic su bstances which are soluble in water are f re

quently found to be nearl y or quite insolubl e in strong water
solutions Of inorganic substances Thus water solubl e salts O f.
-

the alkaloids are generally insolubl e in concentrated water solu —

tions of metallic salts ; pepsin soap an d various other substances

, ,

can be precipitated from thei r sol utions by metallic salts .

69 . O n the other hand it happens sometimes that the pres

ence o f one substance in a solution aids the solution o f another
substance in the same l iqu id as when ammonium chloride facili
,

tates the solution o f mercuric chloride .

70. M i xe d sol v e nt s .When two or more solids are dissolved

in a mix ture o f two or more l iqu ids a s eparation into d istinct lay
-

ers is sometimes the result .

A lthough alcohol and water are miscible in all proportions they

are sometimes separated from each other on the addition o f inor
g a n i c sal ts solubl e in water and organic substances soluble in
alcohol s o that an aqueou s sol ution o f the inorganic salt and an
,

alcoholic solution o f the organic compound form separate layers .

But certain singl e inorganic salts may also cause the partial
separation of mixed solvents by forming a separate solution with
each Hydroalcohol ic solutions o f manganese sulphate and al so
.
,

o f potassium carbonate m ay separate into two la y ers one o f

, ,

which is a concentrated water solution containin g but l ittl e

-
3 6 S OL V E N T S —
S OLU B ILIT Y —
S oL U T I O N s .

alcohol while the other layer consists chiefly o f alcohol contain

,

in g very little o f the salt .

71 . I mmi sci bl e s ol ve n t s Water and ether water and chloro

.
,

form and other pairs o f l iquids which are not solubl e in each
,

other in all pr o portions are frequently employed for the purpose

,

o f trans ferring certain substances from one solvent to the other ,

for removing a d issolved substance from its solution and for ,

separating d i ff erent substances from each other A substanc e .

dissolved in one o f the solvents m ay be divided between it and

the Second solvent or it may be almost completely washed out o r
,

withdrawn from its original solution .

72 . The partial removal o f the solvent from a solution by the

addition o f another l iquid which takes up the solvent with more ‘

or less avidity is frequently practicabl e Thus water may be par .

t i a ll y w ithdrawn from a strong salt solution by the careful add i

—

tion o f a superincumbent layer o f strong alcohol when it may ,

happen that the alcohol gradual ly becomes diluted and the salt
i s partially separated by crystall ization or precipitation from its
solution for want o f su fficient solvent .

73 . By the term ph y si cal pre c i p i t a t i on we mean the separatio n

o f a dissolved substance from its solution by the addition o f a
non solvent liquid miscible with the solvent
-
.

S ince alcohol an d water are m iscibl e w ith eac h other and many
substances which are soluble in one o f thes e l iquids are i nsolubl e
“
in the other various substances in water solution can be thrown
,
-

”
out o f solution by the addition o f alcohol and many other sub ,

stances can be in a similar manner precipitated from thei r

, ,

alcoholic solutions by the addition o f water .

A saturated solution o f K Cl made with pure water at

contains per cent o f the chloride ; but i f made with w ater
‘

mi xed with 1 0 per cent o f alcohol the saturated solution contains

only about 2 0 per cent o f the chloride an d i f mad e with a m ix ,

ture o f equal proportions o f water and alcohol it contains only

about 5 per cent o f the salt .

A saturated solution o f ferrou s sulphate ( F e H S O 6 H O ) z , z

made with pure water contains per cent o f the salt ( at

but a saturated solution o f the same salt made with a m ixtu re o f
60 per cent o f water and 4 0 per cent o f alcohol contains onl y
per cent of the ferrous sulphate .

A saturated water solution of copper sulphate at 1 5 contains

-
°
 S oL VE N T s —
SO LU B I LIT Y —
S OLU T I ON S .
37

per cent o f the salt ; but a saturated solution made with a

mixture o f 60 per cent o f water and 4 0 per cent o f alcohol con
tains onl y 5 per cent o f copper sulphate .

74 . To ai d s ol ut i on w e may employ such means as w ill bring

the solvent into intimate contact w ith the substance to be dis
solved and also any other agencies by which the l iquefaction o f
that substance is facilitated .

T o f a ci l i ta t e t h e s ol u ti on of a s ol i d the solid substance may b e

crushed or powdered in order t o expose a greater sur face to
the action o f the solvent and the sol id and solvent may b e
,

shaken or stirred together to further increa se the fre e dom o f

So l tiu on m or t ar of po r ce a n. li Fi g P f tdp li b kt
15 e r or a e or c e a n as e
di lvi g m l i id b y
. .

t or s so n e ta s n ac s
i l t di p l m t
c r c u a or y s ac e en .

contact between them I f the sol id S houl d rest on the bottom o f

.

the vessel in which the solution i s e ff ected and the solvent r e ,

' '

main at rest over the solid t h e n t h e solution first formed must

,

cover and surround the solid so as to prevent fresh portions o f

solvent from coming in contact with it ; but agitation s erves the
purpose o f distributing the solution throughout the whol e body o f
the liquid .

The solid may be placed in a mortar and triturated with succes

s ive portions o f the solvent each strong sol ution thus form ed be
,

ing poured off from the undissolved remainder and this con ,

t i n u e d until all o f the sol id shall have been dissolved By thi s .

mean s the quantity o f solvent required to complete the solution

may be reduced since it i s practicable to produce a practically
,

saturated solution with each portion o f solvent .

3 8 S OLV E N T S —
S OLU B I LI T Y —
S OLUT I ON S .

A nother eff ective method is that called c i r cu l a tory d i s pl a c e m e n t ,

which consists in placing the sol id substance in a perforated fun

nel dish or basket or in a ba g or on a colander or perforate d
, , , ,

diaphragm j ust be low the surface of the solvent so that the solu
'

, ,

tion formed may at once descend to the bottom o f the vess el per ,

m itting fresh portions o f solvent to freely attack the undissolved

remainder o f the solid until all of it has entered into solution .

H e a t almost always facilitates the solution o f soli ds in l iquids

because the heat opposes the cohesion which holds the molecules
o f the s olid together .

S ol ids which have a tendency to form clots or agglutinations

when wetted shoul d not be powdered t o prepare them for solu
“ ”
tion .S cal e salts o f iron dissolve much more readily when not
crushed o r powd e red ; res ins when d issolved in alcohol or in vola ,

tile oils shoul d be in pieces or in very coarse powder

,
.

A gitation col d and pres sure fac i li ta te th e s ol u ti on of g as e s i n

,

li q u i d s .

75 . A c on t r act i on of vol u me
nearly always results from solu
tion whether the subs tance dissolved be a sol id a l iqui d or a gas
, , .

I n other words the volume o f the resultant solution i s nearly

,

always l ess than the sum o f the original vol umes o f the solvent
and the dissolved matter B ut the Vol um e o f the solution i s .

al ways greater than th e vol ume o f the solvent alone .

When volumes o f water and volumes o f absolute

alcohol are m ixed the total volumes contract to form j u st
°
1 0 0 volumes ( at 1 5

76 . When no chemical action accompan ies the process o f solu

tion there is al ways a l iberation o f heat attendant upon a con
traction o f volume and an absorption o f heat attendant upon an
,

expansion o f volume resulting from t h e solution .

77 When a salt conta in ing a large amount o f water o f crys

.

t a lli z a t i on is dissolved in water the volume o f the solution may

exceed th e sum o f the original volumes of the salt and the water ;
but when an anhydrous salt capabl e o f taking up much water o f
crystallization is dissolved in water a contraction o f volume may
be expected Contraction o f volume occasionally tak e s place when
.

a concentrated water solution o f a salt is diluted with more water

-
.

78 R e l a t i on s of h e a t t o s ol u t i on
. R eference has al ready been
.

made to the l iberation o f heat du e to a contraction o f volum e in

the formation o f solutions But the s tudent shoul d know that .
 S OLVE NT S —
S OLU B I L I T Y —
S OLU T IO N S .
39

the rise or fall o f temperature attendant upon the formation o f

solutions must be a ffected also by various other influences A s .

sol ids must take up latent heat when they become liquefied by
solution it frequently happens that a very considerable reduction
,

o f temperature results when a readily soluble salt is dissolved

in water ; and as any gas must give up l at e n t h e a t when liquefied
'

by solution the temperature o f the water in which the gas i s being

d issolved frequently rises perceptibly B es ides there may be
.
,

various molecular combinatio n s taking place in the formation of

solutions and these may a ffect the temperature Finally chemi
, .
,

cal reactions al so cause changes o i the temperature .

When 1 7 Gm o f H N is compres sed to the l iqu id state it evolves

.
3

44 0 0 units o f heat ; but whe n it dissolves in 1 8 Gm o f water the .

same quantity of H S N evolves 7 5 3 5 heat units The 3 1 3 5 add i .

t i on a l heat units were generated by the chemical reaction by

which the H 3 N and the H 20 formed H 4 N O H .

When 3 0 parts o f absolute alcohol is mixed with 7 0 parts o f

water the temperature rises degrees which is not accounted
,

for by the contraction of volume It is assumed that the alcohol

.

combines in some w ay with a certain number of molecules o f

water .

When ether and chloroform are mixed in equal volum es the

temperature rises
B ut when equal volumes o f alcohol and carbon disulphide are
i x e d the temperature falls
That anhydrous compounds which take up water in molecular
combination d is solve in water with evolution o f heat is well
known ; but there are many exampl es o f the solution o f sol ids a t
tended by a considerabl e elevation o f temperature in which it i s
n ot known what compounds are formed i f any Great evol ution
,
.

o f heat attends the solution o f K O H in water ; but potassium

hydroxide is not know n to combine with water to form any d e fi
n ite compound [ N o system o f a t om i C linking o f K O and H
.
,

is poss ibl e except K O H ] .

A nhydrous calcium chloride takes up water to form a definite

hydrate and this hydration is attended by an elevation o f tem
r a t u r e ; but when hydrous calcium chloride i s dis solved in
p e

water the temperature falls .

79
. F r e e zi n g m i xt u r e s When readily water soluble salts are
.
-

put in a comparatively small amount o f water s a y about twice —

,
4o S OL VE N T s —
S OL U B I I T YL —
S oL U T I O N s .

their weight the temperature o f the water is greatly depressed

—

by the solution o f the salt The temperature may be reduced as .

much as 2 0 by various salts °

.

A m ixture of 3 parts o f crystallized calcium chloride and 2

parts o f snow will cause mercur y to congeal .

Two parts of snow or crushed ice and one part o f common

salt will make a very e ffective freezing mixture for ice cream -

freezers and for other pu rposes .

A m ixture o f 5 parts o f ammonium chloride and 5 parts o f

potassium nitrate with 1 9 parts o f water causes a fall o f 2 0 in the °

temperature o f the water .

8 0 H e a t g e n e ral l y i n cr e a s e s t h e s ol u bi l i ty of sol i d s an d l i qu i d s
. .

Boil ing water frequently dis solves many times as much o f a

metallic salt as c an be dissolved in cold water ; but any substance
which is quite insolubl e in cold water is also qu ite insoluble in “

hot water .

O ne hundred pa rts o f boiling water will hol d 50 parts o f p ota s

sium chlorate in solution ; but when s uch a solution is allowed
to cool to about I 5 only 6 parts o f the salt remain in solution
°

while the remaining 44 parts will cr y stall ize out .

A lum i s soluble in less than one third its weight o f boiling -

water but requires n ine times its weight o f water at 1 5 for its
,
°

solution .

Borax dissolves in one hal f its own weight o f boiling water -

,

but is not solubl e in less than 1 6 parts o f water at I

E ight parts o f water at 1 5 will dissolve no more sodium car °

bonate than i s soluble in 1 part of boiling water .

81 The increased ratio o f solubility o f a solid in water caused

by a ris e o f the te m
.

perature grows more rapidly than the heat

rises ; but the increased solubility resulting from a continued el e
vation o f temperature is o ften ver y irregular .

82 . S ome solids do not dissolve more readily in hot water

than in cold water Thi s is true o f acacia and some other soluble
.

varieties o f gum .

S odium chloride i s only slightl y more soluble in boiling water

than in water at 1 5 1 0 0 parts o f water at 0 dissolves
°
parts
°

of N a Cl 3 6 parts at
,
0 and parts at 1 0 0 °

A solution o f calcium hydroxi de made saturated at 1 5 loses °

about one hal f o f the dissolved hydroxide on being boiled ( W ith

-

ou t contact with the ai r ) .

42 S OL VE NT S —
S OLU B ILI T Y —
S OLUTION S .

ture the sol ution then cooled to any given lower temperature at
,

which it shoul d be kept for a day or two bein g occas ionally ,

shaken and its stren gth then found The results obtained by the
,
.

first method are liable to be somewh at too low and those obtained ,

by the second method are liable to be too high .

8 6 S olubilities are usually stated at

. and this is a very suit
abl e standard temperature for the express ion o f the solubil ity o f
solids because saturated solutions prepared at 1 5 are rarely
,
°

exposed to any lower temperature the average temperature o f the ,

work room being higher .

87 The most satis factory method o f determining the solubil ity

.

o f a salt in water at 1 5 i s to make a saturated solution at about

°

16
°
to 20 to set this solution aside for 2 4 hours at
°
shaking
it occas ionally ; the n filter ; then evaporate a weighed quantity to
dryness and weigh the residue .

I t is o f cours e n ecessary in carrying out this method to know

, ,

precisely what the res idue is wheth er

hydrou s or anhydrous and i f hydrous h ow , ,

much water it contains etc The result ,

.

shoul d be verified by analysis ; a weighed

quantity o f the salt being d issolved in a
weighed quantity o f water and this solution
anal y zed quantitatively the result to serve ,

as a check upon the composition o f the

salt and also upon the result o f a quantita ,

tive analysis o f the saturated solution ,

tm mm”
{i i g
f
fl a
which
ns
shoul
°
d
50
al so be per formed In other .

words the salt u sed to make the solution , ,

the saturated solution prepared from it and the residu e obtained ,

upon evaporating a given weight o f that saturated solution must ,

all be titrated and the results compared with the weight o f the
,

residue I f the salt i s hydrous the resi due must be dried at a

.

given temperature until it ceases to lose weight and i f p ra c t i , ,

cable al l of the water o f cr y stal lization or any other water con

,

t a i n e d in it should be expelled .

Dr R i ce s L y si me t e r
’
88 . . In order to determine the rate o f .

solubility o f a substance at a temperature c onsiderabl y higher tha n

o
that o f t h e ai r in the work room and to obtain a filtered sol ution ,

o f the same temperature as that at which the solution was

saturated D r Charl es R ice devised an instrument w h i c h h e gave
,
.
 S O LVE NT S —
S OLU B I L I T Y —
S OLUT I O N S .
43

the n ame lysimeter , which is here describe d and shown in fig .

17 .

T he lysimeter consists o f a glas s tube a which is 1 5 0 mill i , ,

meters long and 1 0 m ill im eters in external diameter provi ded at ,

one end with a well fit t i n g glass stopper c the oppos ite e n d o f

- -
, ,

t he tube being cup shaped with a con -

,

traction between the cup and the body

A
'

o f the tube a s shown i n the cut .

ground g lass bell e is made to fit into , ,

t h e cup . The bottom o f this bell i s per

f ora t e d as shown in f The ground .

glass stopper b al so fits into the cup

, , ,

and i s to be used to clos e th e cup after

the removal o f the bell .

T he quantity o f solution must be su f

fi c i e nt so that at l east one hal f o f the —

instrum ent can be immersed in it The .

solution may be made and contained in

a glas s cylin der a beaker or a wide , ,

test tube The us e o f the lysimeter may b

-
.

be i l l u s t rat é d by an exampl e as follows ,

assum ing that the solubility o f some sol id

in boil ing alcohol is to be determined : The stopper c
i s inserted int o the tube a and the glass bell e into ,

the cup shaped en d o f the tube A little pledget o f

-
.

pure cotton i s put into the bell e and hel d in place , ,

by a fine platinum wir e pass ing around the c ont ra c

tion or neck behind the cup and over the mouth o f
the bell A su ffi cie nt quantity of alcohol i s put in
.

th e v essel in which the solution i s to be made an d ,

heated by immers ion in hot water the powdered ,

solid being added to the alcohol in su fficient quan

tity to produce a saturated solution a small residue ,

remaining un dissolved a fter cont i nu i ng the boiling

o f the alcohol long enough The lysimeter i s now .

Df n i ii
ig
inserted prepared as described cup shaped end
, ,
—
'
a s
IY im t
downwards and when the instrument has as sumed
,
S f
’ er

the temperature o f the boil ing l iquid the stopper c i s removed ,

.

The alcoholic sol ution then enters the tube through the cotton
filter in the cup To insure uni formity of the solution the liquid
.
44 S O L V E N T s
-
—
S OLU B ILIT Y —
S OLUT I ON S .

may be allowed to flow back through the cotton once or twice .

The stopper c is now replaced the instrument w ithdrawn from ,

the vessel containing the remainder o f the solution and inverted , ,

a fter which the bel l e is removed and the stopper b i nserted in its
place The lysimeter now closed at both ends by the stoppers is
.
, ,

next washed exteriorly with a l ittle al cohol and laid as ide to Cool ,
.

T h e previo usly ascertained tare o f the stoppered tube deducted

from the total we i ght o f tube and contents leaves the net weight
o f the solution contained in it This is then trans ferred to a tared
.

dish orbeaker the tube is carefully rinsed with alcohol the wash
, ,

i n g s be i n g added to the solution which is then evaporated to d r v

,

ness Over a wat er bath an d finally the res idue heated to drynes s
-
,

in a drying oven and weighed .

In us ing the ly simeter with hot solvents the instrument shoul d

be gradually heated to th e temperature requ ired as a too sudden ,

change might cause its fractu re .

89 . Co e fli ci e nt s of sol u bi l i t y
-
The number o f weight units o f
.

any substance requ ired to saturate 1 0 0 weight units o f w a t e r a t '

any given temperature i s the c o e ffic i e n t o f solubil ity o f that sub

-
.

stance at that temperature .

We have stated that it i s the almost univer sal rul e to give the
solubilities o f solids in water ( and in alcohol ) at the temperature
of and the numbers expressing their c o e ffi c i e n t s o f solubil ity -
,

therefore refer to and are correct at that temperature only unles s

, ,

otherwise expres sly stated Thus when we say that the c o e ffi

.
,
-

cient o f solubil ity of borax is this statement mean s that 1 00

weight o f units of water at I 5 will dissolve °

5 w e ight units o f
bo rax to form a saturated solution The c o e fficient o f solubility .

o f sodium arsenate is 2 5 because 2 5 weight units o f the salt

N a H A s O , 7 H O will form a saturated solution w ith 1 0 0 weight
,
.
2

units o f water at
This method o f expressing ratios o f solubility has the a d va n
tage that the solubil ities o f di fferent substances in a constant quan
t ity o f solvent are directly represented by th e c o e ffic i e n t s so that -

comparisons are rendered easy an d direct Thus a substance .

,

whose c o e ffi c i e n t o f solubil ity i s 1 0 is twice as solubl e as one

—

whose c o e ffi c i e n t is 5 in the same quantit y o f solvent

-
, .

90 . A nother and more common method o f stating the solubili

ties o f substances a method employed in all pharmacopoeias is
— —

that O f giving the number o f weight units o f solvent required to

dis s olve on e weight unit of the substance Thus the Pharmac o
.
.
 S OL V N T SE —
S OL U B ILIT Y —
S OL U TIO N S .
45

p oe i a tells u s that sodium arsenate i s solubl e in 4 parts of water at

and that borax is soluble in 1 6 parts The solubilities of .

these two substances are i n i nve rs e r a ti o as the numbers express

ing the respective quantities o f solvent required to dissolve them .

91 Both m ethods o f expression are useful an d in labo ratory

.
,

operations w e find one o f them more direct and conven ient in one
case and th e other preferable in another case
,
.

'

I n this book we shall make use o f both methods according t o

ci rcum stances but the stu dent will observe that the c o e ffic i e n t s
,
-

o f solubility do d irectly expres s the proportions in which sub

stances can be d issolved whereas the pharmacopoeial method does
,

not d i re c t l y e x p r e s s the s ol u bi l i ty o f the substance in a given con

‘

stant quantity o f solvent but the p roportion o f solvent required

,

to d issolve a constant quantity o f the dissolved substance .

92 The student will see that

.

The number o f weight units o f solvent required to dissolve 1

w eight un it o f the soluble substance is the reciprocal o f the num
ber o f weight units o f the solubl e substance required to saturate
1 weight unit o f the solvent and vice versa ,
.

A nd as
The c o e ffic i e nt o f solubil ity o f any sol uble substance is th e
-

number o f weight units thereo f required to saturate 1 0 0 wei g ht

units o f the solvent ,

There fore ,

The number o f weight units o f solvent required to dissolve 1

weight unit o f the soluble substance i s found by dividing 1 0 0 by
its c o e ffi cient o f solubil ity or in other words by m u l tiply i ng th e
-
, , ,

r e ci pr oca l of i ts c o e fi c i en t of s ol u bi l i ty by 1 0 0
-
.

A nd
The number o f weight units o f any solubl e substance required
to saturate I weight unit o f the solvent i s found by dividing the
c o e ffi c i e n t o f solubility by 1 0 0
—
.

93 M ethods o f fixing and expressing t h e str e n gt h of sol u t i on s

. .

The strength or degree o f concentration o f a solution may be

.

fixed or expressed in various ways Probably no one method i s .

equally convenient for all purposes ; but the most generall y use ful
and accurate method is to expres s the strength o f the solution in
per cent by weight .

A mong the various methods in u se are the following

I The emplo yment o f arbitrar y scales o f degrees o f density
.
46 S OL V N T S S OLU B ILIT Y S OLUT I O N S
'

E — —
.

indicated by areometers or h y drometers such a s the scales o f ,

Baum e Twaddell an d others T h e strength of salt solutions

, ,
.
,

syrups acids gas solutions etc i s frequently indica ted by S ome

, , ,
.
,

special hydrometer scale .

2. The actual specific weight o f a solution may be employed to

indicate its relative strength .

3. The strength o f a solution may be fixed a s i s o ften done in ,

pharmaceutical preparations according to the number o f custom ,

ary weight units of the solubl e substan c e contained in any con

v e n i e n t volume o f the solution as for instance the number o f
‘

, , ,

grains or ounces to each fl u i d ou nc e pint or gallon or the number , ,

o f gra i n s in each l iter .

4. The stren g th o f mixtures o f alcoh o l an d water is some

times expres sed i n per cent by weight sometimes in per cent by ,

“
volume and sometim es in arbitrary degrees as in degrees
, ,

”
proo f etc
,
.

5. The strength o f gas solutions may be express ed in per ce nt

by weight or according to the number o f volumes o f the gas dis
,

solved by each volume o f the solvent and in other ways It i s ,

.

the custom to state the strength o f solution o f hydr ogen dioxide

according to the number o f volumes o f availabl e oxy g en o btain
“ ”

able from each volume o f the solution .

6. Volumetric solutions are so prepared that each li t e r o f

finished solution contains as many grams as the number o f units
expressing the mol ecular weight o f th e reagent divided by the ,

number expressing the val ence o f either o f its t w o compone nt

-

radi cals .

7. S olutions may also be made for laboratory us e which con

tain in each ki l og r a m a s many grams as the number o f units ex
pressing the molecular weight o f the dissolved Substance or a ,

convenient decimal proportion thereo f .

8. Finally the strength of solutions may be fixed and ex

,

pressed i n per cent by weight as i s the custom in stating the ,

stren gt h o f acids and other solutions of chemicals This method .

is the most convenient an d scientific especially i f at the same time ,

it in cludes the principle re ferred to in the preceding paragraph s o ,

far as app li cabl e or useful .

The molecular weight o f H Cl being it would be more con

v e n i e n t for laborator y pu rposes to have a solution ( h y drochloric

acid ) containing per cent o f H Cl than to have one containing

per cent .
 C H AP TE R VI .

TH E C LA R I F I C AT I O N O F LI Q UI D S S T R A I N E R S
. . P R E SS E S . FI LT R ATIO N .

94 . U ncl ear liquids r m ixtures o f liqu ids with undissolved

a e

sol id matter or mixtures of two or more li qu ids insolubl e in each

,

other .

L iquids containing suspended i nsolu bl e sol id or liquid particl es ,

or m i xed with any insoluble matter generally require clarification ,

be fore they can be advantageously employed .

The separation o f the undissolved s ubstances i s eff ected by

some one o f the various methods described in this chapter .

95 . Pi e c e s o f solids floatin g or submerged in otherwis e cl ear

l iquids may be removed by means o f per forated spoons or ladles ,

or with an ordinary spoon or by means o f pincers I f the solid

, .

is heavier than the liqui d the latter may be decanted from the
sol id or it m ay be removed by means o f a syphon
, .

Per forated porcelain funnels such as B u c h n e r s funnel ( fig

,
’
.

1 8 ) are very use ful for the s eparation o f

sol ids not too m inutely divided Perfor .

ated discs which can be placed in ordinary

funnel s are also much used ( fi g .

The li quid may also be passed through a

piece o f coarse thoroughl y washed sponge
, ,

or a loos e plu g o f pure cot

ton placed in an ordinary funnel or in a
,

cropped funnel ( fig .

96 . Cl ari fi ca ti on by subs i d e n ce S olid .

matter suspended in a l iqui d may be a l

lowed to subside a fter which the clear F i g 1 8 B h t l f uc ne r unne o
,
l n
. .

p or c e a i
liquid is decanted or drawn off For this .

purpose the turbid l iquid shoul d be put in a tal l or deep vessel

and le ft at perfect rest until all o f the solid matter ha s settled to
the bottom in as compact a layer o f s e d i m e n t as its character may
permit it to form I f the sol id matter is not too finely d ivided and
.

i f its density i s greater than that o f the liqu i d this method o f clari
fi c a t i on is readily carried out But when the sol id particles are
.

47
48 C LA R I F I C ATION O F L I Q U I D S S T R AI N E R S —
,
E TC .

extremely minute and espec ially when thei r density is about the
,

same as that o f the li qu id the operation is slow and di fficult i f ,

not impossible It is however frequently practicabl e to s u ffi

.
, ,

c i e n t l y lower the density of the liquid by dilution or by raising its

temperature .

Whenever admissibl e the clarification may be e ff ected by adding

a rather heavy insolubl e
substance such as purified ,

clay in powder which car ,

ries the other sol id matter

down with it as it descends
to the bottom o f the vessel .

The clay or other s u ffi c i e n t

l y heavy absorbent powder
emplo y ed must be added in
m o d e r a t e quantit y and

Fi g 19 P f
e r or a t e d i d sc and i ts use in an or Fi g 20 Cr o pp d f
e u nne l
f l
. . . . .

d i na ry u nne .

must be thoroughly distributed through the whole bo d v o f th e

turbid liquid by stirring .

97 D e ca n t a t i on A clear l iqui d standing over a solid deposit

. .

o f crystals precip itate or sediment may be poured o ff free from

, ,

s olid matter A compl ete separation o f the liquid by this method

.

i s rarely possible but it may frequently be carried far enough to

,

prove a valuable labor saving process -

.

To pour a l iqui d from one vessel into another without spill ing
is sometimes a di fficult feat but it is on e which every laborant ,

must practice until mastered .

The p ra Ct i c a l precautions to be observed in thi s connection are

I never to qu ite fill any vessel with l iquid but to leave enough
, ,

r oom to admit o f tilting the vessel considerabl y before a n y of the

—
S O C LA R I F I C ATIO N OF L I Q UI S D —
S TRA I N E RS ,
ETC .

A not h er plan is to use a guidin g rod to give the stream o f li qui d ‘

the proper direction .

98 . The trans fer of l iquids from one vessel to another i s also

e ff ected in various other ways as by means o f casseroles pitchers , , ,

pipettes s y phons etc, ,

.

Cas s e r ol e s are dippers with lips and handles ( fig They .

are generally made of p orcelain and ,

are u s ed principally for transferring

conside rable quantiti es of l iqu ids in ,

p ortions from on e vess el to another ,

in th e cours e of lab orator y processes

Fi g 23 P l i
. . or c e a n l ca s s e ro e .

for th e pro ducti on of chemi cals .

Pipettes ( fig 2 4 ) are used for trans ferring smal l quantities o f

.

liquids The y a r e usually o f glas s and gra duat ed

. .

99 . S yp h on s a n d t h e i r u se S yphons o f glass and o f rubber tub

.

ing are indispensable and are used for trans ferring liquids from
,

vessel s which can n ot or should not b e m oved or

disturb ed Clear li quids m a y b e al most com
.

p l e t e l y withdrawn from h eav y precip itates an d

s ediments by m eans of the syph on .

S yphons of glass p orcelain o r earth e nware are

,

also employed for transferrin g solution s of acids

or alkalies an d oth er corros ive li quids from large
contain ers an d for c ontrolling th e gradual addi
,

tion of on e li quid to an other in proc esses of pre

c i p i t a t i on oxidati on
,
etc ,

A variet y of glass Syph on s will b e found u seful

"
in a n y large pharm ac eutical lab oratory Th eir .

construction and op erati on are sh own in figs 2 5 '

to 2 7 ,
Fi g 24 Pi p t t s . . e e .

Flexible pu re rubber tubing o f from 1 0 to 2 0 millimeters diam

eter is extremel y convenient for s y phoning I t may be required .

in lengths varying from 6 0 0 m illimeters to 2 meters .

Two straight pieces of glass tubing connected by a rubber tub

ing j oint make a good syphon .

S yphons work on the principle that l iquids seek their own

level th ro ugh the force of gravita ti on The sy phon is a tube bent
”
.

so that its two l imbs would i f straight meet at an acute angle , , .

When about to be used the instrument is filled with the liquid ,

which is to flow through it ; one limb is then inserted in the vess el

 C LA R I F I C ATIO N OF LI Q U ID S —
S T RA I N E R S ,
ETC .
5 1

from which the liquid i s to be withdrawn and the other limb in ,

the receivin g vessel The greater weight o f the l iqui d in the

.

lon g er l imb o f the syphon will cause it ( the liquid ) to flow d own

Fi g . 25 . i pl
S m e sy p h on .

ward and the atmospheric pressure causes the ascent o f fresh

,

liquid through the shorter limb so that the flow is uninterrupted

until th e level of th e li qu id
in b oth vess els is th e sam e .

When th e level of the two

b odies of liqu id conn ected by
the syph on i s th e sam e it i s
evid ent that th e weight of
th e column of li qui d in on e
limb i s th e sam e as th e
weight of th e li quid in th e
other limb e quilibrium i s
,

established an d th e fl ow Fi g 26 G l s y p h
, f id d t h as s on s or ac s an o er
iv li q id
. .

o c r r os e u s
c eas es ; if n ow on e of th e .

two vessels be lowered the fl ow o f l iqui d through the syphon will

begin again in the d irection o f the lower ves sel .

1 00 . Col at i on Filtration th rough comparatively coarse media

.

i s called colation an d the l iqui d pa rtially freed from solid particles

,

by colation or s tr a i ni ng is called the colature M ixtures o f liquid .

and sol id matter are strained through sieves and throu gh various
kinds o f s tr a i ne rs .

U nbleached muslin i s the most generally u seful straining cloth

for ordinary laboratory operations in the production o f inorganic
5 2 C LA R IFI C ATION O F L I Q U I S S T R AI N E R SD —
,
ETC
.

chemicals The cotton cloth shoul d be boiled in water before it i s

.

u s e d i n order to remove starch or other

~
“
s iz ing and fillin g
” “ ”

material I t shoul d be cut into s quare pieces o f various s izes to

.

su it and always larger than the frame upon which it i s t o be fas

,

tened for use The most u seful S ize of cloth strainer for the
.

manu facturing laboratory is perhaps 60 0 millimeters square and ,

the stand required to hold su c h a strainer shoul d be about 4 5 0

m illimeters s quare and
about 4 0 0 m illim eters
high s o that a ston e ,

j ar of ab out 1 5 liters
capacity may b e placed
un der it The strain er .

must b e larger than th e

fram e in order that a
su ffici ent margin may
b e l eft for fastening the
cloth o n th e woo den
fram e and for the n e c es
”
sary bagging of th e
strain er i n addition to
th e allowance which
m u s t b e m a d e fo r
shrinking .

Th e strainin g cloth
fram e s hould b e strong
en ough to stand con
stant us e and must b e ,

provi ded w i t h strong

po inted nails ab ove o n
w h i c h t o fa s t e n t h e
strainer S quare fram es .

A gm t f rra n ti fi lt
e ti b y 0 1]
en { o u r l € g S a r e much
or c on n u ou s ra on
m f yph e ans o s on s .

better than circular or

triangular fram es on three le g s I n addition to th e strainer .

st ands or fram es on l egs an as sortm ent of square fram es with

, ,

out l e g S i s als o us eful S uch a strain er fram e is called a ten

'

.
“

”
a c u l um ( Fig
. .

Whenever the strainer i s to b e used for straining an aqueou s

fluid it should first be wetted in order to dim inish the diameter of
 C LA R IFI C AT I O N OF L I Q UI D S —
S T RAI N E R S ,
ETC .
53

the openings in the cloth by the swelling o f the threads o f which

it is woven and to establish uni form capillary attraction
,
.

W h en large quantities o f very heavy precipitates are to be

washed or collected on a cloth strainer ca re shoul d be taken t o ,

make the strainer strong enough to bear the weight o f the p re c i p

i t a t e an d th e w a t e r If a .

s ingl e thickn es s of th e mus

l in is not stron g en ough it ,

i s n ecessar y to d ouble it or
to s upport th e sag by broad
musl in ban ds crossing each
other under it unl ess strong ,

er muslin is a t han d wh ich

i s o p en enough to b e S uitable .

Fi g . 28
. M li
us n i
s t ra n e r s tand . Fi g . 29 . T l
e na c u u m .

Clos ely woven cotton cloth is not as su itabl e as a looser fabric .

L inen is rarel y u sed for strainers but flannel is sometimes more ,

Fi g . 30 and 31 . M et hd
o of f ldi g
o n a nd tw i ti g
s n a s ma ll t i
s ra ne r .

e ff ective than musl in and s eamless felt bags are occasionally still
,
-

more e ff ective as in the filtration o f syrups and o f l iquids con

,
54 C LA R I F I C ATIO N OF LI Q U I D S —
S T R AI N E R S ,
E TC .

taining undissolved particles o f vo latile oil or other liquid sub

stances l n suspension .

Pointed straining bags are also made o f musl in and o f flannel ,

“
and o f Canton flannel as well as o f felt ,
.

The manner in which a strainer i s folded and twisted to squeeze

the liquid through a fter it has ceased to run o f its own weight, is
,

shown in figs 3 0 and 3 1 . When the quantity o f wet mass in the

.

strainer i s small in proportion to the s ize of the cloth and the cloth ,

not too large it may be su ffi cient to twist the folded strainer with
,

the hands B ut when larger quantities are operated upon a pr e s s

.

i s necessary ( par .

In most cases however it is most advantageous to allow the

, ,

w e t mass to remain on the strainer until compl etely drained and

s u ffi ciently free fr om moisture t o be spread out t o dry i f the ,

sol id matter be the product and the l iqu id valueless .

Q uantities of liquid exceeding two l iters are usually filtered on

strainers l ined with paper pulp i f neces sary while smaller quan
, ,

tities shoul d be filtered on funn els .

L iquids filtered through cloth strainers and even through paper ,

filters do not always pass through qu ite cl ear from the start ; they
,

shoul d then be returned to the filter until the filtrate runs clear .

To hasten the process the filter o r strainer may constantly be

kept nearly full until all o f the liqu id to be filtered has been added .

B ut the filtration can not be hastened by scraping the sides o f

the filter or strainer i f a clear filtrate i s d es ired Whenever p rac .

t i c a bl e ( as in a large laboratory ) th e strain ing stands u sed for

washing precipitates shoul d stand on an asphalt floor incl ined to
ward on e or more gutters connected with the drain pipes through
.

which the valueles s washings may pass away .

101
. Pr e sse s To expres s the l iqui d from voluminous ma g
.

mas or w e t precipitates hol ding large quantities o f water a stron g ,

screw press is necessary A practical serviceable pres s must not

.
,

be too small becau se satis factory res ults can not be obtained when
,

the quantities operated upon are so g reat as to tax the capacity o f

the press to hol d them This is especially true o f presses con
.

structed l ike the ordinary pharmaceutical tinctu re press in which

the solid m atter subj ected to the pressure i s confined in a cy l inder .

The mass o f w e t soli d matter must be placed in the center o f a

s tr ong press cloth which is then folded so as to securely enclose
,

the mass an d the s ize o f the package must not be so large a s t o

,
 C LA R I F I C ATIO N O F LI Q U I D S S T R AI N E R S —
,
ETC .
.
55

cover the whole botton o f the pres s within the cylinder but should ,

be of s maller diameter than that o f the press block so that plenty ,

o f room will be l eft around the bundle for the escape o f the
liquid expressed from it M ost o f the failures in operating s impl e
.

pres ses are due to the choking occasioned by trying to work on

larger quantities o f material than can be adva ntageously handled
at one time S mall presses o f brittle cast iron with press blocks
.

o f the same material an d Cy linders of tinned or galvan i zed s h eet

iron are therefore useless Presses shoul d instead be made o f
, , .

cast steel or o f hard wood or o f strong porcelain

, ,
.

The pressure shoul d be applied slowly or gradually A fte r a .

Fi g 32 Wi tt ’
s p re s s , ih p
w t res s b l oc k of s t r on g
p li
. .

or c e a n .

twi st or t w o o f the screw the l iquid shoul d be perm itted to run

until it stops before th e screw is turned again The final pressu re .

should be strong .

When no more l iquid can be squeezed out o f the sol id material

in the press cl oth the screw should be tu rned back ; the package
shoul d be removed and the cloth un folded a fter which the con ,

tents may i f necessary be broken up and m ixed and again e n

, ,

fol ded in the cloth replaced in th e pres s and subj ected to ex

,

p ressio n a second time A secon d treatment in the press i s . ,

however rarely neces sary in working upon inorganic substances

,
.
 C LA R I F I C ATIO N O F L I Q U I D S S T R A I N E R S —
,
E TC .

S everal s erviceable presses are pictured here t w o with one ,

screw and one with two O ne o f the best is Witt s press H y

°
.
’
.

d r os t a t i c presses and filter presses required for operat i ng upon

very large quantities of material will be found described in larger
works on chemical technology and in the illustrated price cata
l og u e s o f the makers o f such apparatus .

Cyl inder presses o f from five to ten liters capacity are probably
t h e most use ful in h a rm a c e u t i
p
c a l laboratori es .

102 Corr osiv e l i q u i d s may be .

filtered through variou s filtering

m edia n ot a ffected by th em .

A cids alkali soluti ons so lu , ,

tions of zin c chlorid e and other

c orros ive s olutions when u n ,

c l ear may gen erally b e success ,

fu lly clarifi ed by sub sidence and

d ecantation or by drawing o ff
th e cl ear p ortion by m eans of
glass syphons B ut th ey may .

be filtered when neces sary ,

Fi g 3 3 Cy li d p
. . n er re ss .

through washed sa n d ,

c o a r s e l y powdered

glass or porcelain ,

glass wool asbestos , ,

powdered p u m i c 6
’
"
stone or powdered
,

clay according to cir

,

c um s t an c e s .

1 03 . Pa p e r fi l t e r s .

Filtration t h r o u g h
paper is an extrem ely
important an d valu
able meth od o i clari
l yin g li quids and it is ,

applicabl e to n earl y Fi g 34 M oh d b l w p . .
’
r s ou e s cr e ress .

‘
all l i q u i d s w h i c h are not corrosive or too viscous Filter pap er ,
.

is unsized porou s pap er made expressly for the special us e its

, ,

nam e implies .

Gr ay fil te r pape r i s made o f in ferior material and shoul d nev e r

~
8 C LA R I F I C ATIO N O F L I Q U I D S S T R AI N E R S —
,
ETC .

be spread upon a larger area o f the paper than necessary for i f -

,

finely d ivided precipitates come in contact with a greater surface

so me loss must be occasioned thereby .

Pl a i n fi l te rs are also used in pe r f or a te d f u nn e l s in r i b be d fu n

-

n e l s and in fil t e r bas k e ts ; all o f which facilitate the passage o f th e

,

liqui d through the paper by providing openings and channel s

through which it m a y readily escape .

A s a plain filter when opened form s a cone the apex o f

“ ”
,

which has a n angl e of 6 0 d egrees it fo l ,

lows that th e funn el used fo r such a filter

must b e of th e sam e angl e .

B ut when a plain filter is us ed in a

plain funn el of 6 0 d egrees angl e the ,

li qui d can pass through th e pap er onl y

at the apex o f the filter in the throat o f the
funnel where the paper is not in contact
with it This would make the escape .

of the li qu id very slow which is a d ecided ,

disadvantage except in the washing of

Fi g 35 C g t d f l precipitates
or r u a e
M oreover th e whol e weight
u nne .
,

p id fil t t i
, ,

f or ra ra on
of th e sup erincumb ent liquid restin g upon
‘

th e paper at th e ap ex of th e filter when th e li qu id i s a heavy ,

on e an d the filter full m a y caus e th e paper to break at that ,

.

point To pr event thi s trouble which is som etim es s erious the

. , ,

paper filter may b e supported at its ap ex by an ad ditional con e o r

filter of pap er ( or of p erforated platinum ) or of musl in A paper .

“ ”
filter sho d with a m uslin tip placed in the throat of th e funn el
“
i s to b e preferred to a doub le filter or a pap er sho d filter —
.

Fi g P f 36 e r or a t e d Fi g P f td
37 e r or a e Fi g P f 38 e r or a t e d
l i f l l i f pl i m
. . . .

p p
. .

or c e a n u nne or c e a n un at nu c on e
f fil t t i ra on no ] f d i i gor ra n n f fil t t i
or ra on by
t l
or
p
.

c ry s f a s or or r e s s u re
fil t t i
.

ra on .

are the most useful paper filters for rapid filtration

P l a i t e d fi l te r s
when plain funnel s are used without filter baskets .

A circular piece o f filter paper

.

1 05 H ow t o f ol d p ap e r fi l t er s
. .

may be fol ded into a plain paper filter by making the first fold
 C LA R I F I C ATIO N O F L I Q U I D S S T RAI N E R S —
,
ETC .
59

the center the crease thus made being

l i n e t h r ou g h ,

with the diameter o f the circle ; the second fol d is

through the center o f the first fold and at right angles
third fol d i s n ext made again d ivi ding the folded , .

pap er into two equal s egm ents

of th e circl e th e creas e running ,

fro m the apex to the edge Th e .

folded pap er is now op en ed up

'
until the hal f circle is reached -
,

after which th e flaps are laid

back o n opposite side s against th e
s econd fold an d th e two center ,

edges of th e filter are th en parted

s o that th e con e thus form ed pre
s ents three thickn ess es of paper
on two oppos ite sides w ith a s ingl e
thickn ess of pap er o n the two
oth er oppos ites as sh own in Fig , .

39 .

A plain filter m ay b e mad e out

on e half circl e of filter pap er of -
,

as shown i n Fig 4 0 an d th is
Pl i n p p e fi l t r
a a r -
e .
,
.
,

kin d of pap er filter may b e made

to fit a n y funnel since th e fold can easily b e mad e broader
,

either at the bas e or at the apex o f t h e cone so as to give any angl e

desired This filter as will be seen requ ires the use o f only hal f
.
, ,

Fi g 40 i pl fi lt m d
S m e er a e of Fi g 41 Pl i t d pap
a e er l
fi ter
h lf i l f p p
. . . . .

on e a -
c rc e o a er .

as much paper wh ich makes it the most economical paper filter

,

that can be made .

The pl a i te d fi l te r can be m ade in various ways The most com .

mon method i s su fficiently illustrated by fig 4 1 . .

Plaited filters may be u sed with funnels o f a n y angl e .

60 C LA R I F I C ATIO N O F LI Q U I D S S T R AI N E R S -
,
ETC .

1 06 . treble and even quadrupl e paper filters and clot h

D ouble , .

strainers are Sometimes u sed when a single thickness o f the paper

or cloth is insu fficient to produce a clear filtrate But some tur .

bid l iquids holding extremely finely d ivided sol id matter in sus

pension or containing some insolubl e liquid di stributed through
,

it with which it forms an emulsio n can not be rendered cl ea r ,

by any proces s of filtration The pores of the paper may be .

gradual ly entirely closed by finely divi ded precipitates very v i s

.
,

cous flu ids ( like strong mucilages strong solutions of albumin , ,

“ ”
etc ) do not pas s through filter paper at all and emulsions o f
.
,

mixed liquids pass through without s eparation i f at all .

1 07 . H ot fi l t r at i on M any .

l i q u i d s wh ich wh en col d , ,

refus e to pas s t hrough th e

ord inary filterin g m edia i n ,

clu ding pap er may b e su c ,

c e s s fu l l y filtered wh en h ot .

A gain m any li quids which

,

pass thro ugh the filter slowl y

F ig
jh d t d H i fi l fhi i
z
lre
l ln
r o
n l
t
-

t oi
‘va f r Fi g . 43 . A r ran g e m e n t f o r h ot fil t t i
ra on :

when cold m a y pass les s slowly or even rap idl y wh en hot

, .

Jacketed funnel s ( Figs 4 2 to 44 ) are emplo y ed for hot fi l t ra

.

tion and also con i cal coil s ( F i g

, .

1 08 R apid filtration is in special cases e ffected by hydrostatic

.
, ,

pressure or by suction .

O ne goo d contrivance is a box having perforated Sides and c ov

ered on the outside w ith the straining cloth ( or filter paper next to
the box and c loth ov e r i t ) securel y fastened this box to be pro
'

v i d e d with a tube through which a s y phon can be inserted by

’
 C LA R I F I C ATIO N O F LI Q UI S S T R A I N E R S D —

,
ETC . 61

m eans o f which the filtrate accumulating in the box can be drawn

o ff
. This box is then subm erged in the turbid liquid to be
filtered when the hydrostatic pressure causes the liquid to pass
,

through the cloth ( and paper ) into the box .

Fi g 44 Di ih j ktdf l
e tr c
’
s ac e e u nn e Fi g 45 H ot - w a t e r - c o il
fil t i d wi h fil t t i
. . . .

f or h o t r a t on ; use t ra on .
s t e am e ath .

V arious kinds o f filter pumps are also used to create a

partial v acuum in the receiving vess el int o which the filtrate

Fi g 46 Fil t t i d ra on un er pr es sure by m e ans a fi ter l

p m p w hi h h f
.

k
.

u c ex austs th e ai r r om t h e fl a s .

passes s o as to caus e suction throu g h the filter . O ne such filter

pump is shown in Fig 4 6 . .
62 C LA R I F I C ATION O F L I Q UI D S S T R AI N E R S —
,
ETC .

A perforated filtering disc o f porcelain with a rubber tire

around its grooved edge is placed in the funnel and c ov ,

ered w ith filter paper musl in or both or flannel as may be r e

, , , ,

quired T he funnel i s fitted tightly i nto the neck of a stron g r e

.

c e i vi n g bottle Fig and this is connected by a s ide t be w ith

( 4 7) . u -

the filter pump ( S e e al so Fig . .

Fig 47 U se of p fe r or a t e d di s cs F ig 48 A rra n g e m e nt F ig Ill t t

49 us ra e s
fil t t i d p i
. . . . . .

f or ra on u n er r e s s ure . f or c on t n u o u s fil gm t f
arr a n e en or th e
f i r a t on m i
a u to fl w at c o of
li id i fil t t i
.

qu n ra on .

1 09 . Fig ures 48 and 4 9 illustrate a sim

Con t i n u ou s fi l t ra t i on .

ple arrangement for a continuous fl ow o f l iquid into the funnel

for filtration or for wash ing precipitates .

Continuou s filtration may also be eff ected by a syphon arrange

ment as S hown in Fig 2 7 . .
 C H AP TE R VII
.
.

EV A P O R AT I O N .

1 10. The temperature at which any s u bs ta

state o f vapor depends upon its constitution
sure to which it may be subj ected D i ff eren .

greater or les s differences as to thei r vap o

to thei r composition .

M any substances remain solid at

d u c i bl e ; others may be liquefied but
pose be fore they undergo a
aggregation ; many
gaseous state under
sure ; but numerous nder
ordinary conditions readily converted int o
vapor by su fficient h pressure to which they
are expose d or by both
,

The power w ith w h i c ors res ist compress ion

into the liqu id o r sol id st vapor t e ns i on .

B ut the con version o f solids and liquids into vapors depends

.

’
not i i p on c ompos itio n ,
an d pressure only ; it may ,

form s o f molecular attraction .

attraction and therefore breaks down

contrary aids cohesion B ut the m ol e c
, .

ff e r e n t kinds o f matter may oppos e and

the cohes ion between l ike molecules .

es o ff from ice even at the freezing point

n g the ice is d r y i e i f the avidity o f the
—
.

al ready satisfied .

nt . The boilin g point o f any liquid is the

which it can not continue in the l iquid state
the aid o f increased pressu re .

point o f any given l iqu id i s constant under con

pressure .

r bon dioxide boils at C ; ether at

. alcohol at
water at mercury at and zinc at These
63
64 E VA P O R ATIO N .

boil ing points re fer to the ordinary atmospheric pressur e ; the y

ri se as the pressure i s increased and fall w ith diminished pres
sure .

The boil ing point o f any liquid is in other words the tempera , ,

ture at which the tension o f its vapor i s greater th an the pres

sure wh ich it sustains .

1 12 E v a p or at i on is the formation o f vapor at or from the sur

.

face of a ny solid or l iqui d at any temperature below its boil ing

point .

When comparatively rapid evaporation is des ired it is aided by

the application o f heat by the d iminution o f pressure and by
, ,

other m eans .

When very slow evaporation is desired as i s frequ ently t h e ,

case in the production o f crystallized salts no heat is appl ied , .

E vaporation without the appl ication o f h eat i s called s pon ta ne ou s

e va p or a ti on .

E vaporation depends largely upon mol ecular attraction between

the molecul es o f the vapor and the molecules o f the components
o f th e superimposed air This attraction i s closely akin to that
.

which causes solution .

1 13 Vap or i zat i on as this term is generally u sed means the

.
, ,

formation o f vapor at the boiling point , and it diff ers from e va p o

ration chiefly in the fact that th e vapor which is form ed at the
boiling point o f any l iqu id is not formed at or from the sur face o f
'

the liqu id but in the body of it and mainly a t th e sur face o f

, ,

cont act between the l iqui d and that portion o f the vessel contain
ing it wh ich i s directly exposed t o the source o f heat
,
.

1 14 The r at e of e v a porat i on or vap or i zat i on of any liqu id de

.

p ends upon variou s conditions among which the

, following are the
most important
1. T h e v ol a ti li ty of th e l i q u i d which depends upon its con
,

s t i t u t i on or composition Thin mobile l ess cohes ive liquids are

.
, ,

more volatile even i f o f greater specific weight than thick co

, , ,

h e s i v e l iquids ; but the specific res istance o f any liquid to its con
version into vapor or in other words the relative force o f a tt ra c
, , ,

tion between its molecul es mu st depend primarily upon its chem i

,

cal struct ure .

2.
The te m pe r a tur e w hi c h th e l i q u i d a t ta i ns has a direct and
decided influence upon the rate o f evaporation A boiling liqu id .
66 E VA P O R ATION .

o f w hi ch th e The proportional
a i r c ons i s ts extent
. of surface o f
the evaporating or boiling liqu id which com es in contact with
the air is therefore a matter o f importance not only because
, , ,

greater depth causes increased pressure upon the lower strata o f

the l iqu id but also because actual contact is necessary to the
,

di ff usion o f the vapors into the air This i s an additional reason .

for preferring shallow vessel s rather than deeper ones .

The su rface o f contact between the air and the liquid mav be
increased by stirring the latter .

The humi dity o f the air in contact w ith the liquid also has its
‘

e ff ect upon the rate o f evaporation o f water for th e power o f the ,

a ir to absorb the vapor i s not unlimited .

The rate o f evaporation or vaporization i s greatest when the

ai r is free from vapor o f th e same kind as that being formed and ,

when the air into which the vapor passes becomes saturated w ith
it no further aid i s to be derived from the contact o f the liquid
,

w ith that air Currents o f warm dry air over the surface o f the
.
,

liquid greatly hasten the formation o f vapor and such currents ,

are created by stirring the liqui d as well as by other s im ple

means whereby the saturated air i s removed and replaced by a
,

fresh supply capabl e o f taking up the vapor .

1 15 The obje ct s o f evaporation and vaporization are

.

1, to concentrate solutions by the elimination o f a part o f the

solvent ; 2 to obtain saturated solutions for the purpose o f caus
,

ing crystall ization 3 the completely separate volatile l iquids from

,

solutions and mixtures .

L iquids are evaporated : 1 to drynes s ; 2 to a given volume ; , ,

3, to a given weight ; 4 to a given density

, ; 5 to a certain more or ,

l ess definite cons istence ; 6 to the point at which sol id matter ,

be g ins to separate ; 7 to a constant weight ( i e until there i s

,
. .
,

no further loss o f w eight ) ; or 8 until a certain obj ectionabl e vola ,

tile constituent or impurit y shall have been completely expelled .

116 B oi l i n g ve s s e l s should be deep i f rapid vaporization i s to

.
-

be avoided as far as practicabl e i e when the obj ect i s the —

. .
,

maintenance Of the boiling point purely for its chemical e ff ects .

D eep dishes dishes covered by inverted funnels or by other c ov

,

ers fl a s k s be ak e r s and various other c y lindrical vessel s all these

, ,.
—

are good boil ing vessels but poor evaporating vessel s

-
,
-
.

1 1 7 E v a p or at i on v e s s e l s -
The shallow dishes kettles or
. .
, ,

pans emplo y ed for the vaporization or evaporation o f l iquids

 EV A P O R ATION . 67

shoul d be made o f material s which a re su fficiently good conductors

o f heat not a ff ected by the subs tances with which they must
‘

come in contact and strong enough to resist fracture , .

The most common materials are porcelain other earthenware , ,

glass iron tinned i ron pure tin copper tinned copper enamel ed
, , , , , ,

i ron silver platinum an d aluminum

, ,
.

S ilver dishes are very desirabl e in cas es in which high tem

p e r a t u r e s are sa fe and the metal not attacked by the liquids

heated .

Porcelain dishes which can bear sudden changes o f temperature

w ithout danger o f fracture are the most generally useful evap
orating dishes .

But hot glas s and porcelain vessels should never be put on cold
or wet surfaces ; it is better to let them cool gradually or to put ,

them upon rings O f straw ,

or gromm ets of rubb er

tubing or up on dry cl oths
, ,

tow or cotton .

Glass an d p orcelain v e s
sels s l i ou ld n ot b e heated ,

to o su dd enly an d should Fi g 5 0 R d b t t m d v p o t i o d i h ou n -
o o e e a ra n s
l
. .

f p
, .

o or c e a i n
b e dry on th e o uts i de wh en
.

dry heat as th e bare flam e , ,

is a pplied to them Wire .

gauze o r wire cloth or a

, ,

sand bath o r oth er baths , ,

may b e interpos ed be
twe en the flam e an d th e Fi g 5 1 Fl t b ott m d v p t i o di h of . . a -
o e e a or a n s
p l m or c e a '

glass or porcelain so as to ,

d istribute th e heat evenl y over t h e whol e bo t tom of the vess el .

Th e flam e should also b e well regulated s o as t o b e n ot u n n e c e s

s ari l y h igh an d so that th e h eat m a y b e appli ed graduall
,
y .

A complete assortment o f s izes o f porcela i n evaporating d ishes

i s necessary to every well equipped pharmaceutical laborato ry -

for the production o f chemical s from 5 0 m ill imeters to 40 0 or —

5 0 0 m illimeters diameter .

M etal vessel s except s ilver a re rarely u seful for chemical

, ,

work and enameled iron ( agateware etc ) i s not reliabl e a s th e

, ,
.

ena mel is too l iable to crack off or to become per forated by pin “

”
holes .
68 EV A P O R ATIO N .

118 . M od e s l i cat i on of h e at for the evaporation

of app

or vaporizatio n o f liquids A ccord ing to the temperature r e .

quired the heat may be appl ied : 1 by d irect flame ; 2 w ith but a , ,

piece o f wire cloth interposed between the flame and the ves sel ;
3,
by the san d bath ; 4 through asbestos cloth ;
, 5 by the glycerin ,

bath or an O i l bath or various salt solution baths ; 6 by direct

,
-
, ,

steam ; 7 by steam j ackets ; 8 by steam coils in or around the

, ,

vessel ; 9 by the water bath or I O by a hot air bath

,
-
,
.

The student i s referred to the chapter on heating apparatus

for fu rther in formation on this subj ect .

1 19 D a n ger s of ov e r h e a t i ng in the evaporation o f solutions

.
-
.

The temperature can generally be easily controll ed by means o f

baths with the aid o f t h e r m e t e r s by the regulation o f the flam e
, ,

or fire by gradua l elevation of the temperature and by watching

, ,

the operat ion S houl d there be any signs of da nger prompt

.
,

rem oval of th e flam e or heater or of th e vess el ,

fro m th e s ourc e of h eat i s n ec es sar y ,

.

V acuum pan s are much emplo y ed in the evap —

oration O i s olution s of organic substan ces but ,

not in the op eration s of inorganic pharmaceutical

chemistry
Wh en water soluti ons are evaporated very —

h igh h eat up to th e bo iling po int may b e safely , ,

applied in many cas es s o long as th e s olutions

are dilute but it m ust b e rem emb ered that as th e ,

Fi g 5 1 density of th e s olution increases th e boilin g point

2fi §33
l i ¢e a n
3

also ris es an d the danger p oint may b e reach ed ,

unl e ss th e therm om eter i s u s ed as a gu ide .

I f sol id matter separates from the liqu i d during the process

o f evaporation constant stirring is generall y necessar y to prevent
,

accidents ; S hould the sol id matter form a pellicle over the l iquid ,

the temperature might then rise too high and i f the soli d mat ,

ter deposits on t h e bottom o f the di sh th e latter may crack or

the deposited matter may become overheated .

The stirrers used may be of glass porcelain wood or other , , ,

suitabl e material They may be in the shape o f rods spatulas

.
, ,

spoons or l a d l e s ,
.
.

120 S l ow e v a p or at i on may be perf ormed over a well regulated

.

steam bath water ba t h s a n d ba t h o r air bath in the dr y ing closet

-
,
—
,
-
,
-
, ,

or by spontaneous evaporation w ithout any application o f heat .

 EV A P O R AT I ON . 69

T he evaporating dish should be loosely covered with paper or ,

should be placed under a hood to protect the contents from the

dust .

1 21 . When obj ectionable vapors pass o ff from evaporating

liqu ids the employment o f hoods or fum e chambers i s necessary
unles s it be found practicabl e to carr y on the operation out o f
'

doors in which case the operator may easily avoid the gases by
,

standing with h is back to the quarter from which the wind comes .

122 E xp u lsi on of h y gr oscopi c moi st ure

. S mall amounts o f .

w ater h eld by hygros copic sub

stanc es which can not safely
b e expo sed to heat may b e r e
moved by means o i d esi cca t or s
which consist of glas s covers
placed over ves sels contain ing
calcium chlori de s u l p h u r i c ,

acid dry potas sium hydroxide

, ,

d r y lim e or oth er substances ,

having a great avid ity for

water Th e dishes b eak ers .
, ,

watch crystals or other ves -

Fi g 5 3 D i t i g pp t
. . e s c ca n a a ra us
s els containing th e substance
.
,

Or solution to be subj ected to d e s i c ca ti on are placed immediately

over o r below or beside the vessel containing the calcium chloride
, ,

or other substance employed to absorb the water as it evaporates .

 C H AP TE R VII I .

D I S TILLATIO N .

1 23 . Di st i l l at i on
i s the vaporization o f a liquid in an appar
a t u s so constructed that the vapor which is formed in one vessel

is conducted into another ves sel in which it i s condensed back to

the l iquid state and collected .

The obj ect o f d istillation is the separation o f volatile liquids

from non volatile substances with which the y are m ixed or which
-
,

they contain in solution ; or the separation o f more volatile from

less volatile l iquid s .

The l iquids subj ected t o d istill ation may be m ixtures o r solu

tions consisting o f two or more liquids or solutions o f substances
which are solids when separated from the solvent ; or mixtures o f
solid and liquid substances not forming solutions ; or liqu ids con
taining comparatively small proportions o f other substances which
it is desired to separate .

1 24. M any di ff erent substances have different deg rees o f

volatility within the range o f temperatures produced in ordinar y
distillation while other substances are quite non volatile at thos e
,
-

temperatures .

The volatile l iquid carried o ver by the distillation forms the

product call ed the d i s ti l l a te The les s volatil e or non volatile
.
-

matter le ft in the vessel in which the vaporization was e ff ected

i s called the r e s i d u e This res idue may be either l iqu id or solid
. .

The separation o f a volatil e l iqui d from an altogether non

volatile substance with which it m a y be associated by solution or
otherw i se is easily e ff ected by distillation .

But the separation o f two or several more or less vol atil e liquids
from each other by d istillation i s di fficult an d scarcely possibl e ,

unless thei r respective boil ing points di ff er su fficientl y S uch a .

s eparation i s called fr a c ti ona l d i s ti ll a ti on .

1 25 . The l a te n t h e a t of vapor is the quantity o f heat required

“ ”
to hol d it in its gaseou s state It is called latent becaus e it does
not register upon the ther m
.

ometer or reveal itsel f in any other

w a y than by performing the work o f keeping the molecules of the
volatile substance apart from each other so as t o hold them in
70
 DI S T ILLATION .
7 1

the condition constituting what is known as vapor and the ,

energy requ ired to do that work can not at the same time do any
other work .

The latent heat o f water vapor or steam is about 5 3 7 C for °

.
,

the amount o f heat energ y which is necessary to convert 1 Gram

o f water into vapor ( or to evaporate 1 Gm o f water ) is precisely
the same as the heat energy requ ired to rais e the temperature o f
e
'

5 37 Grams o f water o n degree ( centigrade ) .

The laten t heat o f alcohol vapor i s expressed by about

and that o f ether by about 1 6 3 C °
.

The quantit y o f heat energy required to raise the temperature o f

0
a given quantity o f water from 0 to 1 0 0 C i s a constant quan °
.

tity and the quantity o f heat energy requi red to convert water of
,

1 00
°
into vapor and to hol d it in a state o f vapor i s
,
t imes ,

as great as the quantity o f heat energy requ ired to raise the tem
p e r a t u r e o f the same amount o f water The quantity o f h ea t
energy or thermal energy i s measured in units which stan d for
, ,

the amount o f heat required to rais e the temperature o f one l iter

o f wate r one degree ( centigrade ) The quantit y o f heat energ y
. .

required to raise the temperature o f one l iter o f water from 0 °

to 1 0 0 C is :therefore 1 0 0 heat units or thermal units But the

°
.
, ,
.

quantity o f heat energy required to convert one l iter of water at

1 00
°
into vapor and keep it in a state o f vapor i s 5 3 7 thermal
, ,

units Hence 6 3 7 units o f thermal energy will be required to con

.

vert one liter o f 0 into water vapor of 1 0 0 ° 0

Whenever the vapor produced by one l iter o f water is con

0
d e n s e d o r converted from vapor at 1 0 0 into liquid water at the
same temperature the latent heat of that vapor amounting to
, ,

537 units is released , .

1 26 .The most common method o f causing the condensation o f

vapor in distillation i s t o conduct the vapor through tubes sur
rounded by water o f the ordinary temperature ( between 1 5 °

and 2 0 °
Thi s water is called the c on d e ns i ng w a te r and it -
,

serves the important purpose o f absorbing the heat given up by

the vapor The vapor can not be condensed unless its latent
.

heat be trans ferred to or absorbed by t h e substances with which

it comes in contact ; but the rate at which condensation takes
place i s in di rect proportion to the rate o f abso rption o f the latent
heat o f the vapor by the vessel in which it is condensed by the ,

w ater surrounding that vessel an d by the contiguou s ai r ,

.
7 2 DI S T I L L A T I O N .

The greater part o f the heat lost by the vapor i s taken up by

the condens ing water The heat lost in cooling is precisely th e
.
~

same amount as is required to rais e the same body thr ough th e

same number o f degrees I f one kilogram o f water at 1 0 be
.
°

mixed w ith the same quantity o f water at the equal ization o f

temperature would result in two kilograms o f water o f for
°
th e amount o f heat gained by the water o f 1 0 would be one
hal f o f the di ff erence between 1 0 and an d the heat lost
°

by the water o f 9 0 woul d be the other hal f o f that di ff erence

°
.

I f it be assumed that all o f the latent heat o f the steam in the

distillation o f water is trans ferred t o the condensing water and ,

that all o f the condensing water enters the condenser at a tem

ff
°

p e r a t u r e o f 1 5 and is heated to running o at that tempera

ture and i f it be further assumed that the distillate passes out
, .

having a temperature of then as the latent heat o f water

,

vapor is 5 3 7 thermal units it follows that about , l iters o f

condensing water will be required to take up the latent heat given
up in the f ormation of one liter o f distilled water and nearly ,

5 l iter o f additional water o f I 5 will be requ

°
ired to reduce the
°
temperature of that distillate from 1 0 0 to so that about
°
1 1 liters o f water o f 1 5 woul d have to be supplied to the con
denser l n making each l iter o f distill ed water o f But in
actual practice the amount o f condensing water required is about
twice as great for it i s imposs ibl e t o regulate the operation and
,

prevent waste A ll that can be done in this direction i s to see

.

tha t the condensing water suppl ied runs O ff nearly a s hot a s the
distillate itsel f .

B oi l i n g p oi n t s of mi xe d l i q u i d s When a m ixtu re of s ev .

eral l iquids o f di ff erent boiling points is heated it boils at a ,

temperature somewhat higher than the boiling point o f the most

volatil e constituent o f the m ixture .

1 28 . U se of th e rmome t e r s in distillation In order to regulate .

the temperature in distillation whenever necessary the mercury , ,

thermometer is o ften brought into requisition The slender spe .

c i a l laboratory thermometer o f glas s u sed for this purpose is

represented by Fig 5 4 I t i s long o f very fine bore an d has a

. .
, ,

very small bulb S uch thermometers range from about

.

35
—
°

to + 2 0 0 C but for ordinary purposes the most useful are those

.
,

w h ich re g i ster temperatures from 20 to Wel l made

—
°
74 D I S T I L LATIO N .

are always o f awkwar d shape and their liability t o

R etorts ,

breakage lessens their u sefulness Flasks are to be preferred .

whenever practicable .

Fi g 55 Ill u s trat n i g di t ill t i

s a on on a sma ll s ca e l The c on d e ns e r is a L i big
e c on
d
. . .

e ns e r .

Th e fi tti ngs by which flasks or retorts are connected w ith con

or receivers or both consist o f bent glas s tubing T tubes
d e n s e rs , , , ,

rubber tubing soft sheet rubber and per , ,

f or a t e d rubber stoppers or corks The .

whol e apparatus shoul d be securel y sup

ported the connection s instead o i being ,

rigid should be somewhat elastic to di

minish the danger o f breakage and all ,

the j o ints should be tight .

The c or k bor e r is necessary when -

F i g 56 A l t d gl
ggggt corks are used instead o f rubber stop
: ‘ f e as s
r

pers and only the very best kind o f cork ,

can be used Perforated rubber stoppers o f pu re ( black ) rubber

.

o f all ordinary si zes an d with one two or more perforations for , ,

F i g 57 G l as s fi tt i ng s f or d i t illi g pp t
s n a ara us and f or g a s a pp a rat u s ; e lb ow,
d gl d pi bi g
. .

T t u b e , an t pp
as s -s o e re e ce of tu n .
 D I S T ILLAT I O N .

75

the insertion of glass tube e l bbw s or T tubes sa fety tubes reflex ,

-
,

condensers and thermometers any or all can be obtained from

, , ,

any dealer in chemical apparatus and are so far superior to cork

that they should altogether d isplace the latter ( Fig . .

Fi g . 58 . Thi t l
s e -t u b e a nd f
s a e ty tu b es f or di t illi g
s n fl as k s and
a pp arat u s .

Fig . 59 . Cor k -
bo rer of b ras s tu bing .

Fi g . 60. P f
e r or a t e d ru bb er s to pp e r s.

131 . T he w or m c on d e n s e
or condensing worm i s a simple r , , ,

common and e ff ective condensing apparatus employed in connec

tion with la rge stills especially for the distil lation o f water or o f
,
76 D I S TILLAT I ON .

alcohol I t consists o f a spiral block tin pipe p l a c e d i n a t u b

j

.
,

barrel or tank through which cold water flows

,
.

L i e bi g s c on d e ns e r is shown in Fig 5 5
’
It i s c on s t ru c t e d o f . .

'

two tubes which may be taken apart and cleaned The vapo r .

passes throu g h and is condensed in the inner tube which is sur ,

rounded by the col d water pas sing through the outer tube .

S q u i bb s c on d e ns e r is a modification of L i e bi g s
’
Fig 6 1 ’
. . .

M i ts c h e r l i s c h s c on d e ns e r is a double cyl inder placed i na v e s

’

S qu ibb ’
s u p i ght
r c on Fi g 62 V ti l
er ca i
s e c t on s h w i ng
o c on s t r u c
d i d
. .

’
e ns e r. t on of M i t s c h e r l i s c h s c on e ns e r .

sel o f cold water The doubl e cylinder i s made of t w o tubes

.

tightly fitted together at both ends The va por i s condensed .

be tw e e n th e tw o t u bes and the col d water passes around the

.
,

outer t ube a n d through the inner tube

‘
.

"
1 3 2 S ta n d s for retorts flasks condensers etc a r e m ad e o f
.
, , ,
.
,
)

i ron or o f iron and wood The y S hould be strong e nough and

,
.
,
 D I S T I LLATIO N .

77

Fi g 63 App ar atu s s tan d of i r on f or r e t or t s , Fi g 64 I r on s ta n df orf l

u nne s ,
k d k b k
. . . .

fl as s, c on e n s e rs , e tc . fl as s, ea e rs, e tc .

provi ded with a su fficiently broad base heavy and w ith the center , ,

o f gravity in that bas e .

 C H AP TE R I X .

CR YS TAL S A ND CR YS TALLIZATION .

133 . A cry st al
is a naturally formed geometric s olid boun ded
by smooth plane fa c e s meeting each other to form straight e dg e s
an d soli d a ng l e s The edges are fo rm ed by two contiguous inter
.

s e c t i n g faces ; the sol id angles or corners are form ed by three or

more faces intersecting each other at one point .

Calcspar rock crystal diamond gal ena alum blue vitriol green
, , , , , ,

vitriol E psom salt and quinine sulphate furnish examples o f

, ,

crystals .

134 . Cr y st a l l i za t i on i s the formation o f crystals B ut for our .

present purposes w e shall us e the term to signi fy the preparation

o f chemical products in the form o f crystals .

Crystallizabl e substances are c rys ta ll i c when they occu r in com

p a r a t i v e l y well defined free or detached individual c r vs t a l s such
, ,

a s we s ee in alum copper sulphate sodium carbonate rock crystal

, , , ,

and potassium ferrocyanide ; they are crys ta ll i n e when their crys

t a lli n e structure i s evident throughout their mass but t h e crys ,

tal s are very small imper fect and not detached or s eparabl e from
, ,

each other as in masses o f ferric chloride black antimony sul

, ,

p hi d e
,
camphor and
'
ammonium chloride .

S u bs t a n c e s c on s i s t i n g o f such m inute crystals that they have

the form o f coarse o r fine powder may be either crystal lic o r
crystalline but are alwa y s described as crystall ine Powders con
,
.

“
sisting o f minute cr y stal s are sometimes described as cry stal
meal . When the c rystal s are so small that they can not be recog
n i z e d without the ai d of the microscope the substance made up ,

o f such crystal s i s said to be m i c r o cr ys ta ll i n e -

.

S ubstances which present no indications o f crystalline structure

are called a m or ph ou s .

135 . O nly molecules o f the same kind form cr y stals o r a r ,

range the mselves into regular polyhedral solid bodies except that ,

water ( and sometim es alcohol ) o f crystallization can be inclu ded .

Hence when any substance cry stallizes into well defined crystals
 CR YS TAL S A N D CR YS TALL I ZAT I ON .
79

other substances which may be present w ith it are excluded s o ,

that crystall ization is a good indication o f probable purity .

B ut crystall ization is not absolute evidence of purity for a l , ,

though i t is true in a general way that crystals are chem icall y

homogeneous or consist o f but one kind o f molecules it hap ,

pens quite frequ ently that other kinds o f mol ecules are m e c h a ni
ca lly included in the cr y stals formed or that the exclus ion o f for
,

e i g n substances is not co mplete until a fter repetition o f the proc

ess o f cr y stallization once twice or several times M oreover
, ,
.
,

there are some substances which freely crystalliz e together and

’
the crystals o f which grow in each other s solutions .

136
. There are innumerable distinctly di fferent forms of cr y s
tals ; but as a rul e each particular kind o f matter crystallizes in
, ,

but on e form so that the crystal form of a substance is one o f the

,

means by which it may be identified .

N umerou s di ff erent substances may however crystall ize in the

, ,

same form even i f they can not cr y stallize together to enter into
the formation o f the S ame individual crystals It happens too .
, ,

that a ppa r e n tly the sam e species o f molecules may crystall ize in
two o r three di ff erent form s .

137
. S ubs tances crystallizing in two diff erent forms are called
d i m or ph ou s s u bs ta n ce s ; those crystall izi ng in three forms a re
tr i m or ph ou s or poly m or ph ous .

When di ff erent substances crystall ize in the sam e form they

are said to be h om oe om orph ou s But homoeomorphou s S ubstances
.

are frequently o f altogether dissimilar internal structure .

I s om or ph ou s substances have not only the same crystall ine

form but als o perfectl y analogous internal structure They gen .

e r a l l y contain the same number o f atoms in thei r respective mole

cul es ; the system s o f interatomic linking o f any two or more

isomorphous substances are identical ; they contain the sam e num
ber o f mol ecules o f water o f crystall ization i f any ; they crys ,

t a l li z e together in the same crystals from a common solution ; and

their crystals may grow in each other s solution s ( o r the c ry s ta l o f
’

a less soluble substance may be made to grow in a more soluble

isomo rphou s substance ) . E xamples o f isomorphou s substances
are : the alum s ( although an ammonium alum doe s not contain
the same number of atoms as the corresponding al um formed by
any alkal i metal ) ; the phosphates and arsenates o f the alkal i
metals ; the halides o f the alkal i metals ; the n itrates o f potassium ,
80 CR YS TAL S AND CRYS TALL I ZAT I ON .

rubidium and c aesium the carbonates o f magnesium and calcium ;

the sulphates o f magn esium and zinc ; etc .

S od ium nitrate N a N O and calcium carbonate Ca CO S crys

, , ,

t a llize i n s im ilar forms and their mol ecules contain identical

,

numbers o f atoms ; but they are not isomorphous because their

system s o f atomic l inking are altogether dis similar owing to the
'

fact that sodium i s a monad and calcium a dyad and that the ,

n itrogen o f N a N O i s a pentad while t h e carbon o f the Ca CO 3

3 ,

is a tetrad

Na

S od ium nitrate an d calcium carbonate are accordingly only

homoeomorphous .

E lements having d i ff erent valences can not replace each other

and form isomorphous substances .

D i ff erent substances which cr y stallize in d iff erent form s a re

h e te r om or ph ou s . They never crystallize together in the same
i dentical crystals .

When heteromorphous substances are contained together in

the same solution they may be s eparated from each other by
crystall ization especially i f thei r respective solubiliti es di ff er su f
,

fi c i e n t l y ; but isomorphous substances are di fficult to separate

in this w a y even i f th ey d o not freely enter into the formation
,

O f the same individual crystal s .

L es s soluble substances of cours e crystal lize before the more

, ,

s oluble substances from the same solution .

B ut the presence o f two or more substances in the same solu

tion may caus e one o f these substances to form crystal s having the
.

form belonging to the other or one of the others For instance .

,

copper su l phate cr stallizes normally in the triclinic form but i f

y
,

it crystallizes from a solution containing about one seventh as -

much ferrous sulphate as copper sulphate the copper salt will ,

crystall ize in monoclinic prisms the form o f the crystal s o f fer ,

rous sulphate .

138 . Gen e r a l d e s cr i pti v e t e r m s referring to the forms o f cr y s

,

tals a re so num erou s that they can not be mastered without a

,

more ext e nded study of cr ystallo graphy than is possible in thi s

b ook .
82 CR YS TAL S A ND CR YS TALLIZAT I O N .

The fundamental forms o f this system are the cube the regu ,

lar octohedron and the rhombic d od e k a h e d r on

,
.

I I Th e H e xa gon a l S y st e m ( rhombohedral system )

. A xes .
—

Fi g 71 H m ih d l e e ra Fi g 72 Co m bi i
n a t o n of Fi g 7 3 S l h d ca e n o e r on
h mb h d h mb h d d w i th i ib d h mi
. . . .
. .

r o o e r on r o o e r on a n nscr e e
p im d l h mb h d
.

r s . ra r o o e r on .

CR YS TALL I N E F O RM S OF TH E Q U A D R AT I C SYS T E M .

Fi g 7 4 S q uar e - b as e d Fi g 7 5 Q ua d ti p i
ra c r s m Fi g 76 F or m d f ou n in
d bl p id l
. . . . . . .

ou e y ra m ( Oc c ry s ta s o f th e sul
i
.

t oh e d r on ) p h a t e s of m g a ne s um
i
.

a n d z nc .
 CR YS TAL S AND CR YS TALL I ZAT I O N . 83

f ou r . Three o f these axes are o f equal length ; these are called

the s e c on d ary ax e s The fourth called the pr i m ary ax i s i s either
.
, ,
.

longer or shorter than the other three The s econdary axes a r e .

all in th e same plane and cut one another at angles o f 6 0 de

,

grees ; the primary axis i s at right angles to the plane o f t h e

other three
’

The fundamental form o f this system i s the doubl e s ix s ided -

p yrami d O ther . impo rtant forms are the regular s ix s ided -

prism and the rhombohedrons

,
.

I I I Th e Q u a dr at i c S y st e m ( the dimetric squa re prismatic

.
, , ,

pyramidal or tetragonal system ) Three axes The two s e c .

—
.

a n d a r y a x e s a r e o f equal len g th ; the pr i m ary ax i s i s longer or

shorter The axial angl es are all right angles

. .

Pyramids o f this system have s quare bases .

The dominant forms are the double fou r sided square based -
,
-

pyramid and the right s quare p rism .

IV Th e R h ombi c S y st e m ( trimetric or right prismatic sys

.
,

tem ) The three axes all o f unequal lengths cut each other at
.
—
, ,

right angles .

The fundamental form is the right rhombic double pyramid or ,

rhombic based octohedron -

.

V Th e M on oc l i ni c S y st e m ( monosymmetric or obl ique pris

.

matic system ) The three axes are o f unequal l ength ; the two
.
—

s e con d a r are at right angles to each other the r i mar

y a x e s ; p y
a x i s i s at right angl es to on e o f the secondary axes but form s ,

oblique angl es with the other .

The primary form i s the monocl in ic pyramid .

VI Th e Tri c l i ni c S y st e m ( the a s s ym m e t ri c or doubl e oblique

.
,

prismatic system ) The three axes all o f unequal l en gth and

.
—
,

the axial angles all obl ique .

The fundamental form is the tricl inic pyramid .

139 Cu be s belong to the regular system

. .

Pr i s ms are to be found in all except the regular system .

Prisms with r e c ta ng u l ar s ides i f they are S i x S ided belong to -

the hexagonal system they belong to the quadratic system i f four

sided and s quare based Prisms w ith obliqu e angl es or rhomboid
-
.

sides and ba ses belong to the monocl inic system i f any t w o o f

their axes are at right angles ; but to the triclinic system when
they have no right axial angles Prisms o f the rhombic system .

have rectangular but not s quare bases .

84 CR YS TAL S AND CR YS TALL I ZAT I O N .

Py ra m i d sbelong to all the six systems Those wit h square .

bases belong to either the regular or to the quadratic system ; i f

their faces a re equilateral triangles they belong to the regular
system but they belong to the quadratic s y stem i f their fac es are
,

i s oc el e s triangles Pyramids o f the hexagonal s y stem have .

hexagonal bases and their faces are i s oc e l e s triangl es Pyra g

,
.
-

Fi g 7 7 T t d run ca e oc Fi g 7 8 Q d t i p i ua ra c r sm Fi g 79 S tann i id
(P t i wi h p m id l d
. . . .
. , c ox e .

t h d n
o e ro o as s u m t y ra a en s
f id )
. .

e r r ocy a n e .

CR YS TALL I N E F O RM S OF TH E R H O M B I C SYS T E M .

Fi g 80 Rh om bi d bl
c ou e Fi g Rh m bi p i m
81 o c r s Fi g 82 R h m b i p o c y ra
id W th py m id l d m id l p i m
. . . . .

p y ra m i ra a en s a (P t r s o as
(Z i lph t ) i m lph t )
. . .

nc s u a e . s u su a e .

mids with rhombic or rhomboi d bases belong to the r h om bi c s y s

tem i f all the axes are at right angles ; to the monoclinic syste m
i f any t w o axes are at right angl es but not all ; and to the tr i ,

cl in ic system when there are no right axial angles .

T e trag ons have four angles or corners ; h e x ag ons six ; oc tag ons
'

eight e tc ; te tr a h e d r ons have four s ides ; h e x a h e d r ons six ; oc t o

,
.

h e d r ons eig h t ; d od e k a h e d r ons twelve etc ,

.

1 40 S ome substances crystallize with water ; others withou t

.

”
water o f c rystallization H yd r ou s cr y stals are those containing
.

water ; anhydrous crystal s do not contain it .

 CR YS TAL S AND CR YS TALLIZATIO N . 85

H ydrous crystals may however be quite d ry in the sense that , ,

they do not contain any moisture on their surface O n the other .

hand anhydrous crystal s may contain small quantities o f i n te r

,

s t i t i a l w a te r imprisoned between the individual small crystals o f

which larger crystal s always consist Crystals containing inter .

s t i t i a l w ater d e cr e i ta t e or burst with a slight explos ion when

p
heated .

CR YS TALL I N E F O RM S OF T H E M O N O C LI N I C SYS T E M .

Fi g 83 M on oc li i
n c d ou Fi g 84 M i i pi
o n oc l n c r sm Fi g 85 M on oc li i p i
n c r sm
m id di
. . . . . .

bl e py ra . of s o um a c e ta t e . of ca n e su g ar .

CR YS TALL I N E F O RM S OF TH E T R I C L I N I C SYS T E M .

Fi g 86 T i li i
r c n c pyr Fi g 87 T i li i
r c n c Fi g 88 T i li i p i
r c n c r s m
id ( g p p i l i m th i
. . . . . .

am y s um ) r sm of ca c u os u l
ph
. .

ate .

1 41 . l l i zati on i s hel d by mol ecular a tt rac

Th e w at e r of cry st a

t i on i t i s es sential to the crystalline form o f hydrous crystals

, ,

and is always a molecular proportion .

The p roportion o f water o f crystallization o f salts varies from

5% to 6 0 %
H y drous crystal s are generally formed in water solutions o f -

the c ry stallizing substances an d some salts take up var y ing pro ,

portions o f water o f crystal l ization according t o the degree o f

86 CRYS TAL S AND CR YS TALLIZAT I O N .

concentration o f the solutions Crystal s are o f cours e formed

.
, ,

only i n satu rated or supersaturated S olutions and the strength o f ,

a saturated salt solution depends upon its temperature Crystals .

formed in hot ( and therefore stronger ) solutions generally take

, ,

up less water than t hose formed in cold solutions .

M anganous sulphate crystall ized from a solution saturated at or

below 6 contains seven molecules o f water ; crystallized from a
°

solution saturated at from 7 to 2 0 it contains five molecules ; at

° °

20
°
to 3 0 it crystallizes w ith only four molecules of water
°
.

S odium phosphate crystallizes with twelve mol ecules o f water

at about but with only s even molecul es from a soluti on sat
u rat e d at

S odium carbonate crystallizes with either ten nine s even or , , ,

five molecules of w ater of crystallization according to the tem

e r a t u r e and strength o f the solutions
p .

Copper sulphate generally crystallizes w ith five mol ecul es o f

water But i f an e ffl ore sce d crystal o f nickel sulphate be add ed to
.

a supersaturated solution o f copper sulphate crystals o f the cop ,

per salt containing six molecules of water are deposited I f on .

,

the other h and a crystal o f ferrous sulphate be added instead o f

,

nickel sulphate the crystals o f copper sulphate obtai ned will con
,

tain seven molecules o f water .

Zinc sulphate cr y stall ized at the ord inary room temperature or ,

at any temperature below contains seven molecules o f water ;

°
but cr y stals formed at over 3 0 contain only five molecul es .

These facts emphasize the necessity o f regulating the tempera

ture and degree o f concentration of solution s from which sub
stances are to be crystallized .

1 42 . S alts containing water o f crystallizatio nd o not always

hold all of that water with the same force .

M agnesium sulphate gives up one molecule o f water when dried

at 3 0 to°
at water bath heat it l oses four additional mole
-

cules ; and at a still higher temperature it is rendered an hydrous .

Potash al um contains about per cent o f water o f c ry s t al li za

tion ; heated at 4 0 it gives up 2 7 per cent o f that water at 4 7
°
.
°

it loses per cent ; at 6 0 it loses most of its water ; but long

°

continued he ating at 1 00 is necessar y to expel all

°
.

Crystallized ferrous sulphate , gives up nearly

all o f its s ix molecul es of water o f crystallization at fr om 90 to °
 CR YS TAL S AND CR YS TALLI ZATIO N . 87

1 00
°
but it begins to give o ff some o f it even at the ordinary tem
p e r a t u r e o f the air .

S odium phosphate containing twelve molecules o f water loses

, ,
° °
five molecules o f that water at 4 0 to 5 0 all o f it at 1 00 °

E fii or e s ce n c e means the l oss o f crystalline form through the loss

o f the water o f crystall ization the crystal s fallin g to powder
, .

Hydrous crystals are frequently e ffl or e s c e nt but rarely d e l i q u e s ,

cent .

S olids which neither e ffl or e s c e nor del iquesce are described as

”
permanent in the air .

The solution o f hydrous crystals in their own water o f crystal

li z a t i on i s called a q u e ou s f u s i on .

1 43 . T he obje ct s o f crystallization are : 1 the separation o f ,

crystallizabl e substances from amorphou s substances when they

occu r together in one solution ( This s eparation can also b e e f
.

f e c t e d by d i a lys i s ) 2 the separation o f heteromorphous substances

,

from each other when together contained in one solution ; 3 the ,

purification o f commercial chemicals ; 4 i mprovement o f the ap ,

p e a r a n c e o f the products .

1 44 . Crystals are most readily formed when crystallizabl e sub

stances pass from the liquid or the gas eous condition to the sol id
state for the molecul es o f fluids are more mobile than those o f
,

sol ids and the formation o f crystals is the arrangement o f the

,

molecules into sol ids o f definite form accordin g to the nature

o f each individual crystallizing substance .

But crystallization n evertheless does take place even in sol ids

which thus becom e changed from the amorphous to a crystall ine
condition S ome metals are known to undergo this change ; al s o
.

arsenous oxide melted sugar etc

, , .

1 45 . M e th ods of e ff e ct i n g cr y st al l i zat i on The usual means .

o f inducing solids to assum e the crystall ine form are : 1 insoluble ,

bu t fusibl e crystallizable sol ids are l iquefied by fusion and then

allowed to cool S l owly ( par 2 9 ) 2 volatil e crystallizable solids
.
,

may be crystall ized by sublimation ; 3 soluble substances are ,

crystallized by depos ition out o f their solutions ; 4 som e l iquid s ,

are crystallized by freezing ( for purposes o f purification ) as , ,

e g glycerin , chloro form etc ( Pictet s process ) and 5 many

. .
, ,
.
’

insolubl e or very sparingly solubl e substances are obtained in

, ,

m inute crystals when produced by precipitation .

 C H AP TE R X .

CR YS TALLIZATIO N F RO M S OLUT I O N S .

1 46 .The most common and success ful method o f c ry s t a ll i za

t i on i s that o f soluble solids by inducing them to form cryst a l s
from the i r solutions .

A ny crystallizabl e soluble sol id may be comparatively easily

crystall i zed from its solution unless the substance is so extremely
,

freely solubl e as to be nearly or quite deliquescent .

A crystallizable Substance s eparates from its solution in the

'

f orm of c ry s t a l s whenever the amount o f solvent present i s i n s u f

'

fic i e n t t o retain all o f it in solution .

The ratio o f solubil it y o f a given solid in a given solvent at

any g i ven temperature is a constant ratio A saturated solution .

o f a crystallizable subs tance therefore must deposit cr y stal s

, ,

whenever the proportion o f solvent is diminished by evaporation .

C rystals are also deposited when the temperature o f a saturated

sol ution is lowered i f the cr y stall izabl e substance dissolved is
Solu bl e i n greater proportion at a higher temperature .

Cr y stallization from saturated solutions is therefore e ff ected , ,

e i ther 1 by e vapor a ti on of th e s ol v e n t ; or 2 by r e d u c ti on of th e
, , ,

t e mp e r a tu r e of th e s ol u ti on ; or 3 by both o f these means together

,

1 47 .Water Soluble chemical compounds are g e n e r a l ly pro

-

du c e d in a state of solution and are recovered from their solu

,

tions by cry stall izati on i f they are crystallizable solids .

148 .The s i ze of cryst a l s S ome subs tances naturally form

.

large crystals whil e oth ers form small cr y stal s But much can be
, .

done to incr ease or diminish the S ize o f crystals formed from

solutions .

I f l arg e a nd w e l l d e ve l ope d crys ta ls are des ired their fo rm a

tion must be slow Hence the y must be produced by ver y slow
.

evaporation of the saturated solution or by ver y slow cool ing Of ,

it A s experience has further shown that large cr y stals are more

.

readily obtained from weaker solutions than from stronger ones ,

it f ollows that the best plan i s to make the solution saturated at

not above the ordinary laborator y temperature and to expose
88
90 CR YS TALLIZATIO N F R O M S OL U TIO N S .

o f chlorate nitrate and dichromate o f potassium borax al um

, , , , ,

ferrous sulphat e l ead acetate copper sulphate and many other

, , ,

salts.

T u rbi d a t e d salts which are not a ff ected by alcohol but which

do not bear long exposure to air while in a m oi s t state should r

be washed with alcohol before they are dried as for example , , ,

ferrous sulphate .

15 0 . Gr a n u l a ti on Water solubl e salts may be granulated by

.
— -
.

evaporating their water solutions to dryness during cons tant

-

stirring a fter the salt has begun to separate The solution must .

be fi l t e r e d be fore it is evaporated and the evaporation is carried ,

on without much stirring until a pellicle begin s to be formed or

until salt separat es on the dish j ust above the surface o f the
liquid ; during t h e s ubs e q u e n t evaporation the solution must be
.

stirred to prevent the formation o f larger crystals .

S alts containing water o f crystallization can not be granulated

by evapora tion to dryness because o f the danger of expelling a
part of that water .

In the evaporation o f salts to dryness it is n ecessary to take

into account that som e o f the salts o f volatile and comparatively
weak acids and the salts o f ammonium may be partly d e c om
, ,

posed by the heat Thus a solution o f neutral ammonium sul

.

p hate might bec ome acid during the progress o f the evaporation ,

whil e a solution of potass i um acetate might become alkal ine .

Thes e di ffi culties are corrected by neut ralization .

Granulated salts are generally cry stalline but many are s im ,

ply granular powders without crystallin e form .

M any halides citrates tartrates and other salts may be g ra n u

, , ,

lated in this manner .

15 1 . The bulk or quantity o f product made has great i n fl u

ence upon the s ize a nd per fection o f form o f crystals larger and ,

finer crystal s b e ing more easil y obtained the greater the quantit y
operated upon S mall quantities o f solution sometimes refuse to
.

give good crystals of substances which crystallize well from

larger bodies o f liquid .

152 . When crystall ization is resorted to as a means of elimina ~

tion o f soluble impurities the proces s should be rather slow and

,

therefore performed from solutions saturated at not above the

ordinary room temperature .

15 3 . When the obj ect o f the crystall ization i s S i mply to con

 CR YS TALLI ZAT I O N F R O M S OL U TIO N S .
9 I

ve rt : an alrea dy pure product into good crystals and the quan ,

ti ty; o f soli d to be crystallized i s s o large as to render it desir

able to divide it into two or more portions water i s used as the ,

s olvent only on the first portion the solutions are made at a ,

so mewhat elevated temperature the crystallization i s e ffected by ,

cool ing and the mother l iquor i s u sed as the solvent for s u bs e
,
-

q uent portions o f the salt

. .
.

154 . In manu facturi ng it happens most frequently that the

solutions obtained when water soluble soli ds are produced are -

rather dilute or at all events not saturated s olutions I f the

,
.

product is to be crystallized it is then necessary to concentrat e

“ ”
the solution by evaporation or by boiling it down ,
.

S olutions o f moderately solubl e salts m a y be evaporated until

a pe l l i cl e form s on the surface o f th e solution or until a small ,

s ample o f the solution becomes turbid from the depositi on o f

small crystals on cooling or until sol id particles ( crystals ) begin
,

to form on the S ides of th e vessel near the level o f the l iquid .

Freely soluble salts can not be well crystall ized from solutions
saturated at a high temperatu re .

15 5 . L arger crystals are usually formed in turbid solutions

than in c l e a r on e s B ut clean pure products can not be obtained
'

.
,

from dirty solutions .

A powdered crystallizabl e salt when placed in a saturated solu

tion o f the same substance gradually assumes a d istinct crystal ,

line form The small particl es o f salt serve as n u c l e i for the

.

f o rm a t i on o f crystal s which may gr ow to a considerable s ize .

The size o f crystal s may be increased in a s imilar way This .

i s called n u r s i ng the crystals Gradual changes o f temperature

‘

o f the s ol u t i on c on t a i n i n g an excess o f ( undissolved ) salt promote

‘

the grow t h o f the crystal s becaus e the smallest particles redis,

s olve when the temperature i s increased an d the dis solved salt

deposits on the surface o f the larger particles ( or cr y stals ) when

the temperature falls .

T he vessel containing the solution and salt may therefore , ,

be put in a warm place occas ionally to e ff ect the result described .

156 . S t u n t e d c rys ta ls a re generall y obtained when the crys

t a ll i za t i on progresses t oo rapidly for the numerous crystals ,

formed simultaneously are apt to crowd each other The same .

result is o f course also caused by contact o f the crystals with the

, ,

bottom and s id es o f the vessel .

A

9 2 CR YS TALLIZATIO N F R O M S OL U TIO N S .

15 7 . T h e crystals formed may be either free d

( etached from
e ac h other ) a nd are then
,
usually well developed ; or the y m ay
form clusters clumps crusts or cakes
, , ,
.

D eta hed crystals and clusters o f crystals are formed i n t h e

‘

body o f the solution where they have room and fre ed o m

develop .

Crusts an d cakes of imperfect crystallization are formed o n

the S ides and bottom o f the ves sel .

To obtain particularly perfect crystal s for the purpose o f e x

a m i n i n g their form , a few crystals may be slowly nu rsed to per

f e c t i on in a smal l vessel each crystal being turned occas ionally

, ,

or the Crystal may be suspended in the s olution by a thread so as

to be free to develop in every direction .

When large quantities o f solution are made to deposit cry s

tals a mass o f fine large free cr y stals are usually formed in the
‘

, ,

center while crusts are formed on the S ides and botto m o f t h e

,

vessel .

158 R e t ar d e d cr y st a l l i zat i on O ne o f the i nconvenie nces

‘

. .

attendant upon the crystall ization o f salts from solutions is t he

formation o f supersaturated solutions wh ich sometimes refus e to
'

deposit cr y stals This can generally but not always be remedied

.
, ,

by dropping some crystals o f the same salt into the s u p e r s a t u r

ated solution When once started the crystall ization u s u a ll v con
.

ti n u e s without interruption .

The addition of another salt is a remedy rarely practicable .

But f e ta r d e d or d i fficult cr y stall ization may sometimes be ad

Va n t a g e ou s l y prevented by the very gradual addition o f a non
solvent l iquid to the solution Thus i f some alcohol is very .
,

cautiousl y laid over the surface o f a strong water solution of a -

‘

substance nearly insoluble or only sparingly solubl e in alcohol ,

th e water w ill graduall absorb the alcohol and give up the sa l t

y
which then cr y stall izes i f the process is S low enough .

S ubstances cr y stalliz ing with a large amount of water o f crys

t a l li za t i on s ometimes fail to form crystals when the solutions are

too strong or when the required amount o f water is not p re sent

,
,

as i s the case with ferric chloride .

15 9 . Cr y st al l i zer s
-
The vessel s in which cr ystalliz atio n is
.

f
e fected are called crystallizers They may be deep i f the cr ys .

ta l l i za t i on is to be induced b
y lowering the temperature o f t he
J .
C R Y S T ALL IZ A TI ON F R O M S OLU TI ON S .

solutions made saturated at an elevated temperature and the ,

mother liquor after each crystallization is concentrated by

evaporation with the aid o f heat several cr op s of cr y st al s a re ,

obtained one from each operation I n all such cases the prob
— .

able result will be that the first crop i s better than a n y S ubs e
quent one and that the last crop i s poorer than the preceding ones
,
.

1 63 Whenever crystallization i s performed for the purpose

.

of pu ri fying the substance t o be crystallized each succes sive ,

mother l iquor must contain an increas ing proporti on o f the i m

-

purities and each successive crop o f crystals must be more an d

,

more liabl e to be impure until finally the e n d m oth e r li q u or i s

,
- -

reached from which a product fit for us e without further p u r ifi ca

tion can not be obtained .

U sually only t hree crops o f satis factory product can be Ob .

t ai ne d .

But the end mother liquor i f of su fficient value can be puri fi ed

- -
, ,

by various means according to its nature and its contents f eé fov , f .

ered or utilized in one w a y o r an other For instance w h e nl t he .

,

mother liquor from R ochell e salt has been concentrated s ev eral

—

times it finally becomes dark colored from finely divided c arf f f -

bon and a white o r colorless salt can then no longer be obtai ned
,

from it ; but i f the end mother liquor be rendered strongl y acid

- -
.

by the addition o f hydrochloric aci d to it the valuable tart rate ,

radical is recovered in the form o f cream o f tartar .

1 64 Cr e e pi n g salts
. In the evaporation o f solutions o f cer
.

tain ammonium salts and a few salts o f p ot a s s 1u m and sodium

,

( as for instance the benzoates ) for the purpose o f granulating

, ,

or crystallizing thes e salts it happens that the s alt is deposited ,

on the s ides o f the evaporating dish above th e level o f the l iquid -

,

and that the solution creeps up by capillary action between the

particl es of salt and the crust thus formed by evaporation o f this
solution extends over the top o f the dish and on its outs ide
unless the salt is scraped down from tim e to time But the .

“ ”
creeping may be prevented by slightl y greasing the dish .

165 .The cr ystal s m a y be c ol l e ct e d with casseroles sc oops , ,

ladles spoons or otherwise according to thei r q u a n t i t v S mall

, , , .

crops are u suall y loosened from the cr y stall izer an d poured into a
.

funnel with the mother liquor When ver y small quantities are—
.

cr y stallized the mother liq uor may be allowed to evaporate to

-

dryness .
 C R Y S T ALL IZ A TI ON F ROM S OLU TI ON S .
95

166 The wet crystals must be w as h e d i f the mother l iquor

.
-

is dirty or impure For this purpose they are placed in a per

.

fora t e d funnel or draining cone and af te r th e m oth e r l i q u or , ,

-

h a s ru n o ff the mas s o f cr y stal s may be hastily rinsed wi th a

,

small amou n t o f col d distilled water or w ith a little alcohol i f ,

.

not obj ectionable on chemical grounds Crystals wash ed with .

alcohol are easil y dried

Be fore washing the crystal s w ith water it is necessary to ,
.

break up any clumps .

The water us ed in washing the crystal s usually spoils thei r

appearance somewhat by taking o ff the sharp edges To avoid .

thi s they may be washed with a pure saturated solution o f the

sa substance
l
gC eystals f rmed in sol utions made from pure substances o f
.

( r o .
,

a
g e do not need washing .

51 67 Wet crystals and crystalline products are drai ned in per

.

fl e d funnels or drain ing cones or on musl in strainers When

, , .

atri a l quantities of cry stal s are formed in dishes or beakers thes e

2 vess els may b e tilted in su ch a way as to

‘

L
: 0
-

J all ow th e moth er liqu or or w ash water

o
- - -

to run o ff Th e w e t crystals or mas s .

‘

should b e allowed to stan d lon g enough

to b eco m e thoroughly freed fro m l i quid ,

so that th ey are n early o r quite dry u n ,

less greater despatch is n eces sar y .

F i g 90 P i t i psf di h f on The B uchner funnel ( fig 1 8 ) and the

o s or
d g of y t l
. .
. .
,

ra i ni n cr s a s .

c e n t r 1 fu g a t o r ( fig
9 )
1 are also us ed 1 n .

freeing cr y stal s fro m water .

S mall quantities o f wet or moist crystal s may be drained or

even dried on porous tiles or on pure white blottin g paper or
fi l ter paper Bu t handsome S lender crystal s S houl d not be
.
,

pressed between paper or cloth i f they are so frail as to be broken

or crushed by that treatment .

168 The dr yi n g of crys t al s is a very important matter

. .

S ubstances which are permanent in the air and not a ff ected by

moderate heat m a y be ver y eas il y dried in layers about 1 5 to 2 0
millimeters thick on plates o f glass D ouble thick window glass .

is suitable .

The product shoul d be frequently stirred or turned with a por

c e l a i n spatula or other S u itabl e stirrer .
9 6 C R Y S T ALL IZ A TI ON F ROM S OLU TI ON S .

Hydrous crystals should be dried at temperatures not above

3 0
°
to
E fflo re s c e nt and deliquescent hydrous salts are liable to b e
partially dissolved in their own water i f dried at a too high tem
and this would greatly damage i f not ruin the produ t
‘

r a t u re c
p e .

A lcohol washed crystal s dry rea dily

- .

A nh y drous crystals may in most cases be dried at 1 0 0 to 1 20 ° 0

but i f this i s not convenient they may be exposed a longer time

and dried at a lower temperature .

Wh en crystalline or other salts are dried with the ai d o f heat ,

it is necessary to know whether or not th ey are in any way .

chang ed or inj ured by the heat to which the y are exposed an d ,

the temperature must be regulated accordingly .

S odium bicarbonate when dried with the ai d o f heat i s l iable

to give off C O as well as water A ce 2
.

tates dried with or without th e a i d of

heat are liabl e to lo se acetic acid L ead .

acetate in v ery smal l cr y stals should be

dried in an atmosphere of acetic acid
vapor .

Crystal s dried by expo sure to the air

are liabl e to b e of dull app earan ce .

Cr y stals may b e qu ickly dried by c en

t r i fu g a t i on When drainin g 1 S 1 m p rac
.
'

t i c a bl e as when th e adhering m o ther

,
'
li qu or is dens e or syrupy th e drying i s ,

e ffected in rapidly revolvin g p erforated

drums Granulated sugar is dri ed in that
.

way Th e small centrifugal mach in e

.

gné iif fié gi 3
F

i gi fi
f

g z
te
this text may m t i m e s be
’

g l e 1 S o e
é i fi gg i fi
‘ r

t 21 vantage for dr y i ng e ffl o r e s c e n t
.

an d p re c ipit t a es .
s

salts an d oth er pro ducts di fficult to d ry

in the usual simple w a y ( by expo sure to th e air) .

D esiccators are rarel y used for dr y ing inorganic substances .

The y are glass bells placed upon plates o f glass over ves sels
containing fused calcium chloride calcium oxide concentr ated , ,

sulphuric acid or other ver y h ygroscopic substances which fab

,

sorb the water vapor given o ff from the crystal s or other sub
stances placed above or beside them S e e fig 5 3, . . .

169 . B efore being bot t l e d the produc t mu st be perfectly dry .

,
 CH A PT E R XI .

D I AL Y S I S .

17 1 . is a proces s by w hich crystalloids may be com

D i al y si s
“ ”
p l e t e l y el iminated from colloids when both kinds o f substances
occur together in water solutions I t is the di ff usion o f cr y s
-
.

'

t a ll oi d m a tt e r i n aqueous sol ution through a suitable organic

septum The septum generally us ed is parchment paper This
. .

is tied tightly over a circular frame o f glas s porcelain hard rub

.
, ,

ber or wood so that the fram e form s a vessel resembling a s ieve

, ,

o f which the parchment paper is the sieve cloth or bottom This .

apparatus is called a d i a lys e r and when it i s used the solution ,

which is to be subj ected to d ialysis is placed in the dialyser which

is susp end ed in a large ves sel containing
water as S hown in th e cut , .

172 Cr yst a l l oi d s ar e substanc es which

.

res embl e crystallizable water soluble com -

pounds i n that they pass through s uch

s epta as parchment paper wh en in a state
of s oluti on in water an d placed in a dialys er .

A ll water s oluble crystallizabl e salts are -

crystalloids ; but crystalloids are not n e c e s

s a ri l cr stallizable
y y .

Fi g 92 D i ly
. . a
Col l oi d s ( from c ol l i i m glue and e i d os
ser . , , ,

like ) are water solubl e substances which —

like glue gelatin gum etc are unable to pas s through the d i a ly
, , , .
,

ser in the manner described .

Crystalloids and colloids can therefore be separated from each , ,

other by dial y sis .

1 73 . D ial y sis is emplo y ed in chemical processes to separat e

inorganic cry stalloids from organic colloid s for the purification o f ,

certain chemical products etc ,

.

A r senical compounds lead salts poisonous alkaloidal salts etc

, ,
,
.
,

taken into the stomach m ay be completel y dial y sed out o f the

mixtu re o f the total contents of that stomach and then easily ,

S eparated and identified .

 DI AL Y S I S .
99

S alicylicacid may be freed from impurities by dialysis .

“ ”
The preparation called dialysed iron is a water solution of a
-

compound formed by saturating a dilute solution o f ferric chl oride

with ferric h ydroxide and then removin g by dialysis whatever
ferric chloride remains unchanged together with the ammonium
,

salt left in the ferric hydroxide S houl d th is be incompletely

washed ( or not washed at all ) .

The liquid passing out o f the dialyser is called the di ff usate

.

To perform dial y sis S uccess fully the dial y ser shoul d not be
filled but S hould contain a quantity o f l iquid not over I O to 1 5
,

millimeters in depth .
 CH A PT E R XI I .

P RE CIPIT A TI ON .

1 74 . Pre ci pi t at i on is the formation o f insolubl e sol id matter

in a l iqui d .

The insoluble solid formed is called a pre ci pi t at e .

T h e p r e c i p i t a t e may be absolutel y insolubl e in the l iquid in

‘

which it is formed or it may be so sparingly soluble as to be

,
“ ”
practically insolubl e It may be n early insoluble in that liquid
.

at the ordinary r oOm temperature but more soluble in th e S ame ,

liquid at a higher temperature and may be very soluble in other ,

l iquids .

Precipitation occurs onl y in liquids .

1 75 . It i s important that distinction be made between phys i ca l

p r e c i pi ta ti on and c h e m i c a l pr e ci pi t a ti on .

Ph y si cal pre ci p i t at i on occurs when a su fficiently strong solu

tion of a soli d substance i s mixed with a su fficient proportion of
some l iquid miscible with the solvent but in which the dissolved
substance is insoluble Th e dissolved substance is then more or
.

less completely thrown out o f its solution r e assuming the soli d ,

-

state N o chemical reaction takes place in physical precipitation

.
,

for al l the substances contained in the liqui d before and a fter

the precipitation including the solid substance precipitated were
, ,

already present or added and no new substance is formed .

Ch e mi cal pr e c i pi t a t i on results from the formation o f n e w mole

cules in a l iquid or a mixture o f liqui ds one or more o f the

, ,

new substances being insoluble in the l iquid or m ixture Chemi .

cal precipitation is therefore al ways caused by chem ical r e a c

, ,

tion and the precipitate is in al l cases o f chemical precipitation an

,

insoluble product o f that reaction The chem ical reactions by .

which precipitates are formed may or may not be complete a c

cording to the proportions o f the reacting factors a n d a ccording
to other c ir cumstances attending the precipitation .

It will be seen from the foregoing that ph y sical precipitation r e

s u l t s from a change in the solvent by which it i s converted into

a non solvent while the substance originally held in solution and

-
, , ,

1 00
I OZ P RE CIPIT A TI ON .

chemical compounds by precipitation are with rar e exceptions , ,

s ol u bl e c om pou n d s Hence the compounds o f potassium s o

.
,

d i u m ( and ammonium ) are very largely employed to furnish the

negative radical s of the insoluble inorganic products and the ,

sulphates nitrates and chlorides o f the other metal s are the most
,

common materials furnishing the positive radical s ( the metal s )

toward the formation o f the same products ( S e e Chapter X I X
.
,

V ol I )
. . Thus the factors o f the reactions are chiefly salts .

They must o f course be o f satis factory quality

, ,
.

1 80 . Pr op or t i on s of t h e f a ct or s Whil e the relative quantities

.

to be taken o f the material s are always computed on the ba sis

o f the n umber o f molecules required o f each to complete the
reaction ( as shown by th e chemical equation representing it ) ,

it must be borne in m ind that the exact proportions thu s found ,

although absolutely correct in theory rarely give satis factory ,

results because in the production o f insoluble compounds by pre

,

c i p i t a t i on it is almost invariably necessary that the factor supply

ing the positive radical o f the insoluble product shall be com

p l e t e l y decomposed and for,
this reason the other factor o f the
reaction must be used in excess o f the proportion indicated by
theor y .

Thus when an insolubl e i ron compoun d i s to be prepared by

,

precipitation the iron salt u sed for that purpose must be com
p l e t e l y decomposed ; i f a mercur y compound is to be m ade all
of the mercuric chloride used must be consumed ; i f a l ead com
pound is prepared out o f l ead nitrate not a trace of the lead nitrat e
must be left over E xper i ence has shown that i f an insoluble
.

compound o f any given metal when it i s being formed bv pre i ,

c i p i t a t i on is allowed to come in contact with a solubl e com

,

pound of the same metal contained in the liqu id in which the r e a c

tion is effected the composition o f the product sought may not be
,

normal Pure mercuric iodide is n ever forme d when solutions

.

containing the exact theoretical proportions o f mercuric chloride

and potassium iodide are mixed ; pu re mercuric oxi d e i s not
formed when the exact theoretical proportions o f mercuric
chloride and sodium h y droxide are mixed ; pure normal ferric
h y droxide is not obtained when a mm om a 1 s added to a solution o f
'
ferric sulph ate .

A n e x c e s s must therefore be used o f that factor which sup

, ,
 P RE CIPIT A TI ON . 103

plies the negative rad ical o f the precipitate in order that ever y
molecule o f the other factor m ay be decomposed .

To insure that a pure lead iodide i s obtained from lead acetate

and potass ium iodide an excess o f the potassium iodide is meces
,

sary in ord er that no lead acetate m ay be left undecomp osed for ,

i f lead iodide in the act of its formation as a precipitate comes

in contact with lead acetate in solution the precipitate will not
“ ”
consist o f pure l ead iodi de but o f s o called ox y iodide o f lead
- -
.

How much o f an exces s is actually n ecessary it is di fficult t o

state Perhaps from three to five per cent is a su fficient addition
.

to the quantity theoretically required ; bu t in cases where e x p e r i

ence has shown that the tendenc y toward the formation o f meta
“ ”
compounds basic compounds double salts and other abuor
, ,
-
,

mal or undes ired products i s great an excess o f even ten per

, ,

cent above the quantit y call ed for according to the chemical equa
tion may be requi site A considerabl e exc ess is sa fer than a
.

very small one and no disadvantage can attend the use o f a larger
,

quantity than is reall y necessary except that it would be an u n

ne cessa ry waste Th e practical question be fore the operator is
.

simply which o f the two evil s he wil l choose a slightly increased

,
—

cost o f production without a n y risk o f spoiling the product or the ,

reduction of the cost o f production to a minimum coupl ed with

the danger o f obtaining an unsati s factor y product I n this con .

n e c t i on it i s well to take into consideration the fact that in the

production o f inorganic chemical s the necessary labor and skill

are quite general l y worth much more than t h e cost o f the mate
rials .

181 . Th e s ol u t i on s u se d for mak ing precipitates must be per

f e c t ly cl ear . F i l tr a ti on i s al most invariabl y neces sary to insure
this.

It may be said that within certain limits dilute solutions

, ,

are more favorabl e to free and complete chemical interaction than

strong solutions But the s tr e ng th o r the degree o f concentration
.
,

or dilution which ought to be fixed upon in each case must be

,

determined by several circum stances In some cases the materials

.

emplo y ed may not be s u ffic iently freely solubl e to admit o f the

use o f a n y other than weak solutions .

Comparativel y d ilute solutions should always be made o f any

salts th e complete decomposition o f which i s to be insured ; and
stronger solution s shoul d be made o f a n y alkal ies or salts which
1 04 P RE CIPIT A TI ON .

are to be present i n e x c e s s in the l iqu id in wh ich the reaction

takes place Thus when ferric hydroxide is made from solutions
.

o f ferric c hloride and ammonium h y droxide the iron solution ,

should be weak but the ammonia les s dilute When y ellow oxide .

of mercury i s made the solution o f s odium h y droxi de n e e d not

be very diluted and in fact ou g h t n ot to be so but the solution o f
, , , ,

mercuric chloride m u s t be weak .

D ilute solutions as a rul e make l ight or bulky finel y divi ded

, , ,

precipitates while str ong solutions produce heavier or denser

, ,

coarser precipitates
,
.

But e x pe r i e n c e is the best guide There fore unless the laborant .

,

has had su fficient experience o f h i s own he should be guided by ,

that o f others The directions given in reliable laboratory man

.

u a l s are based upon the experience o f many operators .

The t e mpe r a tu r e o f the solutions is al so a matter o f consider

abl e importance i n many precipitations S ome precipitates are .

liabl e to be decomposed or otherwise inj uriously a ff ected by heat

and therefore require to be made from cold solutions Col d
, ,
.

solutions frequently produce more bulk y and finel y d ivided pre

c i p i t a t e s where hot solutions make denser products .

1 82 . Th e or d e r of m i xi n g t h e sol u t i ons i s o ften one o f the

necessary condition s o f S uccess .

It is necessary to make proper di stinction between the t w o

solutions emplo y ed for the production o f precipitates by meta
thesis and the onl y technical terms I find in us e are the words
,

“ ”
precipitant and f p r e c i p i t a n d ‘
The solutions are necessarily .

mixed by adding one to the other [ The suggestion that both .

solutions be simultaneously poured together into the precipitation

vessel is probably not o f any value in a s ingle instanc e ] The
solution first put into the precipitation vessel was called the pre
”
c i p i t an d ; and the other solution poured into the first one was , ,
“ ”
called the precipitant M any have d iscarded or refused to
.

adopt the term p r e c i p i ta n d becaus e it is scarcel y poss ibl e to pro

nounce the two words so distinctly that one is not m istaken for
the other I shall therefore use the expression pr i m a l s ol u ti on
.
, ,

in this book meaning thereb y the solution which is put in the

,

precipitation vessel firs t ; and will retain the term pr e c i pi ta n t to

designate t he solution which is to be added to the primal solution
“

But which of the two solutions shall we pour into the j ar

—

first ? L et us consider an exampl e The s o called ammoniated .

—
1 06 P RE CIPI T A T I O N .

s h ou l d n o t be pr e ci pi ta te d i n a pr i m a l s ol u ti on c on ta i n i ng a c om
p ou n d o f t h e s am e m e ta l th a t e n te rs i n t o t h e c om pos i ti on of th e
r e c i pi ta t e
p .

A precipitated m e c u ry Compound
should not be produced in a
solution o f a mercu ry salt ; do not make an insoluble iron com
pound i n a liquid containing a soluble iron salt ; do not let an insol
uble lead compound be formed in a solution or mixture containing
a l ead salt ; a precipitated copper compound should not in the act ,

o f its formation be a llowed to come in contact w ith a copper solu

,

tion ; do not let an insoluble zinc compound lie in a solution of a

zinc salt and do not make it in such a solution
,
_
.

I f ammonia water be added to a solution o f ferric sulphate the

reaction will be as follows

0 .

B ut i f a solution of ferric sulphate be added t o ammonia water

the result is

It is clear that i f ammonia water is gradually added to a solu

tion o f ferr i c sulphate the ferric sulphate will at least at the be
, ,

g 1nn 1n
g be present in excess ; but i f the order of m ixing the
,

liquids be reversed the ammonia water will be in excess With

, .

the ammonia present in excess it is impossibl e to obtain any other

products than F e ( O H ) and ( H N ) S O for the F e ( O H ) i s
3 4 Q 4, 3

insoluble in and una ffected by the ammonia water and the a m

m on i u m sulphate ; all o f the ferric sulphate i s decomposed as fast
as it is added and there i s accordingly no ferric salt present in
,

the solution at a n y time But when the solution o f ferric sulphate

.

i s used as the primal solution and the ammonia water a s the p re

c i p i t a n t the ferric h droxide Pe ( O H ) first formed redissolves
y ,
'
in the solutio n o f ferric sulphate

S ubsequently when more ammonia is added the

, ,
basic ferric
sulphate is decomposed
 P RE CIPIT A TI ON . 1 07

F e4O 5 0 4 ) 5 + 1 0 H 4 N O H :

4 O F e O H +5

A ssuming that th e proportions o f the factors are correct we ,

know that when one l iquid is added to the other the pr ecipitant
, ,

is compl etely decomposed as fast as added and the primal solution ,

remains in excess from b eginning to end provided other condi ,

tions are favorable .

T o insure complete decomposition o f the precipitant as

fast as it is added to the primal solution it is necessary to observe
,

the following precautions :

.a The precipitant S houl d be a rather dilute solution wh il e the ,

primal solution should be less diluted ( bu t not concentrated )

.b The preci p itant shoul d be added slowly or gradually and , ,

thi s is best accomplished ( when great caution is necessary ) by

running it into the primal solution through a syphon o f small
diameter O r the prec ipitant may be added in small portions one
.
,

port ion at a time .

.c The primal solution should be wel l stirred as the precipitant ,

is added an d brisk stirring o f the mixture should be continued

,

without interruption until al l o f the precipitant has been used .

It may be readily seen that i f the precipitant be added too

rapidly in rather large quantities and without stirring some o f
, , ,

the newly formed precipitate m ay come in contact with portions

o f the undecomposed precipitant which is the danger to be par
,

t i c u l a r l y guarded against .

1 84
. When ve ry concentrated solutions are u sed the reaction
is liabl e to be incomp lete especially i f the precipitate is bulky
“

.
,

The precipitation is generally more compl ete when hot l iquids

are u sed ; but hot solutions should not be employed unless it is
certain that the precipitate will n ot be 1 n ju r 10 u s l y altered by the
higher temperature .

1 85
. O ccasionally the proportions o f the factors o f the r e ac
tion can not be fixed beforehand in accordance with their
mol ecular weights This happens when the quantity o f the com g
.
-
,

pound contained in the primal solution i s unknown The p rep ip .

i t a n t i s then to be added cautiou sl y a small portion at a time

, ,

until it ceases to cause further precipitation To guard against .

a dding an excess o f the precipitant in such cases it i s best to tes t

 08 P RE CIPIT A TI ON .

the l iquid from time to time by filtering o ff a test sample and

testing that with a drop or more o f the precipitant Complete .

and even precip itation may thus be accomplished i f a d m i s s i bl e ;

but it is generally best to stop the further addition of precipitant
before qu ite all o f the other factor o f the reaction ( that contained
in the primal solution ) has been decomposed and in no case ,

should an excess o f the precipitant be used unless requisite for

some special reason or known to be proper .

1 86 . Th e p r e ci p i t a te Precipitates vary greatly in their physi

.

cal properties The y may be crystalline o r amo rphous he avy or

.
,

light dense or bulky coarse or fine ; they may be granular or

, , ,

curd y or fl occulent or g elatinous A very bulky finely divided

, ,
.
, ,

a m orphous almost pasty or gelatinou s precipitate tenaciously

,

retaining much wate r is call ed a m ag m a ,

.

We have said that hot and strong solutions are l ikely to produce
denser heavier and coarser precipitates wh ereas cold an d dilute
, ,

solutions tend to produce bulkier lighter and finer precipitates ,

.

But the denser precipitates formed in hot liquids generally be

come bulkier i f allowed to remain in th e liquids long a fter they
have become col d and bulky precipitates become denser i f l eft
,

a long time in the l iquids in which the y are formed P recipitates .

should therefore be collected and washed as expeditiously as

, ,

practicable i f it is des ired to prevent such changes The h y d r ox .

ides carbonates and phosphates of calcium magnesium and iron

, , , ,

and aluminum hydroxide when precipitated in the col d are so , ,

bulky and finel y divided as to be nearly gelatinous and they are

. , ,

therefore precipitated from hot solutions instead ; but i f they are

, ,

al lowed to remain in the l iqu id until it becomes cold and washed ,

with cold water the obj ect o f the use of hot solutions is at least
,

partially defeated .

Precipitates which c ontain water or from which water may be ,

split off by rearrangements o f the interatomic linking vary in ,

compos ition according to the temperature o f the l iquids in which

they are formed This variableness may be obse r ved in mag
.

n e s i u m carbonate the carbonates o f zinc and o f lead

, ferric h y ,
”
d r ox i d e and several other compounds
, Precipitates made and .

washed in hot liquids sustain a loss o f water ; those made and

washed in col d l iquids do not O n the other hand some pre .
,

c i p i t at e s take up water when long exposed to its action at the

ord inary room temperature or the y m a y undergo other changes , .

I I O P RE C IPIT A TI ON .

S pecial precipitating j ars o f glass porcela in or

so -
called , ,
'

other e a rt h e a a r e are sometimes used They are tall round

,
.
,

vessels wider at the bottom than at th e top as shown in the cut

, , .

S ome precipitation and decantation vessel s are tubulated or ,

provided with spigot s or taps at various heights as shown in fig , .

9 4 to serve as outlets for the removal o f the supernatant liquid .

whenever the precipitate has subsided su fficiently .

Fi g 95 B k
ea er i h li p
w t Fi g 96 B k ih
W t ou t li p Fi g 97 Pr c i p i t a t i on
p
. . . . . ea er . . .

fl as { s.

But any well glazed acid proof j ars or porcelain o r glass ve s

,
-
,

sel s may be u sed and f or quite small quantities the ordinary

,

E rlenmeyer flasks beakers an d wide mouth bottles

, ,
—
.

1 89 The liqu id in which the precipitate is formed obtained

.
,

by mixing the two solutions ( the precipitant and the primal solu
tion ) contains the by e product dissolved in it It is called the
-
.

m ot h e r l i q u or the same technical term being used to designate

-
,

this liquid as is given to the l iqui d from which the cr y stals are
deposited in the process o f cr y stallization I f the precipitate i s .

heavy enough to s ink down t o the botto m o f the precipitation

vessel or at least to descend below the surface of the mother
,

liquor then the cl ear or nearl y clear l iquid standing above the
,

precipitate is called th e s u pe r n a ta n t li q u i d .

It I s in some cases important to remove the precipitate from the

mother liquor or supernatant liqui d as quickl y as practicable
-

lest the p roduct be unfavorab l y aff ected by too long contact

with it .

1 90 .R e m ov al of t h e mothe r l i q u or or supernatant liquid i s -

necessary be fore the precipitate can be e ffectivel y washed .

 P RE C IPIT A TI ON .
I I I

S hould the bye product contained in that l iqu id be o f su fficient

-

value to warrant its recovery it i s o f course desirabl e to collect , ,

the mother l iquor with as l ittl e loss as poss ible A fter filtration
-
‘

the solution may then be concentrated by evaporation and the

bye product crystal lized out But owing to the necessity o f em
—
.

ploying an excess o f one o f the factors of the reaction the bye

product is rarely pure and must be purified before it can be
,

utilized S hould this be the case the mother liquor may be boil ed
.
—

down t o concentrate it before filtration and the filtrate or the , ,

residue obtained upon its evaporation purified by whatever ,

method m a y be applicable in each case S alts recovered from .

mother liquors a fter p r e c i p i t a t i on s m a y often be purified by r e

'
-

p e a t e d recr y stallizations When the . bye product is to be re -

covered i t is advantageou s i f in other respects unobj ectionable

, ,

to employ strong solutions in per forming the precipitation for ,

the mother liquor will then be less diluted and less concentration
-

by evaporation will be requi red .

I f the by e product is not to be recovered it i s neverthel ess de

-

s irable t o separate the mother liquor from the precipitate as far -

as possibl e before proceeding with the washing process becaus e -

,

the obj ect o f washing the precipitate is the complete removal o f

al l o f the soluble matter and thi s is more speedily e ff ected by first
getting ri d o f as much as poss ibl e o f the mother liquor than by -

removing only a portion o f it and diluting the remainder .

S upernatant l iquids whether mother liquor or washings are

,
-
,

removed from the precipitat e by d e ca n ta ti on either by tilting the ,

precipitation vessel or w ith the aid o f the tubulures or spigots i f

”

a tubulated ves sel i s used or with a syphon The decantation o f

,
.

liquids an d the utility o f the guiding rod and greased rim have
been su fficiently discussed in Chapter V I The p reparation .
,

rigging and us e of c l oth s tr a i n e rs and the u se of pr e s s e s for the,

separation o f l iquids from bulky precipitates are also described in

the same chapter .

191
. Th e w ash i n g A fter the mother liquor has been separ
.
-

ated from the precipitate as far as practicabl e the soluble matter ,

o f which a con siderabl e quantit y stil l remains adhering to and

contam inating th e product must be washed out A s the p r e c i p .

i t a t i on itsel f is generall y performed with aqueou s solutions and

t he by e product i s water soluble
-
the washing is e ff ected with
-
,

water .
 I 2 P RE CIPIT A TI ON .

The water used for this purpose m a y be either hot or cold a c

cording to t h e r e q u i r e m e n t s o f each case When h ot w a te r must
'

or can be u sed it is more e ff ective in removing the soluble matter

, ,

so that a smaller quantity o f hot water w ill do as much work as a

larger quantity o f col d water an d do it more quickly A nother .

advantage gained when hot water can be sa fely used is that it

renders the subsidence of the precipitate easier by making th e
l iqu id lighter and ( in some cases ) the precipitate more dense
,
.

1 92 . R api d w as h i ng is very desirable because prolonged con

tact with water frequently causes the precipitate to contract when
this is not desired or it m a y have the opposite e ff ect when the
,

precipitate w a s produced from hot l iquids .

1 93 .H e at/y pr e c i pi ta te s are the easiest to wash They subside .

rapidly and compa ctly in the precip itation vessel so that t h e

mother liquor can be almost compl etely removed
-
The wash .

water is then added and the precipitate thoroughly mixed with i t

“ ”
by vigorous shaking or s t i r r I n g ; the first washings must then
be thoroughly removed before a second portion o f water is a dded ,

the S haking or stirring repeated and the s econd washings al so

,

separated b efore a third portion o f water is added B y repeating .

the a ff usion and decantation o f water several times the wash i n g

“ ”

will be readily finished .

1 94 .L i g h t pr e ci pi ta te s a n d m ag m a s are not so easily washed

because they do not settle down to the bottom o f the precipitation
vessel either rapidly or compactly S houl d the precipitate remain
.

suspended in the mother l iquor on account Of the too great den

-

s i t y o f that liquor the di fficulty may sometimes be remedied by

d ilution ( with hot water i f admiss ible ) or by warming the mix 3

,
-

ture I f this method should be inadequate or i nadmissible the

.

thick mixture may be turned into a muslin strainer and allowed

to drain The muslin strainer shoul d first be d i ppe d i n h ot w a te r
.

and wrung out before it i s placed on the frame an d bagged to

receive the precipitate or magma S hould the liqui d which passes
.

be turbid it must be returned until it runs cl ear When all o f th e .

l iqu id has passed through the straining cloth the pasty magma ,

on the cloth is returned t o the cleaned precipitation vessel ( or to

any other sui table pot ) an d there thoroughl y mixed with water ,

a fter whic h the mixture is turned into the muslin strainer again
a n d the washings allowed to pas s thr u h Th e se operations a r e
o g .
 14 P RE C IPIT A TI ON .

product i t i s necessary to use chemic al r e ag e n ts t o d e t e r m i n e th e

c ompl e ti on of t h e w as h i ng from the entire absence o f the solubl e

substances in the en d washings The soluble substance contained

.

in the mother liquor and washings is known from the material s

-

employed and the reaction which occurs between them and the ,

reagent required is therefore also known A s the materials

, ,
.

most generally used are sulphates and chlorides the reagents for
the i dentification o f these compounds are much in demand for
te sting washings in the preparation of precipitated products .

Thus the test solutions o f barium nitrate or chloride an d S ilver ,

nitrate are the most common reagents

,
.

A fter completing the washing proces s the n ext step is

-

usually that o f letting the precipitate d r a i n preparatory to d r y ing

it The draining process m a y be eff ected on a cloth stra iner or
.

on a paper filter according to the quantit y The w e t precip itate

,
.

is allowed to l ie undisturbed on the c l ot h or filter until no more

liqu id passes ; the dropping sometimes ceases wh ile the p r e c i p i
tate still retains much water and in such cas es it is worth while
to give the strainer frame or funnel a gentl e tap which o ften h as ,

the e ff ect o f causing some more water to run o ff .

The centri fugal machine may sometimes be advantageously em

ployed to throw o ff moisture from wet precipitates as well as from
wet crystals .

1 99
. The removal o f drained or dried precipitates from strain
ing cloths and filt ers mu st be e ffected with su fficient care I f the .

precipitate has been thoroughl y drained it generall y comes o ff

very easily and i f allowed to d r y completely on the cloth or paper
,
'

it often comes off still more readily ; but large bodies or thick
la y ers of magma d ry too slowly and are therefore generally , ,

spread out on glass plates or on tiles or stoneware d ishes to dry .

When precipitates have been drained on a cloth strainer a s

far as pr acticable they may be loosened or i f necessary scraped o ff
and trans ferred to the plates on which they are to be dried or to ,

dry cloths placed on frames .

To remove precipitates from paper filters the paper mu st be

carefully unfolded so that it m a y not be torn and i f the p re c i p ,

i t a t e adheres to the paper rendering it neces sary to scrape it o ff

, ,

this must be done cautiousl y in order to avoid getting fragm ents

or fibers o f the paper mixed with the product I n un folding the .

paper filter to remove the precipitate it i s well to first place it upo n

 P RE C IPIT AT I O N .
I I5
a clean cloth or sheet o f paper or in a dish or on a glass plate , , .

200 . The dry i n g o f precipitates i s occas ionally di fficult A ll .

products o f this kind must be thoroughly dried The drying may .

frequently be e ff ected on hot plates or on frames or plates in a ,

d rying room or dryin g closet But some precipitate s either do.

not withstand exposure to heat or dry into hard tough cakes that ,

can not be easily reduced to so ft fine powder M any precipitates ,

.

form so ft friable l ight masses when dried at the ordinary tem

, ,

t e r a t u r e an d this is a great advantage because the cakes or lumps

,

so obtained can easily be gently rubbed through a fine sieve cloth

to form so ft fine bulky products , ,
.

S mall amounts o f moist or wet precipitates wh ich can not be

dried in the ordinary w a y without d i fficulty or much delay may
be spread out in thin layers on clean new porous unglazed stone , , ,

ware dishes tiles or bricks which may in man y instances be u sed

, ,

w arm or even hot Common flower pot dishes are o ften u sed to
.

advantag e But porou s dishes tiles and bricks can o f course

.
, , ,

not be used more than once .

Precipitates wh ich are known to be s ensitive and l iable to be

inj ured by exposure to air should be dried as quickly as p ra c t i
,

cable and thos e that are inj ured by light must be d ried in a dark
,

place A ll o f them must be well protected against dust and dirt ;

.

they may be loosely covered with thin muslin or white filter

paper .

201 . Pul v e ri zat i on of pre ci p i t at e s S ome precipitates a r e .

m icro crystal l ine or granula r and form coars e or moderately fine

-

powders when dry without requiring any pulverization B ut pre .

c i p i t a t e s which dry in hard cakes or lumps must be reduced to

very fine powder by s i fting or by trituration or grinding followed

,

by si fting The finer and so fter the powder is the better unless
.
,

it be of perfectly uni form m icro cr y stallin e structure But so ft -

.
,

friable lumps are unobj ectionabl e in several cases according to ,

ci rcumstances .

202 . We have already referred incidentally to the fact that

solubl e salts may also be prepared by metathesis accompanied by
precipitation the precipitate being the bye product It i s n e c e s
,
-
.

sary in all such c a s e s to care fully guard against contamination o f

the solubl e product by the presence o f an undue exces s o f one
o f th e substances used as materials and it may not in frequently ,

be found advantageous to emplo y the exact proportions required

I 16 P RE CIPIT A TI ON .

o f the factors according to the chemical equation representing

the reaction instead of using an excess o f one o f them or it may ,

even be best t o us e an exces s of that factor which contributes the

positive radical toward the formation o f the insoluble bye product -
,

and then als o to mix the solutions in such order as to insure the
preponderance of the right one of th e factors throughout the
chemical interaction It I s evident that m all t hes e cases our fir s t
.

concern is not the composition o f the precipitate but the purity

o f the soluble product .

This method of preparing solubl e inorganic salts i s not gener

ally employed when quit e pure produ cts are desired because it ,

does not generally lead to sati s factory results The solubl e salts.

recovered from the mother l iquors o f p r e c 1p 1ta t i on s u sually r e

-

quire p u r i fi e a t i on by repeated recrystall ization or by other means

to render them fit f or use .

203. A l c oh ol i c s ol u ti ons an d solutions made with glycerin

, ,

acetic acid and other solvents instead o f water sol utions are
, ,
-
,

also emplo y ed in the production o f precipitated chemical s .

A lcohol and other liquids may also be used instead o f water f or

w as h i ng the precipitates in special cases where C ircumstances re ;

quire it .

204. The precipitant may sometimes be a sol id or a gas instead

o f a l iquid or a solution Calcium carbonate placed in a sol ution
.

o f bromide of iron precipitates the iron and leaves calcium bro

mide in the solu tion Carbon dioxide precipitates calcium car
.

bonate from solutions containing calcium hydroxide and barium ,

carbonate from solutions containing barium hydroxide Hydro .

gen sulphide is often conducted into solution s containing com

pounds of arsenic or o f other metals for the pu rpose o f rem oving
the metal s in the form o f insolubl e sulphides .

205
. The purification of commercial ch emicals i s frequ ntly e

e ffected by precipitating the obj ectionabl e impurities from their

solutions I ron m ay be thus removed from solutions o f zinc salts
.
,

the precipitant used being zinc oxide o r zinc carbonate and iron ,

is removed from ammonium chloride by adding ammonia to the

solution of the chloride .
1 18 C H EM I CAL S OLU TI ON WE T ox i D A T I O N ETC
—
.
,

the hydrog en o f the sulphuric aci d which contributes the sulphate

radical toward the formation of the copper sulphate and the two
hydroxyl s o f the molecule o f sulphuric acid which is reduced to
S O , form together the t w o molecules o f water
, ,
.

When silver mercury copper lead or bismuth is dissolved

, , , , ,

in nitric acid w e have again a similar condition reactions i n —

cluding both substitution and oxidation

or ,
to trace the interchanges more clearly

—
j H 20
—
.

When metallic oxides are dissolved in aci ds the bye product i s -

water formed by the hydrogen Of the aci d with the oxygen o f the
oxide

Z n O + H 2S O 4 —
: Z nS O4 — —
j H Q O .

When metallic hydroxides are dissolved in acids the bye prod -

u e t is again water but twice a s much water i s then formed a s

,

when the oxide is used

1, O
-
.

When acids are saturated w ith metall ic carbonates two bye

products are formed namely water and carbon dioxide becaus e
, ,

carbonic acid as soon as formed breaks up into H 20 and CO 2

208 The acids or other chemical solvents are sai d t o be n e u

.

“ ”
t ra l i ze d or saturated by the metal or metall ic compound d is
solved and these expressions are u sed because the point o f
,

neutralization or saturation is frequently determined by the aid

“ ”
of test pap er -
.

But in man y cases the acid m ay be completely saturated by

adding to it an excess of the metal or metallic compound This .

can be safel y done whenever there i s no danger o f the formation

 C H EM I C AL S OLU TI ON —
WE T OX I DA TI O N ,
ETC . 1 19

o f meta compounds or bas ic salts or other undesired products

-
, .

It is safe to saturate sulphuric acid with zinc iron or copper , , ,

or hydrochloric acid with iron or zinc or nitric acid with s ilver , ,

l ead or copper ; but i f salts o f normal composition are sought nitric

acid can not be saturated by mercury used in excess or acetic ,

acid by l ead in excess .

209 . I n Chapter X I X Vol I we have seen that the products

,
.
,

o f chemical solution [ except gases which escape ] must be soluble

in the l iqui d in which the reactions take place ; that acids do not
dissolve metal s and metallic compounds unles s they form water
soluble salts w ith them [ or salts soluble in the acid itsel f i f the
acid is strong or used in excess ] .

When the salt formed is not soluble in water but soluble in ’

the acid then a diluted aci d can not be succes s ful ly employed
,

unless u sed in considerabl e excess and the result w ill then be a

,

solution containing much free acid S olutions o f antimony

.

chloride and o f th e nitrates o f mercur y and bismuth in water

without the presence o f much free acid can not be produced ; but
solutions o f these compound s containing large proportions o f the
acids are made and are u se ful for ce rtain purposes .

When the salt formed is quite solubl e in water and in the dilute
aci d but insolubl e in concentrated acid then the undiluted acid ,

does not dissolve the metal .

21 0 . Th e a ct i on of t h e h e avy me t a l s u p on t h e common i n or
g a n i e ac i d s. G o l d and the p l a t i n u m m e t a ls do not attack any acid ,

but they dissolve in nitrohydrochloric aci d or a q u a r e g ia forming ,

chlorides with the free chlorine .

A l u m i n u m decomposes hydrochloric acid forming aluminum ,

chloride and setting the hydrogen free It does not attack other .

acids .

A n ti m ony is oxid ized by strong n itric acid to insoluble anti

m on ou s oxide . O ther acids are not a ffected by antimony .

T i n decomposes strong n itric acid forming metastannic acid , .

I t al so decomposes hydrochloric acid forming stannous chloride , .

S ulphuric aci d is not decomposed by tin .

B i s m u th quickly decomposes nitric acid forming bismuth u i ,

trate and it als o attacks hot concentrated sulphuric acid but not
, ,

hydrochloric acid .

S i lve r attacks dilute n itric acid forming s ilver nitrate ; it also

,
 C H EM I CAL S OLU TI ON WET OX I DA TI ON ETC
—
I ZO ,
.

decomposes hot concentrated sulphuric acid It does not act upon .

hydrochloric acid .

L e a d decomposes nitric acid but scarcely a ff ects hydrochloric ,

and sulphuric aci d .

Coppe r vigorously attacks nitric aci d an d also decomposes hot ,

strong sulphuric acid but is not dissolved in hydrochlor i c acid or,

diluted sulphuric acid .

N i c k e l decomposes hydrochloric acid sulphuric acid and nitric ,

acid forming nickelous salts

,
.

I r on and z i n c readily decompose the diluted ac ids .

21 1 H y d r oc h l or i c a c i d dissolves zinc aluminum iron n ickel

.
, , ,

and tin ; it does not dissolve lead copper mercury silver gold
“

, , , , ,

platinum arsenic antimony and bi smuth

, ,
.

D i l u te d s u lph u r i c a c i d d issolves zinc iron and nickel Hydro , .

gen is set free B u t i t does not dissolve aluminum lead copper

.
v
, , ,

mercury silver gold platinum tin arsenic antimony and bis

, , , , ,

muth .

Con c e n tr a te d s u lph u r i c a ci d dissolves copper and if h o t it is , , ,

also attacked by mercury silver and bismuth ,

.

The acid not entering into the formation o f the sulphate i s

reduced to 5 0 2
.

M od e r a te ly di l u te n i tr i c a ci d especially when warm dissolves , ,

zinc iron nickel l ead copper m ercury silver arsenic and bis
, , , , , , ,

muth A rsenic i s oxidized to arsenic aci d ; the other metals form

.

nitrates The aci d not entering into the n itrate is reduced to N O

.
,

which oxidizes in the air to red vapors o f N 0 4 or N O or both 2 , ,

according to the temperature .

Col d a n d v e ry d i l u t e n i tr i c a ci d dissolves iron and zinc forming ,

ferrous nitrate or zinc nitrate together with ammonium n itrate .

Con c e n tr a te d n i tr i c a c i d is not attacked by iron but dissolves ,

l ead copper mercur y s ilver arsenic and bi smuth It is not a f

, , , , .

f e c t e d by gol d and platinum It oxidizes tin to insol uble meta

.

stannic acid and antimon y to insoluble antimonous oxide

, .

21 2 The foregoing statements are not to be construed to

.

mean that metal s which are n o t d i s s ol v e d by the acids named

m a y not be superficiall y a ffected to a considerable degree D iluted .

sulphuric acid d o e s take up c opper and form copper sulphate so

that copper vessel s are corroded by it ; but the diluted acid dis
solves the metal s o S lowl y and to such a limited extent that we
would not use diluted sulphuric acid for such a purpose but con ,
1 22 C H EM I CAL S OLU TI ON —
WET OX I DA TI ON ,
ETC .

heat when the evolution o f gas begins again and continues until
saturation is c ompl etely e ff ected .

21 6 . N e u tra l iza ti on is e ffected in solutions by mixing acids

.

and alkalies in the requ is ite proportions adding either the acid ,

to the alkal i or the alkal i to the acid A cid salts are also .

neutralized by alkalies and the alkali carbonates are employed

,

almost as much as the alkal i hydroxides Whenever practicabl e .

the point o f exact neutralization is determ ined by a color reagent ,

and the most common and u seful reagent o f this kind and for
this purpose is l i t mu s which i s generally employed in the form
,

o f li tm u s pape r .

L itmus i s a blue pigment prepared from certain lichens It is .

turned red by aci ds ; alkal ies restore the blue color White u n .

s ized paper dipped in a solution of l itmu s and dried is call ed

litmus paper or test paper The blue litmus paper is made from
,
-
.

the unaltered soluti on o f the pigment ; the red l itmus paper is

made from a litmus solution to which j ust enough dilute h ydro
chloric acid has been added to turn its color red .

A liquid which turns blue litmu s paper red is sai d to have an

a c i d r e a c ti on ; one that turns red l itmus paper blue has an alkaline

reaction ; a l iqu id which does not change the color o f either red or
blue litmus paper is sai d to have a n e u tr a l r e a c ti on on test paper -

or to be n e u tr a l t o te s t pape r The test is made by touching a

-
.

small strip o f the test paper with the liquid or th e liquid with the
-
,

test paper
-
.

In testing l iqu ids w ith l itmu s paper it is necess ary to gu ard

against interferences which might vitiate the test or mislead the
operator It is quite possible for instance to conclude from the
.
, ,

acid reaction o f a liquid which contains a l ittl e carbonic aci d

that the salt in solution i s an acid salt when in reality it may
be perfectl y neutral this may occur when an acid is being neutral
i z e d with a carbonate When a salt o f aci d reaction is being
.

decomposed with ammonia or an acid neutralized with it the , ,

l itmus paper may S how an alkaline reaction produce d by the

ammonia vapor above the l iquid while the l iqu id itsel f is still
slightl y acid or neutral
21 7 . When a strong acid 1 s neutral ized w ith a strong base the ,

salt formed 1 s a normal salt But normal salts formed by strong

.

acids with weak bases have an acid reaction and those formed ,

by w eak acids with strong bases have an alkal in e r eaction E ven .

 C H E M I CAL S OLU TI ON —
WE T OX I DA TI O N ,
ETC . 1 23

aci d salts ( salts still containing some o f the replaceabl e hydrogen

o f the acid ) may have a decidedly alkaline reaction as w e find
to be t h e case with the bicarbonates o f potassium sodium and ,

ammon ium ; and s o called basic salts may have an acid reaction as
-

is the case with solutions o f subsulphate o f iron S everal salts .

( notably sulphates and nitrates ) o f aluminum iron zinc copper , , , .

a n d other metal s have an aci d reaction although their composition

i s normal E ven alum ha s an acid reaction

. .

21 8
. When acids are s a tu r a te d with the metals or with metallic
Oxides hydroxides or carbonates the proportions employed o f
,

the materials are determined be forehand even i f an exces s o f ,

the m etal or metallic compound i s to be u sed and when salts o f ,

normal compos ition are to be prepared an d the reaction on test

paper does not indicate the composition the exact theoretical pro ,

portion s are used .

21 9
. The s a l t s p re p a r e d by chem ical solution i f crystall izabl e
.
, ,

are always recovered by crystall ization because this method i n

sur es a prod uct o f definite composition and fine appearance i f
the proce s s is wel l managed .

M any s a l ts of th e h e a vy m e ta ls crystallize most readily and

,

s a t i s f a c t o r il y a n d o f perfectl y normal composition from strongly

acidulated solutions S olutions o f th e sulphates are acidulated

.

w ith sulphu ric aci d those o f n itrates with nitric acid acetates
, ,

w ith acetic acid chlorides with h y drochloric acid

, .

S alts of the alkali metals on the other han d sometimes crystal

, ,

l ize most readily from alkaline solutions S olutions o f p ota s .

s ium s alts are rendered alkal ine by the addition o f a little car
bonate or hydroxide o f potassium and solutions o f sodium salts ,

with sodium carbonat e or hydroxide ; solutions o f ammonium salts

are rendered alkaline with ammonia water .

B ut there are so many exceptions to these general statements

that no inexperienced operator can be guided by them ; special
directions in individual cases are therefore given in all com , ,

p l e t e working -
formulas .

220. A morphou s salts and those that can not be advantage

,

ou s l y produced in large cr y stals are recovered from solutions

,

obtained by chem ical solution by t u rbi d at i on granulation or , ,

evaporation to dryness or by evaporation until a moist salt resi

,

clue i s obtained which is then spread out on plates to dry

, .

221
. I n addition to the exampl es al ready given we shall men
 C H EM I CAL S OLU TI ON WE T OX I DA TI ON E TC
—
1 24 ,
.

tion now a su fficient number of in stances o f chemical solutio n

to S how how varied such processes are : The production of phos
p h o r i c acid by dissolving phosphorus in nitric acid is an oxida
tion pro cess and at the same time chemical solution ; the produc
tion of R ochelle salt ( tartrate o f potassium and sodium ) from
potassium bitartrate ( acid tartrate ) and sodium carbonate is a
proces s of chemical solution ( neutral ization ) the production o f
ferrous iodide by di ssolving i ron and iodine together in water ;
the solution o f zinc in hydrochloric aci d to ma ke zinc chlori de ;
the solution o f l ead oxide in a solution o f lead acetate to make
solution o f subacetate o f l ead ; making solution o f ferric citrate
from ferric hydroxide citric acid and water ; the production o f
,

solubl e ferric phosphate by dissolving precipitated ferric phos

phate in a solution o f citrate o f ammonium or by boiling s o ,

d i u m phosphate and solution of ferric citrate together ; all of the

“ ”
proces ses by which the scal e salts are made ; the preparation o f
solution o f potassium arsen ite from ars enous oxide and p ota s '

sium bicarbonate ; the solution of ammonia gas in water to make

the solution o f ammonium h y droxide cal l ed ammon ia water ; the
solution o f carbon dioxide in water to produce a sol ution o f car
bonie acid ; the preparation o f solution o f calcium hydroxide from
calcium oxide ( l ime ) an d water ; the formation o f hydrogen di
oxide by dissolving bari um dioxide i n water .

222 By the term w e t ox i dat i on I designate oxidation pro

.

d u c e d in the wet way that is in liquids

—
,
Wet oxidation is
.

closely related to chemical solution and in many cases is nothing

,

el se A s exampl es o f w e t oxid ation we may mention : the

.

method o f turn ing ferrous salts into ferric by heating their solu
tions with nitric acid ; making phosphoric a c i d from phosphorus
with nitric acid ; changing ferrou s compounds into ferric by
adding chlorine water or by conducting a current o f chlorine into
,

the solutions containing them ; producing potassium chlorate by

the action of chlorine on potassium h y droxide in solution ; pro
d u c i n g potassium permanganate by the action o f potassium
chlorate and potass ium hydroxide upon manganese dioxide etc ,
.

In pharmaceutical operations the most useful oxidizing agents

are those that y iel d bye products which can be easil y eliminated
-

or which are unobj ectionable N itric acid is there fore much

.
, ,

used .

In w e t oxidation by nitric aci d heat is generall y applied to

1 26 C H E M I CAL S OLU TI ON —
WE T OX I DA TI ON ,
ETC .

'

nitric acid in the others ; 3 for chlorine put compressed c hl or 1nat e d

,

lime in the middle bulb and a mixture o f 7 volumes o f hydrochloric

Ga s e v l ti
o u on a pp aratu s .

acid and 5 volumes of water in the others ; 4 for generating hydro ,

gen sulphide crushed ferrous sulphide i s put in the middle bulb

,
'

and equal volumes o f h y drochloric acid and water in the others ; 5 ,

Fig . 1 01 . W h b tt l
as o es . Th e l as t two a re W ou l ff ’
s b l
ot t e s .

for the generation of carbon dioxide broken marble i s put in the ,

middle bulb and equal volumes o f h y d r oc hl or 1 c ac i d and water

 C H EM I CAL S OLU TI ON —
WET OX I DA TI ON ,
ETC . 1 27

in the others ; and 6, for nitr 1 e o x ide u se copper tu rnings an d di

lute nitric acid .

Fi g . 1 02 G a s
. e v l ti
o u on a pp a ra t u s .

224 . Whenever it i s n ecessary to w as h the gaseous product

to remove from it any other volatile substances which may a e com
pany it out o f the generator the generator i s connected with ,

one or more w as h bottl es and the gas is a fter having passed

-
, ,

through the wash water con ducted into the receiver where it
-
,

is collected or dissolved in water ( S e e Fig . .

Volatile acids are prepared in apparatu s similarl y constructed ,

and the w h ole process bears cons iderable resemblance to chem i

cal distillation The fittings necessary are practically the sam e
.

as used for small distilling apparatus .

S everal gas solu tions are o f considerable importance as for

-
, ,

instance solutions o f chlorine hydrogen sulphide sulphurous

, , ,

acid etc
, .

225 . When gas solutions are made the exces s o f gas passing ,

out o f the liquid contained in the receiving vessel shoul d be con

ducted int o an end bottle for absorption into a fi x i n g solution
- -

i f the escape o f the gas into the r oom is obj ectionable Thus the .

excess of chlorine or o f n itric oxide may be conducted into a

solution o f s odium carbonate ( S e e Fi g . .
 CH A PT E R X I V .

TH E U S E S OF U N FI N I S H ED P RODU CT S P UR I F I CA TI ON O F CRUDE
—

C H EM I CAL S W H A T T O D O WITH DA M A GED P RODU CT S

—
.

P RO FIT A B LE C H E M I CAL W OR K .

226 . Well trained pharmacists w h o have a moderately

-

equipped laboratory and make u se o f it find it d ecidedly pr ofitable ,

to employ unfinished products as materials I t is clearl y waste .

ful and unworkmanl ike to ad opt an expensive method o f making

any preparation whenever a less expensive method l eads to pre
c i s e l y the s ame result as to the quality of the finished article .

Chemical products in s ol id form i f they are water soluble are

,
-
,

almost invariably obtained first in solution and are a fterwards ,

recovered from their solutions by crystallization o r some other

process frequently involving the expenditure of considerabl e time
and lab or I f the solution contains the chemical compound o f
.

requis ite degree o f purity and i f all that remains to be done in

,

order t o finish the product is its recovery in solid form from the
soluti on then the cost o f that operation i s properly saved in
,

every case where the s olution its el f can be directly employed .

Perfectly pure and in every w a y satis factory chemical products

in a state o f solution in water can be made without mak ing the
solution ou t of the finished sol id substance and it happens quite ,

frequently that liquid preparations are to be made containing suc h

chemical products .

When a large quantity o f pyrophosphate o f ir on i s required in

the form of water solution for the manu facture o f some l iqu id
-

preparation the quantity needed is pr oduced out o f s olution o f

,

ferric sulphate sodium pyr ophosphate ammonia water and citric

, ,

acid or ou t o f solutions o f ferric citrate and sodium p y r op h os

‘

phate and the tedious and di fficult proces s o f turning the pyro
,

phosphate o f iron into scal es i s avoided .

I f large quantities o f solution o f potassium iodide are required ,

it i s cheaper and quite as satis factor y to make the solution out

of iodine i ron and potassium carbonate instead o f making it out o f
,

finished potas sium iodide .

 3 0 TH E U S E S O F U N FI N I S H ED P RODU CT S .

p p
r o r i a t e l y flavored and sweetened s imple el ixi r of proper alco
holic strength t oproduce the desired result .

The foregoing illustrations are su fficient to demonstrate the

value o f technical education for the practice o f pharmacy B ut .

no person ignorant o f pharmaceutical chemistry shoul d under

take to do any such work because he could not know whet h er his
results be right or wrong .

227 . The purification o f cru de commercial chemicals i s a

not inconsiderable part o f the profitable work of the pharmacist .

A m on g t h e common cru de inorganic chemical s which can be

easily purified w a s to be rendered fit for pharmaceutical and
medici nal use we may mention by way o f illustration : boric,

acid alum ammonium chloride copper sulphate ferrous sulphate

, , , , ,

lead acetate lead n itrate potassium chlorate potassium n itrate

, , , ,

sodium carbonate sodium thiosulphate sodium phosphate zinc

, , ,

sulphate The cost o f purification o f t h e s e and many other sub

.

stances i s l ittle o r nothing beyond the valu e of the time and labor .

B rief general reference has been made in various places in

thi s book to the purification of fusibl e solids contaminated with
infusible impurities ; the purification o f volatil e sol ids by subl ima
tion to remove fixed impurities and the removal o f volatile i m
,

purities from fixed solids by ignition ; the purification o f crys

t a l li z a bl e solubl e substances by recrystallization t u rbi d a t i on , ,

granulation and ph y sical precipitation ; the removal o f insol ubl e

substances from solubl e solids by solution a n d fi l t ra t i on the sep
aration of crystalloids and colloids by dialysis ; the purification
of liquids by filtration and by distil lation ; an d the precipitation
of foreign substances from solutions o f various chemical com
pounds by substitution ( as when zinc precip itates iron ) or by
metathesis .

M any individual examples o f the purification o f crude chemi

cal products will be found in Part 1 1 Of thi s volume .

228 . Chemical products which have been damaged or altered ,

or mixed with other substances by accident m ay generally be ,

restored to their original condition or rendered quite pure or , ,

converted into some other valuabl e product by simple methods , .

A cry stal lized salt which has e ffl or e s c e d or which has under

,

gone aqueous fusion i n hot weather ; a h y groscopic or deli

q u e s c e n t substance which has absorbed moisture so that it is no

longer in fit condition to be used ; a ferrous salt which has

 TH E US ES OF U N FI N I S H ED P RODU CT S .

become partially oxidized to ferric ; a compound of

or mercury or any other valuabl e substanc e which
,

partial decomposition from exposure to light ; a salt

dropped on the ground and thus
ru ined by admixture with any othe
minute fra gments o f gla ss from
these things ceas e to have som e
c e u t i c a l chemist shoul d know ho

kind or to reduce the

found impure o r oth
were intended may frequently be °

The restoration o f altered ch

Chapter X V .

229 . The pharmaci st shou l d abl e t repare

any time in an e m e r g e n c
,
is regu
almost any one o f the
called upon to d ispense ,

from the us procure quickly

whatever is ake the prepara
tion ain it from any
othe can be quickly
and eas ily they a re
not easily the most
common s u
it i s eas ier t o make them than to
it has been frequently demonstrated
o f well equipped pharmaceutical schools that
and rarer chem ical preparations organic an d ,

h very high prices are charged by t h os e w ho ,

y because they are new c a n be very readily ,

made by the pharmacist himsel f at far les s cost .

23 0 . A large number o f pharmaceutical chem ical s are o f

such a character that they can not be made to any greater a d
vantage ou a large scale than in very moderate quantities A ll .

such products can be profitably made by any intel ligent well ,

trained pharmacist o f proper business capacity A n extensive or .

generally well equipped laboratory is not necessary for this pur

pose .

A gain i f his whol e time i s not occupied in other directions

,

t h e ambitious educated pharmaci st can hardly find any technical

1 32 TH E US ES OF UN FI N I S H ED P RODU CT S .

work which will a ff ord him greater satis faction than the m anu
f a c t u r i n g o f one or m or e carefully s elected chemical pr oducts
which he can m ak e of unexceptionable qual ity and in cons ide r
abl e quantity O r ganic a s well as inorgan ic products belong t o
.

the list o f chemicals which he can make it his special care to

furnish and any such product can dou btl ess be marketed
,

through the f e gu l a r distributing channels at a remunerative

p r l c e .
1 34 TH E P RE S ERVA TI ON OF M ED I C I NAL S U B S T AN C E S .

23 4 . H yg r os c opi c and absorb

d e li q u es ce n t s u bs ta n c e s m ay
moisture and i f the exact quantity o f moisture they contain i s
,

not known they can no longer be u sed in the same proportion

'

as i f th e y were dry ; and a moist w e t or l iquefied salt may not be ,

adapted for all the uses to which the dry salt i s employed even
i f the percentage o f moisture in it has been determ ined so that
th e correspondingly increased quantity required o f the del i
q u e s c e d salt i s known .

The best plan i s to dry the substance so as to restore it to it s

proper normal condition .

To prevent the absorption o f moisture all hygroscopic and ,

del iquescent substances shoul d be kept in tightly closed bottles

in a dry place The containers shoul d not be too lar g e in pro
.

portion to t he rate of consumption o f the contents .

23 5 . S u bs ta n ce s of c om pl e x ch e m i ca l s tr u c tu r e or cons isting ,

o f mol ecul es composed o f a large number o f atoms are generally ,

less capabl e o f res isting decompos ition than are the s impler .

chemical compounds .

23 6 . Com pou n d s of e l e m e n ts a n d c om pou n d r a d i ca ls of i n

d i ff e r e n t ch e m i c a l e n e r g y decompose more r eadily than those
formed by elements o f decided and powerful pos itive o r nega
tive chemical polarity Thus the compounds formed by nitro .

gen are often unstabl e as are also thos e o f gold silver mer , , ,

cury and several other weak pos itive metallic elements ; but com
pounds formed by the alkal i metal s an d the alkal in e earth metals -

are very stable especial ly when the negative elements to which

,

they are united are al so powerful radical s S alts o f weak bases .

and o f weak acids are usually unstable M etals general ly form .

weak acids when they form any acids at all E lements which .

exhibit g i e at power when exercis ing negative polarity ( as for ,

instance the halogen s) generally form unstable compounds when

,

they as sume positive polarity .

23 7 . Com pou n ds c on ta i n i n g e l e m e n ts e x e r c i s i n
g a n u n u s u a l ly

hi g h pol ar i ty -
va l u e c a p a bl e o f r e d u c ti on
( in other words power ,

ful oxidizing agents ) and , com pou n ds c on ta i n i ng e l e m e n ts e x e r

ci s i n g a n u n us u a l l y l ow pol a r i ty va l u e c apa bl e o
f -
a u g u m e n ta ti on

( in other words powerful reducing agents ) ,are l es s stable than ,

compounds fn a d e up o f elements exerci sing their normal polarity

and the dominant valence which they exhibit when endowed with
that polarity .
 TH E P RE S ERVATI ON OF M ED I C I NAL S U B S T A N CE S . 1 35

23 8 . exerts a decided influence upon a large number o f

L i gh t
chemical compounds inorganic as well as organic This influence
,
.

is in opposition to atomic attraction and its immediate e ff ect i s , ,

therefore dissociation accompanied by changes in th e polarity

, ,

valu e o f two or more o f the component atoms o f the molecule

a ff ected In other words light frequently induces reactions of
.
,

oxidation and reduction in S ingle chemical compounds as w el l

as between two or more kinds o f molecules in contact with each o

other .

The us e o f instantaneou s photography demonstrates the fact

that exposure to light for a period o f second i s suffi cient
to decompose certain very sensitive or unstable chemical com
“ ”
pounds M ost o f the compou nds o f the S O call ed nobl e metal s
.
-

are decomposed by strong light especially direct sunlight an d , ,

the dissociation wrought by its influence i s frequently rapi d .

Preparations o f mercury S ilve r and gol d must be careful ly ,

protected against light and there are many other inorganic com .

pounds and preparations which require sim ilar protection The .

”
s cale s alts o f iron are all sensitive to l ight and liqui d prep ,

a r a t i on s containing such scal e salts m us t a l l be k e pt i n th e d ar k

in order to prevent their deleteriou s alteration .

The pharmacopoeias name specifical ly va r1 ou s medicinal sub

“ ” “
stances wh ich m us t be kept in a dark place or kept in dark ,
”
amber colored bottles
-
or protected against light ; but the
,

l ist o f substances dir ected to be thu s protected should be con

s i d e r a bl y extended The following substances shoul d all be
.

carefully protected against light : f

( B enzoic acid phenol c i t,

r i c a c i d g a l l i,c a c i d ) hydrobromic , ,

acid hydrochloric acid hydrocyanic acid nitric acid n i t r oh y

, , , ,

d r oc h l or i c acid ( s a l i cy l i c a c i d ) sulphurous acid ( t a n n i c a c i d

, , , ,

ta r ta r i c a c i d acetic ether ) a mm on i u m be nz oa te ammonium i o

, , ,

d ide a mm on i u m va l e r a te ( amyl nitrate ) sulphurated antimony

, , , ,

( apomorphine hydrochloride ) chlorine water ( a l l,a r o m a t i c ,

*A
lth ou gh t h e s c o p e o f t h i s b o o k i s li m it e d t o i n o r g a n i c s u b s ta n c e s 1
h a v e i n c l u d e d i n t h i s c h a p t e r t h e o r g a n i c m e d i c i n a l s u b s t a n c e s li a b l e t o
,

c h a n g e b e c au s e s o m e o f t h e s u b s t a n c e s r e q u iri n g p r o t e c ti o n a r e p a rtl y o f

o r g a n i c a n d p a r tl y o f i n o r g a n i c o ri g i n a n d b e c a u s e t h e s e n s iti v e n e s s o f
,

o r g a n i c s u b s t a n c e s fu r n i s h e s a n a l t o g e t h e r l e g iti m a t e ill u s tr a ti o n o f t h e
c h e m i c a l e ff e c t s o f li g h t h e a t a i r e t c u p o n m att e r i n g e n e r a l
, , , .
, M o re
o v e r t h i s li s t m a y s e r v e t o c a ll n e e d e d a tt e n ti o n t o t h e g e n e r a l n e g l e c t o f
.

t h i s w h ol e s u b je c t T h e o r g a n i c s u b s t a n c e s a r e t h o s e p u t i n b ra c k e t s
. .
1 36 T H E P RE S ER VA T I ON O F M ED I CI NAL S U B S T A N CE S .

w a te r s ) all silver compounds iodide o f arsenic ( a tr opi n e a n d a l l

, , ,

i ts s a l ts ) g ol d an d s od i u m c h l or i d e bismuth and ammonium cit

, ,

rate ( c a fi e i n e a n d ci tr a te d ca ff e i ne chloral chloro form c h ry

, , , ,

s a r o bi n, c i n c h on i d i n e and a ll i ts s a l ts , c i n c h on i n e and all i ts

s a l ts , c oc a i n e and a ll i ts s a l ts ,
eucalyptol ) ferric e l a t e r i n, ,

“
chloride all scale salts of iron saccharated ferrou s iodide fe r
,
-
, ,

r ou s l a c ta te ferric val erate ( g ly c e r i te of ph e n ol g ly ce ri te of

, , ,

ta n n i c a c i d ) m e r cu r i c c h l or i d e calomel mercuric c y anide the

, , , ,

mercurous and mercuric iodides t he yel low an d the red oxide o f ,

mercury yellow mercuric subsulphate ammoniated mercury a l l

, , ,

o th e r m e r cu ry c om pou n ds h
( y d r a s t i n i n e a n d ,
a ll i t s s a l ts ,

hy os c i n e a n d a l l i ts s a l ts hy os cy a m i n e a n d a l l i ts s a l ts iodo form )
, , ,

s ol u ti on of a rs e n i c a n d m e r c u r i c i odi d e solution o f f erric acetate , ,

s ol u t i on of f e r r i c c h l or i d e s ol u ti on of f e r r i c c i tr a te
,
s ol u ti on of ,

fe r ri c n i tr a te solution o f ferric subsulphate solution o f chlorin

, ,

ated soda l i thi u m be nz oa te l i th i u m s a l i cy l a te ( methyl sal icylate

, , , ,

m or ph i n e a n d a l l i ts s a l ts naphtol paraldehyde ) phosphorus , , , ,

( physostigmine and al l its salts p il o ca r p i n e a n d a l l i t s s a

,
l ts ) l ead ,

iodide potassium permanganate ( pyrogallol qu inidine and al l i t s

, , ,

salts quinine and all its salts r e s i n of pod ophy l l u m resorcin

, , , ,

s a l ol santonin s od i u m be nz oa t e s od i u m i od i d e sodium sal icylate

, , , , ,

s od i u m pa r aph e n ol s u l ph on a t e ( p
s a r t e i n e a n d i ts s a l,
ts spirit o f ,

nitrous ether ) strontium iodide ( s try c h n i n e a nd a ll i ts s al ts )

, , ,

s y r u p of hy d r i od i c a c i d s y r u p of f e r r ou s i od i d e
, s y r u p of t h e ,

p h o s p h a t e s of i r o n q u i n i n e a n d s tr y c h n i n e ( v e r a tr i n e ) z i nc i o , ,

d ide ,
zi n c ph os ph i d e .

[ A ll a l k a l oi ds a n d a l k a l oi d a l s a l ts
should be protected against
light because experience has S hown that they are very generally
sens itive to its decompos ing e ff ects In fact a l l org a n i c c h e m i c a ls .

shoul d be kept in the dark or in dark amber colored bottle s ] ,

-

[ V o l a t i l e o i l s and ol e or e s i ns a r om a ti c w a te r s and ar om a ti c ,

s i r i ts shoul d all be kept in the dark

p ] .

[ F i x e d o i l s and fa ts oi n tm e n ts c e ra tes and pl as t e rs also r e

, ,

quire protection against ligh t ]

[ A ll c r u de or g a n i c ( vegetable ) d r u g s and especially their ,

p o w d e r s must be carefull y guarded a a 1 n s t exposure to the dam

g
aging actio nof light and of course also the fl u i d e x tr a c ts e x
, , , ,

tr a c ts ,
ti n c tu r e s w i nes and s y r u ps o f all plant drugs A ll
, , .

e l i x i rs ]

In the foregoing l ist the articles named in italics were not ,

1 38 TH E P RE S ER VA TI ON O F M ED I CI NAL S U B S T AN CE S .

alcohol ) ammonium carbonate ammonium val e rate ( amyl

, , ,

nitrite all ethers all aromatic waters ) chlorin e water hydrogen

, , , ,

dioxide solutions gold and sodium chloride ( benzin ) bromine , , , ,

chlorinated l ime ( camphor monobromated camphor ) carbon di

, , ,

sulphide ( all cerates spermaceti chloral chloro form all col

, , , , ,

lodions confections copaiba all plasters eucalyptol ) ferric

, , , , ,

“ ”
chloride all scale salts o f iron iron alum saccharated iodide of
, , ,

iron ferric valerate ( all val erates iodoform ) iodine solution o f

, , , , ,

ferric acetate solution o f magnesium citrate solution o f magn e

, ,

s ium carbonate solution o f chlorinated s od a V a l l e t s mass ( honey

, ,
’
, ,

honey o f rose menthol mucilage al l oleates all oleores ins all

, , , , ,

fixed oils and fats all volatile oils p ancreatin pepsin p a r a ld e , , , ,

hyde ) phosphorus ( pyroxylin ) sodium sal icylate sodium sul

, , , ,

p h i t e ( spirit
,
o f eth e r compound spirit o f ether spirit o f nitrous , ,

ether ) spirit o f ammonia ( all aromatic spirits all syrups tere

, , , ,

bene all ointments )

, .

240 Contact with ai r is inimical to substances liable to ox i d a f

.

tion or which may t ake up carbon dioxide or water from moist

, ,

ai r or which give up water o f crystallization to dry air S u b

,
.

stances liable to undergo fermentation should also be protected

against contact with air .

The most e ff ective means o f excluding air i s to keep the sub

stances requiring protection in small completely fill ed tightly , ,

closed containers o f glass or porcelain Glass stoppered bottles .

-

are generally used and with very satis factory results In som e .

cases where the utmost care is necessary to prevent access o f ai r

,

and moisture the glas s stoppers may be rubbe d over with a uni
,
- ~

form but very thin coating of pure petrolatum so that t h ey make

a smooth air tight fit in the necks o f the bottles
-
.

When the pharmacopoeias direct that any given substance S hall

be kept in small bo ttles th e d e c 1 S I O n as to what s ize is most
“ ”
,

suitable is left to the j udgment o f the pharmacist A S l On g as

. .

the container is filled almost to the complete exclus ion o f air and
remains tightly closed the contents must remain e ffectivel y pro ,

t e c t e d no matter what may be the size o f the vessel

, But when .

the container is opened and the contents used a portion at a time ,

being removed ai r is necessaril y admitted each time A small

“
, .

” ’

bottle then is one that will hold no greater quantity than will
‘

, ,

certainly be consumed in a very short time or before a ny portion ,

can be inj ured ; an d in a few cases that means a quantit y so small

 TH E P RES E R VA TI O N O F M ED I C I NAL S U B S T A N CE S . I 39
that the whole o f it i s probabl y not much more than will be r e
quired at one time In a pharmacy where syrup o f ferrou s iodide
.

i s so frequ ently d ispensed that a pound bottle o f it will be emptied

“ ”
in the course o f a week or two an original bottl e o f that s ize
,

is not too large ; but i f 1 0 0 Gm o f that syrup is more than will

be dispensed in two weeks then an original bottle holding more
“ ”
than 1 0 0 Gm 1 S n ot a small bottle within the meaning o f the
Pharmacopoeia It i s Of course far better to us e stock containers
.
, ,

somewhat too small for convenience than it is to use containers

that ar e at all too large .

24 1
. Impervious containers are nearly always necessary to
the preservation o f medicinal substances and it is therefore bad , , ,

practice to keep chemical s in containers o f paper or wood A ny .

medicinal substance however inexpensive it may be must be r e ,

garded as very valuable whenever it i s u sed with benefit as a

remedy and for that purpose it must be at all times in proper
,

condition I f in order to preserve a given medi cinal agent it

.

S houl d be necessary t o u se a container the cost o f which i s great er

th an t h at o f the medicinal substance itsel f it is nevertheles s clearly ,

inadm i s sible t o use a cheaper container There is no vali d excuse.

for any de viation from that principle In many pharmacies it i s .

the uni form practice to dispense all medicines so far a s practicabl e

in glass stoppered bottles and corks are not used This may
,
.

seem to occas ion in some cases an unnecessary additional expense

to the consumer but the proportion o f cases in which it is de
,

c i d e d l y best from the point Of V iew o f the wel fare o f the patient
is so great and the additional cost i s so trifling that this practice
deserves universal adoption as on e o f the unwritten l aws o f cor
rect pharmacy .

When manu facturers o f chemical products put up t heir g oods

in paper cartoons o r wooden boxes they generally do so under
protest in the form o f a printed label wh ich declares that the
practice is wrong and that the customer w h o insists upon it i n
,

order to save the cost o f a proper container must take the r e

sponsibility for the consequences .

Corks an d rubber stoppers are very unsatis factory and obje c

t i on abl e
. Glass stoppered bottles are now so i n e x p e n s w e that
-

they ought to be generally i f not exclusively used When corks .

are used the top s o f the containers are u sually covered with wax
1 40 TH E P RE S ERVA TI ON OF M ED I C I NAL S U B S T A N CE S .

or para ffin to close up the worm hol es and other de fects in t h e

corks .

24 2 A mong the substances wh ich shoul d be kept in small

.
,

tightly closed bottles ( glass stoppered bottles ) are -

Hydrocyanic acid sulphurous acid ( amyl nitrate a p om or , , ,

phine hydr ochlorate ) chlorine water solution O f hydrogen d i ox , ,

ide gol d and sodium chloride ( chloral chloroform the collodions

, , , ,

elaterin ) saccharated carbonate o f iron s accharated iodide o f iron

, , ,

ferrou s lactate ferrous sulphate ferric valerate ( glycerite o f

, , ,

tannic acid ) mercurous iodide mercuric iodide yellow mercuric

, , ,

oxide yellow subsulphate o f mercury ammoniated m ercury ( hyo

, , ,

s c i n e and its salts hyoscyamine and its salts ) magn esia Vall et s ’

, , ,

mass ( morphin e acetate the ol eates all volatil e oils fixed oils )
, , , , ,

phosphorated oil ( p hysostigmine a nd its salts pilocarpine and its

, ,

salts ) l e ad acetate potass ium hydroxide potassium acetate p ota s

, , , ,

s ium cyanide sodium bisulphite sodium iod ide ( spirit of nitrou s

, , ,

ether ) s y rup o f hydriodic acid syrup o f ferrous iodide the bro

mide chloride iodide and phosph ide o f zinc
, , ,

.
, ,

243 A ll strong acids solution s o f the alkal ies th e solid alka

.
, ,

lies brom ine iodine and other S ubstances o f a corros ive n ature
, , ,

or having a destructive action on corks must o f course be kept , , ,

in glass stoppered bottles -

.

244 M oi st u r e a ff ects all hygroscopic an d deliquescent sub

.

stances A ll such substances must therefore be kept in per fectly

.
, ,

dry small tightly closed ( well made glass stoppered ) bottles

, ,
-
.

Potassium hydroxide potassium acetate carbonate and c yan ide , , , ,

the halides o f zinc ferric chloride and several other substances , ,

are of this class .

 1 42 S OLU BI L ITI E S OF I NOR GAN I C C H EM I CAL COM P OU NDS .

Ve r y s p a r i ng ly s ol u bl e

X Cr e a m o f tartar in ,
20 1 parts o f water at I
N e a r ly i ns ol u bl e
Potassium platinum chloride -
.

24 7 , S od i u m c omp ou n d s A l l are solubl e except the anti .

m on i t e which is nearly insoluble

,
.

V ery fr e e ly s ol u bl e are
m i m d h
‘

H
x y d r o x i d e x
c a r bo n a t e at c h l o r
,
i d e fi bro i e i o d i e Xc l o r a t e A sul x
,

p h a te s s u l p hi t e atbi s u l p hi t e ys t h i o s u l p h a t e NM
)
s
a et
a fe r c itra t e , al e ra t e
‘

y c f e ,
t af t r a f v , ) s ali c l ate
y an d r ‘ bg fl r e
L
and
salt .
3

L e s s r e a d i ly s ol u bl e
-

XB i ca rbon a t e in p arts of water at 1 5 ,

x Py rop h os p h a t e in 1 2 parts of water at , $0 .

xT e t r a bo ra t e ( borax ) in 1 6 parts o f water at x

M
.
,
”

B EAM sparingl y .

24 8 L i t h i u m c omp ou n d s A ll freely solubl e in water except

t h carbonate which dissolves in 8 0 parts o f water at H E /w
. .
‘

, e“ “
ht
A mm on i u m c omp ou n d s A ll offic i n a l ammonium com .

pounds are readil y water sol ubl e the least soluble being the ben -
,

z oa t e and the carbonate which are each soluble in 5 parts o f ,

water at n l wl w p é u i at t f
c a . i g

25 0 B ar i u m sa l ts
. N itrate ghl or i d e bromide iod i d e sul .
, _ _ , , ,

h i
p d e and acetate are r e a di ly s ol u bl e
‘

H y droxide soluble in 2 0 parts of water .

I ns ol u bl e are M M
Carbonate phosphate S ulphate and oxalate , , .

25 1 S t r on t i u m s a l t s
. Chloride ><bromide and y i od i d e a r e .
,

“W i
g
ht I L /
X ua fi fl fik
The acetate lactate and nitrate are r e a d i ly s ol u bl e
, .

The h y droxide i s comparativel y s par i ng ly s ol u bl e A S “L . a

t tu
I n s ol u bl e ar e
3
£
c
Carbonate phosphate sulphate and oxalate “
.
, ,

25 2 Ca l ci u m c omp ou n ds
. .

D e l i q u e s c e n t are
xCh l o r i d e yxb r o m i d e iodide , .

R e a d i ly s ol u bl e

N i t ra t e N i y pp h o s p h i t e ,
p sulphite ace
tat fi
l a
g
c t a t e ,
and S ulphur

m
‘

ated lime W M gwx '

ih
.
 S OLU BI L ITI E S OF I NOR G AN I C C H E M I CAL CO M P OU ND S . 1 43

S par i ng ly s ol u bl e

H y d gq xide in from 6 0 0 to 7 00 parts o f water at

— ,

K Qx ‘
i S u l ph a t e in about to parts o f water at
3 00 40 0
s cc
,

I ns ol u bl e
P
M C
25 3
a bo
r n a te , o a a e 7 ph os
.
x l t ~

p h a

M a gn e s i u m c omp ou n d s
e
R .
.

e a d i ly s
lo C
QS
l u bl e
(
are t h e
A W L

Chl or i d e br om i d e i od ide n i t ra t e fi u l h ate acetate lacta te and

'
‘
, , ,
fs p , ,

the acid citrate

”
.

“ i “
an in s?
re

; a
-

f “
y rox 1.
e ona e oxa 1ate h h ate X oxt
f
ca r , , P O S P 4
.
m
"
4 2
,

25 4 Zi nc c omp or n ds
”

. .

are
D e li q u e s ce n t

m il de r brom ide and iodi de .

R e a d i l y s ol u bl e are
l l é
x S u l p h a t e n i t r a t e na ce t a t e f a e ,
te a n d t pa na p h e nol s u l p h on at e .

L es s r e a d i ly s ol u bl e

I ns ol u bl e Y ‘
A A Q
, 4“
i
l 7 oxalate
7A O xi de ,
sulphide , phosphide ,
h y d rox i d e fl t c arbona t e : ,

phosphat e ol eate , .

25 5 Ca dmi u m c omp oun ds.

‘

S ol u bl e
are the
Chloride bromide iodide nitrate and , , ,

I ns ol u bl e are the
O x ide hydroxide sulphide carbonate oxal ate phosphate
, , , , , .

25 6 . A l u mi nu m c omp ou n ds .

R are
e a d i ly s ol u bl e
x v “ Lb

Chloride bromide iodide , , ,

n itrate , sulphate ,
ot ash
'

M and ammonia alum

m
.

I ns ol u bl e are the
3 M d X
O xide an cfih d rox i d e .
“

25 7 . Ce ri um c omp ou n d s .

S ol u bl e are the chloride nitrate and sulphate ,

.

I ns ol u bl e are the oxide hydroxide carbonate , , and a l at e .

a
ft 25 8 . Cobal t c omp ou n d s .

The co ba l t ou s s a l ts are d e l i q ue s c e n t .

I are th e
n s ol u bl e

O xides h y droxides an d sulphides,

.
m
25 9 . N i ck e l c om p ou n d s .

s ol u bl e
M

N ickelous sulphate an d nickelous chloride are .

\l\\
y
1 44 S OL U BI L ITI E S O F I NOR G A N I C C H EM I CAL CO M P O UN D S .

O xides hydroxides and sulphide are

,
i ns ol u bl e .

26 0 . I r on c omp ou n d s f
Very r e a d i ly w a te r s ol u bl e are -

Ferrous chloride brom ide and iodide , .

Ferrous s ul p hate “
.

Ferric h l or i d e and bromide .

Ferric nitrate subsulphate acetate, , , a n d ; c i t rat e , . iron

The S ca l e - S a l ts o f iron are lu

bl e
vw
w j
f ' “

L ess s ol u bl e

Ferrous lactate is soluble in 40 parts of water at

The I n s ol u bl e I r on Compou n ds are
Ferrous and ferric \ b h a lt
‘

O x i d e sf h y d r ox i d e s sulphides afhoii at e s ox a l at e shp hosp hatg s g

/
n
‘
, , , ,
m

pyrophosphates m e t a p h o s p h a t e s h y po phosphites
, ,
’

26 1 . Ch r omi u m c omp ou n d s .

Wa ter s ol u bl e a r e
Chlorides chrom ium s u l p h a t e ggc h rom i an h yd r i dg ( s o call e d
, c
chromic potass ium chromate potassium di chrom ate and , ,

chrome alum \ x Lw L h “ UK
K
.

i
.

I ns ol u bl e are 3 ‘
”

O xide h y droxide
, .

262 . M an gan e se c omp oun d s .

S ol u bl e are
M anganous chlo ri de brom ide iodide nitrate and sulphate
’

, .

A lso potassium manganate and per anate .

I n s l u bl e are
o
K g r h b x i d e s h y droxide carbo te phosph ate sulphide
, , , ,
.

26 3 . L ead c omp ou n d s .

The only water soluble lead com p ounds are

V
N itr a te:
< acetate and subacetate ?“ “k .

264 .Copp e r comp ou n ds .

The onl y water soluble cupric compounds are -

i
Chloride n i t ra t e y s u l ph at e and acetate
26 5 . M e r cu r y
,
t

c omp ou n d s .
.

kg f

A l l m e r c u r ou s c om
in water ; but mer ou n d s
p ar e i ns ol u bl e
e urous nitrate i s soluble in a mixture of water and nitric acid .

The onl y w a te r s ol u bl e m e r c u r i c c ompou n ds are

-

Y Chloride bromide acetate and cyanide But m ercuric , .

n itrat e is s olubl e i n a mi xture o f n itric acid an d water

“A LL
i

0V i [
1 46 S OLU BI L ITI E S O F I NOR G AN I C C H EM I CAL C OM P OU ND S .

Potassium sodium l ithium ammonium barium strontium

’

, , , , ,
,

magnesium aluminum and gol d , ,

.

L e s s r e a d i ly s ol u bl e is
M ercuric chloride
I ns ol u bl e

S ilver chloride and m ercurous chloride .

N e a r ly i ns ol u bl e
L ead chloride .

D e c om p os e d by w a te r
A ntimony trichloride .

27 4 . B r omi d e s .

R are the bromides oi

e a di ly s ol u bl e

Potassium sodium l ithium ammonium barium strontium

, , , , , ,

calcium magnesium z inc aluminum and ferrous and ferric bro

, , , ,

m ide .

S ol u bl e are
M ercuric bromide and bromide o f gold .

I n s ol u bl e

B romides o f s ilver and l ead .

M ercurous bromi de .

27 5 .I od i d e s .

F r e e ly s ol u bl e are the iodides o i

Potassium sodium l ithium ammonium barium strontium cal
, , , , , ,

c i um , magnesium zinc c admium ferrou s iodide manganous

, , , ,

iodide an d arsenous iodide

, .

I ns ol u bl e are the iodides o f

S ilver lead mercury ( mercurous and mercuric )
, .

27 6 .Cy an I d e s Those o f the alkali metals are fr e e ly s ol u bl e

. .

M ercuric c y anide is s ol u bl e .

C yanide o f silver is i ns ol u bl e .

27 7 .F err ocy an i d e s an d f e rr i c y a ni d e s o f the a l k a li m e ta l s

are water s ol u bl e -
.

Those of the h e a vy m e ta ls are all i ns ol u bl e .

27 8 .S u l phi d e s Those of t he alkal i metal s and the alkaline

.

earth metals are fr e e ly w a te r s ol u bl e —

.

A ll sulphides of the h e a vy m e ta ls are i ns ol u bl e .

27 9 .H yp och l or i t e s of the alkali metal s and alkaline earth -

metal s are s ol u bl e .

280 .Ch l or at e s o f potassium an d sodium are soluble .

 S OLU BI L ITI E S OF I NOR G AN I C C H E M I CAL C O M P OU ND S . 1 47

28 1 . S u l ph i te s
Those o f potassium and sodium are r e a d i l y
.

s ol u bl e ; those o f calcium and magnes ium les s readily s ol u bl e .

28 2 S ul ph at e s
. A ll metallic sulphates are soluble except
.

those o f barium strontium calcium l ead and mercury

, , ,
.

R e a d ily s ol u bl e sulphates are those o f

S od ium ammonium al uminum and ferric sulphate
,
A l so the , ,
.

alums .

S ol u bl e are also the sulphates o f

Potassium lithium magnesium zinc ferrous sulphate man
, , , , ,

ganous sulphate copper sulphate ,

.

V e ry s p ar i ng ly s ol u bl e

Calcium sulphate .

I n s ol u bl e are the sulphates of

Barium strontium an d lead ,

D e c om pos e d by w a te r is the sulphate o f mercury ( mercuric ) .

28 3 .Th i osu l ph at e s o f potas sium and sodium are fr e e ly s ol

u bl e .

284 . S u l ph ur at e d p ot assa and su l ph urat e d l i me are very freel y

soluble .

28 5 . N i t ra t e s . A ll are water solubl e except those of mercury

-

and bismuth which are decomposed by water, .

286 N i t ri t e s o f alkali metal s are soluble

. .

28 7 Ph osph a t e s
. pyrophosphates and metaphosphates Th e
, .

only water soluble phosphates are those o f the alkal i metal s and
-

ammonium .

But some phosphates o f the heavy metal s an d also the phos

p h a t e s o f the alkal ine earth m etal s and ma g nes ium are soluble
-

i n ph os ph or i c a ci d .

O rthophosphates o f i ron are solubl e in orthophosphoric acid

but insolubl e in pyrophosphoric or in metaphosphoric acid .

Pyrophosphates an d metaphosphates o f iron are insoluble in

orthophosphoric aci d but solubl e 1 n metaphosphoric acid .

28 8 H yp oph osphi t e s
. Those o f the alkali metal s and o f .

cal cium are water soluble Those o f the heavy metals a re i n -

.

solubl e .

28 9 Car bon at e s
. The only water soluble carbonates are .
-

those o f potassium sodium and ammonium That o f lithium is .

sparingly soluble .

290 B orat e s
. S odium tetraborate ( or borax ) is solubl e
. .
 1 48 S OLU B I L ITI E S O F I NOR G AN I C C H EM I CAL CO M P OU ND S .

29 1 . M
etallic a ce t at e s are all water solu bl e -
.

29 2 Va l e r at e s
. O nly thos e o f potass ium sodium l ithium
.
, ,

and ammonium are soluble .

29 3 Oxal at e s
. O nly those of the alkal i metal s an d am
.

m on i u m are soluble .

294 Tar t ra t e s
. The normal tartrates of the alkal i metals
.

and ammonium are s ol u bl e ; their bitartrates are s pa r i ng ly s ol u bl e .

Tartrate o f f e r ryl and potassium Tartrate o f f e r ryl an d a m .

m on i u m and tartrate o f antimonyl and potassium are s ol u bl e

, .

'

29 5 Ci tra t e s
. Those o f the alkali metals ammonium and
.
,

o f iron are s ol u bl e .

M agnes ium citrate is solubl e in water containing much citric

acid .

B ismuth citrate is i ns ol u bl e ; but citrate o f bismuth an d a m

m on i u m is solubl e .

29 6 L a ct at e s
. T hose o f the alkal i metals calcium stron
.
, ,

tium magnesium zinc an d i ron are water solubl e

, ,
-
.

29 7 S al i cyl at e s
. Those o f the alkal i metals are alone sol
.

uble .

29 8 Ph e n ol su l ph onat e s
. Those of the alkal i metals barium .
, ,

calcium and zinc are water soluble -

.

29 9 B e nzoa t e s
. T hose o f the alkal i metals ammon ium and
.
,

calcium ar e water soluble

,
-
.

3 00 Ol e at e s
. O nly the soaps a re w a t e r soluble
.
'
-
.

3 01 The student will find it useful to special ly memorize the

.

following
A l l of the offi c i n a l compounds of potas sium sodium and a m ,

m on i u m are water solubl e ; but cream o f tartar is only very -

sparingly soluble .

The hydroxides o f potassium sodium an d ammon ium are

freely soluble [ L ithium h y droxide is soluble in about 1 4 parts
.

o f water ; barium h y droxide dissolves in 2 0

parts of water ; strontium hydroxide is sol
uble in 5 0 parts ; calc ium hydroxide is soluble in
about 6 4 0 parts of water ] .

The oxides h y droxides sulphides carbonates oxalates phos

, , , , ,

p h a t e s ( incl p y rophosphates
. and metaphosphates ) h yp p
O h o s ,

p h i t e s arsenates
,
and arsenites sal ic y lates benzoates and oleates , ,

o f the h e avy m e ta ls are all insoluble .

1 5 0 S OLU BI L ITI E S OF I NOR G AN I C C H EM I CAL CO M P OU ND S .

N i tr a t e ,sodium
B i s u lph i t e sodium ,

P h e n ol s u lph on a te , sodium ( I
A zinc
c e ta t e ,

Va l e r a te zinc ,

B e nz oa te sodium ( I ,

3 05 I n sol u bl e or nearly so in alcohol

.
, ,

A ll metall ic ca r bon a te s ox a l a te s ph os ph a te s py r oph os pha te s

, , , ,

m e t aph os ph a t e s a r s e na t e s a rs e n i te s ci tr a te s and ta r tr a t e s
, , ,
.

A ll metall ic s u lph a te s except ferric sulphate .

A ll the scale salts o f iron

“ ”
-
.

The
Ch l or i d e s o f potass ium sodium and ammonium and mercur , ,

ous chloride .

I od i d e of lead and mercurous iodide .

Cy a n i d e of potassium .

N i tr a te s o f potassium l ead copper and merc ury , ,

.

N i tr a t e o f sodium .

Chl or a t e o f potassium .

S u lph i t e o f sodium .

T h i os u lph a te o f sodium .

B or ax .

P o tas s i u m d i c hr om a te .

P o ta s s i u m f e r r ocy a n i d e and f e r ri cya ni d e .

A m m on i a te d m e r c u r y .

F e rr ou s l a c ta t e .
 CH A P T E R X VI I .

TH E D E N S IT Y OL I D S A N D L I QU I D S T H E M O H R W E S T P H AL
OF S .
-
BA L

AN CE H Y DROM E T ER S P Y C NOM E T ER S E T C
.
, ,
.

3 06 It i s very frequently necessary in laboratory operations

.

to take the density o f various liquids A s this happens most f r e .

quently in the process o f concentrating solutions by evaporation

preparatory to crystall ization and as density is a convenient gu ide
,

to the approximate strength o f solutions we shall su fficiently ,

discuss this Subj ect before w e describe evaporation and crystal

l i za t i on .

But the student must consult special works on weights and

measures specific weight balances and other apparatus an d i n
, , ,

s t ru m e n t s to learn the principles involved in their construction

,
’

and the details o f their care and u se .

'

3 07 . T h e d e n si t y o f any substance i s the relation o f its mass

to its volume It i s expressed in units representing the density
.

o f some known substance adopted as the m edium o f compar i son .

The densities o f solids an d liquids are thus expressed by num

bers the significance o f which i s understood from the fact that
,

the value o f each un it is the density of water The densities o f .

gases o r vapors are compared to and expressed in units o f the

density o f h y drogen .

The term s pe c i fi c g r a vi ty is most commonly employed to ex

pres s densit y ; and the term s pe c i fi c w e ig h t is also used w ith the
same meaning .

A ccordingly th e density specific weight or specific gravity

, , ,

o f water as thes e terms are commonly employed is 1 ; and the

,
‘

,
'

density specific weight or specific gravit y o f hydrogen i s also I

,
.

But water is about times a s heavy as hydrogen so that ,

the density o f water expressed in units o f the densit y o f hydro

gen is I I 1 6 0 ; and the densit y o f hydrogen expressed in units o f
,

the densit y o f water i s or Thes e numbers are

so inconvenient as to forbid the employment o f the water unit to
express the densities o f gases or o f the h y drogen unit to express
the dens ities o f sol ids and l iqu ids .

15 1
1 5 2 B ALAN CE S HY DROM E T ER S PY C NOM E T ER S
, , ,
E TC .

The densit y o f air w a s formerly emplo y ed ( and is still used to

a considerable extent ) for expressin g the densities of gases ; but
it can not be used as the unit o f expression in stating the densi
ties o i sol ids and li qu ids an d there are strong reasons in favor o f
,

the settled preference for h ydrogen as against ai r as the medium

o f comparison o f the densities o f gases .

A ir is about times a s heavy as the same volume o f h y

drogen s o that the density of dry air in hydrogen units is about
,

and the density o f hydrogen in units of the density o f dry

air is about
3 08 S ince I norganic pharmaceutical chemical products are
.

solids a nd l iquids it follows that the unit o f density or o f specific

, ,

gravity or specific weight most important to the lab orant m

, ,

this field o f work is the density o f water The form o f expres .

sion o f the density o f any given solid or liquid is therefore a , ,

number wh ich shows how many times the density of water ( the
unit ) is contained in the density o f that given s ol id or liquid .

Thus the statement that the density or specific weight or specific , .

gravity o f a n y given solid is means that a given volume

o f that solid weighs 8 times as much as the same volume o f
water ; the s p gr o f any l iquid is
. . i f a given volume of it
weighs times as much as an equal volume o f water ; the
sp .
w o f castor oil is
. becaus e one liter o f it weighs 9 6 0
“
Grams ; and one liter o f the o ffi cial solution o f subacetate o f
”
lead weighs about kil ogram s because its density is
For the sake o f uni formit y and precis ion the specific weights
o f all l iqu ids are expressed in numbers carried out to the third
decimal and in a few cases where ci rcumstances require it
, , ,

even four decimals are given .

3 09 .
The densities o f all substances are a ff ected by tempera
ture pressure buoyancy and other conditions It is therefore
, , , .
, ,

necessary to know the c on d i ti ons to which any expression o f

density refers For all ordinar y purposes the standard tem
.

p e r a t u r e o f 1
°
5 C is almost universally adopted and most of
.

the pharmacopoeias of recent date state the specific gravities o f

liqu ids at 1 5 C in numbers which refer to the density o f water
°
.

a t th e s a m e t e m e r a tu r e as the unit of expression B ut some

. p .

pharmacopoeias give the specific gravities o f liquids at I 5 C °

.

in units referring to the density o f water at 4 C °

.

The buo y ancy and atmospheric pressure are generall y ignored

1 54 B ALAN CE S H YDROM E T ERS PY C NOM E T ER S
, , ,
ETC .

cury only far enough to d isplace Gm ( its own weight )

of the mercury .

311 Buoyancy is the e ff ect o f gravitation for mass is meas

.
,

u r e d by gravitation density is the relat ion o f mass to volume and

, ,

a body of greater density is therefore a body acted upon by a

, ,

greater force of gravity L ead bull ets find their w a y to the

.

bottom o f a basketful o f beans becaus e the lead is attracted to

ward the center o f the earth with much greater force than the
bean substance Very heavy ores or other m inerals are there
.
,

fore s ometimes separated from other substances on this principle

, ,

a s grain is separated from the cha ff or as the heav y seeds are ,

separated from the light spongy pulp o f dried colocynth fru it .

Hydrometers a n d various other instruments designed to deter

mine the specific weights or densities o f l iquids and solids are
constructed on the principle o f the law o f buoyancy
.
.

3 12 The density of a sol id heavier than water and una ffected

.

by it m ay be found as follows : weigh the sol id first in air and

then suspended in water ; the di fference is the weight o f the
same volume o f water and the specific weight o f the sol id i s
,

the quotient found by dividing its weight in air by the weight

of the same volume of water
S hould the solid be water solubl e it may be weighed in some
—

liquid by which it is not affected and the density o f which is

known L et us suppose that oil o f turpentine is decided upon a s
.

fulfilling the necessary conditions The di ff erence between th e .

weight o f the sol id i n the air and its weight when su spended in
oil of turpentine is o f course the weight o f the same volume
, ,

o f that oil an d the weight o f the same volume of water i s the

,

quotient obtained by dividing the weight o f the oil by its specific

weight We then divide the weight o f the soli d in the air by
.

the weight of the same volume o f water .

S ol ids which are lighter than water may be weighed i n lighter

liquids or they may be weighted down with heavy substances and
,

thus weighed in water a fter which the wei ght o f the water dis
placed by the heavier sol id is deducted from the weight o f the
water displaced by both solids to find the weight o f the water
displaced by the l ighter sol id .

But the volume of any solid can o f course be readily found , ,

by submerging it in any lighter liquid ( by which it is una ff ected )

i n a graduated c y l inder for the rise o f the level o f the liquid
,
 B A L AN CE S HY DRO M E T ERS P Y C NOM E T ER S
, , ,
ETC . 1 55

must correspond exactly to the volume o f the sol id The densi .

ties of powders are usually found by this means .

'

The densities o f lard and other so ft fats and substances which

can not be weighed suspended in l iqu ids may be found by plac
ing them in a heavier liquid and then gradually adding a l ighter
liqu id until the density o f the liquid i s identical w ith that o f the
sol id which m ay be known to be the case when the solid neither
rises to the surface nor s inks to the bottom of the l iquid but may ,

be made to remain suspended at any point in it ; or the solid may

be placed in a lighter liquid a fter which a heavier l iqu id is added .

until the dens ities o f sol id and l iquid are equal as described , .

The sol id must o f cou rse be insoluble in both liquids and u n ,

a ff ected by either o f them and the liqui ds must be m iscible with

,

each other in all proportions .

3 13
. The densiti e s o f l iquids als o may b e found by weighing
solids in them S ince the apparent loss o f weight o f any solid
when weighed in any l iqui d ( or the di ff erence between the"
,

weight o f the solid in the air and its weight when suspended in
the l iqui d ) must be the weight o f the same volum e of that l iquid .

A s the weight o f I o m i l l i l i t e r s o f water is 1 0 Gm it follows

~

that the weight o f a piece of glass measuring I O cubic centi -

meters must be 1 0 Gm l es s in water than in air and it must ,

be 9 Gm l es s in any l iquid o f the s p gr and 1 2 Gm

. .

l es s in any liqui d o f the s p gr . .

Thus a piece o f glas s displacing I O millil iters o f water must

,
.

los e 1 0 Gm when weighed in water and its loss o f weight in

any other liquid expressed in Gm when divided by I O must
, , ,

give a quotient coincident w ith the s p w o f that other liquid . . .

3 14
. H y dr ost at i c bal a n c e s are specially constructed balances
for determ ining the specific weights o f l iqu ids and solids by
weighing sol ids in liqu ids .

The balances o f M ohr and Westphal are the best hydrostatic

balances an d the most accu rate determinations o f specific weight
,

may be obtained by the M ohr Westphal balances ( Fig

-
.

The soli d to be weighed in the l iquid i s a short glass ther

m om e t e r suspended from the end o f the beam by a platinum wire .

This thermometer i s so constructed that when it is suspended

in air the balance is in perfect equ ilibrium When the ther .

m om e t e r is suspended in any liquid in the cyl inder as shown in ,

the cut it i s buoyed up by the gravitation o f the l iquid so th a t

,
1 5 6 B ALA N C E S HY DROM E T ER S PY C NOM E T ER S
, , ,
ETC
.

weights are necessary to restore equ ilibrium ; these weights S how

the weight of the liquid displaced The weights shown in the .

“
illustration are riders E ach smaller rider is j ust one tenth
.
—

the weight of the next larger except the counterpoise which ,

equals in weight the water displaced and which in the cut i s , ,

attached to the same hook that supports the thermometer .

A s the product obtained by multiplying the power by its dis

tance fro m the fulcrum i s equal to the p roduct obtained by mul

l 0000
‘

Fi g . 1 03 . The M o h W tp h l b l
r es a a ance .

t ip ly in g
the load by its distance from the fulcrum it foll ows that ,

when the distance of the power from the fulcrum is the same
as the distance o f the load from it the power and the load must ,

“ ”
be equal The beam o f the balance is a lever o f the first kind
.
,

having the fulcrum between the power and the load Hence .
,

when the longer arm of the beam or lever is d ivided into ten
equal spaces is must follow that any rider placed in any given
1 5 8 B ALAN CE S HY DROM E T ER S PY C NOM E T ER S
, , ,
E TC .

wire to the hook under the pan and may be weighed in any l iquid
, ,

the sum o f the weights necessary to overcome the force o f the

buo y ancy being the weight o f the l iquid displaced The weight .

o f the water displaced by the plummet m ay be determined once

for all and recorded or engraved upon it and i f that weight be a ,

S imple number o f weight un its such as 1 0 Gm or 5 Gm the di

, ,

vis ion o f the weight o f the other liquid by the weight of th e same
volume o f water is extremely simpl e .

3 16 . When solids o f di fferent dens ities are mixed with each

other and it is desired to separate the heavier from th e l ighter
this separation m ay be e ff ected by adding a li quid which is l ighter
than t h e heavier sol ids and heavier than the lighter sol ids .

3 17 . A Py c n om e te r is a bottl e constructed so that it can be

conveniently used for the determ inatio n o f
the dens ities of l iquids Pycnometers are .

“ ”
o ften called specific gravity bottles .

S everal such bottles are figured here .

The bottle shoul d be made to hold ex

a c t l y 2 5 or 5 0 or 1 0 0 Gm of pure water at

I 5 C ; but many p y cnometers are a d

°
.

j usted to the temper a ture o f instead

of The best pycnom eters are c y l i n
d r i c a l rather than round o f light weight ,

( thin glass ) provided with well ground

,

stoppers wi th vertical capillary tubes bored

through thei r centers O r the stopper o f.

the pycnometer may be a thermometer ,

F ig 1
W 53 Eé i fit gflfggg
- i e t er
whil e a second l onger neck i s provided
with a cap or a perforated ground stop
per The instrument m a y be accompanied by a counterpo i se
.
.

When the p y cnometer is t o be used it is filled to the brim wit h

the liquid to be tested and the stopper o r stoppers then care full y
,

but firml y inserted a fter which the outside o f the instrum e nt i s

,

washed with water or alcohol i f n ecessary and wiped dry with

blotting paper and then weighed with its contents The tare or
, .

weight o f the bottl e must be deducted from the total weight i f a

counterpoi s e is not used The temperature at which the opera
.

tion is performed i s to be observed and the result noted and used

accordingl y This is rendered eas y when a thermometer is fitte d
.

into the bottl e as a stopper to it ; otherwise the temperature o f

 B ALAN CE S HY DROM E T ER S
, ,
P Y C NOM E T ER S ,
ETC . 1 59

the l iquid must be taken by a thermometer immersed together

with the filled pycnometer in a bath and allowed to remain there
until o f the desired temperature throughout its contents .

3 18 .A dju st m e n t of t h e t e mp e ra t ur e I t i s ver y di ffi cult to i m

.

part to a ny l iqu id the preci se temperature at which its densit y

is to be found and to maintain that temperature until the ob
,

s e r va t i on s are compl eted A bath can o f cours e be u sed in

which water is cooled w
.

ith the aid O f ice until

a thermometer inserted in the li quid indicates
the temperature of a little below 1 5 C after °
.
,

which the unmelted portion o f the ice may be

removed ; but the temper ature o f the water
must soon rise again above 1 5 i f the tem °

p e r a t u r e o f the room is much above 1 5 It .

is there fore preferable to take the densities

, ,

o f liquids at any observed temperature near

°
15 C and to make corrections a fterwards
.
,

for the contraction caus ed by a lower tempera

tu re or t h e expans ion caused by a higher tem
p e r a t u r e .

When p n om e t e r s with thermometers are

used the bottle may be fill ed with a liquid
having a temperature a littl e below and
m a y then be hel d in the hand with filter paper ,

between the hand an d the bottle until warmed ,

to Hydrom eter j ars containing liquids

may be warmed in the same manner ; but the
h y drometer itsel f must then also be warmed
at the same tim e so that t h e process is here
much S lower .

3 19 Tables o f coe ffi cients which must be

.

used to make the required corrections for

deviations from the standard temperature will F i g 1 06 P y m t cn o e er
W t h t h m om t e r
. .

i er
be found 1 n spec i al work s on w e I gh t s
e .

measures and specific gravity and in other bo oks , .

3 20 Gr a d u a t e d fl as ks are quite convenient an d su fficiently a c

.

curate for ordinary determinations o f density They should be .

thin flasks o f globe shap ed or pear shaped bodies with long

,
- -

slender necks and so constructed as to hold 5 0 or 1 0 0 or 2 0 0 or

, , , ,
 1 60 B ALAN CE S HY DROM E T ER S PY C NOM E T ER S
, , ,
ETC .

50 0or , Grams of distilled water at I 5 C when filled to the °

.

graduation mark etched upon and around the neck .

S uch flasks are often marked with an etched inscription stating

their capacity in Cc at but they are o f course graduated
.
, ,

by weight the weight does not change with variations o f tem

,

Fi g . 1 07 . D r . Squ i bb p
’
s y c n om e t e r s .

a cubic centimeter is a Cc at any temperature and the

p e ra t u re ,
-
.
,

cubical expansion or contracti on o f the glass flask itsel f is n ot

considered ,

To find approximately the density o f any liquid weigh it in the ,

graduated flask and divide by the weight o f the same volume o f

,

water .
1 62 B ALAN CE S HY DROM E T ER S PY C NOM E T ER S
,
'

, ,
E TC .

sp and man y instruments fail to indicate less di ff erences

.
g r .
,

than Hy drometers are therefore much les s reliable than

the M ohr Westphal balance the pycnometer or the graduated
-
, ,

narrow necked specific gravity flask ( Par

-
but th e ir c On .

Fi g s . 1 09 and 11 0
. Hd y ro m e te rs .

ve n i e nc e is so great that hydrometers are large ly employed when

ever a p p rox 1m a t e l y correct results are su fficient H y drometers .

1 n d 1c a t 1 n
g di ff erences of may be regard ed as e xtremely
 B ALAN CE S H Y DROM E T ER S
, ,
P Y C NO M E T ER S ,
E TC . 1 63

satis factory for all ordinary laboratory operations i n f t h e m anu e

facture o f ch emical products .

The spaces between the graduation marks on t h e hydrometer '

s ca l e s a r e always larger at the top than l ow e r d o w n

~
.

3 24 The hy dr om e t e r ja r ( Fig 1 1 0 ) must be su fficiently roomy

. .

to allow the hydrometer to float freely without coming i n contact

with the s ides and tall enough to leave the upp er end o f the
,

hydrometer protruding above the top o f the j ar when the i n s t ru

ment i s immersed in the lightest l iquid the ,

density of which is incl uded within the range

of the scale .

3 25 I f it is des ired to take observations

.

o f dens ity at 1 5 the h y drometer and j ar must °

both be cooled with cold water be fore they are

used .

The best hydrometers include th e r m om e te rs

within thei r tubes so that the temperature can
“

be observed c on currently with reading off the

density .

T he m e ni s cu s renders the readin g di f

'

3 26 .

fi c u l t but care an d experience will enabl e the

,

operator to obtain satis factory results ; the

dens ity mark at the middle o f the depth o f th e
m e n i sc u s i n d i c a t e s the correct specific gravity .

3 27 L arge hydrometers deman d the us e F i g 1 1 1 R

.
, ,
’
0u s s e au s

o f much l iquid and smaller hydrometers ( each ,

made for a more l imited range of densities ) are accordin g ly o ften

preferred or even necessary ,
.

3 28 T w a dd e l l s hy d r om e t e r s are c omparatively small as the

’
.
,

graduated scales o f thes e hydrometers occupy a space only about

75 mil limeters long The y are made in s.ets o f S i x and as the ,

whol e range o f densities divided up between these six instruments

'

extends Only from O t o 1 7 4 d e g r e e s o r from the s p gr I to

‘

. .

the degree spaces are large enough to be easily read The zero .

’
on Twaddell s scal e corresponds to the density o f water at C .

( 60
°
and each degree above th e 0 represents an increase o f
o f the den sity o f water so that 2 Twaddell i s equivalent ,
°

to the s p gr . and 1 0 T w to s p gr
.
°
. . .

’
It will be observed that Twaddell s hydrom e ters a re i n t e nded
only for li quids heavier than water .
1 64 B ALAN CE S HY DROM E T ER S PY C NO M E T ER S
, , ,
ETC .

O n account o f their small size the Twaddell hydrometers can be

used in the customary graduated cylinders o f 1 0 0 Cc capacity .
,

so that no special hydrometer j ar i s neces sary .

To convert Twaddell degrees into th e correspond ing specific

gravity m u l ti ply th e n u m be r of d e gr e e s by and a dd 1 to .

th e r od u c t
p .

Fi g . 112 . T w dd ll h d
a e
’
s y ro m e te r . Fi g . 113 . B au m e s
’
h d
y r om e t e r s .

B au m e h y dr ome t e r s
were once very generally used ; but
’
3 29 . s

are falling into disuse on account o f their very unscientific scales

o f degrees and their uncertain standards
,
.

The B a um é h y drometer for h e a vy l iquids is as sumed to des

cend to O in water at 5 C and to descend to the point marked .
,

15 in a solution made of 1 5 parts o f sodium chloride in 8 5 parts

°

o f water .
1 66 B ALAN CE S HY DROM E T ER S PY C NOM E T ER S
, , ,
ETG .

Baum e subtract from ,

1 45 the quotient obtained by divi din g ; 1 4 5
by the specific weight

sp . w .

F or l i q u i d s h e a vi e r th a n w a te r .

111 . Baum e degrees into specific weight divide

To '
c on v e r t ,

1 40 by the sum o f 1 3 0 plus the number o f degrees

1 40
sp . w .

°
I 3 o + B

IV To convert specific weight into the correspon d i ng num ber

.

o f degrees B a u m é divide 1 40 by the specifi c weight and from the

'
*
.
,

quotient subtract 1 3 0

sp . w .

3 30 The knowledge o f the density o f a s u bs t an c e a i d s i n l i t s 5

.

id entification and in the determ ination o f its purit y a n d s t r e n gt h fi

,
F
-

and enables u s to comput e the weight f rom t h e volume a n d fi t h e f

'

'

vol u m e f r om the weight It is also a guide in the c on c e n t r at i onl o ff

’ "

solutions by e va p or at i on f or various purposes r .

33 1 S pe c i fi c vol u me fi
. The specific volume o f a t li quid i S t h e < 's '

r e ciprocal of its specific weight .

Its util ity in laboratory work i s great :

To convert any number of grams into th e corresponding num
ber o f mill iliters or any nu m be r o f kilograms into the correspond
,

ing number of l iters m u l ti ply by th e s pe ci fi c v ol u m e ,

.

*T h e t e r m s p e c i fi c v o l u m e a n d i t s e m p l o y m e n t w e r e p r o p o s e d by
t h e a u th o r o f t h i s b o o k i n 1 8 8 3 i n a p a p e r r e a d b e fo r e t h e A m e r i c a n
,

P h ar m a c e u ti c al A s s o c i ati on S e e P r o c e e d i n g s o f th a t A s s o c i ati o n fo r t h e
.

y e an nam e d .
 CH A P T E R X VI II .

RULE S F OR M A KI N G S OLU TI O N S A N D M I X T URE S O F A N Y GI V EN

S T REN GTH ,
AN D F O R D I LU TI N G F OR TIFYI N G A N D M I X I N G
.

,
.

332 To make solutions and mixtures o f any given percent

.

age strength all the quantities and values employed shoul d refer
to weight .

A ccurate results are obtained when all the material s are meas
'

u r e d by weight because mass is not a ff ected by c on t r a c t i on or

,

expansion o f volume .

B ut when the quantities o f the materials or ingred ients are

measured by volume instead o f by weight or when the quantity ,

o f one of two ingred ients is measured by weight and that of the

other by volume the exact strength o f th e mixture or solution
,

can not be directly or easily computed or expressed .

E ven i f t he m ixture or solution is composed o f two l iquids ,

their proportions S houl d be stated and computed by wei ght and

.

not by volume becau se the volume o f the resulting mixture or

,

solution is generally less than the sum o f the original vol u m e s o f

the two component l iqu ids so that the proportion which the vol
,
-

ume o f either o f these two liquids bears to the final vol ume o f
the product can not be known from the proportions e mployed .

A mixture o f alcohol and water one hundred volumes o f which

,

contain fi fty volumes o f absolute alcohol contains an amount of ,

water which s eparately must measure more than fi fty volumes ‘

A statement of percentage strength or compos ition referring to .

volume proportion s i s accordingly unreliable and deceptive .

N evertheless it i s so convenient for many pharmaceutical pu r

poses to prepare solutions and liqui d m i xtures volumetrically or ,

to measu re the solids by weight and the l iquids by measure in

making preparations composed o f both that it i s a common prae ,

tice and the results are i n m os t cas e s suffi ciently nearly accu rate
,

for those pu rposes .

When absolute exactnes s i s necessary however all quantities , ,

and values emplo y ed in working formulas in actual work and in

-
, ,

statements o f strength re ferring to liquids must be expressed in

167
1 68 R U LE S F OR M A K I N G S O L U TI O N S A N D M I X T U R E S .

terms o f weight exclusivel y Gravimetric m e t h o d s f orm u l a s and

.
,
.

expressions are always practicabl e and exact and for nearly all ,

purposes in chem ical laboratory work they are preferable in point

o f convenience as well as scientific accuracy .

3 33 . The following

R u l e f or c omp u t i n g q i t i e s an d pr op orti on s i n mak i n g mi x

u an t
t ur e s a n d s ol u t i on s will be found applicable in most cases :

Having a known quantity ( a ) O f on e ingredi ent o f known value

( )
A and ,
desiring to find the quantity ( )x o f the s econd ingred ient
of known value ( B ) which will be requ ired to produce a m ixture
o f any intermediat e valu e ( c ) M u l t iply t h e k n ow n q u a n ti ty of
—
'

th e fir s t i ng r e d i e n t ( a ) by th e d i ff e r e n ce be tw e e n i ts va l u e ( A )

a n d th e d e s i r e d v a l u e of t h e m i x t u r e ( c ) d i vi d e th e pr od u c t by
th e d i ff e r e n c e be tw e e n th e va l u e of th e s e c on d i ng r e d i e n t ( B )
a n d th e d e s i r e d va l u e of th e m i x t ur e ( c ) T h e q u oti e n t i s t h e
'

q u a n ti ty d e s i r e d of t h e s e c on d i n g r e d i e n t ( x ) .

For the purposes o f the foregoing rul e the term 1 n g re d i e nt

'

applies to each o f the two components o f any mixture or sol u

tion Thus the t w o ingredients o f any sol ution are the solvent
.

and the dissolved substance ; the ingredients o f any dilute alcohol

are the alcohol and water ; and the compon ents o f a n y mixture o f
t w o solutions o f di ff erent stren g th or o f a m ixture o f a stronger
,

and a weaker alcohol or o f a mixture o f a stronger an d a weaker

,

“ ”
opium are also designated as ingredients
, .

“ ”
The value o f each ingredient as well as the valu e o f the
mixture must be expressed in per cent by w eight .

“ ”
I f the ingredients are water and potassium brom ide then the ,

value o f the water is 0 and the value o f the brom ide 1 00 ; in a

mixture of absolute alcohol and water the alcohol has a value o f ,

1 0 0 and wa ter 0 I f opium i s one ingredient and milk sugar the

.

other the value o f the opium may be expressed as 1 0 0 and that

,

o f the mik sugar as 0 i f th e va l u e of th e m i x t u r e i s to be e x pr e s s e d

i n t e r m s pe r c e n t of opi u m ; but i f the value o f the opium be
expressed in per cent o f morphine then the stren gt h o f the milk ,
'

sugar a n d o f the mixture must also be expressed in the sam e

ter ms Thus i f an opium containing 1 6 per cent o f morphine i s
.
1 70 RULE S F OR M A K I N G S OL U TI ON S AND M I X T UR E S .

How much water mu st be added to 3 0 Gm o f potass i um

hydroxide to make a 3 0 per cent s olution o f it ?

( 1 00 — 3 0 ) X 30

3 o—
o

A nswer : Gm o f water 7 0 .

How much z i n c s u l p h a t e must be added to 2 0 0 Gm o f water

3 .

to produce a solution of 4 per cent strength ?

T h e water may be called the first ingr edient and has a value-

o f 0 The zinc sulphate i s the second ingredient and its value i s

.

Then

(4 —
0 )
£ 8 33 3 Gm .

I oo —
4

A nswer : zinc sulphate Gm '

of .

4 How much solution o f 3 per cent strength can be made out

. :

of 4 00 Gm o f a solution o f 1 8 per cent strengt h

-
?

L e t us find how much water must be added .

( 1 8— 3)
=2 0 0 0 Gm .

A nswer : Gm of water must be a dded to the 4 0 0 Gm o f

2 00 0
'

1 8 per cent solution producing therefore 2 40 0 Gm o f 3 per cent , , ,

solution .

5 How. much solution of 5 0 per cent strength must be added

to Gm o f w at e r t o produce a solution o f 3 0 per cent
‘

' ‘ ‘

strength ?

333 ( so —
0 )

5 0 3 0
—

A n sw e r z -
'

5 oo m
cent solution must be added to o f 50 p e r
Gm o f water to produce Gm o f solution o f 3 0 per '
‘

cent strength .

6 .How much zinc sulphate must be added to 60 0 Gm o f a 2 o -

per cent solution o f that salt to increase th e stren g th o f the solu

tion to 2 5 per cent ?
 RULE S . F OR M A K I N G S OLU TI O N S AN D M I X T URE S . 171

—
2o )
40 Gm .

1 00— 25

A nswer Gm o f zinc sulphate added to 6 0 0 Gm o f a 2 0 per

: 40
cent soluti on o f zinc sulphate will make 6 40 Gm o f a solution o f
2 5 per cent strength .

7 : How much o f a borax solution o f 5 per cent strength mu st

-

be added to 8 0 0 Gm o f a borax solution o f 2 per cent strength to

‘
~

produce a solution of 3 per cent strength ?

-

(3 —
2 )
4 00 Gm .

5 3
—

A nswer : Gm of borax solution o f 5 per cent strength

4 00

added to 80 0 Gm o f a solution o f 2 per cen t strength will produce

1 2 0 0 Gm o f borax solution o f 3 per cent strength .

8
. How much alcohol o f 9 1 per cent mu st be added to 3 00 0
Gm o f alcohol o f 4 1 per cent strength to produce a mixtu re con
ta ining 7 5 per cent o f alcoh ol ?

( 75 —
41 )
6 3 7 5 Gm .

9 1— 75

A nswer : 637 5
Gm o f alcohol o f 9 1 per cent strength mixed
with with 3 00 0 Gm o f alcohol o f 4 1 per cent will make 93 7 5 Gm
o f an alcohol o f 7 5 per cent .

How much alcohol o f 4 1 per cent stren gt h mu st be added

9
.

to 6 3 7 5 Gm o f alcohol o f 9 1 p e r cent strength to produce an alco

~

hol o f 7 5 per cent ?

(9 1 75)
—

10 . much glycerin mu st be added to 8 6 4 Gm o f alcohol

H ow ‘

to produce a m ixture containing 1 0 per cent o f g lycerin ?

I o— o )
—
7
=9 6 Gm .

I oo — I o

A nswer : 9 6 Gm o f glycerin ;
 RULE S F OR M A K I N G S OLU TI ON S AND M I X T U RE S .

How much glycerin must be added to 8 6 4 Gm o f alcohol t o

1 1 .

produce a mixture containing 1 0 per cent o f alcohol ?

—
I O )

A nswer : Gm o f glycerin added to 8 6 4 Gm o f al cohol will

777 6
produce a mixture containing 1 0 per cent of alcohol .

12 How much opium containing 1 0 per cent of morphine

.

must be added to 4 2 0 Gm of opium containing 1 8 per cent o f

morphine in order to make a mixture containin g 1 3 per cent of
morphine ?

( 1 8— 1 3)
1 3 10
—

A nswer : o f opium o f 1 0 per cent strength an d 4 20 Gm

700

o f opium o f 1 8 per cent strength when m i xed will make 1 1 2 0 Gm

o f opium o f 1 3 per cent morph ine strength .

3 34To find the relative proportions required o f salt an d

.

water to make 1 0 0 Gm o f any salt solution o f any given stren gth : -

R ul e . S u btr a c t th e d e s i r e d p er ce n t fr om 1 00 ; th e r e maind e r

w ill s h ow th e n u m be r o f Gm o f w a te r r e q ui re d . T he n u m be r

ex p r e s s i ng th e d e s i r e d p e r c e n ta g e s tr e n g th o f th e s ol u ti on w i l l be
th e n u m be r o f Gm o f s al t r e q u i r e d .

Ex To make
. 1 00 grains o f a 4 per cent solution o f cocaine
hydrochlorate u se 4 grains o f c oca I n e hydrochlorate and 96 grains
o f water .

335 To find the quantity of salt ( a ) which must be added

.

to any given quantity of water ( b) to produce a solution o f any

given per cent strength ( c ) and the quantity o f solution ob ,

ta i n e d ( d )
°

R ul e . M ul ti pl y th e gr a m s of w a te r ( b) by t h e d e s i r e d pe r
ce nt o f th e s ol u ti on ( c) t o be m a d e , a n d d i vi d e t h e pr od u ct by

th e r e m ai n d e r f ou n d by s u btr a c ti n g th e n u m be r e x pr e s s i ng th a t
pe r ce n t fr om 1 00 ; t h e q u oti e n t w i ll be th e n u m be r of g r a m s of
1

1 74 R U L E S F OR
‘

M A KI N G S OL U TI ON S A N D M I X T URES .

and 3 0 0

A nswer : kilograms of 8 pe r cent solution will be produced

3 0 0 .

ou t o f 2 4 kilograms o f sodium carbonate and 2 7 6 kilo g rams o f

water .

33 7 . T o find the quantity o f weaker solution o f a ny <

g i v e n

strength that can be made out o f any given quantity o f a stro nger
s olution and thus al so the quantity o f di luent required :
,

R ul e . M u l tipyl t h e g r a m s of th e s t r ong e r s ol u ti on ( ) y
a b i ts

p e r c e n tag e s tr e ng th ( b) , a n d d i vi d e t h e pr o d u c t by th e d e s i r e d
‘
l ow e r pe r c e n tag e s tr e ngth ( c ) ; th e q u ot i e n t i s th e g r a m s of
'

w e a k e r solution ( d ) p r od u ce d by the stronger solution ( a ) The .

di ff erence between d and a i s the number o f g rams o f diluent re

quired ( e )

Formula

d ,
’

and d— az e .

E xplanation
“

c zb a :d , and c Xb
°
z z a .

Ex .I f 20 0 Gm o f a solution o f 5 0 per cent i s to be diluted to ~ ~

30 per cent

and —
2 00 2 1 33 3 3

A nswer : Gm of the 3 0 per cent solution can be made

from 2 0 0 Gm o f 5 0 % solution so that the quantity o f water t o ,

be added is Gm .

. 3 38
To find the quantit y o f stronger solution required t o
.
-

make any given quantit y o f weaker solution and thus al so the

.

quantity of diluent required

 RULE S F OR M A KI N G S OLU TI ON S A ND M I X T URE S .

R ul e . M u l ti l
py t h e r e q uire d q u a n t i ty f
o t h e w e a k e r s ol u t i on

( ) y
a b i ts d e s i r e d pe r c e n t s t r e ng t h ( )
b , a n d di v i d e -t h e pr od u c t

by t h e pe r ce n ta g e s tr e ng th ( c ) of t h e s tr ong e r s ol u t i on ; th e
”

q u ot i e n ti s th e q ua n t i ty r e q u i r e d ( d ) of th e s tr ong e r s ol u ti on Th e .

y f i i d ( ) i h d i ff b w d d
’

q u a n t i t o d l u e n t r e qu r e e s t e e r e n c e e t e e n a
'
an .

Formula

d; and d—
az e .

E xplanation
c z bz a : f; and c s c .

EX How much 2 5 per cent solution will be required to make

’

60 0 Gm of a 20 per cent solut i on A nd how much water

?

and 60 0 —
4 8 0 = 1 2 o .

A nswer : Gm o f 2 5 % solution and

4 80 1 20 Gm o f water will
make 60 0 Gm o f 2 0 % solution .

339 To find the kilos o f water ( x ) required to be added to

.

each kil o o f a solution o f any given percentage strength to dilute .

.

it to any les s percentage desired :

R ul e . D i vi d e th e p e r c e n ta g e s tr e ng t h ( ) a f
o th e s tr ong e r

s ol u ti on by th e pe rce n tag e d e s i r e d ( ),
b
"
a n d s u btr a c t
~

1 fr om th e

q u o t i e n t .

F orm u l a

—
I

EX . A 90 % solution i s to be diluted to
How many kilos
o f water mu s t be add e d to e a ch kilo o f the 90 % solution ?
 R ULE S F OR M A KI N G S OLU TI ON S AND M I X T URE S .

and 1 .
5 O

A nswer : kilo of water must be added to each kilo of the

0 .
5 0

9 0 per cent solution

3 40To find the absolute quantities o f salt ( a ) and water ( b)

.

required to make any g i ve n q u a nt i ty o f solution ( c ) o f any given '

stren gth ( d )

R ul e .
pyM
l tu l ti
h e g r a m s of s ol u ti on r e q u i r e d ( ) y
c b t h e d e

s i r e d pe r c e n ta g e s tr e n g th ( d ) , and di vi d e th e pr o d u c t by 1 0 0 .

T h e q u oti e n t i s t hp g r a m s of s a l t r e q u i r e d ( a ) T h e g r a m s of .

w a te r ( b) r e q u i r e d i s th e d i ff e r e n ce be tw e e n th e g r a ms of s a l t ( a )
a nd th e g r a ms o f s ol u ti on

Formula

a; and c— a: b .

E xplanation
1 00 zdz c :a; and 1 00 >< a _

Ex . H
much sodium h y droxide is required to make 5 0 0
ow

Gm of a 6 % solution ? A nd how much water ?

5 ><6
oo

3 0 and 5 0 0 —
3 0 2
470 .

A nswer : 3 0 Gm o f sodium h y droxide and 4 7 0 Gm o f water .

341
To find the percentage strength o f any salt solution from
.
-

the grams o f salt contained in a given number o f grams of solu

tion
0

R ul e . M u l ti l
py t h e g am s
r o f th e s alt ( )
a by 1 00 and di vide
by th e g r a ms of t h e s ol u ti on
( )
b th e q u o t i e n t i s t h e p e r c e n tag e
1 7 8 RULE S F OR M A KI N G S OLU TI ON S AND M I X T URE S .

i s frequently a convenient method of fin ding

A l l i g a ti on
the proportions requ ired o f two or more ingredients o f di ff erent
values required to produce a mixture o f any value intermediate
between the highest and lowest .

To find the proportions required o f any two I ngredients o f di f

f e r e n t val ues required t o produce a mixture o f any desired inter
mediate value .

R ul e . The n u m be r o fp a r ts r e q u i r e d o f th e w e a k e r i ng r e di e n t
'
( ) a i s th e d i ff e r e n c e be tw e e n t h e va l u e (p e r c e n tag e s tr e ng t h
) f
o

th e s tr ong e r i ng r e d i e n t ( )
b an d th e d e s i r e d v a l u e o f th e mix
tu r e ( ) c .

The n u m be r fp r e q uire d f th e i ng r e d i e n t
o ar ts o
(d)
s tr ong e r

i s th e d i ff e r e n c e be tw e e n th e d e s i r e d va l u e ( pe r c e n ta g e s tr e ng th )
of th e m i x t u r e ( c ) a n d t h e va l u e of t h e w e a k e r i ng r e d i e n t ( e ) .

az b
—
c and dx c— e .

EX
To make a mixture o f 7 per cent strength out o f one o f 3
.

per cent and another o f 1 2 per cent use 1 2 parts o f the ,

3 per cent ingredient and 7 3 4 parts o f the 1 2 per cent ingre

— 2

dient .
 CH A PT E R X IX .

F URN IT URE A ND A PP ARA T U S .

335 The outfit o f a pparatus for a pharmaceutical laboratory

.

in which chem ical preparations are ma de must var y to so great an

extent according to the quantity and variety o f the products and ,

according to other circumstances that a definite d e scription o f ,

such a laboratory i s scarcely practicabl e A fe w general s u g ges .

,

t i on s may however be found useful to pharmacists as well a s

, ,

students w h o desire to undertake to make chemical preparations .

Certain laboratory furniture fixtures and apparatus are o f , ,

course always necessary

,
.

These include wall fixtures such as shelving cupboards a case , , ,

o f drawers good water supply on e or more sinks good ve nt i la

,
-
, ,

tion one or more e ff ective fl u e s with which to connect a drying

,

closet and a hood or fume chamber work tables heating appara , ,

tus a good Stil l for making distilled water a press and a s u ffi

, , ,

cient outfit o f p ots an d pans j ars bottles strainer frames and , , ,

stands dishes funnel s filter stands glassware etc

, , , , , .

F URN IT URE AN D F I X T URE S .

336 . I f th e products made include considerable quantities o f

precipitates an d crystall ized salts requiring dr y ing a dryi ng ,

c l ose t is o f great advantage I n large laboratories two or more

.

d rying closets kept at di fferent temperatures are more serviceable

than one large one ; or a special drying roo m and one or two
closets are us ed S mall drying closets may be heated by means o f
.

steam coils hot water coils or hot air according to circumstances

, , , .

Where steam or hot water can not be had the drying closet may
be heate d by means o f a suitable gas burner or gas stove or by ,

a gasol ine or oil bu rner placed at the bottom The closet must
, .
,

o f course be provi ded w ith openings to admit air below the heat
,

ing appliance used and also at the top so that a current is estab
,

lishe d .The top o f the closet S hould be connected with an e ff e c

tive flue i f possible ; but i f this can not be don e some other means
,

of establ ishing a dra ft should be adopted T he current o f air .

179
1 80 F URN IT URE A ND A PP ARA T U S .

passing through the drying closet need not ( and for most pur ,

poses s h ou ld not ) be strong R acks for shelves or frames are

,
.

so arranged that the circulation of air is not impeded For some .

purposes it is admissible to u se shelv e s made of galvanized iron

wire grating S trips o f plate glass wood or tinned iron are often
.
, ,

employed instead o f shelves .

The moist products to be dried in the drying closet are spread

out upon filter paper or muslin plac ed on the shelves or strips .

It is important to regulate the temperature well so that substances

liabl e to inj ury from too high heat may not be spoiled .

337 . A t i ght f ume ch amber or hood connected with a flue hav

ing a good dra ft is essential i f operations are to be per formed
resulting in the evolution of irritating or poisonous gases such ,

as nitrous vapors chlorine sulphur dioxid e etc The fume cham

, , ,
.

ber S hould have a soapstone bottom and at least two s ides o f it ,

sh ould consist of movable sash with doubl e thick window glass .

338 . The w ork t abl e s must be s trong and heavy They shoul d .

be about meter high and not over meter wide i f placed

l engt hwise against the wall but about 1 meter wide i f out from
,

the wall .

O ne o f the tables should have a tin covered top inclined to

ward and adj oin ing the s ink and this tabl e shoul d be exclusively
,

for apparatu s j ust cleaned and left to be drained .

A nother tabl e adj oining the sink shoul d be covered with sheet
lead and should have a raised edge ( also covered ) all around it
so that operations I n which corrosive or inflammable l iquids a re
used may be per formed more sa fely .

S oapstone tables are most desirable for operations requiring

the continuous use o f powerful burners .

O ther work tables or counters shoul d have wooden tops .

3 39 I f practicable there S houl d be in any large laborat ory a

.

Speciall y planned place for still s pans strainer stands an d the

, ,

press a place where the fl oor i s c ove r e d w i t h a sph a l t and inclined

—
t

toward a drain so that the water which is frequently freely u sed

in connectio n with that kind o f apparatu s will readily run off .

I f an asphalt floor is impracticable a t i n cove r e d low inclined -

, ,

p l a t f or m wit h raised edges is useful A plenti ful and convenient

.

supply o f water with taps or faucets wherever required is very

important here .
1 82 F URN IT URE AND A PP ARA T U S .

should cause the needle t o deviate the same distance from the
center .

4
. The k i l ogr a m bal a n c e should be constructed to carr y loads
o f from 5 to 2 0 0 0 Gm and its sensitiveness should be such that
,

the needl e point deviates from the center by 2 millimeters on

the impuls e o f 5 0 m illigrams when the pans are n ot l oa d e d and on
the impulse of 2 00 milligrams when they are loaded with 2 00 0
Gm each .

O ne or two la rg e r ba l a n c e s may also be neces sary .

A M oh r kVe s tph a l ba l a n ce is o f great value

-
.

A ll balances shoul d be placed on sol id tables where they w 1l l

“

be safe against j arring and inj ury and must be kept well pro ,

t e c t e d against dust They shoul d be kept scrupulously clean and

.

dry and no chemic als S houl d be permitted to come in contact with

,

them They should above all be protected against corrosive sub

.

stances When not in actual us e they must be at per fect rest

.

with the kni fe edges rel ieved from friction

-
.

T he w ei g h ts shoul d also be kept clean and accurate .

“
341 . Gra du at e d gl ass m e asur e s commonly called graduates , ,

are necessary in every pharmaceutical establishment They .

Should be graduated in accordance w ith but one system ; thos e

g raduated according to the ol d system of fluid measure on one
s ide and in cubic centimeters on the other S ide shoul d n ever be
—
,

u sed for any purpos e becaus e such double graduation leads to

frequent errors .

The metric system having now been adopted in every pharma

c op oe i a the worl d over pharmacists S h ould do all in their power
, ,

to shorten the tim e requ ired to compl ete the change from the
Ol d to the new not only because resista nce to the inevitable is
,

u seless but because they will certainly find the new system far
more convenient .

Graduated cylin d ers flasks p ipettes bu rettes an acc urat e , , , ,

pycnometer and a set o f reliabl e h y drometers are required for the

,

analytical work inseparable from the work of producing and dis

p e n s i n g chemical preparations ( S e e Chapter X V ). .

H EA TI N G A PP ARA T U S .

'

3 42 uch can be d on e with the stoves furnaces and burners

. M ,

constructed for use with gas as the fuel Illustrated descriptive .

 F URN IT URE AND A PP ARAT U S . 1 83

catalogues o f such heating apparatus are freel y furnished by deal

ers and manu facturers so that any one may learn more from
them than can be presented in any text boo k A mon g the most —
.

effi cient gas burn e r s are the Fletcher l ow temper ature burner
“ ”
,

Fi g . 115 . Gr a d u at e d g l a ss m e as ure . Fi g 11 6
.

p
Fl t h
e c b er u r ne r
l ow t e m e ra t u r e

which a ff ords a wide range of temperatures from gentl e heat up

to red heat it is so constructed that it can be attached to a pipe
from a bellows when a very hi g h heat i s to be produced and it ,

Fi g . 11 7 . Fl t h
e c e r ra di l b
ca u rn e r .

i s so eff ective that the designation l ow temperature burner is

(

an un fortu nate on e s inc e it emphasizes one o f its merits that th e —

h eat can be t h orou g h l y c on t r oll e d and kept very l ow i f desired

'
‘
 1 84 F URN IT URE AND A PP ARA T U S .

at the expense o f the equally valuable feature wh ic h

'

e n a bl e s the
operator to apply a n e xceptionally high heat -
.

J ewe l ga s h e a te r .

Fi g . 1 19 .
F oot b l ow e r . Fi g 1 20 I
r o n r e t or t f or t h e p d
ro i
u c t on
h
. .

“
th e d ry way and f or ot p
qu r n ii gv
e ry eat hi g h h .
er r oc e s s e s re

Fi g . 1 21 . T ip l B
r e uns e n b u r n e r.
Fi g . 122 . B u ns e n b urne r w t ih c on e
0 .

The Fletcher radial burner ( made by Bu ffalo D ental M f

“ ” g .

Co ) and the Jewel gas stove ( made by Geo M Clark

.

Co . .
.
,

of Chicago ) are particularl y serviceable for heating large vessels .

1 86 F URN IT U RE A N D A P P ARA T U S .

the flame is non luminou s or bluish because the combustion is

-
,

then complete ; but when the supply o f air i s shut off the flame i s
lumi nous yellow and smoky When the current o f gas is t o o
,
.

low in proportion to the air admitted it frequ ently happens that

the gas i g ni te s ba ck the flame reced ing down into the tube to the
,

pin hole orifice o f the g as tip The whole tube the n at once be .

comes very hot so that the rubber tube attached to the burner .

may melt the escaping gas then becoming ign ited and a d e s t r u c
,

tive fi re m ay result I t is therefore dangerous to leave a Bun

. .
, ,

S e n burner i n operation with the gas turned low Whenever it is .

fo und that the o f the B unsen burner has receded to the

Fi g B 1 26 un s e n b u rn e r fl am e s ; t h e c uts p p fl me
c on t r a s t a ro er a
h l t i g wh li g h t d b k i n t o t h
. .

“ ”

fiia
t at th e is
l;
resu n en g as e ac e
l

base or light ed back the gas should be immediately shut off ,

and the burner al lowed to cool off completely before it is again

r e l ighted ; it may be cooled off quickly by letting col d water
-

fl ow upon it .

3 44 I n cases where it i s necessary to allow a Bunsen burner

.

to remain lighted a long time without constant attention it should ,

be placed on a fir e pr oof t a bl e and the gas should be s uppl ied

-

to it not by means of rubber tubing but through a piece o f gas

pipe direct ly attached to t h e bu r n e r ’
.

3 45 The introduction o f a diaphragm o f fine wire netting in

.

“
the tube j ust below the top prevents the flame from striking
, ,
”
back but it also reduces the intensity of the heat o f the flame
, .
 F URN IT URE A ND A PP ARA T U S . 1 87

The mixture o f ga s an d a ir pas sing through the wire netting i s -

ignited above it Gas burners constructed on this principl e can

.

be easily obtained .

S pecial burners are made for u se with acetylene as the fuel ,

and acetylene burners produce a much higher temperature than

gas burners .

3 46. The R oessl er gas furnace i s a very effi cient apparatus

for small crucibl e operations where extremely high temperatures
are necessary It can be used with either gas Or acetylene
. .

I ts construction is shown in the accompanyin g cut I t will .

Fi g . 127 . Ro less er f u r n a ce .

heat a crucible about twelve centimeters high having a d iameter

o f seven centimeters at the top The length o f the chimney m ay
.

be extended to about two meters and to insure a strong dra ft

through it a second burner is used at its foot .

34 7
. When gas is not availabl e g as ol i n e burners m ay be a d
va n t a g e ou s l y u sed
,
an d in many cases a good c oa l stove or a
c har c oa l furnace may be found useful .

S pi ri t l am ps are extremely valuable for small and brief opera

1 88 F URN IT URE AND A PP ARAT U S .

'

tions where a perfectl y s m ok e l e s s fl a m e and h igh heat are de

s ired .

34 8 In the use o f Bunsen burners spirit lamps and other burn

.

ers which a ff ord one sol id vertical

fl a m e the most intense heat i s j ust ,

below the middle o f the flame .

3 49 When a vertical flam e i s .

used it is o ften necessary to dis

tribute an d moderate the heat by
interpos ing w i r e g a u z e or as be s tos -

e l o i n between the flame and the ves

sel he ated The gauze or cloth may .

sometimes incidentally serve as a

support for fl asks beakers and ,

other vessel s to which the heat is

‘

applied But w i re g au z e is soon .

“
burnt out ”
A sbestos cloth is
Fi g 1 28 B t h l p i i t l m p
.

’
ar e s s r a s
much to be preferred
. .

35 0 S a n d ba t hs are frequently useful for supporting flasks

.
-

retorts and dishes which are to be strongly heated serving to ,

F ig 1 29 S hmw i g
o n th e e ff t f th i
ec o e nte r p iti
os on of w i re l h
c ot ;
li g h t d i t h b v b l w i l th
. .

th e g as ay be e e er a o e or e o th e w re c o .

distribute the heat sand bath dishes are used for the
. S h al low -

support of beakers and evaporating dishes and als o flas ks ; deeper

sa nd bath dishes are necessar y for heating retorts which must
-
 F URN IT URE AN D A PP ARAT U S .

ordinary water bath requires watchin g and frequent replenishin g

—

with water to prevent their running dry or too l ow which usual ly ,

results in damage The constant l evel water bath is so con

.
-

struct e d that the water vapor does not escape but is condensed ,

and runs b ack into the body o f the vessel The bath shown in Fig . .

F i g 1 34 S m a ll r ou n db
-
ot t om e d co pp e r Fig 1 35 S ma ll b
fi a t - ot t om e d wat e r
b th h
. .
. .

wa t e r -
a . bat .

Fig 136 W at e r- b at h ih
w t a t ta c hm e nt t o m a nt a i i n a c on s t a n t
lvl
. .

e e of t h e wa t e r .

1 37 is as seen d i ff erently constructed Var i ous kinds may be

, , .

found described in the catalo gu es o f deal ers in chemical a p

paratus .

The water bath when in us e shoul d be kept from one hal f to

— -

three fourths filled with water and the vessel placed upon it
-
,

shoul d not fit so tightly that there is no escape for the steam ,

for the pres sure may then become so great as to throw the vessel
 F URN IT URE AN D A PP ARA T U S .
91

o ff the bath or to cause a sudden outburst o f steam which might

do inj ury .

The temperature a ff orded by the water bath when well man -

aged may be made to range all the w ay from the ordinary

°
room temperature up to about 9 5 C .

35 2 S a l t s ol u ti ons ( for from 1 0 0 to i up °

. l
g y ce r n ( .
.

to and pa r a ffin ( up to are frequently employed in

bath s instead o f water for the purpos e o f imparting heat The .

temperatures aff orded vary according to the boiling points -

‘
.

When temperatures below the respect i ve boil ing points of these

several liquids are required it is necessary to use th e r m om e te r s i n
order to be abl e to guard against a higher he at than that desired .

Thermometers are especially neces sary in w ater baths when the -

temperature mu st not be permitted to exceed a g i ven degree A t .

the same time the water bath may then be placed a greater or -

less distance above the flame an d the flame or fire may be regu ,

lated as c i rcumstances require .

35 3 H ot w a te r c oi ls may be advantageously used to he a t

.
,
.

sa nd or water in large Sand

baths or water baths em -

ployed in the practice labora

tories o f techn ical schools for
the use o f th e classes S uch .

sand baths and water baths

- . -

may be made to a ff ord a

reasonably uni form t e mpera
6
ture anywhere between 3 0
and 7 0 °

354 . H ot ai r c h a m be rs ,

heated with steam or hot w a

ter and tightly closed m a y
, ,
'

be employed for maintaining

nearly uni form temperatures
for various laboratory pur
poses They are u sually made
.
Fi g 1 37 I t t w t h t . . n s a n a n e ou s a er ea er .

o f plate glass i n frames o f wood and the temperature o f the air ,

in them is observed by means o f thermometers .

H ot a i r ov e ns and h o t w a te r ove n s o f copper are used for dr y ing

small quantities o f variou s substances .

355 S t e am h e a t is invaluable in l a r g e manu factu ring labora

.
 9 2 F URN IT URE AN D A PP ARA T U S .

tories E ven small steam boil ers o f very simpl e construction

.

are o f great utility in moderately equ i pped pharmaceutical labora

tories Where steam power is used the steam also furni shes t h e
.
,

heat for pans still s etc , , .

Fi g . 1 38 . S ma ll d i g v
ry n o en in us e .

T he temperature imparted by steam heating apparatus may be -

re gulated so that it can be kept within narrow limits at any

Fi g . 1 39 .
D blou e - wa ll d
e copp er o v en . Fi g . 1 40 .
pp
Co er d i g v
ry n o en .

W i th i n the extreme range o f from a few degrees above the

0 o

m
0

p o t

ordinary room temperatures up to The steam u sed may

be under a pressure o f from three or four pound s to the squar e
1 94 F URN IT URE A N D A PP ARA T U S .

steam may be advantageously used under a pr e s s ur e o f four

pounds or even less .

O TH ER A PP ARA T U S .

35 6 . E thoroughly
a r th e nw ar e
p glazed and acid
o ts , proof are ,

indispensable They can be procured o f all s izes from 5 l iters to

.

3 0 0 liters or even
,
larger The y are used for solution
. filtration , ,

precipitation washing c rystall ization etc

, , ,
.

Wooden vessels ( tubs and barrel s ) may b e u sed for some spe
c i a l prepa rations made on a large scal e .

Glass and porcelain precipitation j ars and w ide mouthed bot -

tles are employed for smaller operations a n d for still smaller ,

'

quantities E r l e n m aye r flasks and beakers .

357 . Porcelain c as s e r ol e s with handles preferably o f wood , ,

ar e most serviceabl e when o f about I liter s capacity

’
Porcelain .

“ ”
or white ware pi tc h e r s may also be used to a considerable extent
for trans ferring l iquids from one vessel to another but not so ,

conveniently as casseroles for h ot liquids .

Tinware cli ppe rs ( well tinned ) may be used for many purposes
in the laboratory .

35 8. B ot tl e s for both solids and l iquids glass stoppered as well ,

-

as others are required in plent y Glass stoppered s o called

, .
- -

“ ”
tincture bottles for acids and other solutions may be used
, ,

as lar g e as o f 1 2 liters capacit y with great advantage i f large ,

quantities o f the liquids a re employed ; but larger bottles are les s

convenient a n d more l iable to breakage .

35 9 . E vapora ti on di s h e s have been su fficiently described in

Chapter VI I crys ta l li z e rs in Chapter I X and m or ta rs a nd pe s tl e s
, ,

in Chapter I .

F u nn e ls for fi l t ra t i on s for collecting and washing precipitates

,

and cry stals and for other purposes have been described in the
,

chapters discussing thos e operations and fl as ks r e t or ts beakers , , , ,

w as h bot tl e s and other requisite glassware including tubing and

-
, ,

fittings were also mentioned to a su fficient extent in preceding

,

chapters S ome apparatus will be more specifically described in

.

Part I I as occasion requires .

S ieves s patulas scoops spoons strainer holders iron stands

, , , , , ,

hammer and anvil cork borer files tongs knives shears and
, , , , , ,

many other implements and tools are needed in laboratories .

 F URN IT URE AND A PP ARA T U S . 1
95

The catalogues o f dealers in chem ical and pharmaceutical a p

parat u s should be consulted for further in formation and detail s .

S uch catalogues are abundantly illustr at ed .

360 . In the training laboratories o f pha rmaceutical an d other

technological schools it i s customa ry to have large water baths -

and sand baths drying closets fume chambers and balance room
-
, , ,

for general use by all students and to is su e t o each student a set ,

o f apparatus for his indivi dual u se and specia l apparatus as r e ,

quired .

361. A n ou tfi t of appa r a tu s su ffi ci ent for the production o f

experimental quantities o f the great maj ority o f the preparations
included in Part I I o f this volume but not including prepa rations ,

requiring special apparatus m ay be as follows ,

A n iron stand with heavy bas e and three rings o f di ff erent sizes
( respectively o f 7 5 1 0 0 and 1 2 5 millimeters
'
d,
iam eter )
“
on the rod ( retort
O ne copper water bath I 5 0 millimeter s diamet er with three
-
, ,

ings and with two opposite handles

r
,
.

O ne R ussia iron dish 1 5 0 millimeters d ia met e r and 2 5 mill i

—
,

mete i s deep for a sand bath ,

-
.

A gas bu rner ( or in its place a coal oil burner or a sp irit

, ,

lamp ) .

O ne N o 4 or 5 mortar an d pestle
. .

O ne or two mm porcelain evaporatin g dishes ( M eisen or

B erl in ware
O n e or two graduated glass measu res on foot each of about , ,

2 0 0 Cc capacity ( metric glass

.

T wo or three thin glass beakers o f about 2 5 0 Cc capacity , . .

O ne glas s flask with wide neck o f medium length and flat bot
tom capacity 6 0 0 Cc
,
.

O ne roun d bottom glas s flask 6oo Cc , .

O ne round glass ( or porcel ain ) dish about I 5 0 millimeters ,

d iameter and 3 5 to 5 0 millimeters deep for u se as a ,

c rystall izer .

O ne 1 5 0 mm glass funnel 60 angle w ith long stem h aving ,

°

bevel ed end .

O ne 1 0 0 mm glas s funnel o f same kind .

O ne E l e nm e y e r flask o f 5 0 0 Cc capacity . .

O ne E l e nm e y e r flask o f 3 0 0 Cc capacity . .

O ne E l e nm e y e r flask o f 2 0 0 Cc capacity . .
1 96 F URN IT URE AND A PP ARA T U S .

O ne E l e nm e ye r flask o f 1 0 0 Cc capacity . .

O ne E l e nm e ye r flask o f 5 0 Ce capacity . .

O ne wi de mouthed 2 l iter bottl e

- -
.

Two wide mouthed I liter bottles

- -
.

Two wide mouthed hal f liter bottl es

- -
.

A dozen 1 50 mm test tubes -

.

O ne double ended 1 5 0 mm horn spatula .

Hal f a dozen glass stirring rods assorted s izes 1 5 0 to 3 00 , ,

millimeters .

T w o packages o f coarse ( rapid filte ring ) filter paper S S .

or S wedish or French ) to fi t the 1 5 0 mm funnel

, .

O ne package o f the same kind o f filter paper to fit the 1 0 0

mm funnel .

Corks t ap e r i n g X X X extra lon g assorted sizes

, , , , .

This outfit wil l enable the student t o m a k e moderate quan

’

tities o f nearl y all the chemicals mentioned in this manual For .

the remaining preparations a few additional pieces o f apparatu s

are requi red such as retorts wash bottles glass tubing rubbe r
, , , ,

tube connections thistle tubes per forated rubber stoppers etc

, , , .
1 98 L A R OR A T O R Y RULE S AND P RE CAU TI ON S .

location where the least danger would result f rom t h e i r being ~

broken E arthenware vessels may be placed und er the stand to

.

catch escaping acids in case o f breakage of a carboy When bot .

tles are fill ed from t h e c a rboy s special acid syphons o f glass

, ,

should be used in order that the carb oy may be le ft undisturbed

in its position and to avoid as far as pos sible all danger o f , ,

spilling .

Whenever a carboy of acid is broken immediate steps must ,

be taken to prevent any greater destructio n than i s unavoidable .

The escaped or escaping acid must be caught up in a j ar or d ish

i f possible or neutralized as far as possibl e with sodium carbo n
,

ate which shoul d be a t all times kept near by for this pur p ose
, ,

and pl enty o f water shoul d be turned or poured upon the a c id

to dilute it I n Order that thi s may be done quickl y and with
.

out hesitation or danger the acid carboys shoul d stand in a place

,

W h ere the floor is covered with asphalt an d inclined toward an

ample drain connected with the sewer and near the h y drant wa t e r .

3 64
. S hould the acid be s u lph u r i c a ci d remember that the ,

ad d ition o f w ater will caus e the gen e ration o f great heat and
steam an d that the m ixture will be liable to boil and spa tter
,

a bo u t especiall y i f the quantity o f water added is comparatively

,

limited It is therefore best to allow the acid to run off unle s s

.
, ,

it can be caught in a large earthenware pot or dish Then soda .

must be used freely and a c opi ous supply o f water .

36 5
. I f hy d ro c hl or i c a ci d escapes in la rge quantity from any
broken vessel throw pl ent y o f sodium carbonate upon it tog et her
, ,

with much water and i f the a i r gets filled with t he irritating vapor
,

scatter some ammonia water about the place so that the vapor
o f ammonia m a y neutralize that o f the acid .

3 66 . N i tr i c a ci d i s more destructive than any o th er It not .

on ly att acks wi t h great vigor any organ ic matter with which it

comes i n c on t ac t but as it does so it fill s the air with su ff ocati n g

, , ,

red nitrous vapors Fire and explosions are l iable to be caused

.

by the action o f nitric acid on wood especially i f the wood i s ,

resinous S awdust which is so e ff ective in absorbing or d inary

.

l iquids should never be thrown upon acids especial ly n itric acid , .

When a l ar ge amount o f nitric acid has escaped ammonia should ,

be freely u sed to neutralize the vapor while soda should also be

util iz e d and an abundance o f water
, .

I n a cc i d e nt s o f this nature the fire hose s h ould be u s ed . .

 L A R OR A T O R Y RULE S AND P RE CAU TI ON S . 1 99
.

367 . When small quantities o f strong acids are spilled or

scattered about they should be immediately neutral ized diluted
, ,

and wiped up The eyes and clothing o f l a bora n t s and especially

.
,

o f careless an d inexperienced beginners are sometimes destroyed ,

by acids The greatest care should therefore be exercised when

.
, ,

ever any strong acid is us ed for even a drop O f it may eas ily do ,

very serious damage A drop or two o f concentrated acid on . _

the floor i f stepped upon will eat through the shoe leather ; on
, ,

the table it may not only make holes in the clothing but may ,

find its way to hands face and e y es , .

D ilute aci ds are al so destructive ; they must be cautiousl y

handled and immediately neutralized and thoroughly washed o ff
when spilled .

368. S trong acids shoul d never be directl y mixed with strong

alkal ies except in case of the escap e o f large quantities o f the
acid as described and then only when plenti ful additions o f
,

water are at once thrown upon the aci d and it is dangerous to ,

be t oo near the spot where the aci d and alkal i are m ixed or to
face it for the temperature o f the reaction is sure to cause the
,

l iquid to spatter about .

When it is neces sary in laboratory operation s to mix a stron g

acid and an alkal i both should be as diluted a s the circumstances
requ ire an d they should be cautiously and g r a d u al ly m ixed i n a
,

capacious vessel .

3 69
. Water must never be added to strong sulphuric aci d for
the result i s liabl e to be disastrou s from the violent reaction
which m ay throw considerabl e portions o f the acid out o f the
vess el in all directions When it i s necessary to d ilute con .

c e nt r a t e d sulphuric aci d the aci d must be s lowly added to t h e

water a s described in the proper place in this book T h e addi .

tion O f water solutions o f alkal ies ammonia alkal i carbonate s

-
, , .

and som e other compounds o f the alkal i metal s i s even more dan .

g e r o u s than the addition o f water alone to strong sulphuric acid .

A ll water solutions and also alcohol ic l iquids act in a s imilar

-

manner when added to concentrated sulphuric acid .

3 70
. S tock bottles containing acid s must be s t rong glass stop -

pered bottl es and not too large,

.

Bottles containing volatile acids such as nitric acid hydro , ,

chloric acid and ac e tic acid must not be entirel y filled unless kept ,

in a ver y cool place and when t h e bottl e i s mor e than h al f filled

,
 OO . L A R OR A T OR Y RULE S AN D P RE CAU TI ON S .

with such an acid the contents should be cool when the bottle is
’
opened and the operator s face shoul d be turned away because ,

i f the acid i s not cool there may be when the stopper is removed
, ,

an out rush o f acid vapor great enough to do inj ury to the eyes
-

and the respiratory organs .

371 A ll acids shoul d be kept in a cool place

. .

372 When a drop or more of dilute acid acci dentally gets on

.

the clothing a littl e dilute ammonia shoul d be applied .

3 73 A l k al i e s are not so dangerous as the strong m ineral

.

acids but they are corros ive enough to do a great deal of damage
,

i f allowed to come in contact with organ ic matter They destroy .

clothing and eat into wood When strong lye i s spilled it shoul d
,
.

be at once diluted with pl enty o f water the dilute li quid w i ped ,

up very dilute sul p huric or h y drochloric acid next applied and

, ,

finally more water .

3 74 B ottles containing solutions o f potass i um hydroxide

.
,

sodium hydroxi de or ammonia mu st be strong glass stoppered —

bottles ; and bottl es containing ammonia solution must not b e

ent i rely filled must be cool when opened and opened cautiously
, , ,

the face o f the operator bein g averted a s in the case o f opening

bottl es containing volatil e acids L oss O f eyesight has resulted
.

from opening filled and not su fficiently cool bottles o f strong a m

mon ia water owing to the g reat rush o f gaseou s ammonia from
the container .

375 When solid K O H or N a O H i s to be dissolved in water

.

it i s best to add the alkal i to al l o f the water an d to add it ,

gradually i f the solution i s to be a concentrated one Great evo .

l u t i on o f heat attends the solution o f the strong alkalies in water ,

probably due to condensation caused by mol ecular combination .

376 The glass stoppers o f bottles containing solutions o f

.

K O H or N a O H must be coated with petrolatum “

U nless this .

is attend ed to it usually happ ens that the stopper become s so firmly

cemente d to the neck o f the bottle by the chemical action o f th e
alkal i upon the ground sur faces of the glass that the removal
o f the stopper i s impossibl e and the neck o f the bottl e must be
cut or broken O ff in order to recover the contents .

37 7 B romi n e is a terribl e substance to deal w ith i f allowed to

.

escape It rapidl y evaporates and fill s th e room with its vapor

.
,

which i s so irritating and destructive that it can not be inhaled

without grave danger and it attacks the e y es severel y It also
, .
20 2 L A R OR A T O R Y RULE S AN D P RE CAU TI ON S .

floor near the bromine in order that the vapors o f the H 3 N an d

th e B r may neutralize each other
2
.

I f l iq uid bromine i s allowed to act upon any part o f the body

it may quickl y produce serious wounds wh ich are not only very
pain ful but qu ite di fficult to heal .

The vapor attacks the eyes and face and the respiratory o rgans .

S houl d the e ff ects be so severe as to requ ire alleviation a littl e

a mmonia vapor may be v e r y c a u ti ous ly inhaled from diluted a m

monia water and the face and eyes freely bathed with col d water
, .

3 78 . Ph osph oru s and al so the m etal s potass ium and so d ium

, ,

a re fi r e dangerous
-
.

Ph os ph oru s mu st be k e pt in water contained in glas s stop -

pered bottles in a safe place When required for use it must be .

-
handled and divided i n water or in a moist condition and it can ,

n ot be with sa fety wiped dry for weighing S hould it ignite

. .

it must be at once thrown into water I f i gnited while held in .

the hand or between the fingers it may caus e severe wounds .

P otas s i u m an d s od i u m must be kept in a l iquid hydrocarbon in

tightly stoppered bottl es T hey ignite when expo sed to the ai r
.

or come in contact with water .

3 79 .E th e r petroleum spirit ( benzin ) an d other i nfl ammabl e

,

l i qu i d s must be kept in strong tightly closed containers ( not ,

filled ) in a cool place away from any l ight or fire and when
, ,

re quired for use they shoul d not be brought near any flame I t .

must always be remembe red that the vapors o f inflammable vola

tile liqu ids may be conveyed through and wi th the air and be
come ignited by a flame a cons iderabl e distance from the vessel
c ontaining the liquids E xtraordinary precaut i ons mu st be taken
.

t o prevent fire when any distillation or other o p eration is per

f ormed in which a volatile inflammable liqu i d is h eated A ll s uch .

operations shoul d be performed on the fir e table near the sink

and in such manner t h at th e inflammable vapor can not c ome in
contact with the flam e i ndirectly or directly supplying the heat .

I n fl a m m a bl e v a p ors f or m ex pl os i v e m i x t u r e s w i t h ai r .

3 80 . in a laboratory may be caused not only by s tron g

F i re
acids phosphorus ether and other i n fl amm abl e s and explosives
, , ,

bu t more easily than el sewhere from the careless handling o f

matches and heating apparatus because heat is s o constantly ,

util ized S trict discipline in this direction is accordingl y i m

.

p e ra t i ve .
 L A R OR A T O R Y RULE S AN D P RE CAU TI ON S . 20 3

M atche s mu st be kept in a sa fe place Gas shou ld never be .

le ft burning except wh en necessary Water baths shoul d never .

-

be permitted to become em pty while in u se .

Whenever the laborato ry is abou t to be closed for th e n ight ,

or temporarily d eserted at any time a ca reful insp e ction must be ,

m ade to see t h at no flame o f any kin d is l eft burning and n o

o p eration continued which is l iable to prove dangerous or to cau se
any inj ury or loss by fire explos ion or any damage t o materials , , ,

or to pr oduct s in pr ocess o f preparation .

In the training labo ratories o f technical school s the employment

o f common large sand baths and water baths for the us e o f the
- —

cl asses dim inishes the l iabil ity to da nger and damage by rendering
unn ecessary the constant u se o f gas burners as well as by sub
s t i t u t i ng the far sa fer baths for m a ny operations in which i n

fla mm abl e Substanc e s are employed .

O perations and experiments involving danger can be en ti rely

avo ided in co llege labo ratories an d the risks o f accid ents be t hus ,

reduced to such as may happen anywhere as t h e result o f g ross

carelessness or stupidity .

38 1 . I n al l laboratory wor k the operat ors s houl d k ee p a

:

j o u r n a l o r record o f every o peration and o f each important step

in it T o save tim e it i s generally advantageous or even n e ce s
. .

sary to keep t w o three or even more preparations und er w ay

,

con currently .

A l l ves sels contain ing either material s unfinished products or , ,

fin ish ed products must be l abe l e d so explicitly t h a t no mista ke

can be made To leave any subs ta nce or mixture or s olution
.
, , ,

unlabe led trusting to m e mor y to know what it is must be r e

, ,

garded as inadmissibl e in a laboratory N othing shoul d be l e ft

’

unlabel ed for even an hour T he label on the vessel shou l d not .

only indicate plainly what it contains but wha t the contents are to
be used for the d a te a n d a ls o the nam e o f the labo rant ha ving
, ,

the matter in han d .

N ote s should be made i n the lab ora tory j ournal o f all prepa ra .

t ions made date when commenced material s u s ed and quantit ies

, ,

o f them m et hod adop ted ( i f there i s a choice ) any interestin g

, , ,

instructive or important observations made in regard to the

results t he date on which the preparation is finished the quan
, ,

tity o f product ob ta ined and its character or qual ity and what ,

w a s done with the by e product i f anythi n g -

, .
20 4 L A R OR A T O R Y RULE S A ND P RE CAU TI O N S .

3 82. in finishing the op e rat i ons u n d e r

U nn e ce s sar y d e l a y
taken in the laboratory is very l iable t o caus e loss or waste o f
material s as well as o f the tim e an d labor already be s t ow n This .

appl ies to analytica l processes as well as t o the production o f

chemical preparations N o preparation shoul d be started at an
.

hour when it woul d be impracticabl e to give i t the attention

necessary to carry the process up to a point at which furthe r a t
tention may be deferred without d isadvantage or risk .

U nfinished products especially i f moist are generally more

, ,

liabl e to decomposition or damage from exposure than fini shed

preparations .

3 83 . H ow t o c l e an ap p ar a t us A ll laboratory apparatus and

.

implements as well as the fu rniture must be k e p t clean O pera

, ,
‘

.
:

tors w h o do not clean -their apparatus an d utensil s thoroughly and

keep them in perfect order and ready for u se an d w h o leave t h e ,

table in d isorder soiled or w e t are wholly unfit l aborant s

, , .

E very p iece o f apparatus should a fter using it be as thoroughly

'

, ,

cl eaned a s any dish plate or tumbler set before properly fastidious

,

p ersons at the dinner table .

But chemical apparatu s an d especially mortars and pestl es

, ,

require at times chemical agencies to clean them particularly i f ,

they have been permitted to remain long in contact with sub

stances which act upon them chemically or which are absorbed .

“ ”
D irt i s only m isplaced matter an d even pharmacists a n d
,

chemists are apt to recognize or notice only colored dirt B ut .

white or colorl ess dirt is quite as obj ectionable and sometimes

more so than the more obtrusive kinds Hence all chemical an d .

pharmaceutical apparatus must be scrupulously cleaned and

rinsed .

Insolubl e substances rubbed into th e pores o f mortars an d

pestles or adhering to glass an d glazed surfaces should be con
verted into soluble substances to facil itate their removal Thus .

iron stains may be removed with the aid o f nitric acid or hydro
chloric acid or i f necessary both togethe r ; insoluble mercury
, , ,

compounds are removed with nitric acid ; antimony compounds

with s tr ong hydrochloric acid ; iodine stains with potash solution ;
organic extr ac tive with strong potash sol ution ; arsenic and its
compounds with strong nitric acid ; silver compounds with stron g
ammonia or with nitric acid or the two used alternat ely ; l ead
,

compounds with n itric acid etc , .

 RT

O R A TO R Y M A N U A L O F I N O R G A N I C
C H E M I CA L PR E PA R A TI O N S .
210 I N T RODU CT OR Y .

to s om e so selected that the product obtained from each

e x te n t

m a y serve as one o f the materials for the next lesson The stu
.

dent may for instance first be given the iron and sulphuric aci d
, ,

to make ferrous sulphate ; he may then make not only ferrous

sulphate in large crystal s but also t u rbi d a t e d and precipitated fer
,

rou s sulphate dried ferrou s sulphate ferric sulphate ferric sub

, , ,

sulphate ferric hydroxide ferric p y r op h os ph a t e f e r r i c citrate

, , ,
'

etc He may be furnished the materials for t h e preparation o f

.

sodium phosphate and then make several phosphates an d pyro

phosphates from the same material s It i s also use ful to requir e
.

students to recover the bye products wherever practicable and

-
,

to accou nt for the materials furni sh ed them by producing as l arge

a yield o f each product as may be practically obtainabl e .

The directions an d notes are su fficiently explicit to enabl e i n

dividual students as wel l as other l abo ra n t s to do the work suc
c e s s f u l l y and s a t i c f a c t or y results are certainly unattainable with

out such explanations as can not be repeated to each individual

student .

The work ing formulas incl uded in this work are applicable not
-

only in the practice laboratories o f technical schools but a l s o ,

i n the laboratories o f manu factu ring pharmacists an d chemists .

 W EI G H T S AN D M EAS U R E S .

A ll weights and measures in u se in the U nited of S tates

A merica are derived from the metric prototypes in the custody
o f the O ffice o f S tandard Weights and M easures at Washin gt on .

The prototypes referred to are the U S N ational Prototype . .

S tandard M eter and the U S N ational Prototype S tandard . .

Kilogram both made o f iridium platinum and furnished to the

,
-

A merican Government by the I nternational Bureau o f Weights

and M easures in 1 890 .

The ol d customary weights and measures as well as thos e

‘

o f the m etric s y stem are based upon and adj usted to the material
,

metric standards mentioned .

TH E M E T R I C S Y S T EM .

T he me t er is the length o f iridium platinum prototype meter at-

Washington .

1 meter is equal to 1 0 decimeters .

I m eter is equal to 1 00 centimeters .

I meter is equal to 1 0 0 0 m illimeters ( mm ) .

Th e k i l ogr am is the mass o f t h e iridium platinum prototyp e -

kilogram at Wash ington .

I kilogram is equal to 1 0 0 0 gram s ( Gm ) .

1 gram is equal to 1 0 0 0 m illigrams ( m ) .

The l i t e r i s the vol u m e of one kilogram o f pure water at 4 C °

.

in va c u o.

1 liter is equal to 1 00 0 milliliters ( ml ) .

[ T h r e ti c a l l
°
e o
y the volume o f 1 kilogram o f pure water at 4 C .

i n va c u o is I cubic decimeter ; but the liter in actual use being

-
,

always obtained by weight can not consistently be called a cubic

,

decimeter especially as it seems probable that the actual lite r

,

measures less than a cubic decimeter ] -

.

I cubic decimeter i s equal to 1 0 0 0 cubic centimeters ( Co )

- —
.

1 A merican yard is meter .

1 A merican commercial pound i s kilogram .

1 A merican liqui d gal lon is th e volum e o f Gm o f

pure water at 4 C i n va c u o
°
.
 W AT E R .

AQ UA .

H 20 2 18 .

The Pharmacopoeia of the U nited S tates defines aqua as

”
natural water in its purest attainabl e s tate I t must be color .

less clear i nodorous and tasteles s S houl d not contain more

, , ,
.

than 1 00 milligrams o f fixed impuriti es in one liter and not more ,

than trace s o f organ i c matter .

S pri n g w at e r usually contains inorganic salts cons isting chiefly ,

o f the chlorides sulphates and carbonates o f calcium mag

, ,

n e s i u m etc S uch water i s called h a r d w a te r because when used

, .
,

with soap it produces insoluble compounds which cause a sense ,

o f harshness Hard water can be rendered les s so by boiling it

.
,

because the calcium and magnesium carbonates which are hel d ,

in solution by the carbonic acid present depos it a s soon as that ,

acid is expelled by the heat S pring water i s generally unfit for .

pharmaceutical uses on a cc ou n t o f the m ineral impurities it con

.

tains .

W e l l w at e r o ften contains organ ic matter derived from s e w

age etc especial ly in thickl y inhabited places and must not be
, .
, ,

used unl ess careful examination shows it to be su fficiently pure .

Water contam inated w ith organic substances contains ammonia .

The presence o f organic matter in su fficient quantity to impa rt

odor to the water shoul d at once condemn it Where pure water .

is not obtainabl e for ordinary purposes small quantities o f organic ,

impurities may be partially removed by adding a l ittle alum ; the

ammonia and carbonates present caus e the precipitation o f
aluminum hydrate which as it s ettles carries other impurities
, , ,

with it .

R ai n w at e r is pure i f coll ected in clean vessels as it descends

from the c lbu d s a fter the rain has continued long enough to
puri fy the atmosphere from dust etc F alling o ff roo fs and col , .

l e c t e d from the condu its in the usual w a y it i s rarel y pure

I ce when melted a ff ords a comparatively pure water
, ,
.

21 2
21 4 W A T ER .

W ith a l ittle potassium permanganate and then W ith alum The .

first portion o f the d istillate should be rej ected a s lon g as it does

not hold the necessar y tests .

D istilled water may be kept in large bottles the necks o f which

“ ”
are closed by l oos e plugs o f pure cotton ( absorbent cotton ) i n
stead o i glass stoppers .

Te st s . S houl d yiel d no residue on evaporation . I n applying

the permanganate test described above to distill ed water t h e ,

rose red tint should not onl y remain a fter five m inutes boiling
-
’
,

’
but should not be entirely destroyed even a fter ten hours stand
,

ing in a covered vessel subsequent to the boiling .

I t should not be a ff ected by test solutions o f barium chloride

—

( p
s u l h a t e s ) s ilver
,
nitrate ( c hl or i d e s,) ammonium oxalate ( ca l
ci a m ) ,
or mercuric chloride with or W ithout the subsequent addi
tion o f potass ium carbonate ( ammonia and ammonium com
pounds ) .
 A CI D S .

Caution in the handl i ng and use o f acids has been ur g ed in th e

chapter devoted to l aborat orv rules and precautions The most .

su itable containers for con stant use in the laboratory are the
“ ”
common glas s stoppered aci d bottles o f about two l iters c a
p a c i t y .

The removal o f the glass stopper which has become fast in the
neck o f an aci d bottle is attended with risk Gently tapping th e
.

stopper with a wooden block or stick warming the neck o f the

,

bottle with a cloth dipped in hot water or by cautiously rotating

it whil e held over the flame o f a gas burner or spirit lamp and ,

inverting the bottl e in a vessel containing enough warm water to

m
cover the whol e bottle neck are a ong the best means o f loosen
-
,
;

ing the stopper su fficiently to render the application o f t h e

stopper wrench success ful A block o f wood with a deep groove
.

in the center is an e ffective stopper wrench I f the bottle is .

nearly filled and the aci d volatile ( as nitric hydrochloric or ,

acetic acid ) and concentrated the face should be turned away

,

when the stopper is removed .

The acids o f di fferent manu facturers and d i ff erent pharma

c op oe i a s are not o f uni form strength It is there fore important
.
, ,

that the laborant shoul d know the particular stren gth inten ded
by the d irections or formula followed and the stren gt h o f the
,

acid he actuall y emplo y s in order that the quantities or proportions

may be adj usted as the circumstances may requi re The em .

ployment o f acids which are stronger or weaker than thos e pre

scribed by the manual is o ften practicabl e i f the quantities be
modified accordingl y ; but in many cases the particular strength
prescribed can not be altered without disadvantage or failure .

A s the acids are so many and so extensively used and as many ,

metall ic salts of the organic acids must necessarily be included

in any such manual as this all o f the common acids organic as
, ,

well as inorganic are placed together in alphabetical order under

,

the general head o f acids before the other compounds are de

scribed .
216 A CI D S .

A C E TI C A CI D .

A CI DU M A CE T I C U M .

Formerly prepared by acetic fermentation o f dilute al c ohol ,

or o f weak saccharine liqu ids It is now made by dry distillation

.

o f wood O akwood billets are heated in closed sh eet iron c y li n

.
-

ders one o f the numerous products being impure acetic aci d or

, ,

w ood vi n e g ar which is a fterwards purified

,
.

The impure acetic acid obtained by the destructive d istillation

o f wood is called p y roligneous acid and has a disagreeabl e smoky ,

Odor from the empyreumatic products contained in it E ven .

some o f the better grades o f acetic aci d con tain empyreumatic

matters and only chemically pure acid is entirely free from them
,
.

To get ri d o f thes e impurities the aci d i s treated W ith l ime and

soda the acetates o f calcium and sodium are freed from the tarry
,

matters and then decomposed by sulphuric or hydrochloric acid

,
.

A nearly pure acetate o f sodium can thus be made from the impure
acid an d by distil ling a m ixture o f thi s sodium acetate with sul
,

p h u r i c acid a purer grade o f acetic acid is obtained which can ,

be further purified by again neutral iz ing W ith sodium carbonate ,

decomposing the acetate with sulphuric aci d and distilling as ,

before A pure sodium acetate is finally Obtained from wh ich

.
, _

pure acetic acid may be made as follows

S odium acetate
S ulphuric acid

R educe the acetate to a coarse powder ; introduce it into a dis

tilling flask ; warm the flask ; connect it w ith a condenser an d
receiver ; add the sulphuric acid through a funnel tube a littl e at ,

a time and continue the distillation until 1 2 parts o f distillate

,

have been collected .

Test the produ ct with volumetric test solution o f potassium -

hydroxi de to determine its strength and then dilute as required .

Pr op e r t i e s . A solution composed o f 3 6 per cent of h y drogen

acetate and 6 4 per cent o f water .

A cl ear colorless liqu id o f a disti nctl y vinegar like odor

, ,
-
,
'

a
218 A CID S .

To neutralize 3 Gm o f glacial acetic acid shoul d require not

less than ml o f normal solution o f potassium hydroxide ( cor
responding to at least 99 per cent o f absolute acetic acid )
A t low temperatures it crystallizes into an ice like mass and -
,

when it onl y partially congeals it has the appearance of a s u p e r s at

u r a t e d solution .

When glacial acetic aci d is diluted with water its specific gravity
increases with a simultaneous fall in temperature until the m ix
ture contains about 77 to 8 0 per cent o f hydrogen acetate U pon .

the further addition o f water however the specific gravity de

, ,

creases an d the temperature o f the mixture rises A n acetic aci d o f .

47 per ce nt strength has the same specific gravity as the ofli c i a l

glacial acetic acid which is more than twice as strong
,
.

The corrosive nature o f glacial acetic acid renders it n e ce s

sary to be very cautious in handl ing it especially in removing ,

the stopper from a full bottl e which has been standing in a warm
place as vapors o f the acid are l iable to is sue from the bottle w ith
,

a rush at the moment the stopper is removed .

Glacial acetic acid is a remarkably e ff ective solvent for resins ,

volatil e oil s glucosi des alkaloids and many other organic sub
, , ,

stances I t also dissolves normal bismuth nitrate

. .

B E N Z O I C A CI D .

A CI DU M B E N Z O I CU M .

HC7 H5 0 2
: 1 22 .

B enzoic acid i s contained in benzoin to the extent o f from 1 0

to 1 9 per cent and may be obtained by subl imation The benzoin .

i s coarsely powdered and spread in a thin layer on a flat tinned

i ron pan This pan for 5 0 0 Gm o f benzoin ought to be about
.
, ,

3 00 mm in diameter and about 35 mm deep A sheet o f porou s .

paper i s fastened over the pan a fter which a cone or dome o f

,

thick paper i s tied securely around the edges o f the pan Th e .

apparatus i s then placed on an iron plate covered with a thin layer ,

o f san d Heat is now applied gradually until th e odor o f benzoic

. .

, ,

acid becomes quite noticeable through the paper but the tempera ,

ture must not be raised too high for the product will then become
,

fu s e d and discolored .
 A CID S . 219

Benzoic acid can also be made by the wet way : boil ing benzoin “

w ith calcium or sodium hydroxi de and decompos ing the benzoate ,

o f ca l cium or sodium with hydrochloric acid S odium carbonate .

may also be us ed :

B enzoin .

S odium carbonate
Hydrochloric acid su fficient , .

D igest the benzoin with the sodium carbonate previously d i s ,

solved i n 1 0 parts o f water for three hours at about 60 C Then

,
°
.

boil the m ixture a few minutes filter and neutralize with hydro , ,

chloric acid Collect the precipitated benzoic acid an d puri fy it

.
,

by dissolving it in 2 0 times its weight o f boil ing water digesting .

the solution with a l ittle animal c harcoal filtering concentrating , ,

the solution by evaporation and crystallizin g , .

Benzoic acid i s now manu factured c hi e fl y from toluol ; but al so

’

from hippuric acid and from naphthalin This artificial benzoic .

acid is generally pure chemically but di ff ers from pure natural

, ,

b enzoic acid by being more compact and inodorous N atural .

benzoic acid o btained from benzoin by subl imation is very so ft ,

and bulky an d is fragrant B enzoic aci d prepared from benzoin

, .

by the w e t process is however scarcely fragrant The a g reeable

, ,
.

odor o f sublimed benzoic acid s eems to be du e to ethyl benzoate ,

or to some volatile oil or both existing in the resin and aeco m

, ,

panying the aci d when subl imed The fragrant benzoic aci d pre .

pared from benzoin by sublimation i s the only kind prescribed by

several pharmacopoeias .

In the trade the natural benzoic acid is styl ed as E n g l ish and ,

the artificial as German Benzoi c A cid

“ ”
.

Benzoic aci d has marked antiseptic properti es and a solution ,

o f one part o f benzo i c ac i d and one part of borax in I OO parts o f

water i s o ften employed The bora x aids the solution o f the
.

benzoic acid .

B enzoic acid must be kept in tightly closed bottl es i n a c ool ,

place and well protected against light

, .

D e scri pt i on —
N a tu r a l
( that prepared from S
be nz oi c
iam a ci d

benzoin by sublimation ) i s white or yellowish white in scales or ,

needles o f silky lustre and has an agreeable benzoin l ike odor

,
-

an d a somewhat pungent taste M elts at .

2 20 A CID S .

i s white consists o f lustrous needles i s

A r ti fi c i a l be nz oi c a ci d , ,

odorless and has a warm aci d taste M elts at

, ,
.

B enzoic acid is soluble at 1 5 in about 4 0 0 parts o f water and in

°
,
i

2 parts o f alcohol ; in 1 7 parts o f boiling water and in I part o f ,

boiling alcohol ; also in to 3 parts o f ether and in 1 0 parts o f

glycerin I t is also soluble in fixed and in volatil e oil s
. .

B O R I C A CI D .

A CI DU M B OR I C U M .

H sB O3 =6 2 .

Borax in powder ,

N itric aci d
D istilled water .

D issolve the borax in 2 50 parts o f boil i ng d istilled water and ,

filter wh ile hot A dd the acid to the hot filtrate and stir S e t
. .

aside in a cold place for a d ay .

Collect the crystal s on a musl in or paper filter an d wash them

with a small quantity o f col d distilled water .

R e dissolve the washed crystal s in 2 00 parts o f boilin g distilled

-

water an d set the solution as ide until quite col d

, .

Place a loos e layer Of clean cotton in the throat o f a glas s fun

nel and collect the crystal s upon it D rain thoroughly Trans fer . .

the product to a dry musl in cloth or a sheet o f bibulous white

paper spread it out an d dry it in a moderately warm place
, ,
.

R e act i on .

+ 2 N aN O 3 j 5H ZO
— -
.

N ot e s . I t will be s een that

parts o f borax requires 2 003 8 1

parts o f nitric aci d o f 6 3 per cent stren gth A sl ight excess o f .

acid is however necessa ry ; hence 5 8 parts is or d e re d i n s t e a d o f

, ,
‘ ’

55 for 1 0 0 parts o f borax N itric acid i s preferred

. to h y drochloric
acid because sodium n itrate i s more readily soluble than sodium
chloride S ulphur i c acid i s not employed becaus e it is not so read
.

ily washed out .

,

The yiel d is theoretically about two thirds o f th e weigh t of —

.
,
2 22 A CI DS .

R e a ct i on .

N ot e s I f the materials are pure and i f n o foreign organic

. ,

matter be permitted to get into the d ish the product will be per ,

f e c t l y clea r and colorless The heat applied should not be greater

.

than necessary Boroglycerin i s a remarkably tenacious sub

.

stance which whil e warm can be d rawn into slender threads o f

, , ,

great l ength I t i s readily solubl e in water in alcohol and in

.
, ,

glycerin .

Gly c e r i tu m B or og ly c e r i n i ; U S .

A glycerin solution o f glyceryl borate ( boroglycerin or boro

-

glyceri de ) i s ordered by the Pharmacopoeia prepared as follows ,

'
Boric acid ,
i n fin e powder 3 1 Gm
Glycerin .

Heat 6
Gm o f gl y cerin i n a tared porcelain dish to not over
4
C ; add the boric aci d gradually and stir well When all
°
1 50 . .

of the boric acid has been added an d dis solved continue the heat , ,

stirring constantly to prevent the formation o f any film on the

sur face o f the mixture until the weight o f the contents o f the
,

d ish s h a l l have been reduced to 5 0 Gm Then add 5 0 Gm o f .

glycerin mix well and trans fer the p roduct to a suita ble con
, ,

t a i n e r which must be tightly closed

, .

N ot e s . The preparation i s a perfectly clea r colorless thick , ,

liquid . It is hygroscopic .

C I T R I C A CI D .

A CI DU M C I T R I CU M .

H 3 C6 H 5 O 7 H 20 :. 210 .

Contained in various plant j uices especially o f lemons l imes , ,

and Currants The j uice is allowed to ferment enough to d e c om

.

pos e the sugar Then follows clarification with albumen a fter

.
,

which the j u ice is treated with prepared chalk and the calcium ,

m
citrate deco posed with sulphuric acid

L emon jti i c e
Prepared chalk
S ulphuric acid
 A CI D S . 223

Heat the lemon j u ice to the boil ing point and gradually ad d the ,

chalk until it no longer causes e ff ervescence Collect th e deposit .

‘

on a muslin strainer and wash it with hot water till the filtered
liquid passes colorless M i x the deposited calcium citrate w ith
.

2 0 0 ml o f water and gradual ly add the sulphuric acid previously

,

diluted w ith 3 0 0 ml o f water Boil gently for hal f an hour keep

.
,

ing the mixture constantly stirred S eparate th e aci d solution by.

filtration wash the i nsoluble matter w ith a little distil led water
’

, . ,

and add the washings to the solution Concentrate this solution .

to the density o f then allow it to cool and a fter twenty four ,

-

hours decant the l iquor from the crystal s o f calcium sulphate

which have formed continue the evaporation of the solution until
,

a pellicle forms and then s et aside to cool and crystall ize I f

, .

neces sary pu ri fy the aci d by recr y stallization

,
.

R e act i onThe free citric acid in the lemon j uice i s neutral ized
.

by the calcium carbonate whereby calcium citrate i s formed

,

0 s o i') 2 + 5
2 H 3 C6 H S O 7 H 2O ) °
+3 C3 C 3
2 C3 3 Ce
H H 20 — —
l3 C0 2 .

When the calcium citrate is treated w ith sulphuric acid the fol ,

lowin g reaction occurs

C3 3 Cal 1 5 0 7 ) -

N ot e s . A small amount o f acid calcium citrate al ways remains

in the liqui d a fter the treatment with chalk This acid salt pre .

vents the precipitation o f coloring matter and a fter the removal ,

o f the neutral calcium citrate the aci d citrate can be decomposed

,

by milk o f lime yi elding nor m al citrate

,
.

The precipitated calcium citrate i s washed with warm water

until the washings are n early colorl ess A fter cool i ng it is de .
,

composed by sulphuric acid added in excess to prevent the forma

tion o f aci d citrate which would prevent crystall ization o f the
,

citric acid The calcium sulphate is washed and then thrown

.

away ; but the last o f the calcium sulphate does not separate until
the solution has been evaporated down to s p gr The final . .

evaporation to cr y stallization must not be ca rried too far as the ,

free sul phuric acid present woul d then blacken the product when
su ffi ciently concentrated to decompose the citric acid .

R ecrystallization i s neces sary to render the crystal s colorless

22 4 A CI D S .

and pure . S ometimes the solu tion must be decolorized by animal

charcoal .

D e scri pt i onColorl ess translucent prisms ; odorl ess ; having

—
, ,

an agreeable purely aci d taste ; e ffl ore s c e nt in warm air and

, ,

deliquescent when exposed to moist air .

S oluble at 1 5 C in part o f water and in parts o f

°
,
.
, ,

alcohol ; in about part o f boiling water and in parts o f ,

boiling alcohol ; also s olubl e in I S parts o f ether .

H Y D R I O D I C A CI D .

A C I DU M H Y D R I O D I CU M .

HI :

A solution o f hydriodic acid or d iluted hydriodic acid con

, ,

ta i n i ng 1 0 per cent o f hydrogen iodide may be prepared by a ,

process similar to that prescribed by the Pharmacopoeia for mak

ing the syrup with the exception that water is added instead o f
the same quantity o f syrup at the end ,
.

D iluted hydriodic acid i s a colorl ess odorles s liquid o f aci d ,

taste It shoul d be kept in glass stoppered bottles entirely filled

.
-
,

and placed i n a cool dark place I t is very unstable ; but may be

'

, .

preserved for a time with the ai d o f sugar .

T he offi c i a l

S y ru p o f H y d r i od i c A ci d

is made as follows

Potassium iod ide

Potassium h y pophosphite
Tartaric acid
Water
D iluted alcohol .

S yrup .

D issolve th e;
two potassium salts in water and the tartaric acid ,

in 2 5 ml o f diluted alcohol M i x the two sol ution s in a vial

.
,

shake it thoroughly an d place it in ice water for hal f an hour

,
-
,

occasionall y shaking Then fil t e r the m ixture through a small

. -
,
226 A CI D S .

connec t it with a well cooled receiver and d istill nearly to dry ,

ness A ssay the distillate and dilute it with enough distilled water
.

to make the final product contain 1 0 per cent o f hydrogen bro

m ide .

R e act i on . 2 KB r —
l

O th e r M e th od s .

Hydrobromic acid m ay al so be made from bromine and hydro

gen sulphide as described under the title o f A mmonium Bromide ,

and from potassium bromide with tartaric acid a s follows :

Potassium bromide
3 Tartaric acid
D istill ed water

D issolve the bromide and the acid separatel y each in , ,

parts of distill ed water Filter the solutions M i x them stirring

. .
,

well Filter out the cream o f tartar A ssay the solution and
. .

adj ust its stre n gth to 1 0 per cent .

V a l u a t i onTo neutralize
. Gm o f diluted hydrobromic
acid ( 1 0 per cent of H B r ) requires 1 0 ml of normal solution o f
potassium hydroxide E ach ml o f the volumetric test solution
.

corresponds to 1 per cent of hydrogen bromide Ph e n olp h t a l e i n .

i s the indicator u sed .

O ne ml o f normal solution o f K O H is the equivalent o f

Gm o f absolute H B r .

D e scr i pt i on clear colorl es s odorless strongly aci d l iquid

—
A , , ,

having a s p w o f about . . at
I t is to be kept in glass stoppered bottles in a cool dark place
-
, .

H Y D R O CH LO R I C A CI D .

A CI DU M H Y D R O CH L O R I CU M .

H CI : 3 6 4 . .

Hydrochloric acid is prepared by double decomposition between

sodium chloride and sul p huric aci d
 A CI D S . 2 27

N a C1+ H , s o and

T he hydrochloric acid o f the Pharmacop oeia o f the U nited

S tates contains per cent o f H Cl and has a s p w ; o f about .

at I t is a colorles s corros ive fumin g liquid o f s u ff o

, , ,

cating acid odor and intensel y aci d taste and reaction When
,
.

diluted with twice its volum e o f water the ac i d ceases t o give O ff

fumes and becomes o dorless .

“ ”
The acid styled G P in the trade usually holds the p harmaco
.

p oe i c a l tests a s to purity .

The customary fi ve pint aci d bottles hol d six pounds o f h y

- - -

d roc h l or i c acid .

The white vapors given off by strong hydr ochloric acid are due
t o th e d ifference in th e proportion o f moisture contained in the
ai r and in the acid a s well as to the formation o f ammonium
chloride when the aci d vapors meet ammonia in th e atmosphere .

V al uat i on To neutral ize

. Gm o f o fficial hydrochloric acid ,

diluted wi th 1 0 ml o f water should requ ire ml o f normal

,

solution o f potassium hydroxi de E ach ml o f this volumetric .

solution corresponds to I per cent o f absolute H Cl Ph e n olp h .

t a l e i n i s used as the indicator .

O ne ml o f normal solution o f p ota s s i u m hydroxi de i s the

‘

equival ent o f Gm o f absolute H CI .

A cti on on me t a l s D issolves
iron and z inc readily ; it al so acts
on n ick e l and alum i num an d warm aci d attacks tin Hydro
,
.

chloric acid does not attack platinum gold s ilver mercury lead , , , , ,

copper arsenic anti mony and bismuth

, ,
-

D il u t e d H y d r oc h l or i c A c i d .

Hydrochloric acid 1 00 Gm
D istill ed water 219 Gm

M ix them Keep the product in glass stoppered bottles

.
-
.

D iluted hydrochloric acid contains 1 0 per cent o f hydrogen

chloride .

S pecific gravity : about at 1 5 C °

.

I t does not fume in the a i r and i s without Odor but otherwise, ,

it corresponds in properties to hydrochloric acid .

To neutral ize Gm o f diluted h y drochloric aci d should r e

 A CI D S .

quire 1 0 ml o f normal potass i um hydroxide solution ( each ml

corresponding to I per cent o f the absolute acid ) p h e n ol p h ta l e i n ,

bein g u sed a s i ndicator .

D I LU T E D H Y D R O C Y A N I C A CI D .

A CID U M H Y D R OCY A N I CU M DI L U TU M .

H CN : 27 .

M ust contain j ust 2 per cent o f hyd rogen c y anide

Potassium ferrocyanide in coarse powder , .

4 parts
S ulphuric acid 3 parts
0

'
The apparatus necessary consists o f a long necked flask fitted -

w ith a twice perforated stopper carrying a sa fety tube and the

bent tube connecting the flask w ith a L i e bi g s o r other suitable ’

condenser th e exit tube o f which shoul d dip into th e liquor in

,

the receiver The receiver shoul d be tared S houl d be lar g e

.
,

enough to perm it the final adj ustment o f strength without a

change o f vessel and shoul d be placed in broken ice or ice water
,
-
.

Put 1 6 parts o f distilled water in the receiver .

The ferrocyanide is to be d is solved in 20 parts o f water an d'

then introduced into the flask The acid i s diluted by addin g it .

gradually t o twice its weight o f water and a fter connecting the , ,

whole apparatus together properly and making a l l the j oints tight ,

the cold diluted aci d i s poured in through the sa fety tube Heat .

the flask on a sand bath to the bo iling point and continu e apply
-
,

ing a moderate heat until there i s bu t l ittle l i qui d mixed with the
sal ine mass remaining in the flask Then detach the receiver and .

a ssay a su fficient portion o f the contents The d istillate is then .

to be diluted with d istilled wate r so that the finished product will

have the required strength ( 2 per cent ) .

R e act i on . 2 K, F e Cy 6 —
I
K
+ 2 es
F 6 + 6 H Cy .

N ot e s . A flask is used instead o f a retort because more con

I f a retort be used it shoul d be directed upward to pre
ve n i e n t .

vent contamination o f the distillate from spurting .

The heat requ ired is not far above the boiling point o f w a ter .
 230 A CI D S .

immediatel y a fter bottl ing and not much bel ow 2 per cent before
,

consumed in dispens ing .

This preparation is frequently used in extremely critical cases

and it must therefore be absolutel y rel iable It shoul d accord
, , .

i n g l y be tested from time to time and th rown away when no

longer o f proper strength .

O ffici a l A l t e r n a te Pr oces s .

The Pharmacopoeia also gives an easily performed proces s for

the extemporaneous preparation o f diluted hydrocyanic aci d ,

which is as follows

Silver c yanide parts

6
H y drochloric acid .
5 parts
D istil led water 55 parts

M ix thes e ingredients in a glass stoppered bottl e adding the -

,

cyani de last and shake well When the precipitate has subsided
,
.
,

pour off the clea r liquid which will be the finished product con
, ,

taining 2 per cent of H Cy .

R e a ct i on .

A n ot h e r M e t h od .

D iluted hydrocyanic acid may al s o be conven ientl y made from

potassium cy anide w ith tartaric acid :

I t W ill be s een from this equation that 6 5 parts o f dry p ota s

s ium cyanide and 1 5 0 parts o f tartaric acid will furnish 2 7 parts o f
H CN . Hence the following formula may be used :

Potassium cyanide
Tartaric acid
D istilled water .

D issolve the cyanide a nd the tartari c acid separately each in , ,

20 0 parts o f distilled water

‘
A dd the solution o f tartaric acid to
.

the other stirring well F ilter out the precipitated cream o f tar
,
.

i tar A ssay the filtrate and add enough distilled w ater to make
.

the product contain exactly 2 per cent o f H CN .

 A CI D S . 23 1

T heoretically the quantity o f product obtained from these pro

portions should be 4 5 0 parts .

The diluted hydrocyanic aci d prepared in this way may co ntain

in solution a minute amount o f tartaric acid and o f cream o f
tartar .

D e s cr i pt i on D iluted hydroc y anic acid is a color less l iquid o f a

—

str o ng and characteristic odor and taste resembl ing thos e o f

i
,

bitter almonds w e t t e d w i t h water or o f volatile o i l o f bitter a l ,

mond B ut as it is e xtr e mel y p oi s on ou s it is dangerous to taste

.

or to smell it without first d iluting it considerably .

Pr e se r v a t i on D iluted h y droc y anic acid frequently undergoes

.

some change by which a dark colored deposit i s formed in it A c .

“ ”
cording to S qu ibb it may turn ne arl y as black as dilute ink
,

within a y ear and a hal f i f k e pt i n g l a s s s toppe r e d bot tl e s and

,
-
,

this change does n ot occur when the acid is put up in corked vials .

The action which the acid thus appears to have upon the ground
sur face o f glass has not been explained .

The preparation should alwa y s be kept in a cool dark place , .

D I LU T E D H Y P O PH O S PH O R OU S A CI D .

A C I DU M H Y PO P H O S P H O R O S U M D I L U TU M .

H P0 2H 2
—
66 .

Cal cium h y pophosphite

O xalic acid

D issolve the hypophosphite i n 1 0 0 parts o f distilled water and ,

the oxal ic aci d in 5 0 parts Filter both solutions A dd the s o

. .

l u t i on o f oxal ic acid to the solution o f calcium hypophosphite

. ,

stir ring well Filter Wash the calcium oxalate on the filter
. .

w ith distilled water and mix the washings with the filtrate .

E vaporate the liquid to 1 3 2 parts .

R e act i on .

Ca PO 2H 2 ) 2

= Ca C O + 2 H 2 4
PO 2 H 2 + 2H 2 O
232 A C1 D S .

N ot e sThe product contains 1 0 per cent of

. . H PO 2H 2
. It
must be kept in a glass stoppered bottle -
.

LA CTI C A CI D "
.

A C I DU M L A CT I C U M .

H C3 H 5 O 3 2 90 .

M ilk sugar
-
y ields by fermentation
,
lactic acid ,

C1 2H 2 2 O 1 1 + H 2 O 2
4 H C3 H 5 O 3 .

S everal other organic substances as dextrin glucose etc are , , , .

,

al so capabl e o f unde rgoing lactic fermentation .

W h e n a m ixture o f 1 0 0 parts Of sugar dissolved i n su fficient

'
’

water to yiel d a solution o f about sp g r with 8 to 10 . .

,

parts o f old cheese and 5 0 parts o f prepared chalk i s exposed

, ,

for Several weeks to a moderate heat Such as is a ff orded in a ,

sunny place in the summer calcium lactate is formed which i s ,

found crystall ized in the l iquid The lactate o f calcium is r e c r y s .

t a l l i z e d i f necessar y and decomposed by sulphuric acid yielding

, , ,

lactic acid and calcium sulphate .

L actic aci d is al so prepared from milk sugar and skimmed -

milk a mixture Of 3 0 0 Gm o f m ilk sugar and 4 liters o f m ilk be

,
-

ing exposed to a temperature o f 2 0 to 3 0 C and the acid ° °

.
,

n eutralized from time to time w ith sodium bicarbonate until the ,

lactic fermentation ceases The solution o f sodium lactate is .

then evaporated t o a syrupy consistence dissolved in alcohol , ,

and decomposed by sulphuric aci d a fter which the lactic acid is ,

neutralized with chalk an d the lactate o f calcium in turn de

,

composed to obtain a purer product ( S e e also F errous .

,

L actate )
The lactic acid o f the A merican Pharmacopoeia
D e s cri pt i on —
,

contains 7 5 per cent o f absolute lactic acid ( H C3 H O 3 ) and 2 5 5

.
.

per cent of water It is a colorless s y rup y liquid without odor

.
, , ,

and o f a pure acid taste A bsor bs water on exposure to moist.

air S p W about
. .
‘
. M iscible with water alcohol and ,

ether in all proportions .

V al u at i on . To neutralize Gm o f lactic ac id 75%

23 4 A CI D S .

Pu ri fi cat i on The most common impurities in commercial n it

.

ric acid are H zS O 4, Cl N 2O 4 and iron nitrate T h e chlorin e

, ,
.

is derived from the chlorides in the nitrates employed Chili salt .

peter al so contains sodium iodide which gives rise to contamina ,

tion with iodine Chloride The iron comes from the iron cylinders
.

in which the distil lation is conducted in the manu facture o f nitric

acid on a large scale A bsolute n itric aci d . sp gr ) does . .

not attack metallic iron and the strong acid generated i n the ,

iron cylinders attacks the metal but l ittl e Hence iron cylinders .

can be used The yellow or reddish color o f crude strong nitric

.

acid i s due mostly to nitrogen tetroxide N 2O 4 Thi s impurity ,

.

° °
may be removed by heating the aci d t o about 8 0 t o 90 C
whereby it is driven off .

The purification o f nitric acid is e ff ected on a large scale by

r e distillation from glass retorts
-
The first portion d istilling over .

contains the nitrogen oxi de chlorin e and iodine A s soon as the ,

.

d istillate i s colorless and free from chlorine the receiver i s ,

changed and the distillation continued until about one eighth

,
-

remains To fix the sulphuric acid in the cru de nitric acid a

.
,

l ittle potassium nitrate is added before th e d istillation .

Pur e ni t r i c aci d is made directly from pure potass ium nitrate

and pure sulphuric aci d .

D e scri p t i on colorless fuming l iquid o f su ff ocating odor ;

—
A , ,

extremely corrosive S p w about . at C ontains 68

. .

per cent o f H N O 3 .

The aci d which manu facturers designate as C P usually . .

satisfies the pharmacopoeial requirements .

Va l u at i onTo neutralize
. Gm o f the offi cial nitric aci d
requires 3 4 ml of normal solution o f potassium hydroxide .

E ach m 1 o f thi s volumetric solution corresponds to 2 per cent

o f absolute H N O 3 Ph e nol p h ta l e i n is the indicator used
. .

O ne ml o f normal potass ium hydroxide solution is the e q u i val

ent o f Gm o f H N O s .

A cti on on me t a l s
Gol d platinum iridium rhod ium and
.
, , , ,

chromium a r e not a ffected by nitric acid Iron l ead and silver are .
,

scarcely attacked by concentrated nitric acid but diluted nitric ,

aci d dissolves them A ntimony tin and tungsten are oxidized

.
,

but not dissolved M ercury silver and bismuth dissolve readily

.
, ,
 A CID S . 23 5

e specially in wa rm nitric acid with the evolution o f n itric oxide ,

( N O ) which in contact with the ai r

,
at once oxidizes to nitro ,

g en tetroxide ( N which appears as red fumes .

D i l u te d N i tr i c A ci d .

N itric acid
D istilled water

M ix them Keep the product in dark amber colored glass

.
-
,

stoppered bottles .

D iluted nitric acid contains 1 0 per cent by weight of absolute , ,

nitric acid .

S pecific gravity : about at 1 5 C °

.
.

'
To neutralize Gm o f dilut ed n i t r i c a c i d should require
1 0 ml o f normal solution o f potass ium hydroxide ( each ml cor

responding to 1 per cent o f absolute acid ) p h e n ol p h tal e i n bein g ,

used as ind ic ator .

N I TR O H Y D R O CH L O R I C A CI D .

A C I DU M N I T R O H Y D R O C H L O R I CU M .

Nitric acid
Hyd rochloric acid

M ixthe acids in a large glass beaker and when e ff e s ve s ce n c e , ,

has ceased pou r the mixture int o a glass stoppered bottle which
,
-
,

shoul d not be more than hal f filled Keep it in a cool dark place .
,
.

R e a ct i on .

N ot e sWhen strong nitric and hydrochloric acids are mixed

.

both decompose and free chlorine is formed in the l iquid wh ich

, , ,

therefore is capabl e o f dissolving gold and has long been kno w n

, ,
'

“ ”
under the name o f aqua re gi a The medicinal value o f the .

'
preparation al so depends upon the free chlorine ( and n itros yl
chloride ) it contains .

The e ff ervescence which always takes place should be allowed

to cease before th e product i s bottl ed th e acids should be cold ,

when mixed and the finished preparation should be kept i n a c ool

,

pl a c e .
23 6 A ID S
C .

The pharmacopoeial direction to keep it in bottles not m or e .

than hal f fill ed is intended to prevent the poss ibl e bursting o f th e

bottle shoul d the evolution o f ga s not have been complete d be fore
it w a s bottl ed .

Care must be exercised in handling this aci d Chemical action .

must be completed before it or any mixture conta ining it shoul d , ,,

be dispens ed When mixtures o f nitrohydrochloric ac id w ith

.

organic substances have been made explos ions h a ve happened a

shor t tim e after they had been bottl ed .
.

D e s cr i pt i on .
—
A
gol den yell ow fuming an d extremely corrosive
-

l iquid having a strong odo r o f chlorine and a strongly aci d r e

,

action R eadily dissolves gold le a f

. . .

D i l u te d N i tr ohy dr och l or i c A ci d .

Hydrochloric acid
D i stilled water

M ixthe acids i n a capacious gl as s vesse l and when e ff e rve s

’
'

, ,

cence has ceased add the distilled water Keep the product in
, .

dark amber colored glass stoppere d bottles in a coo l place

-
,
-
, .

D e scri pt i on A
co l orless o r pal e yellowis h l iquid having a faint
—
,

o dor of chlorine and a very aci d taste,

.

O LEI C A CID .

A CID U M OL E I C U M

H C1 8 H3 3 0 2 2 28 2 .

Impure oleic acid known as red O i l i s ob t ain ed as a by ‘

, ,

product i n: th e manu facture o f candles Fats consist o f o l ein .

,

palmitin an d stearin which are the glycerides o f oleic p almitic

,
. .

and stearic aci ds .

T he soli d fa tty aci ds ( palm itic and stearic acids ) are separ ated
for use in makin g candl es and the resid ue call ed red oil; is
“
,
”
,

crude ol eic acid which still contains som e o f the soli d acid s
,

n am ed .
 Pu r i fi e d O x a li c A ci d .

Commercial oxalic aci d 1 parts

Hydrochloric acid parts
5 Q
Water .

Put the oxalic acid in a porcelain dish and add 7 0

hot water Boil for a few minutes L et it settl e D e cant the
. . .
m
solution whil e still hot from th e undissolved portion ( which con
s ists mostly o f oxalates and may b e reserved for further treat
ment i f profitable )
, A dd th e h y drochloric acid to the hot s o
. .

l u t i on obtained .S ti r well Cool rapidly stirring the liquid to

.
,

get small crystal s Coll ect the crystal s an d wash the product
.

with a very small quantit y o f cold water .

R ec rystallize the product once or twice as may be requ ired .

N ot e s
. The less soluble oxalates remain undissolved w h
commercial oxal ic acid is treated with l ess water than is r e q u i r
for complete solution The remaining oxalates are d e c om p os e i j i
.

by the h y drochloric acid which is used in considerable

,

I t is best not to allow the oxal ic aci d t o form large crystal s from“
th e solution containing hydrochloric acid ; small crystal s are m o ré
i l ’
’

'

readily washed free from th e H Cl R e c ry s ta l l i zat i On fr om a h ot} ? i

.

saturated soluti on i s necessary to complete the purification a nd

?

, s
L"
it m ay be found necessary to repeat it .

Pure oxal ic acid volatil izes on platinum without res idue .

PH O S PH O R I C A CI D
'

A CI DU M PH OS PH O R I CU M .

H 3 PO4
°

2
9 8 .

Phosphoric acid can be m ade in various ways It is most com .

m on l y made from phosphoru s by oxidation with nitric aci d .

When strong nitric acid i s u sed the reaction is m ore rapi d and
l ess heat is then appl ied ; when th e acid i s diluted the action be ,

ing les s violent more heat is requisite

,
.

It requires parts of phosphorus to make 1 0 0 parts o f the

O ff i cial phosphoric acid The usual process i s as follows :
.

M ix 5 1 0Gm o f nitric aci d w ith 5 0 0 ml o f distilled water in a ,

'

tubulated retort capabl e o f holding ml Place the retort .

 A CID S . 2 39

upon a sand bath or on a wire gauze support connect it loosely

-
, ,

w ith a well cooled receiver A dd 8 0 parts of phosphorus In

. .

sert a funnel through the tubulus o f the retort and then gradual ly
apply heat until the reaction beg i ns R egulate the heat so as to .

pre vent the action from becoming violent checking it i f need be , , ,

by the addition o f a l ittle distilled water Continue the d igestion .

until all the phosphorus i s dissolved and return to the retort , ,

from ti me to time any liquid which may collect in the receiver

‘

.
,

When all the phosphorus i s dissolved trans fer the contents o f

the retort to a tared porc elain dish an d heat the l iquid at a tem ,

o f nearly but not above C until the excess o f nitric °

p e r a t u r e 1 90 .

acid is expelled and an odorl es s syrupy liquid remains Cool ,

.

the d ish and contents an d add enough distill ed water to mak e

> +h e total weight of the product 2 8 5 Gm .

< c Test the product for n itric phosphorous and arsenic acids all
, ,

f which must be removed i f present .

m a: I f n itric acid be present evaporate the l,

iquid until it ceases
33 3th give any further reaction for that acid ; then l et it cool and

i l u t e it with di stilled water until the prescribed weight ( 2 8 5

E m ) is restored .

I f phos phorous acid be found in the phosphoric acid add ,

o f nitric acid and again heat the mixture until reactions

o s p h or ou s and nitric acids cease and restore the pre ,

weight ( 2 8 5 Gm ) by dilution with distilled water as

(“
Befor e
S houl d arsen ic be present d ilute the phosphoric acid with,

75 0 ml o f distilled water heat the liqui d to about 7 0 C an d

°
, .

then pass through it a stream o f hydrogen sulphide gas for hal f

an hour Then remove th e heat but continue pass ing hydrogen
.
,

sulphide through the dilute phosphoric acid until it becomes cold .

Close the vessel tightly set it aside for 2 4 hours filter the l iquid
, , ,

then heat the filtrate until al l odor o f hydrogen sulphid e has been
expelled filter again and finally evaporate the now purified phos
, ,

p h o r i c acid until its weight is reduced to 2 8

5 Gm .

The product must be tested as to its stren gth in the manner

prescribed below and diluted or concentrated as may be required
, , .

Pr eserve the product in glass stoppered bottl es -

.

R e act i on s . Probably firs t

2P + 2H NO
24 0 A CI D S .

N ot e s The phosphorus used must be f ree from sulphur ;

.

otherwise sulphuric acid will be form ed from the latter and con
t a m i n a t e the product This r esult m ight however be prevented
.
, ,

by using an excess o f phosphorus so that some of it remains u m

dissolved the phosphorous acid being oxidized to phosphoric acid
,

by a fresh portion o f nitric aci d a fter removing the undissolved

p hosphorus and sulphur .

A s the phosphorus fuses collecting on the bottom o f the retort ,

or flask where it presents but a l imited surface o f contact for

,

the acti on o f the nitric acid the oxi dation is slow H igh heat ,
.

'
renders the a c t i on t oo violent unl ess the nitric aci d has been ,

properly diluted as in the usual process described above N itric

,
.

acid o f sp gr i s considered m ost suitabl e Whenever th e

. . .

reaction i s from any cause too violen t there i s danger that par ,

t i c l e s o f phosphorus may be thrown t o the surface o f the liqu i d

'

an d ignited the heat from the combustion fracturing the vess el

,

and scattering the burning phosphorus the aci d l iquid and t h e , ,

r e d nitrou s fumes The temperature need not exceed 5 0 C °

. .

A flask can be u sed in place o f the retort and the heati ng can ,

be do ne in a water bath In tha t cas e the neck o f the flask

—
.

shoul d be covered by a watch crystal the convex side d ownward , ,

so that the liquid formed by the condensation o f the rising vapors

m a y run down into the flask again S hould th e flask or retort .

break from a n y cause while undissolved phosphorus remains in

it the use o f the water bath instea d o f a san d bath would prevent
,
- -

the ignition o f the phosphorus .

S hould the liquid a fter the phosphorus has been dissolved

, ,

contain both phosphorou s and arsenic acids and should it then ,

be concentrated to les s than three times the weight o f the phos .

~

p h or u s con sumed the phosphorous acid may be oxid ized by

,

the conce ntrated nitric acid s o violently that the liqui d froths
over the s ides o f the dish unles s a littl e water is added The .

a rseni c then separates as a brown powder o f reduced metal .

I f the liqu id contains phosphorous acid but no nitric acid the , ,

phosphorous acid m a y be lost during the subsequent evaporation ,

hydrogen phosphide being formed unl ess nitric acid be added

to prevent it .
24 2 A CID S .

j ar placed i n ice water ; then 6 parts o f bromine di ssolved in

-

dilute hydrobrom ic aci d is very cautiously added A fter the .

reaction 5 40 parts o f n itric aci d is added A fter 2 4 hours the i

.

phosphoru s is nearly or quite dissolved ; i f a n y o f it remains u n

di ssolved a fter that pe riod heat may be sa fely appl ied to hasten
,

its oxidation The iodine bromine and excess o f nitric acid

.
,

are then driven o ff by heat .

T he slow oxidation o f phosphorus by moist air at a l ow tem

p e r a t u r e has als o been practiced .

O rtho phosphoric aci d has also been prepared by h eating a

-

soluti on of glacial phosphoric acid ( metaphosphoric acid ) in

water the reactions being : 2 H P O l H O H , P 2O 7 ( p y rop h os
'
—
— - _ :
, 3 ,

p h or i c acid ) and then H 4,

P2 O 7 + H O 2 H 3
PO 2
2

A considerabl e quantity o f pyrophosphoric aci d may h ow ,

ever remain undecomposed

,
.

A morphous phosphorus i s readily oxid ized by nitric aci d With

out danger o f fire .

The reaction be g ins a fter a few hours generally without the ,

application o f any heat and having once commenced it progres ses

,

very r apidly I f a capacious vessel is employed no danger n e e d

.
,

be apprehended .

Pr op er ti es . A n aqueous solution containing

per cent of 85
ortho p h osphoric aci d and 5 0 per cent o f water It is a clear
—
.
,

colorl ess liquid without odor o f a strongly acid taste an d reaction

, , .

S p w not less than

. . at Its s p vol is . .

V a l u at i e n To neutralize
. Gm o f O ffi cial phosphoric acid i

( 57 )
8 0 should requ i re 1 7 ml o f n o r m a l s ol u t i o n o f potassium
hydroxide E ach ml o f the volumetric test solution corresponds
.

to 5 per cent o f H 3 P O 4 Ph e n ol p h ta l e i n is used as the indicator

. .

The phosphoric acid shoul d be somewhat diluted with water be

fore the potassium h y droxi de solution is added .

O ne ml of normal solution o f potassium h y droxide i s the

e q u i va l e n t 0 f
.
Gm o f H 3 P O 4 when forming K H PO , Q

(p h e n o l p h t a l e i n being then used as an indicator ) it is e q u i v a l

n t to o f H 3 P O when forming K H PO ( methyl orange
4 4
-

being the indicator used in this test ) .

 A CI DS . 24 3

[ 3
K P O 4 shows an alkal ine reaction with all color indicators ;
K Z H PO 4 i s neutral to p h e n olp h ta l e i n but alkaline toward methyl
o range and Congo red ; K H 2PO , g ives an acid indicator with
-

p h e n ol p h t a l e i n but a neutral reaction with methyl orang e ] -

D i l u t e d P h os ph or i c A ci d .

Phosphoric acid . 1 00 Gm
D istill ed water 75 0 Gm

M ix them Keep the product in well stoppered bottles

.
-
.

D iluted phosphoric acid contains 1 0 per cent by wei g ht of , ,

absolute H 3 P O , .

S pecific g r a vrty : about at 1 5 C °

.

Gm o f diluted phosphoric acid shoul d require for neut ral

i zat i on 1 0 ml o f normal potassium hydroxide solution ( each
ml correspondin g t o 1 p er cent o f the absolut e aci d ) phenol ,

p h t a l e i n being used a s ind icator .

M E T A P H O S PH O R I C A C I D .

H P0 3 =:8 0 .

[ Glacial phosph ori c acid .

]
This i ce - l ik e solid i s formed by heatin g the ordinary phos
p h o r i c acid to redness or by
,
dissolvin g phosphorus pento xide in
col d water and heatin g A s found in commerce it usually con
.

tains much sodium phosphate .

S AL I C Y LI C ACID .

A CI DU M S A L I CY L I C U M .

H C 7 H 5 0 3 =1 3 8 .

M ethyl sal icylate e x i sts in th e volatil e oil o f gaultheria which ,

contains about 90 per cent o f this compound ether S al icylates .

have also been found in sweet birch an d mother plants S alicylic .

acid is manu factured as follows

A solution o f sodium hydroxide i s saturated with phenol the ,

m ixture evaporated to dryness with constant stirrin g and the ,

244 ACI DS .

residue whil e sti ll h ot is powdered ; the po wder i s heated in a

, ,

retort over an oil bath t o 1 00 C wh ereby all moisture is driven

-
°
.

o ff then a current o f dry carbonic acid gas is pass ed into the

retort u ri d e r sl ight pressure the temperature being raised to
' ‘

C and finally to 2 2 0 25 0 C
°
1 80
°
.
,
The residue now consists °
—
.

o f sodium carbonate and sodium hydroxi de together with sodium

salic y late ; it i s dissolved in water and hydrochloric acid is added , ,

by which the salicyl ic acid is precipitated while sodium chloride

remains in solution .

R e acti ons .

C6 H 5 O H + N a O H z C6 H 5 O N a + H 2O ; then

n
'

C6 H 5 O N a l— C —
N a C7 Hg
O3 ; and

N ot e s uch depends upon a careful re gulation o f the tem

. M
t e in this process Potassium hy droxi de cannot be used in
“

p e r a u r .

place o f the sodium h y droxide the resul t being then para oxy ,
-

benzoic acid instead o f sal icyl ic acid T he chemical reactions i n .

“
c l u d e also the formation o f
’
sodium salicylate o f sodium -
,

N a C7 H 5 O g + C6 H s O N a z N a C7 H 4 N a ) O s l Ce H s O H
— —
;

thi s compound is decompos ed by th e H Cl yielding salicylic acid

and sodium Chloride .

The crude salicy l ic acid is purified and decolorized by fil t r a

tion o f its solution through animal Charcoal and repeated r e ,

crystall ization To perfectly remove the resinous impurities

.
,

dialysation i s resorted to .

When oil o f wintergree n i s treated with sod ium hydroxide and ’

the methyl salicylate o f sodium boiled m eth y l alcohol and s o ,

d i u m salicylate are formed .

Precipitated salicyl ic aci d ( amorphous ) i s not su ffi ciently pu re

for medicinal uses The crystall ize d acid is required S ublimed
. .

salic y lic aci d o ften has the odor o f phenol and acquires a red ,

d ish tint On exposure to air or sun light The purest acid i s that ,

purified by dial y s is .

'

D e scri pt i onf Fine white l ight prismatic needle s h a p e d c ry s

“
— -
, , , ,

tals per m an e h t in the air free from odor o f carbol ic acid , but
,
¢
l ‘

,
 46 A CI DS .

N ot e s The pharmacopoeias contain sulphu ric acids varying in

.

stren gt h from per cent to 9 8 per cent That o f the U nited .

S tates Pharmacopoeia i s required to contain a t l e as t per cent

o f absolute acid and in al l ofli c i a l formulas wherever sulph uric
,

acid is ordered the quantity prescribed is based upon the a s s u m p

,

t ion that the acid has that strength .

S ulphu ric acid is extremely corrosive and destructive I t must .

there fore be han dled with great caution It reacts violently with .

all volatile oils and with a number o f other substances When it .

i s mixed with water or with alcohol the chemical action which

takes place causes a rap id and great ri se o f th e temperature .

Hence the only safe way to make thes e m ixtures is to add the
acid very slowly an d in a small stream to the water or t h e
alcohol stirring constantly It is al so re c ommended that a very
, .

large vessel be used one holding at l east three times as much as

—

the total quantity o f mixture to be made for i f the l iquid shoul d ,

become so hot as to boil or spurt damage might otherwise result .

Whenever it may be necessary to add fuming sul p huric acid

N ordhau sen or nearly absolute sulphuric acid to a
weaker sulphuric aci d in order to produce a mixture o f definite
strength as for instance to make an acid containing exactly
, , ,

9 8 per cent o f absolute hydrogen sulphate the stronger acid ,

should be added to the weaker A nd when a strong sulphuric .

aci d is to be diluted with a comparatively small amount o f Water ,

the order o f mixing shoul d be as stated be ore the acid must

f i —

be added to the water an d not the water to the acid .

The acid sold by manu facturers and dealers under the d e s ig

“ ”
nation chemicall y pure ( C P ) is generall y su fficiently pure . .

for pharmaceutical purposes fulfilling the requirements o f the ,

Pharmacopoeia .

S ulphuricacid is customarily put up in bottles containing one ,

“ ”
or two or nine poun ds The ordi nary s o called five pint acid
, .
—

bottle holds nine pounds o f concentrated sulphuric acid .

D e scri pt i on —
A
colorl ess oily odorless extremely corros ive
, , ,

liquid . Sp . w not less than

. at

A ct i on on me t a l s
Concentrated sulphuric acid attacks copper
.
,

and i f hot it also attacks mercury s ilver and bismuth D iluted

, , ,
.

s u l p u h r i c acid attacks and dissolves iron zinc and nickel but , , ,

 A CI DS .
24 7

does not dissolve platinum gold silver lead c opper mercury , , , , , ,

aluminum ars enic antimon y and bismuth

, , .

D i l u te d S ul ph u r i c A c i d .

S ulphuric aci d
D istilled water .

Pour the acid slowly in a small stream into the d istilled water
, , ,

under constant stirring .

Keep the liquid in glass stoppered bottles -

.

N ot e s
When sulphuric acid and water are m ixed a cons ider
.

able rise o f the temperature and a contraction o f volum e take

place I f the l iquids a re mixed too rapidly or the water added
.
,

to the acid inst ead o f vi ce v e rs a the heat generated may be so ,

great as to cause serious accidents by violent boil ing or spattering .

The diluted sulphuric acid obtained by the for egoing formula

,

contains 1 0 per cent of absolute H S O z 4 .

F u m i ng S ul ph u r i c A c i d ,
or N
This or d h a u s e n S ul ph u r i c A c i d —

'

i s a m ixture o f S O 3 an d H zS O 4 or poss i bly H S O 7 It is al so , , ,

“ ” “
called p y r os u l p h u i i c acid and d isulphuric acid
’
It i s made .

by distilling ferrous Sulphate which has been fi r s t d r i e d to a cer

'

tain point :

4 F e S O , l
—

Fuming sulphur i c acid i s a thick l iqu id extremely corrosive , ,

and gives off dense fumes

alle r s A ci d D r ops
’
H .

L I QUOR A CI D U S H ALLER I .

This i s a m ixture o f equal parts by weight o f alcohol and sul

p h u r i c acid The acid must
. be added to the alcohol gradually and
cautiously with co nstant stirring in order that the tempe rature
, ,

m a y n ot ris e so high as to cau se the li qu id to boil The l iquid .

contains alcohol sulphuric acid ether and ethyl sulphuric acid

, , ,
—
.

I f the alcohol was pure the preparation is colorl ess ,

.
2 48 A CI D S .

A R O M A TI C S UL P H U R I C A CI D .

A CI DU M S U L PH U R I CU M AROM A TI C U M —
U . s .

S ulphuric acid
Ti n ctu re o f g inger .

O il of cinna m on
A lcohol su fficient ,
.

Add the acid s l ol and in small stream to 8 0 0 ml o f alcohol ,

stirring constantly being careful not to add the acid so rapidly

,

as to cause the mixture to boil When the mixture has cool ed .

add the tincture and the volatile oil Finally add enough alcohol to .

make the product measure mil liliters .

Keep it in glas s stoppered bottl es -

.

N ot e s . A romatic sulphuric acid contains about

per cent o f 20

sulphuric acid chiefly in the form o f ethyl sulphuric aci d or acid

,
-

eth yl sulphate It also contains some e t her and various other

.

products formed by the chem ical action o f the sulphuric acid on s

the other ingredients .

D e s cr i p t i on —
is a pale yellowish brown liquid o f aromatic
It -

and strongl y acid taste B ecomes darker by a g e through the car

.

bon i za t i on o f the organic matter by the sulphuric acid .

S UL PH U R OU S A CI D .

A C I DU M S U L PH U R OS U M .

The sulphurou s acid o f the Pharmacopoeia o f the U n ited

S tates is an aqueous solution representing per cent o f H S O 3 , Q ,

corresponding to per cent o f sulphur dioxide ( S O 2 ) .

It is prepared as follows

S ulphuric acid
Charcoal in coarse powder
,

D istilled water .

S odi um carbonate .

Put the aci d and the charcoal in a flask o f about 5 0 0 ml ca

p a c i t
.
y Connect the flask by mean s o f bent glass tubing and peg;
f or a t e d rubber stoppers w ith a wide mouthed bottle o f about
 A CIDS .

S ulphurous acid deteriorates rather rapidl y by oxidation to

sulphuric acid .

colorles s solution with strong Characteristic

D e s cr i p t i on —
A
odor o f burning sulphur and sharp acid taste and reaction I ts ,
.

specific gravit y is at 1 5 C °
.

A noth e r M e t h od .

S odium bisulphite ,

D iluted sulphuric acid ,

D istill ed water o f each su ffi cient ,

.

Intro duce the sodium bisulphite in a su itabl e roomy flask pro

vi d e d with stopper sa fety tube and delivery tube and connected
, ,

with a wash bottle Containing some distilled water and in turn

-
, ,

connected with a receiving bottle conta ining cold distilled water ,

previously freed from air by boiling .

A dd the diluted sulphuric acid a littl e at a time through the , ,

sa fety tube being careful not to add the acid too rapidly s o as
,

to cause a t o o rapi d evolution o f the gas .

When the water in the receiving bottle has been saturated bot
tle the product .

R e act i on .
—

l
—
2S O, .

N ot e s This process i s not as ec onomical as the o fficial method

.
,

but it is more convenient and may o ften be found pre ferable .

Theoretically Gm o f sodium bisulphite y iel ds 6 4 Gm o f

S O , or enough to saturate one l iter o f water ; but allowance
,

must be made for the S O 2 hel d in the wash bottle an d that r e -

ma i n i ng in th e various parts of the apparatus so that much

more than that quantit y is consumed The quantity of diluted .

sulphuric aci d requ ired is a bou t fi ve times the amount o f s o ‘

d i u m bi sulphite .

The size o f the vessels the amount o f water in wash bottle ,

- -

and receiver the temperature o f th e water in the receiver and

, ,

certain other details are indicated in the o ffi cial process already
,

described The en d bottle containing sodium carbonate shoul d

.

not be om it ted .

-
Two receiving bottles may be alternatel y used until the water ,

in both shall have been saturated E ach bottl e can then be shaken .

occasionally .
 A CID S . 25 I

T A R T A R I C A CI D .

AC I DU M T A R T A R I CU M .

H 2C 4 H 4 0 6
= 1 50

Tartaric acid occurs in grapes and in other fru its in the form ,

o f acid potassium tartrate from which it is manu factured ,

.

The following formula is based on S cheele s process

’

Cream o f tartar
Prepared chalk .

Calcium chloride
S ulphuric acid .

D istilled water su fficient ,

.

Boil the cream o f tartar with ml o f water and gradually ,

add the chalk stirring constantly When e ffervescence has

,
.

ceased add the calcium chloride d issolved in 80 0 ml o f water

, .

When the calcium tartrate has subsided decant the liqui d and , ,

wash the tartrate with water until tasteless Pour the sulphuric .

acid previously diluted with

,
ml o f water on the calcium ,

tartrate mix thoroughly boil for hal f an hour with repeated

, ,

stirrin g and filter through musl in E vaporate the filtrate at

,
.

a low temperature until it acquires the specific gravity l et

it cool an d then separate and rej ect the crystal s o f calcium sul
,

phate formed A gain evaporate the clear liqui d until a pellicl e

.

forms and then set asi de to cool and crystall ize L astly puri fy
, .
,

the product by re crystall ization -

.

4 0 6 l K2 C4 H 4 0 6 l
R e act i on .
—
CaCO 3 Ca C4 H — — —

H zO —
l CO z
-
, and K2C4 H 4 O G+ Ca Cl z
z Ca C4 H 4 O e —l —
2 K C1 ; finally ,

Ca C4 H 4 0 6 + H z S O 4 2 H Z C4 H 4 O 6 + Ca S O 4 .

N ot e sTartaric aci d crystallizes best from a solution contain

.

ing a small amount o f free sulphuric acid Calcium h y droxi de .

can be used instead o f calcium carbonate .

D e s cri pt i on
Colorless prisms having a sharp but pleasant
.
—
,

aci d taste R eadily soluble in water an d alcohol and slightly

.
,

soluble in ether The crystal s are anh y drous and not d e l i q u e s

.

cent .
 A CIDS .

V ALE R I A N I C A CI D .

A CID U M VA L E R I A N I CU M .

( A c i d u m Va l e r i c u m —
Va l e r i c A c i d .
)
H C5 H 9 0 2: 1 02 .

T his acid exists in valerian anthem i s angeli ca hu mulus an d , , ,

V iburnum being form ed by the oxidation o f volatile oil s or other

,

natural constituents and accordingly pres ent in larger proportion

,

in ol d lots o f these plants which have been somewhat exposed

to the air I t is now prepared by the action o f chromic anhydride
.

upon amyl alcohol a s illustrated in the process for the man u fa c

,

“ ”
ture of s odium valerate S e e S odium Valerate . .

Val e ric aci d may be conveniently prepared by a d d i n g s u l p h r i c

acid to a strong solution o f sodium valerate in water The oily .

layer ris ing to the surface o f the m ixture is valeric acid This .

is separated from the watery liquid containing the sodium sul

phate then deprived o f water by repeatedly shaking it with s trong
,

sulphuric aci d and a fter separation from the sulphuric acid the
, , ,

product i s distilled .

D e s cri pt on i —
A
thin oily colorles s l iquid having a very char
, , ,

a ct e ri s t i c
,
sharp disagreeabl e penetrating valerian like odor
, , ,
—
.

Its taste is p ungent acid extremel y disagreeabl e S oluble in

, , .

from 2 6 to 3 0 parts o f water S oluble in all proportions in alco

’
.

hol a n d e t h e r Its s p w i s about

. at 0 C
. .
°
.
2 54 ALU M .

T u r bi d a te d A l u m .

Potash alum
Boiling water
D iluted sulphuric aci d

D issolve filter and cool the solution rapidly stirring it con

, , ,

s t a n t l y to as low a temperature above the freez ing point of water

,

as may be conveniently attained Collect dra i n and dry the crys .

,

t a ll i n e salt .

D e scr i p t i on .
—
A 1um consists o f large colorless octohedral , ,

cr y stal s sometim es modified by cubes or occurs in crystalline

, ,

fragments w ithout pd o r but h a v m g a sweetish and strongly

, ,

astringent taste O n exposure to the air the crystals are l iable

.
,

to absorb ammonia and acquire a whitish coating , .

S oluble in 9 parts o f water at 1 5 C and in

°
part o f boil ing .
,

water i t is also freely soluble in w arm glycerin but is insoluble

, ,

i n al co hol .

T he salt has an acid reaction upon litmus paper .

D ri e d A l u m .

ALU M E N E X S I CCA T U M .

E xpose parts of crystallized pota sh alum for several days

1 1

to a temperature o f about 8 0 until it has thoroughl y e ffl or e s c e d °

.

Then heat it in a porcelain dish gradually up to being care

ful not to permit the temperature to rise above and continue
the heating until a porous white mass remains Weigh ing 6 part s ,
.

When col d powder it and keep it in a well closed bottle

,
—
.

N ot e s . Potassa alum cont ains

”

per cent o f water of crys

t a ll i z a t i on .When kept heated to 4 0 C it loses about pe r cent °
.

of that water ; at 4 7 C it loses per ce nt ; at 6 0 C it loses most

°
.
°
.

o f its water bu t the pieces still retain to a great extent their shape
, ,

and the produc t which is not porous yiel ds a clear solution with
, ,

water A t 8 0 C the salt falls to powder but still retains a con

.
°
.
,

s i d e r a bl e amount o f water L ong continued dry ing at 1 0 0 C .

- °
.
 ALU M . 255

expels al l the rest o f the water and l eaves an en t irely water soluble
product but not a li g ht and porous one
,
.

'

When first e ffl or e s ce d at 80 C a n d t h e n at once gradually to °

.

°
between 2 0 0 and 2 0 5 C and kept at that temperature until its
°
.

weight is reduced to that o f the anhydrous product the result is ,

a l ight and porous dried alum .

°
When alum is at once heated to 92 C it undergoes aqueous .

fusi on and i f then s e t a s i d e to cool the liquid does not sol idi fy
’

until a fter long standing .

A porous and light product is to be much preferred and such ,

a product can not be obtained i f the alum be per mitt ed to d is

solve i n its water o f crystall ization When heated at a too l ow .

temperature the alum may form a glassy mass which c an not be

rendered porou s I n this glassy Condition the alum is said to
.

retain 1 4 mol e cul es o f water wh ich can be expelled at a higher

temperature but the product i s then heavy and non porous
,
.
-
.

D uring the latter part o f the proces s o f heating the alum it

swell s and foams considerably from the water vapor formed .

Hence the dish u sed shoul d be large enough or onl y about one ,

fourth to one third filled The alum should not be S ti rred during
-
.

the heating i f stirred it will not yield a l ight product .

A s it is impracticabl e for the student to regulate the tempera

°
ture so as to maintain it at between 2 0 0 and he may not
succeed in making a perfect product ; but he can veri fy in a gen
eral way the statements here made and may even produce a better
dried alum than is obtained by the o ffi cial process
which is as follows :
“
Place 1 00 grams o f alum [ in small pieces ] in a shallow p orc e
lain capsul e so as to form a thin layer an d heat it on a sand bath ,

until it l i q u e fi e s Then continue the appl ication o f a moderate

.

heat with constant stirring until aqueous vapor ceases to be dis

, ,

engaged and a dry white porous mass is obtained wei ghing 5 5

, , ,
'
,

grains When cold r e d u c e t h e product to fine powder

.
, .

D ried alum shoul d be kept in tightly closed bottles E xpos ed .

to a moist atmosphere it absorbs water quite rapidly even to the ,

extent o f about 1 8 molecules or over 50 per cent o f its weight , .

D e s cr i p ti on
Porous white masses o r a white granular pow
—
,

der odorles s sweetish a stringent S lowly solubl e in 20 parts o f

, , , .

water at
2 56 ALU M .

A M M O N I A A LU M .

ALU M I N I E T AM M ON II S UL PH A S .

A l u m i n u m A m m on i u m S
-
ul ph a te .

A 1H 4 N .
2
1 2H 2O
z
4 53 .

A luminum sulphate . 25 parts .

A mmonia water ( 1 0 7 o f H 0 3
N ) 1 3 parts .

Diluted sulphuric acid 35 parts .

Water 10 parts .

M ix t hed iluted acid and water in a porcelain dish A d d the .

ammonia water gradually stirring wel l ; Then add the aluminum

,

sulphate ; heat to bo il ing for a few minutes ; fi l t e r S e t aside to ‘

cool and crystallize .

A dditional quantities o f cry stal s may be obtained on evapora

tion o f the mothe r liquors -
.

R ecrystallize the product once or tw ice to puri fy it .

N ot e s The alum inum sulphate required m a y be obtained from

.

cryol ite by the proces s described under A l u m i n i S ulphas .

D e s cri p ti onColorl ess transparent octohedral crystals ; odor

—
, ,

less ; ta ste sweetish astrin g ent

,
“ ”
Commercial alum is now ammonia alum while the o fficial ,

“
alum i s potash alum .

For most o f the purposes for which alum is used the ammon ia ,

“ ”
alum is as e ff e ctive as the p otash alum B ut dried alum or .

“ ”
burnt alum must be made from potash alum and when alum ,

i s prescribed for pharmaceutical or medicinal purposes the o fficial

“ ”
alumen i s Of course the kind intended
, ,
.

A mmonia alum is somewhat more readily soluble in water than

the potash alum ; but in other re spects their ph y s ical properties
are alike O n warming th e ammonia alum with solution of
.

potassium hydroxide the odor o f ammonia is developed .

ALU M I N U M A C E T A T E S OLU TI O N .

[ A f ter the German and S wiss Ph a rm a c op oe i a s .

j
A lum inum sulphate 222 parts .

A cetic acid 3 0 0 parts .

D istilled water 480 parts .

2 58 ALU M I N U M HY DROX I DE .

This preparation may also be made by m etathes i s from alu

minum sulphate and barium chloride .

D e s cr i p t i on .
—
Colorless crystals . S olubl e in 5 part o f water
at 1 5
°

U sed as a disin fectant and an astringent .

A l u m i n u m Chl or i d e S ol u ti on .

L I QUOR ALU M I N I CH L OR I D I .

S olution
o f aluminum chloride i s o ften employed as a di s i n
f e c ta nt Pure aluminum chloride is not necessary for thi s pur
.

pose A good product i s obtained as follows

.

Calcium
A lum in powder
,

Water .

D issolve
the cal cium chloride in 5 parts of water and the alum
in 1 5 parts o f boil i ng water M i x the solutions Filter A dd. . .

enough water to mak e the whole product weigh 2 0 parts .

The product contains aluminum chloride potassium

N ot e s .
,

chloride and a trace o f calcium sulphate

,
.

A LU M I N U M H Y D R OX I D E .

ALU M I N I H Y D R OX I D U M .

A lum in powder
,

S odium carbonate
D istilled water su fficient ,
.

D issolve each salt in 1 5 parts o f distill ed water filter the s o ,

lutions and heat to boiling Then having poured the hot solu .

t i on o f carbonate o f sodium into a capacious vessel graduall y pou r ,

into it the hot solution o f alum with constant stirring and add ,

about 1 0 parts o f boil ing distilled water L et the precipitate sub .

side decant the clear l iquid and pour upon the precipitate 2 0
, ,

parts o f hot distilled water A gain decant trans fer the p r e c i p i

.
,

t ate to a strainer an d wash it with hot distilled water until th e

,
 ALU M I N U M HY DROX I DE . 2 59

wash ings give but a faint cloudiness with test solution o f barium -

chlori de Then all ow it to drain dry it at a temperature not

.
,

exceeding 4 0 C and reduce it to a uni form powder

°
.
,
.

R e act i on
“

N ot e s It i s nec es sary to have a decided exces s o f alkal i pres

.

ent throughout the process and as equal parts of alum and ,

sodium carbonate l eave only about ten per cent exces s o f the
alkali and as this exces s i s not too great thes e proportions
, ,

are u sed U nles s a su ffi cient exces s o f alkal i be present from

.

th e beginning to the end o f the reaction and the l iqui d still ,

remains alkal ine a fter all the alum has been decomposed the ,

product will contain sulphate This explains w h y it is directed .

that the al um sol ution must be poured into the alkal i solution ,
i

and not v i c e v e rs a it als o accounts for the inj unction to ad d

,
“

the alum solution slowly an d with constant stirring .

A luminum hydroxide is a very l ight voluminous precip itate , ,

forming an almost gelatinous magma which settles very slowly ,

i f at all and is there fore di ffi cult to wash It will o f course

,
.

settl e less readily in a den se liquid than in one les s dense Hence .

the addition o f hot water greatly facilitates the washin g by de

cantation But prolonged contact with boil ing water changes
.

the constitution o f the hydroxide from A l ( O H ) 3 to O A l O H and ,

the latter compound i s insolubl e in aci ds Hence th e l iquid in .

,

which the hydroxide i s suspended mu st not be boiling but only ,

hot .

T he washed hydroxide i s to be dri ed without much heat in

order to avoid its becoming hard an d gritty
-
.

A luminum hydroxi d e may al so be prepared from cryol ite as ,

described und er the title o f A luminum S ulphate .

It is chiefly prepared as a preliminary step in the preparation

o f sulphate chloride nitrate acetate and other aluminum salts
, , , , .

When prepared for this purpose th e hydroxide a fter h av i n g bee n

’

well washed is s imply drained but not dried be fore dissolved in

,

the proper acid .

260 ALU M I N U M N IT RA T E .

D e s cr i pt i onwhite light amorphous odorless and tasteless

—
A , , ,

p ow der insolubl
,
e in water and in alcohol .

AL U M I N U M N I TR A T E S OLU TI O N .

L I QUOR ALU M I N I N I TR A TI S

Contain ing about 10 per cent o f A l ( N O 3 ) 3 9 H zO —

37 5 .

A lum powdered
, 33 parts
S odium carbonate 3 0 parts
N itric acid 20 parts

'
D is solve the alu m and the sodium carbonate separately each ,

in 4 5 0 parts o f boiling water ; filter the solutions ; pour the sol u

tion o f alum into th e s olution o f sod ium carbonate stirring ,

briskly A dd 3 0 0 parts o f boiling water D igest the m ixture at

. .

a gentle heat until the evolution Of carbon dio xide ceases ; wash
the precipitate with hot distilled water first by decantation and ,

a fterward on a muslin strainer until the washings cease to ,

give a precipitate with test solution o f barium chloride L et

-
.

the ma gma drain thoroughly an d then dissolve it in the nitric

,

acid E vaporate the solution to 2 6 0 parts

. .

N ot e s The reaction taking place between the alum and s o

.

di a m carbonate and notes on that part o f the process are given

, ,

under the titl e aluminum hydroxide

,
.

This solution is employed as an astr i ngent and disin fectant .

A LU M I N U M O L EA T E .

ALU M I N I OLEA S .

Potash alum ~

White Castile soap in fine powder ,

D issolvethe alum in ml o f water and the soap in ,

ml o f hot water Pour the col d soap solution gradually into

.

the alum solution Warm the mixture until the ol eate se p arat e s
. .
262 ALU M I N U M S UL PH A T E .

aside to crystallize or evaporate to a syrupy cons istence and

, ,

s et it as ide to solidi fy on cooling .

R e a ct i on .

-
3 Ca F e2 then
Al N aO ) 3 —
3 N a H CO g ( O H )3 —
3 N a 2 CO 3 and finally , ,

N ot e s This aluminum sulphate is us ed for the preparation of

.

alum ( see alum and ammonia alum ) .

The q uantity o f sod ium bicarbonate indicated may not all be -

required .

It i s necessary that the diluted sulphuric acid should be com

w
.

p l e t e l y saturated ith aluminum hydroxide or in other words , , ,

that some o f that hydroxi de shoul d remain undissolved in the

aci d Hence it is recommended that only three fourths o f the
.
—

diluted acid be u sed at first and that a fter all o f the aluminum
,

h y droxide shall have been added the remainder o f the sulphuric ,

acid be added gradually according to the indications The whole .

quantity named can probabl y be sa turated with the al uminum

hydroxide obtained from the quantity o f cryolite used unless a
.

portion o f the hydroxide be lost in the proces s o f washing .

But the results are somewhat variable an d it i s therefore ne c e s

sar y to proceed cautiously .

Pu r e A l u m i n u m S ul ph a t e .

A lum 3 0 p arts
S odium carbonate 3 0 parts
S ulphuric acid 9 parts

D issolve the alum and the sodium carbonate each in 40 0 parts

‘

,
'
o f boil in g water filter an d pour the hot alum solution i nto th e
, ,

hot s olution of sodium carbonate stirring constantly D ige st , .

the mixture at a gentle heat until the evo l ution o f carbon d ioxid e
ceases Wash the precipitate with hot water until the w ashings
~

no longer yield a precipi tate w ith test soluti on o f barium chloride .

Then l et the precipitated aluminum hydrate dr ain as fa r as pos

‘
'

s ible and dissolve it with the ai d o f g e nt l é he at i n t h e s ulp hju ri q

, l
t

s
- —
 A M M ON I A . 26 3

acid previousl y diluted with 5 0 parts o f water ; filter the sol ution
, ,

evaporate it with constant stirring over a water bath until a , ,

nearly dry white salt remains .

N ot e s . A luminic hydroxide i s first prepared artic le . S ee

A luminum Hydroxi de p 2 5 8 for reaction and notes Then the
,
.
, .

sulphuric acid is saturated with the aluminum hydroxide Care .

must be taken not to l ose any of the hydroxide in the process

o f washing it for i f the quantity is insu fficient the acid can not
,

be saturated an d the product will then contain free sulphuri c

acid I f there is any reason for believing that any portion o f the
.

al um inum hydroxide has been wasted the amount o f sulp h uric ,

acid used may be reduced so as to in sure its saturation .

D e scri p ti on Pure aluminum sulphate i s a white crystalline

—

powder ; odorless ; taste sweetish astringent Permanent in the , .

°
ai r i f pr operly prepared S oluble in parts o f water at 1 5
.

Insoluble in al cohol .

A M M O N I A WA T ER .

L I QUOR AM M O N II
’

H Y D R OX I D I .

H 4N OH : :
35 ,
dissolved in water .

A mmonium chloride in coarse powder ,

. 80 parts
L ime 1 00 parts
D istilled water water each
, ,
s u fli c i e n t

S lake the lime with 2 parts o f water ; add the ammonium

chlori de to 2 0 parts o f water ; m ix the whol e well an d i m m e d i ,
.

ately introduce the mixture into an iron flask Connect the flask .

at once by means o f corks glas s tubes and rubber stoppers

, , ,

w ith a Woulff bottl e of the capacity o f 2 0 parts Connect this .

with a second Woul ff bottl e o f the sam e s ize and th is in turn ,

w ith a receiver o f the capacity o f 1 6 0 parts and containing 20 ,

parts o f d istilled water Conn ect the receiver with still another
.

bottl e containing 1 6 part s of distilled water The W ou l fi bot

'
.

tles are to be empty The second VVou l fi bottle and the receiver
.
‘

must each be provided with a siphon sa fety tube charged with a

very short column of mercury .
264 A M M ONIA .

The iron flask is placed in a sand bath and heat is appl i e d —

, :

Th e receiver is to be cooled by cold water A ll joi n t s be i ng

'

.
.

tight the heat i s gradually raised and continued until no more

,

gas passes over .

R e act i on . 2H 4 N C + Ca
1 OH ) 2
: I
-
Ca Cl z .

N ot e s For experimental pu rposes a glass flask may be used

.

instead o f that o f i ron but the proces s cannot then be continu ed

,

until all the ga s has been obtained which the ammonium chloride
will yield .

T he water i s added to the lime and ammonium chloride in

order to facil itate the reaction The calcium h y drate must be.

allowed to become cool be fore mixing it with the ammonium

chloride .

A t the c onclusion o f the operation there will be considerable

quantities o f liquid in all fou r bottles The W ou l fl bottl es will .

contain discolored ammonia solutions ; the third bottle or receiver ,

contains a strong solution o f ammonia wh ich is to be diluted ,

with distill ed wate r until o f the required strength ; the terminal

bottle contains weaker ammonia solution which may be strength ,

ened by charging it with an addi tional quantity o f gas obtained

by heating in a fla sk the contents o f h e W ou l fi bottl es t ‘
.

I f ammon ium carbonate i s used instead of chloride l ess heat ,

will be requ ired but in that case the gas must be passed through
,
“

a bottle containing milk o f l ime to fix the carbon dioxide .

In order to prevent accidents which may cause s erious re sults

the Pharmacopoeia directs that stronger ammonia water shall
be kept in s tr ong glass stoppered bottles onl y partially filled , ,

and pu t in a cool place I f the containers a re not su ffi ciently

.

strong and are too nearl y full and kept in a warm place they
, ,

may burst The gas is extremely caustic and acrid To inhal e

. .

o r smell ammonia without due caution i s attended with danger ,

and a full container with tightly fitting glass stopper sho uld -

never be opened especially i f it i s not co ol without turnin g the

, ,

face aside from it .

Val u a t i om water solutions o f ammonium hydroxide are

T wo -

contained in th e Pharmacop oeia o f the U nited S tates O ne i s .

called a qua ammoni ac ammoni a w at e r and i s required t obe o f a

, ,

strength correspond ing to 1 0 per cent o f H aN ; the ot her is called

2 66 A M M ON I U M A CE T A T E .

N ot e s . T he solution obtained i s usually stronger than

per 10

cent in which case it s imply requires dilution with the proper

,
:

proportion o f alcohol I f the solution be found to contain les s

.

tha n 1 0 per cent o f H 3 N the receiver may be reconnected and

the process continued S houl d the stronger water o f ammonia
.

used fail from any caus e to furnish s u fli c i e n t H 3 N to give the

product the requisite strength put a fresh porti on of ammonia ,
-

water in the flask and repeat the process .

I t has the s p gr and the s p vol

. . . .

A r om a ti c S pi r i t f
o A mm oni a .

A mmonium carbonate in translucent hard ,

pieces
A mmonia water '
O il o f lemon .

O il o f lavender flowers
O il o f nutme g
A lcohol
D i stilled water .

T o the amm onia water contained in a flask add ml o f

, , 1 40

d istilled water and a fterwards the ammonium carbonate reduced

,

to a moderately fine powder Close the flask and agitate the .

contents until the carbonate is dissolved Introduce the alcohol .

into a graduated bottl e o f suitable capacity add the oil s then , ,

gradually add the solution o f ammonium carbonate and a fter ,

wards enough distilled water to make the product measu re one .

liter S e t the liquid aside during twenty four hours in a cool

.
-

place occasionally agitating then filter it through paper in a

, , ,

well covered funnel

-
.

K eep the product in glass stoppered bottles in a cool place -

, .

D e scri pt i on nearly colorless liquid when freshly prepared

.
—
A ,

but gradually acquiring a somewhat darker tint

It has a pungent ammoni acal odor and taste
,
.

°
S pecific gravity : about at 1 5 C .

A M M O N I U M A C E TAT E S OLU TI O N .

L I QUOR A M M ON II
‘

A CE T A T I S .

S
[ pi r i t us M i n d e r e ri
j
A n aqueous solution containing about 7 per cent o f ammon ium
 A M M ON I U M A CE T A T E .
26 7

acetate ( H 4 N C H 3 O 77 ) together with small

2
quantities of z
z

acetic acid a nd carbonic acid .

A m monium carbonate
D iluted acetic acid

A dd the ammoniu m carbonate gradually to the col d diluted ”

acid and sti r until it is dissolved

,
.

This preparation should be freshl y made when wanted .

R e act i on .

H 4 N H CO 3 H 4 N N H zCO z f 3 H C2H 3 O 2
.
— —

: H
3 4 N C2
H 3 O 2+
H z O —
2 C0 2.

N ot es. T h e ammoniu m carbonate u sed must be in hard

translu cent pieces free from white pulverul ent bicarbonate
, .

To make a preparation such as the Pharmacopoeia intends ,

the diluted acid should be col d in order that the free carbonic
aci d which is formed may d issolve in su ffi cient quantity in th e
liquid T he presenc e o f this carbonic acid renders it i m p ra c
.

t i c abl e to determine the point o f neutral ization by means o f test

.

paper ; but the preparation as made is slightly aci d The solu , , .

tion shoul d have a pure acidulous sal ine taste or th e sal ine ,

taste modified only by that o f the carbonic acid ; a sl ight excess

o f acetic acid is des irabl e ; but any exces s o f alkal i is obj e ctionabl e .

E ven when neutral the sol ution gives an acid reaction to l itmu s
paper owing to the carbonic acid
.
.

When the ammon i um carbonate dissolves in the acetic aci d the

temperature is lowered on account o f the liberation o f carbonic ,

aci d gas This fall o f the temperature o f the l iquid i s a dvantage

.

ous as it aids the solution o f another portion o f the gas

, .

I n some pharmacopoei as ammonia water i s u sed instead o f ,

ammonium carbo nat e In this case the temperatu re rises Test

‘

. .

paper can be used to ascertain the reaction when thi s method -

i s followed but it i s directed th at the solution shall be not

, ,

neutral but slightly acid

,
.

The prep aration must not be filtered as that would expel nearly
all the c a rb o nic aci d
"

. .
2 68 A M M ON I U M C I T RA T E .

A M M O N I U M CI T R A T E S O LU TI O N .

L I QUOR A M M ON II CI T R A T I S .

A so lution o f ammonium c itrate each ml o f which contain s

Gm o f ( H N ) 3 C6 H O 7 is o ften employed in cl ea r ing cer
“

4 5

tain l iquids containing iron compounds and liable to becom e

cloudy or to form precipitates S mall additions o f s uch a solu
.

“ ”
tion to the preparations known as beef wine and iron and ,

el ixirs containing phosphate or pyrophosphate o f i ron assoc iated

with organic substances prevent the formation o f certain pre -

c i p i t a t e s containing iron or dissolve them when formed S uch

, .

a solution may also be advantageously employed in the prepar a

tion o f solubl e phosphate and pyrophosphate o f iron .

It i s prepared as follows :

Citric ac id 5 0 0 Gm
S tronger ammonia water ( 2 8 70 o f H 3N ) 43 0 ml
D istilled water .

D i ss olve
the aci d in the ammonia water N eutralize pe rf ectly .

by adding as much ammonia water as m ay be required T hen .

add enough distilled water to make th e whole measure ml .

S ol u ti on f
o Di -
a mm n i m H
o u -
y d r og e n Ci tr a te ,

may be prepared by adding 2 5 0 Gm o f citric aci d to ml

o f th e sol utio n o f normal ammonium citrate j ust described and
the n diluting with enough distilled water to make the whole
m easure ml .

E ach ml of this s olution contains Gm o f di ammonium -

hydrogen citrate ( H 4 N ) 2H C6 H O 7 5
.

T his solution is frequently us ed in the p re p a rat l on o f the

so l ubl e phosphate an d pyrophosphate of iron .

A M M O N I U M B E N Z OA T E .

A M M O N II B E N Z OA S .

H 4 N C7 H 5 0 2 : 1 39 .

D istilled
water
Water o f ammonia su fficient , .
«

27 0 A M M ON I U M B ROM I DE .

is first precipitated but redissolv es A fter the l iquid has st ood

.
.

for some time u nder the pressure o f the g as the bicarbonate is ,

separated When no more crystals a re formed a stratum o f

.

al cohol cautiously laid over the mother liquor will cause t h e

dep osition o f an additional crop T he salt may best be preserved .

in g l a s s tubes filled with carbon dioxide and sealed

‘

A n oth e r M e t h od .

D issolve the ammonium carbonate from p owdered or d i

ou t

nary ammonium carbonate by macerating it with twice its weight

o

o f alcohol for a few minutes A fter separating the alcoholic .

solution o f the c arbonate wash th e undissolved ammonium bi , ,

carbonate with another portion of alcohol us in g the same qua n ,

tity as be fore E xp ose the product t o the ai r until the alcohol

.

ha s evaporated and then bottl e it ,

.

The carbonate may also be removed by maceratin g th e o rdi

nary ammonium carbonate for t w o hours w ith tw ice its weight
o f water .

D e scr i pt i on
Colorless crystals or a white crystalline powder
.
—
,

o f ammoniacal ta ste and faintly ammoniacal odor ( or nearly

S oluble in
°
odorless i f qu ite dry ) parts o f water at 1 5
.

I nsoluble in alcohol .

AM M O N I UM B R O M ID E .

A M M ON II B ROM I DU M .

H 4 N B 1 2 98
‘

I ron wire
B romine
A mmonia water
D istilled water .

Put the iron wire into a flask add 5 0 parts o f wa rm ( not ,

h ot ) water and then gradually add 9 parts o f bromine

, Pu t a .

loos e plug o f cotton into the neck o f the flask and shake g ently ,

from time to time until a green ish l iqui d i s obtained having no

odor o f bromine Filter this solution o f ferrous brom i de a dd
.
, ,

the remainder o f the bromine to the filtrate and shake g e ntl y ,

so that a uni form solution m ay be obtained .

 AM M ON I U M B RO M I DE . 27 1

Pour this solution into the ammonia water previously diluted

with 5 0 parts o f distilled water S hake well Heat the mix . .

ture over the water bath for hal f an hour Then filter When
-
. .

the liquid has passed through the filter wash the residue u p on i t ,
'

with some hot distil led water lettin g the washings run into the ,

filtered solution .

E vaporate the liqui d in a porcelain d ish until a pellicl e begins

to be formed Then stir the contents w ith a gla s s rod whil e
.

continuing the evaporation until a granular salt remains S houl d .

this not be per fectly white or colorles s redissolve it in its own ,

weight o f boil ing d istilled water add a su ffi cient quantity o f a m ,

monia water to render the solution sl ightly alkaline to test paper -

,

boil the l iqu id a few m inutes filter it an d evaporate the filtrate , ,

to dryness as be fore .

R e act i on .

2F e + 2 B r2 2 2F e Br then 3 F e B r then
F e B r2 . 2 F e B r3 + 8 H 4
N OH r 8 H 4 N B r + F e O F e 2O 3 + 4 H zO
. .

D e scri pt i on é Colorl ess transparent crystal s or a white crys

—
, ,

t a l li n e granular salt odorless o f pungent saline taste S olubl e

, , .

°
in parts o f water and in 3 0 parts of alcohol at 1 5 C ;
,
.

in parts o f boiling w ater and in 1 5 parts o f boiling alcohol

,
.

A n oth e r M e th od .

B romine 25 parts
A mmonia water .

Water .

Hydrogen sulphide .

S hake parts o f water with 5 parts o f brom ine Conduct

20 0 .

a stream o f hydrogen sulphide into the l iqu id When the liquid .

i s no longer rendered turbid by th e hydrogen sulphide add a n ,

other 5 parts o f bromine and again d irect hydrogen sulphide ,

I nto the liquid until the red color disappears R epeat the addi .

tion o f bromine 5 parts at a tim e and the treatment with h y

, ,

d rogen sulphide until all of th e bromin e has been used and con ,

verted into hydrobromic acid by the current o f h y drogen sul

p h id e .

Filter out the sulphur and h eat the filtrate to expel the exces s
27 2 A M M ON I U M C ARB ONA T E .

of hy dro g en sulphide from the l iqui d When filter pap er moist .

e ne d with a soluti on o f lead acetate is no longer blac kened by

the l iquid fil t er again S upersaturate the filtrate with a m

, .

monia ( abou t 6 0 parts will be required ) .

E vapor at e the s olution of ammon ium bromide until salt be

gins to separate Then add a l ittl e more ammonia a fter which
.
,

c ontinue the evaporation to dryness stirrin g constantly , .

R e act i on .

B r2 + H 2 S 2 2H Br+S ; then
H B r+ H 4 N O H :
.
H 4 N Br —
H 20 .

A M M O N I U M CA R BA M A T E .

A M M ON I I GAR D A M A S .

H 4N H Z N CO z ) 2
7 8 .

D issolve th e ammonium carbamate from powdered ordinary

ammonium carbonate with strong alcohol and evaporate the a l
c oh ol i c solution to drynes s by the aid o f very moderate heat ( not
°
exceeding 2 5

D e s cri pt i on .
-
A whit e powder readil y oluble in water and in
s
alcohol .

AM M ON IUM C AR B O N ATE —
O FFI C I N A L .

A M M O N II C AR B ONA S O FF I C I N AL I S .

( H a r ts h or n S al t .
)
A pproximately H 4 N H CO g H 4 N H 2N C0 2
. = 57 1 .

This i s a somewhat variabl e m ixture o f ammonium hydro g en -

carbonate and ammonium carbamate .

It i s manu factured on a large scal e by heating a mixture o f a m

m on i um su l phate ( or ammonium chloride ) and calc ium carbonate ,

when the s o called ammonium c arb onat e s ubl ime s and is con
-

d e nse d .
2 74 A M M ON I U M C H LOR I DE .

nine parts of warm ammo nia water ( containin g 1 0 per cent o f

H 3 N ) in a closed bottle Cool the solution so that crystals may
.

be formed Collect and drain the crystals quickly and press

.

them gently between cloths or bibulous paper Bottle at once . .

R e act i on .

H 4 N H CO s H 4 N H 2 N CO z
.
2 C0 3 .

D e s cri pt i on
Colorless crystals o f ammoniacal odor and ta ste ;
.
—

soluble in their own weight of water at

A M M O N I U M CH LO R I D E P U R I FI E D —
.

'
A M M ON II CH L OR I D U M P U R I F I CA T U M .

H 4 N C12 5 3 4 .

The impurities l iable to be present in crude sal ammonia c or

crude commercial ammonium chlori de are the chlorides and sul
,

p h a t e s o f iron and o f calcium The iron compounds may be .

both ferrous and ferric but are usually ferrous O f the i m

, .

purities mentioned the most common i s ferrous chloride This .

does not discolor the ammonium chloride until the sal ammoniac
i s exposed to the air s o that the ferrous salt is oxidized to ferric .

The sal ammoniac shoul d be tested for ferrous salt ferric salt , ,

sulphates and calcium with test solutions o f potass ium ferri

,

cyanide potassium ferr ocyan ide bari um chloride and a m

, , ,

m on i u m carbonate o r Oxalate successively in the u sual w a y , ,

.

S houl d all o f the impurities named be present they may be r e ,

moved as follows

D issolve the I mpure ammonium chloride in about twice its

weight o f water or les s Heat the sol ution t o boil ing Filter
, . . .

A d d solution o f barium chlorid e in small quantities to the hot

filtrate and stir well A s soon as a further addition o f barium
.

chloride no longer causes turbidit y in a filtered test p ortion of the -

l iquid add a sol ution o f ammonium carbonate or oxalate to com

,

p l e t e l y pre c ipitate the calcium and the excess o f barium Filter . .

Then add to the filtrate about 2 5 ml of strong chlorine water for

each kilogram o f ammon ium chloride in solution Boil for .

t wenty or thirty minutes Then add enough a mmo n ia water t o

.
 A M M ON I U M C H LOR I DE . 27 5

render the l iqu id alkaline and to impart an ammoniacal odor to it .

Filter again E vaporate the filtrate to

. sp w and then . .

set it asid e to crystall ize or evaporate nearly to dryness and dry

,

the granulated salt perfectly in the usual way .

When salts o f organic bases are pres ent in the crude sal a m
moniac made from gas l iquor they should be destroyed by boiling
1 00 parts of the crude product with 1 2 5 parts o f water an d 1 5

parts o f concentrated nitric aci d until no more acid vapors are

evolved The residue may then be treated as before described
.

to remove the chlorides and sulphates o f calc ium and iron .

S houl d ferrous chloride be found to be the only impurity pres

ent treat the solution o f the impure ammonium chloride with
,

chlorine water an d ammonia as described S hould the product .

be not entirely free from i ron a fter one treatment repeat the ,

add ition o f chlorine water boil again , a dd ammonia in exces s as

,

before and again granul ate or c rystall iz e the product .

When ferric chloride is the only impurity the process o f p u r i fi

cat i on I S simple
”
Crude ammonium chloride
Water
A mmonia water
D issolvethe ammonium chloride in the water heated to boiling .

A dd the ammonia water Continue the boiling for a few minutes

. .

Filter E vaporate to granulation D ry the product thoroughly

. . .

Pu r e A mm oni u m Ch l or i d e

may be readily made from pure diluted hydrochloric aci d and pure
ammonia water :

hydrochloric acid ( 1 0 % o f
D iluted H Cl )
A mmonia water ( 1 0 % o f H N ) 3

A dd the ammonia water gradual ly to the acid stirring well ,

.

E vaporate to granulation or crystallization and d ry the product , .

R e act i on . H 3N + H Cl N Cl .

Pure ammonium chlori de i s a colorless crystall ine

D e s cri pt i on —
,

or a white g ranular salt ; odorless taste sal ine cool in g S oluble

, , , .
27 6 A M M O N I U M I OD I DE .

in 3 parts o f water o f and in its own weight o f boiling w ater .

N earl y insoluble in alcohol R eaction neutral

. Volatilises w 1th .

o u t residue when strongly heated .

AM M ON IUM IOD ID E .

A M M ON I I I OD I D U M .

Potassium iodide
A mmonium sulphate
A lcohol
D istilled water

the salts each in 6 parts o f d istilled water ; filter the

D issolve ,

solutions ; m i x them ; evaporate the filtrate to about 1 5 parts ;

set the liquid as ide in a cool place for a bout twelve hou rs ; add
the alcohol to the s ol u t i on a n d set the mixture in an ice water
'

bath until cooled down to separate and rej ect the crystals o f
potassium sulphate wh ich are now separated and add a little
, ,

ammon i a to the cl ear solution and evaporate it to dryness .

Put the product in a dry bottl e which must be tightly closed

, ,

and kept in a dark place .

R e acti on . 2 KI +

N ot e sThe alcohol i s added to facilitate the separation o f the

.

potassium sulphate which is insoluble in diluted alcohol whil e

, ,

the ammonium iodide is soluble The solution may a fter standing

.
,
°
twelve hours be cooled to 5 on an ice water bath be fore the alco
,
-

hol i s added the cl ear solution then separated from the crystal s
,

o f potas sium sulphate by throwing the whol e into a cooled glas s

funnel having a loose plug o f moist cotton placed in its throat .

The filtrate may then be evaporated to dryness and the ammon ,

ium iodide extracted from the d ry salt mas s by means o f warm -

alcohol which will leave the potassium sulphate undissolved The

,
.

alcoholic so lution of ammon ium iod ide may then be allowed to "

evaporate until the dry salt is obtained The yield o f ammonium .

iodide from 6 parts o f potass ium iodide should be about parts ,

which i s soluble in 5 0 parts o f warm alcohol .

278 A M M O N I U M OXALA T E .

happens that the liquid gradually acquires an acid reaction ; this

shoul d be corrected by th e addition o f enough am monia to restore
.

a s l i g h tly alkal ine reaction before the l iquid i s set as id e to crys

tal li ze .

D e s cr i p t i on .
—
L ong colorless prismatic c rystal s or
, fused , , a

white mass O dorless Taste sharp and bitter Hygroscopic

. . . .

S oluble at I 5 in hal f its w eight o f water or in 2 0 parts o f alcohol ;

°

very soluble in boiling water and in 3 parts o f boiling alcohol , .

A M M O N I U M OXALA T E .

AM M O N II OX A L A S .

( H 4 N ) 2
2 C 0 4 H 2 0 = I 42

O xalic acid
Boiling distill ed water
A mmonium carbonate su fficient ,
.

D issolvethe acid in the water neutral ize with ammonium car ,

bonate raising the temperature at the end o f the neutralization

, , ,

to the boilin g point ; filter whil e hot ; and set aside to cool and
crystallize .

R e acti on . 2 + 3 H 2CzO ,

N ot e s . A bout
Gm o f ammonium carbonate will be required
83
to saturate 1 0 0 Gm o f oxalic acid Instead of 8 3 Gm of ammon .

ium Carbonate the correspondin g quantity ( 2 7 0 ml ) of ammonia

,

water ( 1 0 per cent ) may be used The solution shoul d be ren .

dered exactly neutral to test paper filtered whil e hot and set -
, ,

aside to cool slowly When the solution i s dilute and the cooling
.

and crystall ization slow very handsome needle shaped crystals ,

-

may be obtained By evapo rating the mother l iqu or and again

.

crystallizi ng additional crops o f the salt are recovered ;

,

D e scr i p t i on —
This salt crystallizes in rhombic prisms e asily ,

solubl e in wate r .
 A M M ON I U M PH O S PH A T E . 27 9

A M M O N I U M PH O S PH A T E .

A M M ON II PH OS PH A S .

Prepared by adding strong ammon i a solution to diluted phos

p h o r i c acid until a slightly alkaline reaction on test paper is pro -

d uc e d .The solution is then evaporated the alkal ine reaction ,

being maintained by adding a l ittle more ammonia from time to

time as required The crystals formed upon allowing the solu
, .

tion to cool are collected and quickly dri ed on bibulous paper

placed upon a porous tile .

A mmonium phosphate must be kept in well stoppered bottles -

.

Transparent colorless p risms inodorous of a

D e scri pt i on .
—
, , ,

somewhat alkal ine salin e taste R eadily soluble in water ; insoluble

.

in alcoh ol .

AM M O N IUM SU L PH A T E .

A M M ON II S UL PH A S .

H
( 4N )2 S O ,
= 1 3 2 .

A mmonia water
D iluted sulphuric acid

A dd the aci d gradually to the ammonia water stirring th e ,

l iquid S hould the solution not be alkaline in its reaction on test

.

paper add enough additional ammonia water to render it alkaline

, .

Filter E vaporate to crystall ization D uring the evaporation test

. .

the l iqu id from time to time with l itmus paper and add more ,

ammon ia i f n ecessary to prevent the solution from acquirin g an

acid reaction or to render it alkaline again shoul d it become acid
,

by the loss o f ammonia .

R e act i on .

t i on Colorless and odorless cr y stals soluble in

D e scri p .
—
,

parts o f water at
 A M M ON I U M VALERAT E .

AM M ON IUM V ALE R A T E .

A M M ON II VALER I ANA S .

N H 4 C5 H 9 0 2 2 1 19 .

Prepared by saturating valeric aci d with dry ammonia gas ,

usuall y generated from a mixture o f equal parts o f ammonium

chloride and lime The heat produced by the chemical union keeps
.

the salt in a liquid condition and on cool ing the valerate cr y stal
,

lizes The salt cannot be crystallized from an aqueou s solution

. .

A solution of ammonium valerate may be readil y prepared by

dissolving 1 0 2 Gm o f valeric acid in 6 1 Gm o f stronger water o f
ammonia ; i f d iluted w ith distilled water until it measures 2 3 8
mill il iters each ml o f this solution will contain
,
Gm o f the
salt .

N eutral ammonium valerate easily parts with ammonia and be

comes acid ; in solution it i s to be care fully neutral iz ed with a m
monia water .

t i on
Colorless crystalline plates solubl e in water and
D e s cr i p .
—
,

alcohol and having the odor o f the acid They should volatilize
,
.

com pletely .

A N TI M O N Y CH LO R I D E .

A N TI M ON I C H L OR I D U M .

S bCl 3 2 226 .
5 .

A ntimonou s oxide
Hydrochl oric acid ( 3 2 % o f H Cl )

Heat gentl y together in a porcelain dish stirring well until t h e , ,

acid ceases to dissolve any more o f the oxide Then rai s e the .

te mperature slowly to the boiling point and continue boiling until

a drop o f the liqu id deposits cr y stals on cool ing Then pour the .

l iquid int o a retort provided with a thermometer in the tubulure

and distill heatin g th e retort in a sand bath
,
The distillate at .

first consists o f h y d r oc h l or i c acid which is to be collected separ

.
,

atel y A s soon as the boiling point rises to 2 0 0 and a drop of the

.
°

distillate solidifies on a cold surface change the receiver and con ,

28 2 A N TI M ON Y ox 1 D E .

D e scr i pti on .
—
A
yellowish red l iquid o f the odor o f h y drochloric-

acid It gives a white precipitate whe n mixed with water S p w

. . .

about s p v ol It can be diluted w ith

. . times its
'

own weight Of water w i th ou t p e rm a ne n t preci pitation

‘

A N TI M O N Y OX I D E .

A NTI M ON I OX I D U M .

S b20 3 2 28 7 ( or S b4 0 6 :

Purified antimonou s sulphid e in very fine powder ,

. . 1 00 parts
Hydrochloric acid 3 5 % of H Cl ) 53 0 parts
A mmonia water ( 1 0 % o f H 3 N ) 1 1 5 parts

Water .

Put the hydrochloric acid in a flask capable o f holding 1 0 0 0

parts of water H eat to about
. A dd the fi nely powdered a n
t i m on y s ulphide in small portions shaking well and waiting a fter
, , ,

each addition until the evolution o f hydrogen sulp hide has nearl y
ceased before adding another portion Of the sulphide of antimony .

°
Continue the heat at 50 and add hot water from time to time to
maintain the volume o f l iquid in the flask or to keep the flask ,

about hal f filled When all o f the antimony sulphide has been
.

added and the evolution o f h y drogen sulph ide becomes very slow ,

heat the contents o f the flask to boil ing and continu e the boiling
for hal f an hour still adding enough hot water from time to time
,

to keep the volume o f the contents o f the flask nearly constant .

V
Then let the l iquid cool Filter it through muslin into a porcelain
.

d ish A dd j ust enough water to produce a sl ight but permanent

.

turbidity Boil the l iquid again for about five minutes Filter
. .

again Pou r the fil trate slowl y into 2 5 0 0 parts o f water contained

.

in a glas s or stoneware vessel stirring the mixture dil igently du r ,

ing the addition o f the antimony solution to the water L et the .

precipitate subside S iphon o ff the supernatant l iquid and add

.

to the precipitate 2 5 00 parts o f hot water stir well l et stand until , ,

t h e precipitate has settled and then draw o ff the wash water , .

.

R epeat this w ashing once more in the same manner with another , ,

2 5 0 0 parts o f hot water and siphon o ff the l iquid Then add

,
.

th e ammonia water to the precipitate let the mixture stand for an ,

h our stirring frequently

,
Collect the precipitate on a filter a n d
.
 A N TI M ON Y OX ID E . 28 3

wash it with boiling water until a test portion o f the washings -

a fter acidulation with nitric acid no longer produces a clou dines s

,

with test solution o f silver n itrate Then drain the oxide and dry
-
.

it at a temperature not exceeding

R eacti on s . S b2 S 3 + 6 H Cl z s C13 + 3 H 2 S ;

then —
I oH Cl ; and ,
finally ,

l
—— 2 H 4 NC1+ H zo .

N ot e s . A very large exces s o f hyd rochloric acid i s used in

order to hold the antimony chloride in s ol t i on N evertheles s the .
,

action o f th e acid upon th e antimony sulphide is slow A high .

temperature is necessary The operation shoul d be carried out

.

under a h oo d with a goo d draught to carry off the vapors o f h y

drogen sulphide .

S ome hydrochloric acid is lost by volatilization during the

process o f heating it with the antimony sulphide A hydrochloric .

aci d o f les s than 3 5 per cent s p w ) st r en g th does not dis

. . .

solve the antimony sulphide completely .

The antimonous sulphide should be pu r e and in very fine i m ,

”
palpable ) powder I t may be tested before being u sed to see
.
,

that it is soluble in the strong hydrochloric acid without any res i

due .

The purified antimonous sulphide o f the Pharmacopoeia a l ,

though nearly or qu it e free from arsenic may contain some lead , .

The lead chloride derived from an impu re antimony sulphide i s

washed out fro m the pre cipitated oxychloride o f antimony by
“ ”

means o f hot water .

S odium carbonate may be used in stead o f ammonia water ( u s

ing 9 5 parts of t h e carb onate in place o f 1 1 5 parts o f ammonia
water ) .

D e scri p t1 0n heavy l ight grayish or nearly white odorless

.
—
A ,
—
, ,

and tastel ess powder insolubl e i n water and in alcohol It turns

,
-
.

yellow when heated but becomes white again on cooling

, .

A n ot h e r M e t h od .

Hea t powdered antimonou s sulphide in the ai r until sulphurous

28 4 AN TI M ON Y OX Y C H LOR I DE .

vapors cease to be g iven o ff and a fus ed g lassy residue is

, oh

ta i n e d :

The glassy antimonous oxide is translucent and may be reduced

to a white powder .

T his method of preparation i s called roasting .

A N TI M O N Y OX Y CH LO R I D E .

A N TI M ON I O X Y C H L OR I D U M .

( A lgaroth s Powder’

) .

2 S bO Cl . S b, O g -6 3 o 8
r . .

Prepared by pou ring a solution o f antimony chloride ( see

A ntimon y Chloride S olution and A ntimony O xide ) into a l arge
quantity o f water The d irections given under the titl e A ntimony
.

O xide down to and including the washing o f the p recipita t ed

oxychloride with hot water may be foll owed ( the treatme nt o f
the washed precipitate w ith ammonia being omitted ) The prod .

u e t is then dried with the aid of heat .

It is a white insolubl e powder

,
.

A N TI M O N Y L P O T A S S I U M T A R T R A T E
-
.

A N TI M ON I E T POT A S S I I TA R TR A s .

[ Tartar E metic ] .

2 K S bO C4 H 4 O6 I .

A ntimonous oxide parts

4
Potass ium bitartrate 5 parts
Water 5 0 parts

M ixthe oxide and the cream o f tartar with enough water to

form a paste and set this aside for twent y four hours Then add
,
-
.

the remainder o f the water and boil the m ixture in a porcelain

capsule for fi ftee n m i n u t e s s t i r r i n g f re q uently and replacing the
,' ,

water lost by evaporation Filter whil e hot evapo rate the filtrate
.
,
 286 AN TI M ON I C S UL P HID E .

Rinse the crystals hastily with a little weak soda solution and ,

d r y them by pres sing them between bibulous paper [ These .

“ ”
crystal s are the s o called S c h l i p p e s S alt
-
’

D issolve 1 00 parts o f thes e crystals in 4 0 0 p arts of distill ed

water Filter i f necessary D ilute the filtrate with s ix hundred
.
, .

parts o f distilled water and pour the dilute solution slowly and
,

w ith constant stirring int o a mixtu re o f thirty six pa rts ( by -

weight ) o f sulphuric acid and s ix hundred parts o f distill ed

water .

Wash the precipitate as rapidly as possibl e by a ff usion and de ,

cantation with distilled wat er let drain expres s the remainder

, , ,

o f the w ater and d ry the precipitate with the ai d o f gentle heat

, .

Keep it in a tightly corked b ottle protected from light , .

R e act i on .

4s S 3 + 4 S z+

then , 2 N a3 S bS 4 + 3 H 2 S O 4 + I O H zO

Th e direction t o wash the crystal s o f S c h l i p p e s s alt i s

N ot e s .
’

given for the purpose of removing sul pharsenate which i s mor e ,

readily soluble and a l ittl e sodium hydroxi de is added to the wash

,

water in order t o prevent oxidation .

The sulphuric aci d must be l n excess ; otherw is e the p roduct

will be dark colored .

The washing must be done with distilled water and should not ,

be long continued A ffusion and decantation is therefore t o be

.

preferred .

S everal formulas prescribe an excessive proportion o f sulphu r

equal weights o f sulphur and antimony sulphide
—
.

D e scri pt i on orange red odorl ess insoluble powder

.
—
An -
, , .

“
This preparation i s identical with the sulphurated antimony
“
o f the B ritish Pharmacop oeia an d with the ol d golden sulphuret
o f a n t i m ony i I t is redder than the sulphurated antimony o f the
’

Pharmacopoeia o f the U nited S tates and the Kermes M ineral o f

the old p harmacopoeias both o f which contain S b,, S but not
, 3 ,

s Ss .
 A N TI M ONOU S S UL PHI DE . 28 7

A N TI M O N OU S S UL PH I D E .

A N TI M O N I S U L PH I D U M N I GR U M .

S b2 S 3 z 3 3 6 .

N ative antimony trisulphide ( antimonite ) purified by fusion , ,

and as free from a rsenic as it can be obtained constitutes the ,

“ ”
antimony sulph ide o f the Pharmacop oeia .

D e scri pti on .
—
D ark
steel gray striated crystalline masses o f -
, ,

metall ic lustre form ing a black o r grayish black lustrel ess pow
,
-

d er whe nreduced to a very fine state o f division ; odorless ; taste

l ess ; insoluble i n water and in alcohol S oluble in s tr ong hydro .

c hloric aci d with evolution o f hydrogen sulphide .

Pu r i fie d A n ti m ony S u lphi d e .

A ntimon y sulphide
Water of ammonia

R educe the antimony sulphide to a very fine powder S eparate .

the coarser particl es by elutriation and when th e finely divi ded ‘

, ,

sulphide has been deposited p ou r off the water add the water o f , ,

ammonia and macerate for five days agitating the mixture f r e

, ,

quently T hen let the powder settl e pour off the water o f a m
.
,

monia an d wash the residue by repeated a ff usion and decantation

,

o f water Finally dry the product by the aid o f heat

.
, .

N ot e By this treatment al l but traces o f arsenic i s removed as

.

soluble ammonium sulph arsenite -

.

D e s cri pti on . An
impalpable heavy grayish black lustreles s
-
, ,
-
, ,

odorl ess tasteless insolubl e powder

, ,
.

S ul ph u r a t e d A n t i m on y .

Ch i e fl y antimonou s sulphide with a very smal l amount o f anti

mon ou s oxi de .

Purified antimony sulphide

S olution o f sodium h y droxid e
’

D iluted sulphuric acid su fficient ,

.
28 8 A N T I M O N OU s S UL PHID E .

M ix the antimony sulphide with the solution of sodium h y d rox

ide and 3 0 parts of distilled water and boil the m ixture gently ,

for two hours constantly stirring and occasionally a dding d is

, ,

til led water so as to preserve the same volume S train the l iquid .

immediately through a double musl in strainer and drop into it , ,

while yet hot d iluted sulphuric acid so long as it produces a pre

,

c i p i t at e .

Wash the precipitate with hot distilled water until the washings
are at most but very slightly clou ded by test solution of bariu m
°
chloride ; then dry the precipitate at 2 5 an d rub it to a fine pow
der .

R e act i on .

First ,
then
2 N a3 S bO 3 + 3 H z S O 4 z
3N a2S O4 + s O 3 l 3 H zO
— —
,
and
z N a3 5 b5 3 + 3 H , s o ,

N ot e s The antimony sulphide must be in the form o f an i m

.

” “
palpabl e powder This product is n ot the same as the sulphur
.

”
ated antimony o f the B ritish Pharmacopoeia ; the B R preparation
consists mainly o f s S 5 ( see A ntimon ic S ulphide ) ; neither is ‘
“ ”
it the Kermes M ineral o f the ol d pharmacopoeias The Phar .

m a c op oe i a o f the U nited S tates nevertheless gives this prepara , ,

tion the title o f the B ritish ofli c i a l precipitated antimony sulphide

“
a s well as the synonym Kermes

D e s cr i p t i on . A
reddish brown or brown red odorless taste
— — -
,

less insolubl e powder I t is redder than Kermes M ineral but

, .
,

not so red as the antimonic sulphide or sulphu rated antimony o f

the B ritish Pharmacopoeia .

O x ys u lph u r a te d A n ti m ony .

( KE R M E s M I NERAL . K ERM E S A N TI M ON I ) .

Purified antimon y sulphide 1 part

S odium carbonate 25 parts
0

Put the sodium carbonate together with 2 5 0 parts o f water , ,

into an iron pot and heat to boil ing A dd the sulphide a n d c on

, .
'

t i n u e boiling for two hours stirring constantl and replacing the

y , ,
29 0 AR S ENOU S A C I D .

I f sodium hydroxide be u sed instead of the carbonate the prod ,

u c t i s nearly the same in composition but has an altog e ther ,

di ff erent appearance .

Kermes mineral does n ot deserve a place in any pharmacopoeia ,

an d ver y few pharmacopoeias now contain it I t i s a rel ic of the .

times when peculiar physical properties du e to extraordinary

methods o f preparation were often without reason hel d to be , ,

indicative o f extraordinary m edicinal virtues .

D e scri pt i on Prepared care fully in strict obedience to the d i r e c

.
—

tions g iven kermes mineral i s a beauti ful velvety dark purplish

, , ,

bro w n p ow de r
~
M inute crystal s o f a n
. timonou s oxide may be seen
under the microscope as shin ing particles in the product .

The Pharmacopoeia o f the U nited S tates ( 1 8 90 ) gives t h e

“ ”
synonym Kermes M ineral to the antim onous sulphide p r e c i p i
t a t e d from a solution o f sodium sulphantimonite by the addition
o f sulphuric acid ; but t hat is n ot the kermes mineral o f the ol d
pharmacopoeias .

The N orwegian Pharmacopoeia directs the preparation of

kermes m ineral by m ixing 1 part o f antimonous oxide with nine
parts of prec i p i tated sulphide .

A R S E N OU S A CI D S OLU T I O N .

L I QUOR A CI D I A R S E N OS I .

A rsenou s oxide .

H y drochloric acid
D istilled water su fficient , .

Boil the arsenous oxide with the aci d diluted with 2 5 0 m l o f the
water until dissolved F ilter the solution pass enough distilled
.
,

water through the filter to make the product measure 1 l iter an d ,

m i x t h e whole well
, .

N ot e s The presence o f h y drochloric acid materially aids the

.

solution o f the arsenous oxide When dissolved in the water the .

oxide is p oba bl y con v e rt e d i n t o arsenous acid

s
r

A s, 0 3 +3 H , 0 —
2H 3 A s o, .

This preparation was formerly e rroneou sl y call ed solution o f

 ARS ENOU S I OD I DE . 29 1

chloride o f arsenic ; it probably contain s ve ry l ittle arsenou s

chloride .

D e s cr i p t i on .A colorles s solution with an aci d reaction

—
It .

g i ve s‘
a b right yellow precipitate with hydrogen sulphide .

A R S E N OU S I O D I D E .

AR S E N I I OD I D U M .

A 3 1 3 =4 54 5 ° °

0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0

Triturate until finely powdered and thoroughly m ixed Pu t .

int o a flask and heat gently on a water bath incl ining the fla sk -
,

in di ff e rent directions until fusion takes place Pour the fused

, .

mas s upon a porcelain slab and l et i t cool then break it int o . ,

pieces and keep it in well stoppered bottles in a cool place .

D e scr i pt i onThe product consists o f glossy orange red crys

— -

t a lli n e masses or scales having an odor o f iodine I t decomposes .

on exposure to ai r and light .

S ol u ti on o f A r s e ni c an d M e r cu r i c I od i d e .

D oN OVA N s
’
S OLU TI O N .

A rsenic iodide
M ercuric iodide
D istilled water su fficient , .

Triturate th e iodides with 1 5 parts o f distilled water until dis ,

solved Filter th e liquid and pass enough distilled w ater

.

through th e filter to make the product w eigh 1 0 0 part s .

Keep the product in a dark place .

'
N ot e s . No
chemical reaction takes place in dis solving the t w o
iodi d es together ; but the mercuric iodide i s soluble in the solution
o f arsenic iodide although almost insoluble in water
, .

The arsen ic iodide must not contain free iodine The prepara .

tion does not remain unchanged a long time It must be odorless .

and only pale yellowish not having any odor o f iodin e nor a —
29 2 AR S ENOU S OX ID E .

reddish color A s soon as it acquires the odor o f iodin e or

. a

reddish color it should be thrown away .

D e scr i pti on A
clear pal e yellowish liqu id without od or but
“
—
.
,

havin g a n a useous metallic taste .

A R S E N OU S OXID E .

AR S EN I OX I D U M .

A 840 6 =3 96 .

i um th e P h ar m a c opoe i as
( A c d u m A rs e n os
.
f
o .
)

A heavy sol id ccurring either in transparent colorles s g las sy

, o

masses or white porcelain l ike or in white powder ; very

,
-
,

poisonous .

For medicinal u ses it must be in extremely fine powder I t .

may be powdered by trituration in a porcelain mortar ; but it

should be kept moi st with alcohol while triturated t o prevent t h e
risin g of the poisonous dust .

Forms a permanent solution in 8 0 parts o f water D issolves .

slowly unless the solution is aide d by heat .

BAR IUM A C ETA TE .

B AR II A CE T A S .

B a Cs o z 2 - H 20 2 273 °

Barium carbonate
A cetic aci d
Water

D issolve filter and evaporate to crystallization D ry the crys

, , .

tal s in a desiccator over sulphuric acid or with the aid o f heat , .

Keep the product in a t i g h t l y closed bottle .

D e scr i pt i on .
—
White deliquescent odorless ; readily solubl e
, , .
2 94 B AR I U M C H LOR I DE .

R e ac ti on .

B a ( N O g ) 2+ ( H 4 N ) 2CO 3 z B a CO 3

N ot e s . A mmonium carbonate is prescribed instead of p ot a s

s ium or sodium carbonate because it is scarcely possibl e to re

,

move all potassium or sodium salt from the precipitated barium

carbonate while ammonium salt is easily removed A mm onia
,
.

water i s added not only to convert the ordinary carbonate int o

the normal salt but also because the barium carbonate is some
,

w hat sol uble in ammonium nitrate solution but not in the a m ,

m on i a c a l l iquid obtained by the addition o f an excess o f a m

mon 1 a .

'
D e s cri pti on .
-
A h e a vy
white insolubl e odorles s and tasteles s
, , ,

powder . Completely soluble in nitric acid and in hy d r oc t r i c

acid
O th e r M e t h od s .

From heavy spar ( barium sulphate ) the carbonate of bar i um

can be obtaine d by heating to redness an intimate mixture made
o f 1 0 parts o f powdered heav y spar 2 parts o f powdered charcoal , ,

and 5 parts o f potassa and then washing the fu sed mass with
,

water when the undis solved residue is barium carbonate

, .

The impure native barium carbonate call ed w itherite may be

converted into chloride as described under the titl e B ariu m C hlor
ide and the pure carbonate then made from the chloride by pre
,

c i p i t a t i on with ammonium carbonate .

BAR I UM CH L O R I D E .

B AR II C H L OR I D U M .

Powdered witherite
Hy drochloric acid of H Cl )
Barium sulphide .

Water .

M ix the witherite thoroughl y with its own weight o f wate r .

. in
 B AR I U M C H LOR I DE . 295

a porcelain dish Then add gradually the hydrochloric acid

.
, ,

previously mixed with 1 0 parts o f water stirri ng well waiting , ,

a fter each addition o f the dilute acid until the e ff ervescence has
subsi ded be fore adding more When the interaction becomes .

tardy heat the dish over the water bath to facilitate the satura
,
-

tion o f the acid When all o f the acid has been added
.
,

evaporate the unfiltered liquid to dryness and heat the dry ,

residue at about 1 0 0 for hal f an hour Then add 5 0 pa rt s o f

°
.

bo iling water ; stir well continuing the heating and sti rring about
,

Filter A dd to the filtrate a solution o f barium

'

fi ve m i n u t e s . .
.

sulph ide until no fu rther precipitation is produced by it Filter . .

again A cidi fy the filtrate wi th hydrochloric acid so that it j ust

.

shows a distinct acid reaction on l itmu s paper Then evaporate .

the solution to the densit y o f about and s et it aside in a cool

place to cr y stallize .

R ecrysta ll ize the salt two or three times as m a y be necessary , .

R e a c t i on .

N ot e s . The mineral wit herite i s an impure native barium

ca rbonate containing var y ing amounts o f calcium strontium an d
, ,

iron compounds together with other mineral substances A very .

large excess o f witherite must necessaril y be used becau se much ,

o f it may consist o f substances other than barium carbonate and it ,

is further requisite that a fter the satu ration o f the acid a con
, , ,

s i d e r a bl e amount o f barium carbonate shall still remain in order

that during the evaporation of the solution to dryness the i ron

, ,

and calcium ma y be precipitated The remaining iron and any .

other heav y metals present are removed by precipitation with

barium sulphide which mu st however be emplo y ed with great
, , ,

caution to avo id using an excess The final solution still contains .

chlorides o f the alkal i metal s and o f calcium and strontium which ,

mu st be removed by t e cr y stall ization o f the barium Chloride

“
-

which is less freely soluble than the others so that the latter ,

remain in the mother liquors The concentrated solution o f .

barium chloride can al so be m ixed with alcohol which p r e c i p i ,

tates the salt whil e the calcium and strontium chlorides remain
in solution .

A pure barium chloride may o f cours e be at once obtained , ,

by saturating pure h y drochloric acid with pure bari u m carbonate .

29 6 B AR I U M C H R OM A T E .

D e s cr i p t i
Colorless cr y stals sol uble in 3 parts of water at
on .
—
,

in 2 parts at and in parts o f boiling water The .

solution is neutral .

B AR I U M CH R O M A T E .

BAR II C H RO M A S .

B a Cr O 4 : 2 53 .

Barium acetate
Potassium dich romate
Water .

D issolve the di chromate in 7 5 parts of hot water and filter .

D issolve the barium acetate also in 7 5 parts o f water and filter .

A dd the latter sol ution to the former stirring well Wash the , .

precipitate by a ff usion and decantation o f cold water Collect .

,

dra in and d ry it .

R e acti on .

: 2 B a Cr O 4

D e scr i pt i on .
—
An insoluble lemon y ellow powder -
,
use d as a
pigment .

BAR I UM D I OX I D E .

B AR II D I OX I D U M .

13 3 0 2 : 1 69 .

When a current o f air is conducted over barium oxide heated

at 4 5 0 C the oxide is converted into dioxide The barium di
°
. .

oxide is employed i n the preparation o f hydrogen dioxide .

D e sc
r i p t i on —
A heav y grayish white or pale yellowish white
,
-
,
—
,

coars e powder . O dorless and tastel ess N early insoluble in cold .

water .
2 98 B AR I U M H YDROX ID E .

B AR I U M H Y D R OX I D E .

B AR II H Y D R OX I D U M .

Ba ( O H ) 2 2 1

Barium chloride .
.

S odium "h y droxide

Water .

D i ssolve the barium chloride in part s o f hot wate r and -

the sodium "hydroxide in 8 4 0 parts of water M i x the solutions . .

Heat to boiling Filter while hot S e t asi de to crystallize

‘

. . .

R ecrystallize the hydr oxide twice from hot water D rain t h e .

cr ystals on a p l a t i ni i m cone by means o f a filter pump Preserve .

the pr oduct in tightly stoppered bottles .

BAR IUM OX I D E .

B AR II OX I D U M .

B aO : 1 53 .

Prepared by heating barium nitrate to white heat in a Hessian

crucible covered with a fire clay cover The R oessl er furnace .

may be used for this purpose when the quantity is sm al l .

Pr op e rt i e s
. Grayish white porous pieces f orm ing barium hy
-
, ,

d r ox i d e wi t h water .

B I S M U TH ; P U R I FI E D .

BI S M U TH U M PU R I F I CA T U M .

Biz -
2 08 .

Commercial bismuth
Potassium n itrate

Triturate the bismuth with ten parts o f the potassium nit rate
until the t wo substances are wel l m ixed Heat the mixture in .

a crucibl e to complete fusion sti r uninterruptedly with a cl a y

,

rod ( or pipe stem ) and keep the mass in a state o f fusion for at
-

least hal f an hou r Then pour the fused mass into a vessel o f
.
 B I S M U TH .
2 99

hot water D ry the undissolved res idue consisting o f bismuth

.
,

and som e bismuth oxide mix it well with 1 part o f potassium ,

nitrate and fus e th e m ixture as be fore an d separate the sla g from

, ,

the insolubl e bismuth oxide and the ingot o f metal .

N ot e s Commercial bismuth contain s arsenic sulphur an d

.
,

selenium T hey are converted into ars enate sulphate and s el enate
.
,

o f potassium by fus ion with the potassium nitrate Thes e salts .

together with the excess o f potass ium nitrate are water soluble —
,

and thus separated by the water The bismuth is fu sed together .

in one lump A ny bismu t h oxide formed rema i ns I n pulverul ent

.

form when the slag o f salts has been washed off and can be ,

recovered .

A n ot h e r M e th od .

B i smuth
S odium nitrate
S olution o f sodium hydroxide ( 5 70 o f
9 parts
Water .

M ix the bismuth an d sodiu n itrate and heat the mixtu re in m

a n iron dish at low red heat When the mass begins to swell
'

s tir uninterruptedly with an iron spatula for about an hour or

until the metal is finely divided and thu s scarcely distingu ishable
in the mixtu re Then remove the dish from the source o f heat
.
,

and add to the hal f cooled contents the sol ution o f sodium h y d r ox
-

i de
. Heat the mixture to boiling stirring well Trans fer the , .

whol e to a paper filter let the l iquid run ofi wash the finely ,
‘
,

divided bismuth remaining on the filter and dry it ,

.

S om e bismuth oxide i s mixed with the me tal thu s purified ,

and it i s possible that some bismuth arsenate may also remain

with the product .

B I S M U T H B E N Z OA T E .

BI S M U T H I B E N Z OA S .

Freshly prepared and still moist bismuth hydroxide i s digested ,

at about 8 0 C with an excess o f benzoic acid mixed with ten

0
.
,
.

times its weight o f water in a porcelain dish over a water bath -

for about hal f an hour .

3 0 0 BI S M U TH B E N Z OAT E .

[ The quantity o f bismuth hydroxide required for 1 00 Gm ,o i

benzoic acid is about that corresponding to 1 7 5 Gm o f bismuthous
Oxid e ]
The insolubl e product ( which 1 s s a 1 d to yiel d ab out 6 4 to 6 5; _

per cent o f bismuthous oxide on ignition ) is washed as rapi dl y

'

as poss ible with col d water and dried at a temperature n ot e x ,

'

°
c e e d i ng 8 0 C .

A n oth e r M e t h od .

Cry stallized normal bismuth n itrate

Gl y cerin
S odium benzoate
D istilled water su fficient ,
.

Crush and then p Ow d e r the bismuth nitrate in a deep porcelain

dish Pour upon it the gl y cerin and stir well together Place
. .

the dish over a water bath and heat until the bismuth nitrate is
-

dissolved A dd 6 5 parts o f distilled water

. .

D issolve the sodium benzoate in one l iter o f water at a tem

p e ra t u r e o f about 4 0 to 5 0 C ° °
.

A dd the bismuth solution grad ually to the solution o f s odi um

benzoate stirring well L et the precipitate subs ide decant t h e
,
.
,

°
mother l iquor and wash the precipitate with warm wate r ( 40
-
,

)
°
—
5 0 C by decantation
. until the washings gi ve no furthe r
reaction for n itrate D ry the product first at the ordinary tem
.
,

p e r a t u r e and finally at not over 8 0 C R educe it to fine powder °

. .

D e scr i pt i on white amorphous odorless and ta steles s p ow

—
7 A , ,
'

der insoluble in water D ecomposed by hydroc hloric aci d or by

,
.
’

nitric acid with the s eparation of benzoic acid .

B I S M U TH CIT R A T E .

BI S M U T H I C IT RA S .

B i C6 H 5 O 7 2
3 97 ’

B ismuth subnitr ate 10 parts

’
Citric acid 7 parts
‘

'

Boil them with 4 0 parts of distilled water until a drop o f the ,

mixture yi elds a cl ear solution with ammonia water A dd 5 00 .

3 0 2 BI S M U TH HY DROX I DE .

D e s cri p t i onwhite odorless and tasteless powder readily

.
—
A , ,

soluble in amm onia water but insoluble in water and in alcohol , .

S oluble in solutions o f alkal i citrates .

B i s m u th an d A m m on i u m Ci tr a te .

BI S M U TH I E T A M M ON II C ITR A S .

Citrate o f bismuth 1 part

Water o f ammonia su fficient ,
.

M ix the citrate o f bismuth with two parts of distilled w a ter t o

a smooth paste and gradual ly add water o f ammonia until the
,

salt i s d issol ved and the liquid has a neutral or only fai ntly
,

alkal ine reaction T hen filter the solution evaporate it to a syrupy

.
,
‘

consistence spread it on plates o f glass an d dry it in scales Keep

, , .

the product in small wel l stoppered bottles protected from light

, , .

D e s cri pt i on scales soluble in water O dorl ess Taste

.
—
S mall ,
. .

slightly acidulous and sl ightly m etallic O n being kept for some .

time it becomes only partially soluble in water ; but the addition

o f ammonia e ff ects complete solution .

B I S M U TH H Y D R OX I D E .

BI S M U T H I H Y D R OX I D U M .

Bi ( OH )

Cr y stall ized normal bismuth nitrate 1 0 Gm

N itric acid 1 3 Gm

D istilled water ammonia water each su fficient

, , .

D is solve the bism uth nitrate in t h e nitric acid and 1 0 0 Gm o f

water previously mixed Precipitate with a mmonia in excess.
,

by pouring the bismuth solution gradually and with constant stir

ring into 3 5 Gm o f ammonia water D ecant the liquid from the .

precipitate A dd to the precipitate 1 0 0 Gm o f distilled water

.

m ixed with 1 0 Gm of ammonia water and let the mixture stand

.

for a few hours to decompose any subnitrate wh ich m a y be con

,

t a i n e d in the precipitate Wash the product by a ff usion an d

.

decantation o f cold d istilled water until the wash ings give n o

 BI S M U TH N IT RA T E .
3 3
0

further reaction for nitrate and l eave no residue on evaporation .

D ry the product without heat .

R e act i on .

3.

D e scri pt i on —
A white fine odorless and tastel ess powder
, , .

B I S M UT H N I TR AT E .

BI S M U T H I N IT RA S .

( T r i s n i tr a te f
o B i s m u th .
)

Bi N O ? ) 3 5 H , O : 484
. .

Proceed as in th e formula for making subnitrate of bismuth

up to the p oint where the precipitated subcarbonate has been r e
d issolved in nitri c acid E vaporate this solution to c rvs ta ll i za t i on
. .

D ry the crystals by gently pressing them between white filter

paper an d at once put them in a glass stoppered bottl e
, .

Th e salt i s in large transparent crystals colorles s

D e s cri pt i on —
, ,

i f pure D ecomposed by water solubl e in dilute n itri c acid and

.
,

in glycerin also in glacial acetic acid

,
.

Gly c e r i te of B i s m u th N i tr a te .

Normal bismuth n
i trate
Glycerin

Powder the crystal s by trituration in a mortar Then add the .

glycerin al l at once and stir until the salt has dissolved

, ,
.

N ot e s .I f the crystal s are triturated w i th the glycerin espe ,

c i a ll y with a s m a l l q u a n ti ty of glycerin there i s danger that n itro ,

glycerin may be formed and explosion result .

The solution i s used for preparing certain other bismuth prep

a ra t i on s by doubl e d e composition as the ol eate
'

salicylate and
, , ,

vale rate .
3 4
0 B I S M U TH OLEA T E .

B I S M U TH OLEA T E .

BI S M U T H I OLEA S .

B i C1 8 H 3 3 O2 3
: 105 °

Normal bismuth nitrate

White Castile s oap in fine powder ,

Put the crystals o f normal nitrate of bismuth into a mortar ,

powder the salt and then add al l at once 1 0 0 ml o f glycerin ;

, , ,

stir occas ionally avoiding friction or pressure until the n itrate

, ,

is dissolved which will be accompl ished in a few hours D issolve

,
.

the soap in ml o f water and then add slowly the solution ,

of nitrate o f bismuth Warm the mixture rej ect the water y

.
,

mother liquor and wash the oleate twice with warm distilled
-
,

vva t e r .

R e act i on .

Bi N 0 3 ) 3 + 3 N a C1 8 H 33 O2
B i C1 8 H 33 O Z ) 3 +3 N 3 N O 3 '

N ot e s The normal nitrate o f bismuth i s to be powdered before

.

add ing the glycerin and the glycerin is added all at once to prevent
,

possible explosion o f nitro glycerin which might be formed —

, .

This oleate mu st be fused by very gentl e heat over a water bath ,

-
,

to get rid o f the last portions o f water The yield is about 3 6 .

Gm and the product is a white or yel lowish white ointment con

,

taining about 2 0 per cent o f bismuth .

B I S M U TH O X I D E .

BI S M U T H I OX I D U M .

B i 20 3 : 4 66 .

B ismuth subnitrate 1 part

S olution o f sodium hydroxide ( 5 70 o f
N aO H ) .
4 parts

M ix in a porcelain dish and boil the m ixture for ten minutes .

~
 BI S M U TH S U B CAR B ONA T E .

B I S M UT HY L CAR B O N AT E .

BI S M U TH I S U B CA R B O N A S .

[S u bc ar bon a t e o f B i s m u th ]

B ismuth in small pieces, 5 Gm

0
N itric acid 1 5 0 ml
A mmonia water . 1 2 5 ml

S odium carbonate 2 5 0 Gm

M i x 8 00 ml o f the nitric acid with 1 0 0 ml of distilled water in a

capacious glas s vessel a dd the bismuth an d set aside for twenty
, ,

four h ou r s t o dis solve D ilute the solution with 2 5 0 ml o f dis

‘

till ed water ( until permanent turbidity results ) stir well again , ,

set th e liquid aside for twenty four hours and then filter D i -
, .
~

l u te the filtrate by gradually adding to it ml o f distilled

water and m ixing well N ow add slowly the ammonia water
,
.
, ,

through a small siphon stirring constantly and actively Trans , .

fer the whole to a wetted muslin strainer and let drain When , .

the liquid has drained o ff pou r upon the precipitate 8 00 ml o f dis

tilled water m ixing well and then let drain again N ow t rans fer
, , .

the precipitate to a suitable vessel add the remainder o f the nitric ,

'
acid and when all has dissolved also add gradual ly 1 0 0 ml o f
, , ,

distilled water and set the solution aside for twenty four hours
,
-
.

Then filter .

D issolve the sodium carbonate in 3 0 0 ml o f distilled water with ,

the aid o f heat filter t h e solution and set it as ide until cold
, , .

N ow pour the col d solution o f bismuth nitrate very slowly int o

th e solution o f sodium carbonate with constant and brisk stir ,

ring Trans fer the whole to a wetted muslin strainer and a fter
.
, ,

draining thoroughl y wash the precip itate with distilled water as

, ,

expeditiously as practicable until the washings become tasteless , .

L astl y pr ess out the moisture a s fa r as practicable dry the pre

, ,

c i p i t a t e on bibulous paper or on muslin at a gentle heat an d , , ,

then powder it by rubbing it through a fi n e sieve by means o f a

so ft bru sh .

R e ac t i on . First a s olution o f bismuthous n itrate is made

 BI S M U TH S U B CAR B O N A T E .
3 7
0

This is poured into a large quantity o f water containing a m

monia whereby bismuthyl n itrate i s thrown down the ammonia
, ,

being added to n e i t t r a i i z e the free n itric acid so as to prevent it

from retaining any bismuth nitrate in the l iquid Then the pre .

c i p i t a t e is redissolved in nitric acid to form again the B i N O 3 ) 3

( .

Finally ,

N ot e s . A s the bismuth usually contains arsen i c the aci d solu

tion first prepared contains bismuth arsenate ; when the l iquid
is diluted with water until permanently somewhat turbid th e ,

arsenical salt precipitates be fore the bismuthyl nitrate does and ,

’
hence a fter twenty four hou rs rest most o f th e arsenate is
,
-
,

found deposite d as a white precipitate and i s then filtered away , .

'
The rest o f t h e arsenic remain s in the mother liquor a fter the -

precipit ati on of the bismuth nitrate with ammonia as am monium ,

arsenate S e e also the notes under the title B ismuthyl N i t ra t e

. .

D e scri pt i on .
—
A
s oft white or pale yellowi sh odorl ess and taste
, ,

less powde r which becomes converted into oxi de by heat I t i s

, .

quite insolubl e in water but shoul d g ive a cl ea r solution with ,

n itric acid .

A n oth er M e th od .

Purified bismuth in small pieces ,

N itric acid .

A mmonium carbonate
D istill ed water su fficient ,
.

M ix the n itric aci d with 1 5 0 ml o f distilled water and add t h e ,

bismuth in succes sive portions When eff ervescence has ceased .

,

apply for ten m inutes a temperature approaching that o f e bu lli

tion Then decant the solution from any insolubl e matter that
.

may be present E vaporate th e solution until it is reduced to 1 00

.

ml and add this in smal l quantities at a time to a col d filtered

,

solution o f the ammonium carbonate in 2 liters o f distill ed water ,

stirring constantly during the admixture Collect the precipitate .

on a filter and wash it with di stilled water until the washings

pass tasteless R emove now as much of the adhering water as
.

can be separated from the precipitate by sligh t p r e s s ure wi th the

30 8 BI S M U TH SU B GALLA T E .

hands and finally dry the product at a temperature not exceeding

,

C .

D e s cr i pt i onsoft white odorl es s and tastel es s powde r i n

.
-
A , , ,

soluble i n water but completely soluble in dilute nitric acid with ,

e ffervescence .

BI S M U TH S U B G ALLA T E .

BI S M U T H I S U B GA L L A S .

Crystallized normal bismuth nitrate 1 00 Gm

Glacial acetic acid 200 Gm
Gallic ac id 33 Gm
'
D issolve the bi smuth nitrate i n the acetic acid and dilute the -

solution with 5 0 0 Gm of d istilled water Filter A dd gradually . .

to thi s liquid a solution o f th e gallic aci d in Gm of col d dis

tilled water Wash the precip itate with tepid distilled water
.

until the washings are free from nitric acid D ry the product .

at from 7 0 to 8 0 C on blotting paper spread upon porous tiles

° °
. .

D e s cr i pt i on .
—
A
sulphur yellow odorless and tastel ess powder ; ,

insoluble in water or in alcohol Probably practically identic a l .

“ ”
with the preparation called d e rm a t ol .

B I S M U TH Y L N I TR AT E .

BI S M U TH I S U B N I TR A S .

Chi e fl y O B i N O g H zO = 3 0 4 . .

B ismuth in s m a l l p i e c e s
,
'

N itric acid
S odium carbonate
A mmonia water
D istilled water su fficient ,
.

M i x 8 00 ml o f the nitric acid with ml o f the distilled

water in a capacious glass vessel add the bismuth and set aside
‘

, ,

for twen ty four hours to dis solve D ilute the solution with
-
.

ml o f distill ed water s o that th e turbidity pr o duced by the

,

addition o f the water no longer disappears on stirring ; stir well ,

a n d again set it asi d e for twent y four hours Then fi l t e r —
, . .
3 1 0 B I S M U TH S U B N IT RA T E .

baskets o f stoneware are used for suspending th e bi smu t h i n th e

acid when bismuth preparations are prepared on a moderately
large scale the acid being placed in a stone pot and the basket
,

containing the bismuth suspended j ust below the surface of t h e

acid U nless the vessel in which the solution is effected is su f
.

fi c i e nt ly large to obviate all risk and inconvenience from t h e viol

ence of the reaction the metal shoul d be added in portion s each
, ,

porti on to be entirel y dissolved before more is added The c a .

p a c i ty o f the vessel ought to be about three times th e combined

volume o f the aci d and water used to d issolve the metal .

The strong solutio n can not be filtered through paper for the ,

acid liquid is s o corrosive a s to destroy the paper not o nly de ,

feating th e filtration but also discoloring the solution I t is best .

to filter through coarsely powdered glass or glass wool or ,

washed asbestos ; sometimes the solution i s filtered throu g h cot

ton previously immersed i n dilute nitric acid D ecantation is t h e .

easiest method and generally su fficient especially when large

, ,

quantities are operated upon A fter dilution however filtration

.
, ,

th rough paper i s entirely practicable .

The obj ect o f first preparing subcarbonate o f bismuth 1 5 t og et

rid o f the ars enic which the metal contained This arsenic is .

hel d in t h e acid s ol ution as bismuth arsenate nearly al l o f which

'

, .

precipitates upon dilution o f the l i q ui d with water a nd i s re ,

moved by filtration after standing twenty four hours T he r e —

.

m a i n d e r of the ars en ic i s l eft in the last mother liquor as a m -

m on i u m arsenate together with the ammonium nitrate after p r e

,
;

c i p i t a t i on o f the bismuth subnitrate with ammonia .

The character and composition of subnitrate o f b ismuth de

pend greatly upon the me thod o f its preparation A mong t h e .

most important influences that a ff ect the character o f the product

are these : The rel ative quantity o f water used in the precip ita -J

tion ; the l ength o f time the precipitate is exposed to t h e m oth er

'

liquor ; the amount and temperature o f the water used for the
precipitation ; the quantity o f water and the len gth o f time con
s umed in washing ; the us e or omission o f ammonia ; an d the
‘

greater or less care be s t ow n upon the various details of the

process .

The process given above probabl y y iel ds the most u ni form and
‘
"

satis factory results In order to insure succes s each step of the

.
 B I S M U TH S U B N IT RA T E .

3 I I

pr ocess shoul d be carried out in strict accordance with the precise

directions given .

O ther processes prescribe that the solution o f bismuthous nit

rate be evaporated to crystallization and the crystals a fterward
tr eated with a definite quantity of water The evaporation must .

not be carried so far that a cake fo rm s on the botto m o f the dish ,

for then the salt will be hard and d i fficul t to manage The clear .

crystal s removed from t h e mother l iquor are carefully made dry

by gently pres sing them between blotting paper which operation ,

must be very carefully carried out so as not to soil the crystal s

with fibers from the paper N o heat must be u sed in drying the
.

crystals Triturate one part o f the cr y stall ized salt very thor
.
'

oughly with four parts o f distilled water an d then pou r this ,

mixture into a large vessel containing twenty one parts o f boi l -

i ng distilled water stirring constantly

,
L et cool ; d ecant ; and .
-

wash t h e pre c ipitate on a strainer w ith ten parts o f cold distill ed

water gradually added A fter drain i ng as rapidly a s poss ible
,
.
,

=
press out the last o f the w a s h w a t e r by means o f a screw pres s ,

°
and dry the product on filter paper at not over 3 0 C .

In order to obtain a good product the n itric aci d u sed must be ,

pure distilled water must be used and the aci d solutions must
, ,

not come in contact with wood or other organic substances or ,

with metals .

Whenever th e precipitated bismuth subnitrate is permitted to

r e m a I n long in contact with the mother liquor in which it has been

thrown down it becomes more dense and at the same time takes
, ,

up more nitric acid This must be avoi ded L ong contact w ith
. .

much water al so renders the preparation heavier but at the same

—

tim e more basic Col d l iqu ids w ill y ield a voluminous p r e c i p i

.

tate ; hot water mak e s the precipitate more dense I f the water .

°
u sed for precipitating is 5 0 C the precipitated subnitrate w ill
.

have a compos ition corresponding to about 7 7 per cent o f B i Ofi ; z

i f the water i s boil ing hot ( 1 0 0 C ) the subnitrate will have a

0
.

composition corresponding to about 8 0 to 8 1 per cent o f B i O g 3

.

A ccording to L oewe the precipitate i s not a ffected by a solution

,

o f ammonium n itrate and hence it can be washed with such a

,

solution without danger .

T he precip itate must be dried at a l ow temperature ( not over

3
°
0 but mu st be thoroughly dry before i t i s put awa y
'
.

A fter removing all water that can be gotten rid o f by pressing

3 12 BI S M U THY L C H LOR I DE .

it the precipitat e should be dried i n layers I f not thoroughly

,
.

dried it decomposes by the influence o f light and acquires a nitrous

odor I f dried properly in layers these can be eas ily broken and
.
,

powdered by rubbing the pieces through a fine wire s ieve by

means o f a soft brush I f dried at too high a temperature the .

pieces are hard not so readily powdered and apt to yiel d a coarse
, , ,

harsh powder .

Good subnitrate of bismuth i s soft and bulky .

D e s cr i p t i on
fine white powder odorles s almo s t tasteless ;
—
A , , ,

insolubl e in water alcohol and glycerin , ,

.

B is muth subnitrate is always a comparatively heavy substance ,

but it must be a s bulky as it can be made The product varies .

extremel y in this p articular A relatively very heavy and coarse .

preparation is not fit for medicinal uses .

B I S M U TH Y L CH LO R I D E .

BI S M U TH I O X Y C H L OR I D U M .

( O x y chloride o f B ismuth ) .

O B i Cl z z

B ismuth
N itric acid
S odium chloride
D istilled water su fficient ,
.

the aci d w ith 3 0 ml of water ; dissolve the metal in the

M ix
mixture D i ssolve the sodium chloride in 4 0 0 ml of distill ed water
.
,

and filter Pour the acid solution o f bismuth n i trate gradually

.

a n d with constant s t i r r 1 n g 1 nto the solution o f sodium c h l o r i d e f

'

Wash the precipitate with distilled water first by decantation ,

and a fterwards on a filter until the washings are t asteless D rain

'

, .
,

and then d ry the product between bibulous paper with the aid
o f gentle heat .

R e a ct i on . O B i N O g + N a Cl z N a N O + O B i Cl .

D e s cr i pt i on .
—
A fine white odorles s and tastel es s powder
, , .
 BI S M U TH T AN NA T E .

D issolve the bismuth nitrate in the glacial acetic acid D issolve .

the pota ssium iodide and the sodium acetate in 2 liters o f distilled
water M i x the clear solutions constantly stirring pouring the
.
, ,

bismuth solution gradual ly into the Other .

A y ellowish brown p reci pit ate i s formed which chan g es t o

-
,

lemon yellow and finally to brick red Wash the precipitate by

-

,
-
.

°
decantation and dry it at 1 0 0 C .

S houl d be kept protected from light .

D e s cripti on 7 A brick red m 1 e ro crystalline powd er , o dorless ‘

— - -
.
, ,

tastel ess insoluble in water an d in al cohol

, .

0 11 i gni tio n i t shoul d yield n ot les s tha n 6 6 per ce nt of B i zO s .

BI S M U TH TA N NA T E .

BI S M U T H I T AN NA S .

N ormal bismuthous nitrate

Gl y c e r i
Tannic acid
S ol ution o f soda ,
2 40 ml or , s u fii Ci e n t
‘
.

T riturate the bismuth nitrate pow der ; ad d the gl ycerin an d to

s tir until dissolved ; then gradually ad d solution o f soda until a

precipitate no l onger forms stirring wel l ; wash the precipitate,

with distilled water until the washings are tast e l es s ; drain ; add
the tannic acid to the moist hydroxide mix well and set aside for , ,

tw o hour s st irrin g fr equent l y

,
Then trans fer the mixture to a .

filter wash with di sti lled wate r un til t he washings a re tasteless

, ,

and dry the product .

D e s cri pt i on —
A di rty white or p ale yellowish
-
,
odorless and
tastel ess powder
'

BR OM IN E .

BR O M U M .

B r2 : 1 60 .

B romine is a heavy dark red fuming liqui d o f a p e culiar su f

,
-
, ,

f oc at i ng odor a nd its vapor is terribly irritating and dange rous to

th e eyes and respiratory organ s .
 C AD M I U M C AR B ONA T E .
3 5
I

Commercial bromine usually contains some chlorine and iodine .

I t must be kept in small glas s stoppered bottl es in a cool place

-
.

S e e als o Part I I Vol I and Part I o f this volume

, .
, .

S ol u ti ons o f B r om i n e .

Water solutions o f bromi ne are frequently requi red for surgical

and other uses They may be prepared with the ai d o f potass ium
.

bromide O ne such solution which i s commonly employed con

.
, ,

t ains 1 0 Gm o f bromine an d 20 Gm o f potassium bromide dis

solved i n one liter o f distilled water ; another contains 20 Gm o f
bromine 1 0 Gm o f potassium br omide and 8 00 m 1 o f d istil led
,

water B ut as bromine i s soluble in 3 0 parts o f water at

. a
simple water solution containing any quantity o f bromine below
-

three per cent may be readily made as requ ired .

CAD M I U M CAR B O N AT E .

CA D M I I C AR B ONA S .

Cd CO 3 : I 72 .

Cad mi um
N itric aci d ( 68 70 o f H N Os )
A mmonium carbonate
Water .

Granulate the cadm ium by pouring the fused fn e ta l from a

height o f about four fe et int o a vessel o f water A dd the g ra n u .
,

lated metal gradually to the nitric acid previously diluted with

about one h al f its volume o f water : When all o f the cadm ium has
-

been added and the reaction has subs ided set the solution ( with ,

the undissolved residue o f metal ) on a water bath and heat until -

e ff ervescence has entirely ceased D ilute the solution with about

.

3 0 parts o f water L et the

. whol e stand at rest for a few hours .

Filter Put the filtrate in a large vessel an d add 4 00 parts o f hot

.

wate r.

D i s s olve the ammonium carbonate in 1 5 0 parts o f water A dd .

a small portion o f this solution gradual l y to the solution o f cad

mium nitrate t o precipitate iron from it When a test portion o f .

t he c adm ium n itrate solution shows no further test for iron filter ,
3 16 C ADM I U M C H LOR I DE .

the l iquid and pour it into the remainder o f the solution o f a m

m on i u m c arbonate Wash the precipitated cadmium carbonate
.

by decantation until free from nitrate and ammonium salt col lect ,

it and dry it
,
.

R e act i on s .

t h en ,

D e scri pt i on .
—
An insolubl e amorphous
, ,
o dorl ess and tastel ess ,

white powder .

C A D M I U M CH LO R I D E .

CA D M I I C H L OR I D U M .

Cd Cl 2 . 2H 2O
:

S atu rate
hydr ochloric aci d with cadmium carbonate digest the ,

solution with a slight exces s o f the carbonate filter and evap , ,

orate t o dryness D issolve the d ry salt in two thirds o f its own

.
-

weight o f hot distilled water acidulate with hydrochloric acid , ,

and set the liquid aside for several hours to crystallize D ry the .

cr y stal s with the ai d o f moderate heat or in a d siccator over , e

sulphuric acid .

D e s cr i pt i on .
—
Colorless crystals readily solubl e in water and in
,

alcohol .

CAD M I U M I OD I D E .

CA D M I I I OD I D U M .

Cd I 2
2 6
3 5 .

Granulated cadmium
Iodine
D istilled water

Put th e metal iodine and water into a flask and place this in
,

w arm water br keep its contents at about

,
until the odo r o f
iodine has passed and the metal i s nearl y al l disso l ved The n .

heat to boil ing for a few minutes filt er hot evaporate to satur a
“

, ,

tion and s et aside to cool and crystalliz e D rain th e crystals a n d

,
.
3 18 C AL C I U M B EN Z OA T E S .

in a large porcelain dish and d issolve with the aid o f mod

M ix
c rate heat Filt er and evaporate to crystal lization
.
,
.

D e scr i p t i on . White crystalline readily solu bl e in water

—
, , . Ef
fl or e s c e n t . O dorless ; taste saline bitterish ,
.

C AL CI U M B E N Z OA T E .

CA L C I I B E N Z OA S .

Ca C7 H 5 0 2 ) 2 -4 H 20 2 3 5 4 ~

L im e part
Ben zoic aci d 4 parts
Water parts
S lake
the l ime in a porcelain dish with a part of the water
’

When the reaction has been completed add the remainder o f the
water mix thoroughly and then add t he benzoic aci d Boil th e
, ,
.

m ixture a few minutes until the benzoic acid i s dissolved Filter .

the S olution while hot E vaporate the filtrate to one hal f i t s vol
.
-

ume and s et it aside to cool Collect the crystals and drain an d .

dry them R ecover the remainder o f th e salt from the mother

.

l iquor by evaporation in the usual way .

N ot e s Very large long crystal s can be obtained by spon

.
,

t a n e ou s evaporation o f a saturated solution The crystal s may-

.

'

be dried with the ai d o f gentle heat When the mot her l iquor .
-

ceases to yield enough to warrant further evaporation the benzoic ,

acid m a y be recovered from it by precipitation w ith a su fficient

amount o f hydrochloric acid .

D e scr i p t i on .
—
L ong white needles soluble in about 2 5 parts o f
, ,

water at and in a smaller proportion of boilin g wat e r .

C AL CI U M B R O M I D E .

C AL CIT B ROM I DU M
Ca B r z z -
z oo .

A mmonium bromide 3 parts

L ime 1 part
S lake the l ime with 6 parts o f water and triturate it in a mortar ,

addin g enough water to form a liquid mixture D issolve the a m .

 C AL C I U M C AR B ONA T E .
319

m on i u mbromide in 8 parts o f water heat to the boiling point , ,

and th en add the m ilk o f lim e until the evolution o f amm oni a

ceases Then filter the solution and evaporate the filtrate to dry
.

nes s stirrin g constantly so as to produce a granulated salt

,
.

R e act i on .

D e scri pt i on white granular salt ; odorless ; taste s harp

—
. A , ,

sal ine D el iquescent S oluble at 1 5 in

. . part o f water and in °

1
p art o f alcohol ; extremely readily soluble in boilin g water o r
alcoh ol The solution is neutral to test paper
.
-
.

C AL CI U M C A R B O N A T E ; P R E CI PI T A T E D .

CA L CI I C AR B ONA S PR A E CI PI T A T U S .

Ca CO 3 -
1 00 .

Calcium chloride fused ,

S odium carbonate
D istilled water s u fli c i e n t
,
.

D issolve the calcium chloride in 1 0 0 parts o f the water and the ,

sodium carbonate in another equal quantity Filter the solu tions . .

Heat both solutions to about 8 0 C P our the solution o f calcium °

.

chloride into the solution o f sodium carbonate stirring constantly , .

Wash the precipitate by decantation ; then collect and dry it .

R e act i on . Ca C12 + N a2CO 3 z Ca CO S l — —

2 N a Cl .

N ot e s Hot solution s are used to insure a dens e precipitate s o

.
-

that the process o f washing may be easier ; when col d solutions are
used the precipitated calcium carbonate is a very bulky magma ,

diffi cul t to wash free from s odium chl oride .

The precipitate should be washed until the washings cease to be

ren d ered turbi d by test solution of s i lver n itrate and then dried ,
°
at 1 00 C .

A n ot h e r M e t h od .

Prepa re a solution of calcium chlori de from white ma rble a s ,

described under the titl e o f Calcium Chloride removing iron , ,

aluminum and magnesium by e mplo y ing chl orine water and m ilk
o f lime R ender t h e s ol u t i on alkaline by us ing a s uffi c iency o f
. ,
3 20 C AL C I U M C AR B ONA T E .

milk o f lime Filter Then acidulate the liqu id with hydrochloric

. .

acid Precipitate th is solution w i th e i th e r ammonium carbonate

.
'

or sodium carbonate .

D e scr i pt i on . A
very fine perfectly white powder odorless
—
, , ,

tasteless and insoluble in water and in alcohol U nder the micro

,
.

scope the precipitated calcium carbonate is seen to be micro crys —

t al l i n e .

Pr e par e d Ch a lk .

Triturate 1 00 0 Gm o f chalk with a little water until reduced to

a very fi n e p owder by the l evigation
“ ”
Thr owthe m 1x t u r e int o .

a vessel capabl e of holding about twenty l iters and nearly filled

with water stir th e mixture well and a fter a brie f tim e decant
, , , ,

the supernatant li q u id while y e t white and turbi d from the sus,

pended particles o i the finel y divided chalk into another vessel ,

.

To the residue in the first vessel add a fresh portion of water sti r ,

well aga 1n and a fter allowing the coarser particles to subside as

,

be fore decant once more a dding the second turbid li quid to that
, ,

previou sl y d ecanted S e t the m 1 x e d l iquors aside and when the

.
,

fine powder has subsided perfectly pour off the wa er and collect ,
t
,

an d d ry t h e p ow d e r .

N ot e This p roces s o f separating the coarse gritty particles

.
“

“ ”
f rom the levi gated cha lk is called elutri ation the obj ect bein g ,

to obtain a very soft finely d ivided product ,

.

I nstead o f dr yin g the product as a mas s the moist powder m a y ,

“ ”
be formed into cones by trochiscation .

light amorphous cream colored nearly white

D e s cr i p t i on —
. A , ,
-
, ,

ver y soft powder or coni cal lumps ; odorles s and tasteless I ri s ol

' ‘
“
.
,

uble in water and in alcohol .

C AL CI U M CH LO R I D E .

CA L CII C H L OR I D U M

Ca C12 : I

White marble in powder ,

H y dr ochloric acid of H Cl )

Chlorine Wate r w i t gb u gg .
” “
u
,

L ime .
i
,
3 2 2 C AL C I U M HY DROX I DE .

v apor ceases to be disengaged cover the pot well and set it asid e ,

until the contents are cool Put the slaked lime into an iron w ire .
-

s ieve and by gentl y shaking cause the fine powder to pass through
,

t h e sieve rej ecting what is left

,
Put the powder into a bottle and .

cork tightly .

N ot e s . O nly recently prepared calcium hydroxid e is fit to be

u sed for any o f the purposes for which slaked l ime is prescribed ,

as it s oon becomes contaminated with carbonate It should be .

-

perfectly white .

The water shoul d be added to the lime all at once ; otherwise ,

when too l ittle water i s added at first the hydrate formed will be
“

coarse and hard and does not a fterward disintegrate re adily o n

,

addition o f mor e water .

Good Clean white calcium oxide must be us ed to obtain a s u ffi

, ,

c i e nt l y pure and white h y droxide .

Ca l ci u m H y d r ox i d e S ol u ti on .

( L I QUOR C AL C I S . L I M E W A T ER )
.

A saturated aqueous solution of calcium hydroxide contains

a bout per cent o f that compound .

L ime
D istilled
water
Water su fficient
,
.

S lake
the lime by the gradual addition o f 6 parts o f water then ,

add 3 0 0 parts o f water and stir occas ionally during hal f an hou r;
A llow the mixture to settle decant the l iqui d and throw this away , .

N ow add to the res idue 3 00 parts o f distil led water stir well wait , ,

a short time for the coarser particles to subside and pour th e ,

l iquid hol ding the undissolved l ime in suspens ion into a glass
, ,

stoppered bottle Pou r o ff the clear liquid when wanted for use
.
.

N ot e s The obj ect of rej ecting the soluti on first made is to r e

.

move dust and alkalies A fter thi s washing th e calcium hydroxide

.

furnishes a purer product .

At C water dissolves about

.
of its weight of cal
c i u m h y droxide .

When a sol ution o f calcium h y droxide is exposed to the ai r ’

,
 C AL C I U M HYP O PH O S PHIT E .
3 3
2

which happens each time the stopper i s r e m ove d from th e c on ’

t a i n e r some CO from th e air precipitates calcium carbon ate from

, 2

the liquid thereby reducing the quantity o f Ca ( O H ) in solution

, 2 .

But i f an excess o f the hydroxide is allowed to remain in the stock

bott l e t h e solution i s kept saturated
’

.
,

S yr up o f L i me .

Triturate th e l im e and sugar thoroughly in a mortar so as to ,

‘

form a h om og e n e ou s powder ; then add the m ixture to 5 0 0 ml o f

‘

boiling water contained in a bright copper or tinned i ron vessel

, ,

boil for five minutes constantly stirring and then strain D ilute
, ,
.

the strained l iqui d with an equal volume o f water an d filter ,

through white paper Then evaporate the filtrate in a tared cap

.
,

sul e t o 7 0 0 Gm all ow it t o cool add to it enough water to make

, , ,

the product measure 1 0 0 0 ml an d mix thoroughly ,

.

Keep th e syrup in well stoppered bottles -

.

The preparation contains a chemical compound formed

N ot e s .

b y the lime with the sugar cal led calcium sucrate which may , , ,

however d issolve more l ime I t is best to dissolve the sugar in

,
.

the water heat t o boiling and then add recently prepared calcium
, ,

h y droxide in powder The calcium hydroxi de may be prepared

.

by slaking 6 5 Gm o f cal cium oxide w ith 4 0 Gm o f water The .

calcium h y droxi de may also be dissolved without heat .

D e scri pt i on A clear colorless syrup o f alkal ine tas te

‘

—
. .
, ,

C AL CI U M H Y P O PH O S PH I T E .

CA L CI I H Y PO PH O S P H I S .

Ca ( PO zH )2
-

2
l 7o .

Phosphoru s
L ime
D istilled water .

Carbon dioxide .

Put the phosphorus in a bottl e containing 2 0 parts of a saturated

solution o f sod ium chloride and large enough to be only about
3 4
2 C AL C I U M HYP O PH O S PH IT E .

hal f fil led by these contents Heat th e bottle gradually by plac .

i n g it in a vessel o f hot water ( about until the ph osphorus

becomes liquid S hake the bottl e until col d Wash the g ra nu
.
. .

lated phosphoru s t w o or three times with distilled water .

Place the l ime in a porcelain dish and a dd 20 parts of water .

When the l ime has been completely converted into calcium h y

d r ox i d e and intimately mixed with the water to form a creamy
mixtu re add the granulated phosphorus and stir well Heat the
, .

m ixture at about stirrin g frequently until the phosphorus ,

i s all dissolved which may be known by the fact that the evolution
,

of phos phine ceases .

N ow ad d enough distille d water to make the liquid measure

about 4 0 parts filter it and conduc t into th e filtrate a current o f
, ,

carbon dioxi de as long as any precipitate continues to be formed ,

k eeping the l iqu id at about 60 during this part o f the process °

.

Filter ou t t h e calcium carbonate .

E vaporate the filtrate over a water bath to drynes s bein g care -

,

ful not to permit the temperature to exceed R edis solve the

dry salt in s i x t i m e s its weight o f hot distilled water ( not over
'

filter again ( i f necessary to make the solution perfectly

°
clear ) and evaporate it at 4 0 in a porcelain dish to about one
,

hal f its volume L et it cool Collect the crystal line salt which
. .

has been formed drain it well and dry it w ith the ai d o f gentle
, ,

heat .

E vaporate th e mother liquor to on e hal f its volu m e let it cool

-
- -
, ,

a n d c ollect and dry the second crop o f crystalline sal t in th e same

manner as the first E vaporate the s econd mother liquor in the

.

same w ay .

R e act i on . PO Z H Z ) 2
—
2H 3
P .

N ot e s .When phosphorus is digested with alkal ine hydroxides

—
whether potass ium sodium o r calcium hydroxide the products ,
—

are hypophosphites and hydrogen phosphide The reaction is .

completed when no more phosphine ( hydr ogen phosph ide ) is

evolved This gas is known by its strong garl ic odo r O wing
. .

to its inflammable nature care should be taken that no accident

may happ en To guard against danger from a too rapid evolution
.

of phosphine and from th e explos ive decomposition o f the hy

,

O
p p h o s p hi t e th e temperature
,
must be kept within sa fe lim its a s ,

directed .
3 26 C A L CI U M I OD I DE .

the ferrous lactate and potassium citrate with 5 0 ml of hot

“

R ub
distilled water u ntil dissolved F ilter the solution A dd it t o
‘

. .

ml o f syrup o f hypophosphites m ix well an d evapor ate t o , ,

ml .

This preparation should be freshly made when w ant e d , .

C AL CI U M I OD ID E .

CA L C I I I OD I D U M .

Ca I 2
: 293 .

Iodine
I ron
L im e
Water su ffic ient
,
.

D ig estthe iron and 1 5 parts o f the iodine with 3 0 parts o f

water in a flask until all odor o f iodine ceases and a green
, ,

solution of ferrous iodide is obtained Filter this then ad d the .

,

remainder of the iodine and dissolve , .

S lake the l ime with 6 parts o f water and triturate the cal ,

c 1 um h y droxide with enough w ater to make a smooth l iquid m ix

tu re A dd this m ilk o f lime g r a d iI a lly to the s ol u ti on o f ir on
'

iodides until the iron has all been precipitated Then filter the .

l iqu id and evaporate it to dryness sti rring constantly , .

R e act i on s .

F e +2 I =F e I
' '

then F el i [ I F eI then
'

— :
z

l H 20
‘

— -
.

white granular salt ; odorless ; taste acrid

D e scr i pt i on —
A , ,

sal ine reminding o f iodine D el iqu escent R eadily solubl e in

,
. .

water and in alcohol .

C AL CI U M LA CT A T E .

CA L C I I LA CT A S .

Ca C 3 H O 3 ) 5

L actic acid
Calcium oxi de
D istilled water
 C AL C I U M OX I DE _
.
3 7
2

S lake the calcium oxide w ith about 5 0 parts o f the water ; add
the remainder of the water to the lactic acid Then add the m ilk .

o f lime gradually to the diluted lactic aci d in a porcelain dish

heated to about 90 C over a water bath Filter the solution
°
.
-
.

whil e hot S eparate the crystals deposited on co ol ing and dry

.
,

them bet w een blotting paper E vaporate the mother l iquor to .

-

obtain more crystals .

Re acti on .

N ot e s The mother l iquor may be evaporated to drynes s to

.
-

obtain all o f the calcium lactate ; but this product i s granular and
not pure .

D e scr i pt i on . Colorl es s inodorou s crystals solubl e in

—
,
parts ,

o f water . Freely soluble in boiling water Insoluble in alcohol . .

C AL CI U M OX I D E .

CAL CI I OX I D U M .

( Calx . L ime ) .

Ca O 56
‘

z .

Fill a Hessian crucible with pieces o f wh ite marble or with ,

any suitabl e calcium carbonate and subj ect it to a red heat until ,

compl etely decomposed so that the res idue no longer e ffervesces

on being mixed with dilute hydrochloric acid a fter havin g been
first mixed with its own Weight o f water .

Keep the product in tightl y closed bottles in a dry place .

R e act i on . Ca Cn Ca O + CO 2 .

D e s cr i p t iHard white masses or pieces ; odorless ; tast e

on —
,

sharp c austic In contact with ai r it attracts water and carbon

,
.

dioxide an d falls to powder S olubl e in 7 5 0 parts o f water at

,
.

and in about parts o f boil ing water Insol uble in .

alcohol .

I f 8 Gm o f Ca O be m ixed with 5 Gm o f water a chemical inter

action shoul d a t once ensue and the calcium h y droxid e formed ,

should be completel y solubl e in h y dr ochloric or nitr i c acid .

 C AL CI U M P H O S P H A T E .

C A L CI U M PH O S PH A T E .

CA L C I I PH OS PH A S PR A E CI PI T A T U S .

Precipitated Tri Calcium Phosphat e ]

[ -

B on e —
is obtained by the calcination of bones I t is the
as h .

i n org a m c res idue left on burning bones to whiteness and c on s 1 s t s ,

m ainly o f tri calcium phosphate with about ten per cent o f cal
-

c i u m ca rbonate an d a l ittle calcium fl uoride and magnesium phos

phate I t is used in the manu facture o f glacial phosphoric acid

. ,

precipitated cal ciu m phosphate s odium phosphate etc , ,

.

I t should be wh ite or but sl ightly grayish odorless an d almost , ,

completely soluble with but sl ight e ff ervescence in dilute hydro

, ,

chloric acid .

Precipitated tri calcium phosphate -

is prepared as follows

Bone ash in fine powder

-
,

H y drochloric acid .

A mmonia water su fficient ,

.

D igest the bone ash with the acid diluted with

-
ml o f ,

water until dissolved Boil the solution a few minutes ; filter ;

, .

then add ml o f boil ing water N ow add ammonia water .

until the mixture acquires an al kaline reaction Collect the pre .

c i p i t a t e on a muslin strainer wash it with hot water until the

,

washings cease to produce a precipitate with test solution o f

s ilver nitrate acidulated with nitric ac i d D ry the washed pre .

c i p i t a t e at a temperature not exceeding 1 00

°
C .

R eact i onWhen the crude tri calcium phosphate is disso l ved

.
-

in hydrochloric acid the reaction occurri ng is as follows :

,

When ammon ia is added to the solution both the acid calcium

phosphate a n d the calcium chloride are decomposed ,

H
4 4 N C1+ 4 20 + C3 3 P0 4 )
H 2 ‘
33
‘

0 C AL CI U M P H O S P H A T E .

S odium phosphate parts

‘

35
‘

D istilled water . 2 0 0 parts

S tirrin g constantl y . D ecant

the mother l iquor Wash the pre -
.

c i pi t a t e by decantation U ntil the acidulated washings no longer

produce a precipitate With s ilver nitrate solution D ry the .

product .

T hi r d M e th od .

Calcium carbonate
H y drochloric acid ( 3 2 70 o f H Cl )
Calcium hydroxide .

Phosphoric acid ( 8 5 70 o f H 3 P O
S odium phosphate
Chlorine water su ffi cient ,
.

D istilled water su fficient ,

.

i “

M ix the w ith 6 0 parts o f distilled water and

h y d r oc h l o r i c acid ,

add th e c al c i um c a rbonat e When e ff ervescence has ceased heat

' '

f
;

the mi xtur e until solution is e ffected .

L et the liqui d cool and then add enough chlorine water to i m

part a distinct odor o f chlorine and m 1 x well Heat again until , .

the odor o f chlor i ne ceases .

1 N OW add the calcium hydroxide stir well and let the mixture , ,

s tand for hal f an hour at a temperature of 3 5 t o 4 0 C ° °

.

Filter the solution add the phosphor i c acid to the filtrate filter
, ,

again and let the solution get cold

,
.

D issolve the sod i um phosphate in 3 0 0 parts o f hot distilled

water filter and let the solution cool to about 2 0 C
,
°
.

Pou r the solution o f calcium chloride gradually and with con

stant stirring into the solution o f sod ium phosphate .

L et the mixture stand s t i rr 1n g frequently until the p r e c ip i

, ,

tate becomes cr y stall ine .

Trans fer the precipitate to a cloth strainer and wash it with

distilled water until the washings ( acidulated w ith n itric acid )
no longer give a precipitate with silver nitrate test solution -
.

L et i t drain thoroughl y ; squeeze out as much o f the water a s

practicabl e using strong pressure ; d ry the precipitate with the
,

aid o f mod rate heat an d reduce it to fine powder

e , .

D e scri pt i on . A
light white microcrystalline powder ; odorless
—
, , ,

t asteless ; insolubl e in water and in alcohol but soluble in solution ,

o f ammonium citrate .
 C AL CI U M S UL P H A T E .
33 1

S yrup o f Ca l c i u m L a c toph os ph a te .

Precipitated calcium carbonate

L actic acid
Phosphoric acid .

O range flower water

S ugar
Water .

To lactic acid m ixed with 1 00 ml o f water and contain e d

th e ,

in a 1 cap a c i ou s mortar gradually add the calcium,

portions until it is dis solve d Then add the phosphoric acid a nd

,
.
,

triturate u ntil the precipitate at first formed i s dis solved A d d

I 5 0 ml o f wate r and filter rinsing the mortar with 7 5 ml o f
, ,

water and passing the rinsings through the filter To the mi xe d

,
z
~
.

filtrate s add the orang e flo wer water , and hav ing a d ded t he ,

sugar d issolve it by agitation without he at and strain L astl y

, , , .
,:

pass enough water through the strainer to make the product

m easure 1 00 0 ml and m ix thoroughly , .

C A L CI U M S U L PH A T E .

'

JCA LCI I S UL PH A S ’
.

0 2 1 72

calci um s ulphat e Or gypsum conta ins two m olecules

[

”
N ative
“
’

'

o f wat er F rom it t he d ri e d c a l c i u m sulph ate or plas ter i s

“ ”
’

~ " :

made .

DR I ED . C
.
A L CI U M SU L PH A T

[ S urgica l Plast er o f Pa r i s

A p o w der c on t a m m g about 9 5 per ce nt , by w e ight , o f calcium

t

sulphate [ CaS O and about 5 p er cent o f wat e r ; p r e

pared from the purer varieties o f native gypsum by care fully heat
ing until about three fou rths o f the wat e r h as bee n expelle d
D ried calcium sulphate shoul d be kept in w ell closed vessels ,

care fully protected from moist ure .

N ot e s
‘

The k i nd o f f d r i e d calcium sulphate req ui red m om

.
.
' ‘

d l tak s up h w ry f o r crysta llization and

that r e a 1
y
_ _ e ; tv
e a t e r n e c e s s a
33 2 C AL CI U M S UL P HI DE .

at once sets to a hard mass A n anh y drous calcium sulphate does .

not do this Hence when the gy psum is dried the heat must not
.

exceed 1 0 5 C for i f that temperature is exceeded the product

°
.
,

“
wil l be anhydrous and usel ess S o called dental plaster o f .
—

paris is well adapted for surgical plaster bandages and casts I t .

i s sold by dealers in dentists supplies

.
’
.

D e scri pti on . Plaster o f paris is a fine white po w/der without , ,

d
o or or taste .

From moist air it attracts water becomes granular and th en , ,

los es the propert y o f hardening with water .

Whe n mixed with hal f o f its weight o f water dried calcium ,

s ulphate form s a smooth cohesive paste which rapidly hardens

, , .

It is So lubl e in about 4 1 0 parts o f water at 1 5 C ; in 3 882 °

.

pa rt s at 3 8 C and m 4 7 6 parts at 1 0 0 C In alcohol it i s

°
.
,
0
.

uble .

C A L CI U M S UL PH I D E ; CR UD E .

CA L x S U L PH U R A T A .

S ulphurated L im e .

A mixture containing at least 60 per cent o f Ca S .

D ried calcium sulphate in fine pow de r , .

7 0
Charcoal in fine powder , 10
S tarch in fine powder , 2

M ixthe powders thoroughly pack t h e mixture l ightly into a ,

crucibl e cover this loosely an d heat it to bright redness continu

, , ,

ing that heat until the contents cease to have a black color L et .

the crucible and contents cool R educe the product to powder . .

and at once put it into smal l glass stoppered bottles -

.

R e acti on . and

N ot e s The starch seems to rende r the m ixtu re more ea si ly

.

c on ver t ed by the he at The reduct ion is not complete and the

.

,
3 34 C AL C I U M T E T R A T H I OS U L P H A T E .

-
CAL C I U M T E T R A T H I O S U L PH A T E S OLU T I O N .

S O L U TI ON OF S UL PH URA T ED L I M E .

V l e mi n g k x S olution
’
. s .

S ublimed sulphur
L ime
Water .

parts o f water to the lime and make a uni form m 1x t u r e

A dd 10

o f them Dry and si ft the sulphur add it t o the lime mixture

. .
, ,

m ix well and then ad d z 5 parts o f wa t er Boil together f or one

,
.

"

hour stirring const an tl y an d replace t h e w ater lost by evapora

, ,

tion su fficiently to obt a i n I o parts of finished clea r soluti on L et .

s ettle and decant .

Kee p the product in well closed bottl e s

The solution c ontains calcium sul phide
N ot e s . an d calci um ,

thio sulphate .

The reactions a re
-

Ca O + H zO : Ca ( O H ) and

3 Ca ( O H ) 2+ I zSz z Ca S S 4 + Ca S Dg S + 3 H 2Q

It will be found that the theor etical p roportions o f sulphur and

calcium oxi de required by these reactions are 8 parts o f sulphur

employe d N ormal calcium sulphide 1 s Ca S and a soluti o

. n o f it ,

dissolves large quantities o f sulphur form ing according to many , ,

authorities v arious compounds The chie f constituent is h ow

,
.
,

ever Ca S S or calcium t e t rat h i os u l p h at e

,

d ark red brown liqui d having an odor of

'

D s cr i p t i on A hy
e
— -

droge n sulphid e .

CA R B O N .

P u r i fi e d A n i m a l Ch ar e oa l .

The pharmacopoeial process for the purification of animal char

co al is a s follows
Put I oo Gm o f bone black into a c a p a c i ou s flask and add 200 -
_
,
'

Gm of the o fficial hydrochloric acid and 1 0 0 m l o f boiling wa f er .

Connect the flask with an upright condenser A pply h e a t h y .

,
 C AR B ON .
335

m eans o f a sand bath to the flask an d keep the contents boil in g

-

gently for about eight hours Th en add 5 0 0 ml o f boil in g water .

and trans fer the mixture to a muslin strainer When the l iqu i d .

has run o ff return th e c h a rc oa l t o the flask A dd to it 1 00 ml

'

.
,

Of hydrochloric acid a nd the same quant ity o f boiling water boil ,

for t w o hours an d then again add 5 0 0 ml o f boiling water

, , , ,

trans fer the mi xture to a plain paper filter and when the l iqui d
.
}
, ,

ha s passed off wash the res idue with boil ing water until th e
,

washings no longer produce a precipitate but only a slight

cloudines s with s ilver nitrate test solution - -
.

D r y the washed charc oal perfectly in a drying oven and i m ,

mediately put the product in bottles and close thes e tightly

’

N ot e s The hydrochloric acid removes from the crude animal

.

charcoal or bone black all o f the calcium phosphate ( a l ittl e over

,
-
,

8 0 per cent ) and some other inorganic substances but leaves to ,

gether with the carbon the s iliceous matter ( which amounts to

about 4 per cent The product there fore i s less than 1 6 per
.
, ,

cent o f the weight o f the bone black used -

.

I f the bone black imparts color to soluti on o f K O H when boiled

-

w ith it it has not been completely carbonized I n that cas e it

,
.

shoul d be t fe a te d with that alkal i before it is boiled with hydro

chloric acid The bone black may be freed from animal matter
.
-

by percolating through it a 2 per cent solution o f K O H u n t i l t h e

liqu id pas ses colorless and then water until the percolate be ,

comes tasteless
‘

When purified animal charcoal has been kept a long tim e it is no

longer e ff ective as a decolo ri zing agent but can be renewed by
‘
'

[
,

being heated to dul l rednes s in a covered crucible and then allowed

to cool .

D e s cri pt i on .
—
A dull black odorless tasteless insoluble powder
-
, , .

CA R B O N D I OX I D E .

CA R B O N E I D I OX I D U M .

[ Carbonic A cid Ga s ]
CO 2 : 44 .

Put into a flask a convenient quantity o f marble or chalk i rf ,

small p i e c e s a i1 d add enough d istilled water to cover it Con

'

, .
33 6 C AR B ON D I OX I DE .

h ect this generator by means o f the required fittings with a wash

bottle containing distilled water and provide the wash bottl e with ,
-

a bent glas s t ube for conducting the gas wherever it may be n e

«

c e s s a ry A dd hydrochloric acid g radually through a safety tube

.
, ,

to the marble and water .

R e a ct i on .

N ot e s When calcium carbonate either in form o f marble o r

.
,

chalk is u sed for generating carbonic acid gas by doubl e d e c om

,

position with hydrochloric acid the by prod u ct o f calcium chloride ,

-

may be recovered or its solution may be used for the preparation

,
.

o f precipitated calcium carbonate .

When sulphuri c aci d is employ ed instead o f H Cl calcium sul ,

phate is formed Chalk an d sulphuric acid are not readily mixed

.

for making car bonic aci d in the manu facture o f m ineral waters
on a large scale owing to the fact that the whiting used contains
,
.

enough moi sture to render it lumpy so that a portion o f it is not ,

acted upon by the acid Chalk moreover contains animal a nd .

, ,

bituminous matters and therefore yiel ds an impure carbonic , , ,

acid gas o f disagreeable odor and taste which are with great di f ,

fi c ul t y removed Chalk i s nevertheless very generally employed

.
,

and sulphu r i c acid is used in pre fere nce to hydrochloric acid be ,

cause the latt er is not only dearer but requ ires a larger acid
chamber The reaction when chalk ( whiting ) and sulphuric
.
,

acid are the material s u sed i s : ,

Ca CO g l H S O 4 z Ca S O 4 + H zO + CO 2
— —

The prompt removal o f the calcium sulphate from the g enerator

as soon as the chalk has been consumed is n e cessary in V iew o f , ,

the fact that a hard mass is s oon formed by the r esidue which ,

wi ll be found t roubl e s om e t o remove

‘

A ssuming that the chalk used contains 90 per cent o f Ca CO a ,

and the sulphuric acid 9 2 per cent o f H S O 4 it will requ ire 1 0 z , ,

0 0 0 parts o f chalk and parts o f acid to produce parts o f

CO , At 20 C
. Gm o f carbonic acid gas measures
°
.

liters .

S odium bicarbonate furnishes a pu rer carbonic acid gas than can

be obtained from chalk .

“
C arbonic aci d water or s o c a lled soda water is water sat
,
.
-
,
3 38 C ER I U M OX I DE
'
.

other salts are made from the sulphate The oxal ate is mad e .

from the cerous sulphate and sodium oxalate .

D e s cri p t i onwhite powder tasteless and insolubl e in water

.
—
A , ,

but readily soluble in dilute acids .

CER I UM OX I D E .

CE R I I OX I D U M .

Ce O 2 : I 7 I .

'

Heat cerium oxalate in a Hes sian crucible to rednes s and let

the contents cool

D e s cr i pt i on .
—
A reddish powder ; insolubl e in water .

CER I UM S UL PH A T E .

CE R I I S UL P H A S .

Ce 2 ( S O , ) 3 5 66 .

Ceric oxide i s dissolved in sulphuric acid .

The ceric sulphate may be reduced to cerous sulphate by means

of sodium thiosulphate .

D e scr i pt i on .
—
Colorless ; soluble in water .

CH LO R I N E .

C H LORU M .

( 212 2 7 0 8 .

M anganes e dioxide
H y drochloric acid
Water

A s a generator flask o f ample capacit y and provided with

u se a

well fitting per forated rubber stopper carry ing the thistl e tube ,

sa fet y tube and del ivery tube ; Connect the gene rato r in t h e
‘

usual w a y with a wash bottl e c ontaining water a n d havin g a

-
,
 C H LOR I NE .
3 39

Id e li ve ry tube wh ich m a y be in turn connected with the vessel , ,

i nto which the c t r i n e g a s is to be conducted .

The manganese dioxide must be coarsely powdered and the

fi n e powder removed from it It is put in the generator all con .
,

n e c t i on s are made tight and then the mi x ture o f acid and water
,

poured into the fla sk through the thistl e tube .

5
Th e flask i s then heated by means o f a Bunsen burner and san d
b ath until t h e evolution o f chlorine begins ( at about 5 0
'
°

T he bu rn e r m ay t h e n be withdrawn to be replaced a gain only

‘

when the reaction se ems s o slow as to require it .

"
T h e ch lo rine i s w a s h e d by pas sing it through water .

R e acti on .

N ot e s .
S e e Chlorine S olution
The hydrochloric aci d m ay be .

a dded gradually a s r e q u i r e d and further addition discontinued

when no fu r th e r evolution o f chlorine i s des ired To stop the liber
’

.
_

ati on of c t r i ne entirel y the l iquid in the flask is poured off from

t h e remain in g manganes e dioxide This l iqui d containing man .
,

ganese chloride may be reserved for the recovery of the salt

‘

from it .

Kipp s apparatu s may be used to advanta g e

’
.

Chl or i n e S ol u ti on .

( H LOR I
C NE W A T ER ) .

A water solution o f Chlorin e containing

-
less than per n ot

c ent o f that element T his is not a s at u ra t e d solution but it is

i
'

.
,

s u fficiently strong and it woul d be di fficult to com ply with a r e

,

u i r m n t of greater chlorine strength becaus e water is d e c om

q e e

posed by c h l or i n e h yd roc h l or i c acid being formed and a strong er

h ,

s olution de teriorates more r ap i d ly f A saturated solution at I 5 °

C contains about
. per cent o f C12 .

A pp ar at us r e q u i re d .
ml capacity ; a sand A flask o f about 5 00
bath an d Bunsen burner ; a Woul ff bottl e o f about one l iter s ’

capacity ; two glas s stoppered receiving bottl es each o f one liter s

- -
,
’

capacity ; glass tubing per forated rubber stoppers rubber tube

~

, ,

connec t ions and sa fety tubes ; and glas s stoppered containers o f

-
,

ambe r colored gla ss and o f 20 0 or at most 2 5 0 ml capacity

-

The flask to be used as the generator the Woul ff bottl e in w

.

hi ch ,
3 40 C H LOR I NE .

the gas i s washed an d one o f the receivin g bottl es are con nected
,
—

by means o f the stoppers an d tubing and provided with the sa fety ,

tubes .

A vessel of water is al so necessary in which the re c eivers may

be placed to cool them with the aid o f crushed ice .

M a t e r i al s
Coars ely powdered manganese dioxide freed from
.
,

fi n e powder 2 0 Gm ; o fficial hydrochloric acid ; di stilled water

,

which has been boil ed a few m inutes and allowed t o cool again ;
a su fficien t quantity o f ice ; and some loo se cotton .

“
Pr oce ss Put the manganese dioxide ( 2 0 Gm ) into the flask
.

an d place this on the sand bath —

.

Put about 1 2 0 m l o f water into the wash bottle -

.

Put 4 0 0 m l o f water into each receiving bottle

' -
.

Place one o f the receiving bottles in the vess el o f wat e r kept

-

°
at a temperature o f about 1 0 C by m eans o f the ice and put into .
,

the neck o f that bottle som e loose cotton around the glass tube
through which the chlorine i s to enter it .

N ow pour into the flask or generator through the thistle tube , ,

a mixture o f 7 0 ml o f hydrochloric acid and 5 0 ml of water .

A pply gently heat to the sand bath so as to warm the fl ask -

.

Increase the heat gradually so that the liberation o f chlorine,

may proceed rapidly e n o u g h bu t not violently The chlorine i s

‘

to be passed through the water in the wash bottl e and then from -

the upper part o f that bottl e into the receiver .

When the air in the receiving bottle shal l have been wholly dis -

placed by the greenish yellow chlorine gas remove the bottle c lose
-
, ,

it with its glass stopper and put the s econ d receiving bottle ( con
,
-

taining like the first 4 0 0 ml o f boil ed and cooled water ) in its

, ,

place .

S hake well the receiving bottle j ust removed s o th a t t he chlor

ine may be dissolved in the water .

Continue the evolution o f chlorine and collect the washed gas

as before exchanging the two receiving b ottles altern ately in
,
—
, ,

the manner described until the water 1n both shall have be com e
,

thoroughly satu rated with chlorine .

Then pour the saturated solution into the amber colored stock -

bottles filling each of them complete l y close the filled bottles

, ,

tightly by their glass stoppers and keep them in a cool dark , ,

place .
34 2 C H LOR I NA T E D L TM E .

D e s cri pt i ongreenish yellow l iquid havin g t he p e cu l i a r su f

'

.
—
A —

f oca t i n g odor and disa g reeable taste o f chlorine It decolorizes .

dilute solutions of litm us indigo and other ve g etable coloring

,

matters .

Ch l or i n a t e d L i m e .

( B leaching Powder .
“
Chloride o f L ime .

A sl i ghtly grayish white or quite white granular , dr y pow der

, , ,

evolving the odor o f h y pochlorous acid ( a somewhat chlorine lik e -

odor ) It has a nauseous acrid sal ine taste Very hygroscopic

.
, ,
. .

D ecomposes on exposu re to air O nly partially solub l e in water .

R eacts with alcohol and with glycerin

”

Its principal or most important constituent i s c al c i u m h ypo

‘

, ,

chlorite Ca ( O Cl ) g which readily decomposes on the addition o f

,

an acid giving off free chlorine The chlorine th us l i be ra t e d i s

,
. .

“ ”
termed the availabl e chlorine o f the chlorinated l ime and th e
”

, ,

A merican Pharmacop oeia requires the preparation to c ont ai n an d

produce not less than 3 5 per cent o f available chlorine .

C alcium chlori de constitutes a large proportio n of t he chlorin

at e d lime .

Bleaching powder is p roduced by th e action of c t r i ne on; -

slaked lime
Chlorinated l ime must be kept 1 n tightly closed ves sels to com ,

p l e t e l y exclude air and moisture and should be stored i n a cool , ,

dry place .

When damp the chlorinated l ime should be rej e ct ed .

It 1 5 largely us ed a s a bleaching agent and as a di sin fectant

f T o produce chlorine gas for purpos es o f disin fect i on chlorin ,

ated lime may be put in a dish m 1x e d with s ome diluted aci d or ,

vinegar and placed in the roo m which i s then kept closed for a
,

s u fli c i e n t period .

CH R O M I U M A C ET A T E .

CH R O M I I A CE T A S .

Cr ( C2H 3 0 -
2 29 .

Chrome alum
S odium carbonate
A cetic acid -

Water .
 C H ROM E AL U M .
’

343

D issolve the chrome alum in 4 0 parts and the sod ium carbonate .
,

in 2 0 parts o f water A dd the sodium carbonate solution to the

.

chrome al um stirring well Wash the chromium hydroxide w ith

,
.

warm water by decantation D rain w ell and d issolve it in the .

,

acetic aci d with the aid o f moderate heat E vaporate to dryness . .

R e ac t i on .

and then

D e s cr i pt i on
greenish very soluble salt extremely di ffi cult
.
—
A , ,

to crystallize The solution when ma de below 6 0 i s violet but it

.
°
,

becomes greenish when heated .

CH R O M E ALU M .

ALU M EN C H R O M I CU M .

4 99 .

Potassium dichromate 4 parts

S ulphuric acid of H Q S O4 ) 5 parts
Water 9 parts
S tarch I part
Put the water in a large enough porcela in dish to hol d at least
twice the total quantities operated upon S e t the water into rap id .

rotary motion by stirring with a glass rod A dd the sulphuric .

acid in a thin stream D issolve the potassium dichromate in the

.

mixture Then add the starch a small quantity at a time stir

.
,

ring cautiously When the reaction is nearly ended heat the

.
,

l iquid i f n e c e s s a ry until it acquires a bl u ish green color Filter

, ,
-
.

the solution and set it in a c ol d place to cr y stallize .

R e a ct i on .

2K Cr , O , 8H , S OH 3 C l 4O H 20
1 2H 0]4
—
— — — — L
2 ,

3 CO Q .

N ot e s The temperature of the reaction i s very h igh and the

.
,

chemical interaction liable to be violent unless the starch be added

ve ry slowly I t is necessar y that the mixture should remain hot
. .
3 44 C H RO M I C AN HY DR I DE .

throughout the whole reaction but no appli cation o f heat from ,

without is necessary nor should it be resorted to until after the

,

violence o f the action has subsided The liqui d must at the end be .

bluish g reen and not olive green S hould the bluish green color
-
,
-
-
.
-

be a ttained without the application o f heat no heating is n e c e s ,

sary S hould on the other hand the l iquid be ol ive green heat it
.
, , ,

cautiously until it acqu ires a bluish green color -

.

In case the crystallization should be much retarded evaporate ,

the solution somewhat and then set it in a cold place S hould

,
.

it still fail to crystallize drop I nt o it a few crystals o f chrome

alum to start the crystal lization .

A s the salt is e ffl ore s ce nt it must be kept in tightly closed bot

tles in a cool place .

D e scr i pt i on D ark
purple transparent crystals, solubl e in 7
—
,

parts o f water at The col d solution is reddish blue but -

,

above 7 0 it becomes bluish green

°
-
.

CH R O M I C A N H Y D R I D E .

A CI DU M C H R O M I CU M .

Chromic A ci d . U . S .
]
Cr O 3 : I oo .

Potassium dichromate
S ulphuric acid of H 5 O4 ) 2

N itric acid ( 6 8 % o f H N O ) 3 .

Water .

Put 5 parts o f water in a porcelain dish capable o f holdin g about

ten times that quantity ; set this wate r into rotary motion by brisk
s t 1 r r 1 n g W i th a glas s rod A dd slowly and in a small stream
.

parts of the sulphuric acid D issolve th e coarsely powdered p o .

t a s s i u m di chromate in the m ixture appl y ing gentl e heat to facil i ,

tate the solution L et the l iquid stand ( at the ordinary room

.

temperatur e ) for about twelve hours in the dish which should be ,

covered to keep out dust A mass o f cr y stal s o f acid potassium

.

sulphate will now be foun d on the bottom o f the dish .

D ecant the red liquid from the crystals Heat it in a large .

3 4 6 C H RO M I U M HYDROX I DE .

'

S ol u ti on i
o Ch rom i c A ci d ; B P . .

The B ritish Pharmacopoeia contains a formula for a solution “

o f chromic acid I t directs the solution of 1 part o f chromic a n

.

hydri de i n 3 parts o f distill ed water Thi s s ol u t i on h a s the s p w

'

. .

and its stren g th is per cent expr e sse d in terms o f

c h r om 1 c acid ( H Cr O 4 ) corresponding to 2 5 per cent o f chromic
2 ,

anhydride ( Cr O 3 )

CH R O M I U M H Y D R OX I D E .

CH R O M I I H Y D R OX I D U M .

'

Cr ( O H ) 3
—
I O3 .

Prepared from chrom e al um as describ ed under the head o f

chrom ium acetate .

I t m a y als o be prepare d f ro mch ro mium sulphate as follo ws

‘

, ,

Chromium sulphate
A mmonia water "

Water .

D i ss olve
the chrom e alum in a n e q u a l w eight o f water and add
‘
‘

the ammonia B oil for twenty m inutes

. . Wa sh and dry the pre
c ip i t a t e .

"
Chromium hydroxide may also be prepared by conducting a
strong current of hydrogen sulph ide into a solution o f pota ss ium
dichromate until the precipitate formed becomes green and then ,

washing and drying it ; but this product contains much sulphur .

D e scri pti on .
—
A green I nsoluble pow der
, .

CH R O M I U M S UL PH A T E .

CH R O M I I S UL P H A S .

Cr 2 ( S O 4 ) 3 1 H
5 , O : 66 2 .

D issolve parts o f dry chromium hydroxide m 2 5 parts o f

24

s ulphuric acid of strength in a porcelain dish at a tempera

ture o f about 40 to A violet s ol u t 1on is obtained f rom which
°

cry stals are obtained on cool in g T h e temperat ure must not be

“

. i
 CO PP E R A CET AT E .
3 47

perm itted to exceed 6 0 at any time as t he solution then becom es

°

green and does not yiel d any crystals until a fter standing for
several w eek s 1 -

I t 18 sai d t h at s ome d 1 l u t e alcohol to t h e p urpl e

solution o f chromic sulphate facilitates the crystallization Of the

Des r ci pti on Purpl e or violet crystals solubl e in l ess than thei r

—
,

ow n w ei gh t o f wa ter .

C O PP E R A C E T A T E .

CU PR I A CE T A S .

Cu CzH g O z ) 2 H
‘

.
2 O; 19 9 :5 .

S ubacetate o f copper
D iluted acetic acid
Water

Tri turate the ve rdi gri s wi th eno ugh water to form a smooth ,

th in p a ste Then add the acid mix well tran sfer the mixture t o
.
, ,

a porcelain capsul e an d heat it over a water bath at not over 8 0

,
°

C. F ) until solution i s e ff ected Filter while hot S e t

. . .

aside to cool and c rystall ize Coll ect and dry the Crystals on blot
.

t in g paper in a cool place

‘

R e a ct i on . Cu zO C2H 3 O z ) 2 —
1 — 2H C2H 3 O z } H 2O « -

N ot es. .
T o o btain good crystals a sl ight exces s o f acet ic aci d
must be present during the evaporation and c ry st a l l i za t i On S houl d
“

. .

the l iquid become unclear fro m blu e di basic copper acetate

"
,

through los s o f acetic a ci d by evapOrat i on more acid must be ,

added .

A dditional crops o f Crystal s can be obtained from the mother -

l iquor On evaporation
The t otal p roduct should be at least equal to the we ight o f t he :

ve rdigris used The crystal s shoul d be d i s t i n c t d e e p green and

.
, ‘ _
,

should make per fectly clear solutions with water or with ammonia ,

water ,
'

M as t be kep t in a fw e ll (forke d bo ttle , a n d i n a c oo l place

fl

.
3 4 8 C O PP E R A CE T A T E .

S e c on d M e t h od .

Copper sulphate
L ead acetate
A cetic acid su fficient , .

D issolveeach salt s eparately in 6 parts o f water I f necessary .

add a little acetic acid to the solution o f the lead acetate to render
it clear Filter the solutions M i x them Filter Collect the
. . . .

filtrate containing the copper acetate evaporate it on a water bath ,

-

at not over 8 0 C ( 1 7 6 F ) until a pellicle begins to form taking

°
.
°
.
,

care to keep acetic acid present in excess Then set aside to crys .

t a l l i ze .

R e act i on . Cu S O 4 5 H 20 .
—
Pb ( C2H 3 0 2 ) 23 H zO

Cu ( C2H 3 0 2) 2
H ,O .
—
PbS O , —
H
7 20

T hi r d M e th od .

Copper sulphate 25 part s

S o l ution o f sodium hydroxide ( 5 per cent )
,
165 parts
A cetic aci d ( 3 6 per cent o f H C H 3 O ) 2 2 3 6 part s
Water .

D issolvethe copper sulphate in 2 5 0 parts o f water and filter .

Pou r this solution into the solution o f sodium h y droxide stirring ,

briskly Wash the precipitated copper hydroxide thoroughly by

.

a ffusion and decantation o f water until the washings are tasteles s .

L et it drain Put the moist copper hydroxide in a porcelain d ish

. .

A dd th e acetic acid Heat gently until solution is e ff ected E vap

. .

orate to crystallization taking care to keep an excess o f acetic aci d

,

present in t h e l iqu id .

F ou r t h M e t h od .

Copper acetate may also be prepared by adding a solution o f

copper sulphate to one o f bar 1 um acetate until n o fu rthe r p r e c i p
i t at i on results Care shoul d be taken to add neither more nor less
.

than is necessar y The l iqu id must be well stirred and set aside
.

for a d a y or tw o before it is filtered and the filtrate evaporated to

c r vs t a ll i z a t i on .

n e ac t i om (311 5 0 4 + 13 3 Cs Oz) -
Cu CzH aoz ) 2+ B a S O 4 ’
3 5 0 C O PP ER N IT RA T E .
“

stirrin g well R ej ect th e precipitat ed barium sulpha te? F il t e f t h e

’

s ol ution o f copper nitrate acidi f y it w ith n i t r i c a c i d and evaporate

, ,

it to obtain the product in crystals .

R edissolve the crystals in distil led w a ter ac i di fy w i t h ni t ri c

“ '

, ,

acid and recrystal l iz e

,
.

R e acti on . Cu S O 4 5 H zO + Ba N O 3 ) 2= Cu N O 3
.
2
. H
3 2 O ~

A noth er M e t od h .

Copper nitrate may al so be ma de by s a t ura t ifig d i lut e d nitric

’

"
acid with metallic cop per a n d c ry s t a ll i zi ng a t ab o ut 25 C ' ‘ ‘

.
,
0

R e act i on .
—
H
ta 2 0 —
4 — 2N O .

D e scr i pt i on .
—
B eauti ful , t ra n s p a re nt
l de e p- bl ue crystal s readily ,

solubl e in water .

C O PP E R OLEA T E .

CU PR I OLEA S
‘

Cu ( Cm H a z) 2
O 2 76 2
5 5

Copper sulphate
White castil e s oap ,
i n jfi ne po wde r .

D issolve th e copper sulphate in five liters o f water and the soap ,

in three l iters of hot wa t e r Po ur the soa p sol u t i on into that o f m ,

— ~
~

the copper sulphate sti r ri n g w e l l W a s h the precip itated oleate

‘

, .

twice using ten liters o f h ot w ate r ea ch time Collect the dark

, .

green ol eate squ eeze the water out of i t , and fuse it by very gentle
,
p

heat over the water b ath i

,
-
‘

R e act i on . Cu S O g+ 2 N a C1 8 H 3 3 O 2;
3 A
-
Cu ( C 18
H 3 3 0 2) 2
—
N as,

The product i s about 2 90 Gm of a dark g reen Wax y

N ot e s . .
-
,

plaster conta in ing

,
per cent o f coppe r oxi de .
 C O PP ER OX I DE .
35 1

C O P P E R OX I D E .

CU PR I OX I D U M .

Cq 79 5 . .

Heat copper nitrate strongly until n o more red vapors pass off

and the residue i s a fine black powder ,

.

2 Cu N O 3 ) 2: 2 Cu O + 2 N ZO4 + Oz .

Cupr ic oxide is insoluble in water but readily solubl e in dilute ,

hydrochloric nitric sulphuric and acetic aci ds

, ,
.

C O PP E R S U B CAR BO N ATE .

CU PR I S U B CA R B O N A S .

Cupric sulphate
S odium carbonate
Water .

D issolve the blu e vitriol in 2 0 parts o f hot water and filter D i s .

solve the sodium carbonate also in 2 0 parts o f water and filter .

A dd th e hot copper solution slowly or in small portions to the hot

sodium carbonate solution in a large vessel being care ful not to ,

let the l iquid run over from the active e ffervescence Wash the .

precipitate with hot water by decantation and then dry it .

D e s cri p t i on .
—
A
green powder having a variabl e composition .

Insolubl e 1 n water but readily soluble in acetic sulphuric hydro , ,

chloric and nitric acid s .

C OPP E R S UL PH A T E .

C U PR I S UL PH A S .

Copper in fil ings
,

S ulphuric acid
N itric acid
Water O O O O O O O O O O O O O O O O O O O O O O O O O O O O O O
35 2 C O PP ER S UL PH A T E .

M ix the ingredi ents in a flask and heat at first gently and a fter ,

wards raise the temperat u re gradually to the boil ing point Boil .

until the evolution of gas ceases evap orate the solution to dryness , ,

dissolve the res idue in four times its weight o f water filter and ,

evaporate to crystallization D ry the crystals without the aid o f

.

heat .

R e a ct i on .

Gr anu l a te d
pp co er o f s ul
copper rph
e duced
a t e to. S ulphate ,

coarse powder i s dissolved in an equal weight o f boil ing water

, ,

and the solution filtered and evaporated during constant stirring

-

until nearly dry a fter which the residue is dried by spreading it in

,

thin layers on pape r and exposing it to currents o f dry a i r

. .

Precipitated copper sulphate may be made by di ssolving the sal t -

in its ow n Weight of boil ing water and filtering the solution into ,

an equal volume o f alcohol .

Tu r bi d a te d co er s ul ph
may be made by dissolving 2 0 parts
pp a t e

o f coarsely powdered copper sulphate in 2 0 parts o f boiling water ,

acidi fying with I part o f diluted sulphuric acid filtering the solu ,

tion W hile hot and stirring the filtrate briskly until col d The
, .

granular salt thus obtained is collected on a filter drained dried , ,

at the ordinary temperature and bottled The mother l iquor is , .

evaporated to one hal f its weight and an additional amount o f

-

product obtained f rom it in the same manner A ll of the remain .

ing salt may be recovered by evaporation nearly to drynes s and ,

finishing the drying by exposure to the air .

P u r i fi ca ti on o f Com m e r ci a l B l u e Vi tr i ol m a y be e ffected as
follows :
Put the bluestone or blue vitriol into a porcelain dish A dd 3 .

parts o f w ater A ppl y heat an d bring t he solution to the boiling

‘

point Then add small quantities at a time o f nitric acid stir well
.
, ,

and continue heating When the liquid no longer gives o ff nitrous

.

vapors on the further addition o f n itr i c acid boil it a few minutes ,

longer and th en l et it cool A dd to the col d solution enough

,
.

water o f am monia to impart a permanent ammoniacal odor to it .

L et it stand a few hours Filter E vaporate to dr yness and heat

. .
,

the residu e strongl y until it becomes nearly white Then let it .

cool dissolve it in
,
parts o f water filter the solution add , ,
3 54 AM M ON I U M C O PP ER S UL PH A T E .

d uce d to a dry powder this product is to be kept in a tightly stop

“

pered bottle .

This preparation is nearly simi lar in composition to the crystal

l ine ammoniacal copper sulphate which is more uni form o f hand , ,

some appearance and prepared as follows ,

*

A m m oni a c a l Coppe r S ul ph a t e .

Copper sulphate in powder ,

A mmonia water
A lcohol o f 8 5 % strength
D iss olve the sulphate o f copper in the ammonia water containe d
in a porcelain capsule without applying h eat ( Heat is generated ,
.

by the chem ical solution ) When the l iqui d has become cold .
,

filter it Put the alcohol in a tall narrow cylinder Then run in

.
,
.

under the alcohol 1 0 ml of water by mean s o f a funnel tube reach

ing to the bottom o f the cylinder Final ly add the copper solution .

through the same tube so that it may form a separate layer under
the water S e t it asi de w ithout disturbing it and well corked fOr
.
, , ,

one to fou r weeks and then decant the mother l iquor and throw
, ,

i t away Collect the crystal s and dry them as rapidly as poss ible
.

w ithout the aid o f heat by gently press ing them between bibulous
paper avoiding exposure to the a n as far as practicable Put th e
, .

product at once into a bottle and cork it tightly .

D e scr i p t i on
The preparation i s in handsome dark blue
—
.
,
—
,

needl e l ike crystals having an ammoniacal odor an d a nauseous

—
, ,

metall ic taste S oluble in I 5 parts o f water

. . .

“ ”
It is not ammonio copper sulphate wh ich may be made by -
,

mixing solutions o f the sulphates o f ammonium a nd o f copper .

A mmoniacal copper sulphate readily absorbs oxygen from th e

air and hence acts as an oxidizing agent on substances present in
,

its sol ution Thus sodium thiosulphate is rapidly converted int o

.
,

sulphate ; asparagin and gl y cocoll to oxalic and carbonic acids ,

etc.

Coppe r P otas s i u m S ul
ph a t e .

0
Copper sulphate
Potassium sulphate
Concentrated sulphuric acid
Water .
 G OLD .
355

D issolvethe copper sulphate in 1 5 0 parts o f hot water and the ,

potass ium sulphate in a si milar quantity of hot water to which ,

the sulphuric ac id has been added M i x the solutions L et th e . .

m ixture stand until cold Collect the light blue crystals and dry
.
-

them E vaporate the mother liquor to one hal f and l et coo l again
.
- —

to obtain a second crop . .

A l u m i n a te d Coppe r .

L
( pa is D i vi n u s . Cuprum A l u m i nat u m .
)
Copper sulphate 1 5 parts
A lum 1 5 parts
Potassium nitrate 1 5 parts

Camphor I part
Powder the salts an d mix them Fu se the m ixed powder in a .

porcelain dish stirring well L et the ma ss cool

, Powder it
. . .

Finally add the camphor and mix the whol e intimately by tritura
tion.

G OL D ; PUR E .

AURU M P URU M .

A uz 1 97 .

Gold in coin or scraps

,

H y drochloric acid of H Cl )
N itric acid ( 6 8 % o f H N O 3 )
Ferrous sulphate
D istilled water .

Put the gold in a flask with the hydrochloric acid A ppl y gentl e .

h eat A dd the nitric acid a l ittl e at a time until the metal is com
.
, ,

p l e t e l y dissolved ( leaving only the precipitated silver chloride

formed by the s ilver contained in the gol d coin or scraps i f a l ,

loyed with s ilver ) . Filter the solution through a paper filter ,

washing the silver chlori de on the filter with a l ittl e distilled water
and ad ding the washings to the filtrate E vaporate the filtrate to .

a syrupy con sistence weigh it and dilute it with ten times its
, ,

weight o f d istilled water .

D issolve the ferrous sulphate in 2 5 0 parts o f distilled water ,

3 56 G OL D .

ac idulate the solution with 5 parts o f diluted hydrochloric acid ,

h eat to boil ing filter and let the filtrate cool

, , .

A dd the solution of ferrous sulphate very gradually and with

constant stirring to the solution o f gol d chloride S e t the mix .

ture in a warm place for an hou r Then col lect the yellowish .

brown precipitate o f metall i c gold upon a paper filter wash it first ,

with a littl e diluted h y drochloric and a fterwards with distilled

water D ry the product with the ai d o f moderate heat
. .

R e act i on s . First ,
2A u C1
+3 2
—
2 A u Cl 3 ; then ,
2 A u C13 - t
—
6 F e S O4

N ot e s Coin gold and gol d employed in making j ewelry and

.

gold vessels is allo yed with e ither s ilver or c op p e r or both The ,

.

s ilver forms insoluble s ilver chloride when the gol d coin is dis
solved i n the hydrochloric and n itric acids [ This s ilver chloride .

s h oul d be collected and may be reduced to metallic s ilver when ,

convenient as described under the title of S ilver ; Pure ] Cop

,

per dissolves together with the gold but remain s in the liquid ,

when the gol d is precipitated w ith ferrous sulphate .

The solution o f gol d chlori de and that o f ferrous sulphate

should be per fectly clear when about to be mixed Ferrous chlor .

ide may be u sed in place o f ferrous sulphate .

The precipitated gol d i s chemicall y pure and so finely divided

that it is easily dissolved in h y d roc h l or1c and nitric acids mixed
together .

O xal ic acid ( pure ) may be used instead o f ferrou s sulphate for

the precipitat ion o f the gold .

The amount o f crystallized oxal ic acid required for 12 parts o f

gold i s about parts .

G OL D CH LO R I D E .

AUR I CH L OR I D U M .

A u C13 :

Pu re gold
H y drochloric acid H Cl )
N itric acid ( 68 % H N Og)
35 8 G OLD C H LOR I D E ,

The pure gol d required is precipitated as described und er

Gold .

The gold an d sodium chloride o f the A merican

D e scri pti on .
—

Pharmacopoeia consi sts o f equal w eights o f gol d trichloride and

“

sodium chloride It is a c oarse orange yellow granular p owder ;

.
, ,

odorless ; taste saline m etallic I t i s sl ightly deliquescent in moist

, .

air R eadily solubl e in water A lcohol dissolves the gold chloride

. .
,

leaving the sodium chloride which should constitute not more ,

than one hal f by weight o f the whol e quantity added t o the a lc o

-

11 0 1 .

A n ot h e r M e th od .

This preparation may be made as follows

Pure gold
H y drochloric acid
N itric acid
D istilled water
D ry pure sodium chlori de

the gol d in the mixed acids A dd the water D i s

D issolve . .

solve the sodium chloride i n th e liquid E vaporate the liqu id over .

a water bath to dryness

-
.

N ot e sIn this formula which is constructed a fter that o f t he

.
,

German pharmacopoeia there is rather more hydrochloric aci d a nd

,

less nitric acid prescribed than in other working formulas .

A noth e r M e th od .

( A fter the S wiss Pharmacopoe ia ) .

Pure gol d 65 parts

H y drochloric acid ( 2 5 70 o f H Cl ) 1 80 par t s
N itric acid o f H N O g or , sp . w) 60 parts
S odium chloride 1 00 par t s
D istilled water 1 00 parts

M ixthe acids D issolve the gold in the mixture with the aid
.

o f gentl e heat E vaporate the solution over a water bath to the

.
-

consistence of syrup so that upon cool ing it forms a sol i d salt

,

mass D issolve this gold chloride in the distilled water add t h e

.
,

completely dried ( decrepitated ) sodium chlori de and evaporate ,

to drynes s over a water bath -

.
 H YD RO G EN .
3 59

HYD R O GEN .

Hydrogen gas when req uired for laboratory operations may be

, ,

m a de as follows
.

Zinc granulated 7 0 parts

S ulphuric acid 1 00 parts
Water 5 0 0 parts

Put the zi n c in a wide mouthed hal f gallon bottl e provided w ith

- -

a twice per forated rubber stopper fitted with thistle tube and a ,
-
.

bent del ivery tube Connect the del ivery tube with a wash bottle
.
-

’
o f about a quart s capacity containing a pint o f water and provi d e ,

the wash bottl e with the neces sary del ivery tube which may be , ,

in turn connected with any bottle or tube into which the hydro g en
,

i s to be conducted .

A dd the sulphuric acid to the zinc through the thistle tube as ,

requ ired .

The most convenient apparatus for producin g hydrogen as well .

,

a s hydrogen sulphide an d several other gases is Kipp s apparatus ,

’
.

R e act i on . Z n + H zS O 4 : Z n S O 4 —
~

H 2
.

S ixty fiv e Gm o f zinc i f al l consumed will furnish 2 Gm o f ’

—
, ,

hydrogen according to thi s equation O ne cubic decimeter o f .

-

h y drogen at 0 C bar 7 6 0 mm weighs about

°
.
,
Gm and 2 Gm
. .
, ,

o f hydrogen there fore occupies about

, cubic decimeters
,
-
.

H YD R O G E N D I OX I D E S OLU TI O N .

L I QUOR H Y D R O GE N I I D I OX I D I .

A water solution containing when fresh about

-
3 per cent o f , ,

hydrogen d ioxide H Q O corresponding to about 1 0 volume units

, Q,

o f free oxygen obtainabl e from each volume unit o f the solution .

required for the preparation o f about 1 liter : Two

A p p ar at u s
hal f gallon bottles White pap er filters o f 3 0 Cm diameter and
-
.

o f such character as to admit o f rapid filtration A funnel to .

correspond to the size o f the filter .

3 6 0 HY DRO G EN DI OX I DE .

M at e r i a l s
Barium dioxide 3 0 0 Gm ; phosphoric acid
.
'

about 1 0 0 ml ; diluted sulphuric acid about 2 ml ; starch in , , p o w

der about 1 0 Gm ; distilled water about 1 l iter
, ,
.

Pr oce ss Put . ml o f col d distilled water into a hal f gallon

5 0 0 -

bottle A dd graduall y the coarse powder o f the barium dioxide

.
,

and shake a fter each addition to break up any lumps that might
be form ed When all o f the barium dioxide has been added shake
.

the bottl e vi g orously so that the contents may form a uni form
mixture
Place the bottl e in a vessel o f water cooled by additions o f
broken i c e so that the contents may be kept at a temperature
°
somewhat below 1 0 C 5 0 F ) for about hal f an hour D uring
.
°
. .

'
that time s hake the bottl e thoroughly every few minutes Con .

t i n u e keepi ng the mixture cool and shaking it occasionally an d

strongly until the barium dioxide shall have been converted into
hydroxide which may be known by the fact that but l ittl e water
,
'

i s separated on standing and that a uni form m ixture may be

'
obtai ned; w i th out d i ffi c u l t y by shaking ,
.

Put into the other hal f gallon bottle 9 6 ml o f phosphoric acid

-

and 3 2 0 m l o f distilled water and cool thi s mixture to about ,

10
0
C Take o f this l iquid 5 0 ml an d set that aside To the
. .

remainder o f the mixture o f phosphoric acid and water add in ,

four equal portions the well m ixed magma from the first bottle
,
-
,

shaking the mixture vigorousl y an d cool ing it a fter each add i

tion N ote the reaction o f the mixture upon l itmus paper and
.
, ,

when it shows an alkaline reaction add cautiously enough o f the ,

reserved dilute phosphoric acid to render the reaction again acid .

R epeat th e vigorous shak ing of the bottle and the gradual

addition o f more phosphoric aci d until the l iqu i d no longer be
comes alkal ine upon long continued strong shaking ( S houl d .

the reserved portion o f the mixture o f phosphoric acid and water

prove insu ffi cient t o e ff ect a slightly acid reaction m ix a suffi cient ,

additional amount o f phosphoric acid and distilled water in the

sa me proportions as before an d add o f this as much as may be
'

necessary ) .

When t h e whole mixture shall have been finally thoroughly

shaken until the l iquid portion has acquired a neutral reaction on
test pape r set the bottle aside and let it rest until the supernatant
,

liquid occupies abou t two thirds o f the volume o f the whol e mix
-
3 62 HY DRO G EN DI OX I DE .

ml o f the diluted solution ) 1 ml may be taken ( using 1 0 ml o f

,

a mixture made o f 1 0 ml of the S olution and 90 ml o f distilled

water ) The number o f ml o f permanganate solution decolor i zed
.

by each ml o f the solution o f hydrogen dioxide when multipl ied

by gives a product expressing the number o f volumes o f
oxygen yi e l d e d by one volume of the solution o f H 2O 2 The
‘
.

number o f m 1 o f permanganate solution decolorized by each ml o f

solution o f hydrogen dioxide when multiplied by gives a
product express ing the per cent o f H 2O contained in the prepara 2
.

tion E ach
. ml o f the solution o f H 0 2 should require not 2

less than 3 0 ml o f the volumetric permanganate solution or each ,

ml shoul d require not l es s than ml The reaction which .

takes place in the assay process is

Thus molecules o f K M n O 4 are requ ired for 5 molecules of

2

H 20 2 A s the mol weight o f K M n O 4 is 1 5 8 and that o f H 20 2

. .

is 3 4 an d as the permanganate solution i s a decin ormal one

,

it follows that each ml o f the volumetric solution containing ,

Gm o f K M n O 4 corresponds t o Gm o f H 0 2 or to 2

Gm o f a va i l a bl e O 2.

The first reaction by which the barium dioxi de is de

N ot e s .

composed is

B a O 2 + 2 H zO z B a OH ) 2

T he completion o f thi s facil itated by cool i n g the

r e a c t 1 on IS

water below 1 0 C and may be known to have been attained

°
.
,

when a magma has been formed from which bu t l ittl e water

separates on standing .

The barium i s then precipitated by means o f phosphoric acid .

I f necessar y a little sulphu ric aci d may be u sed as directed ,

by
the Pharmacopoeia to c ompl ete the separation o f the barium
,
.

A ll that then remains to be done is the filtration o f the liquid

and the ad 1u s t m e nt o f its stren gth to the prescribed standard .
 H YD RO GEN DI OX I DE .
363

T he filtration i s frequ ently difficult . A doubl e filter is ne ce s

sary and starch is added to further aid the clarification .

S mal l quantities o f phosphoric and sulphuric acids are u m

avoidably left in the product an d their presence tends to pre
,

s erve it .

Hydrogen d ioxide i s very unstable an d its uses depend upon ,

that fact ; it decomposes into water and oxygen Heat and light .

hasten this decompo s ition Hence it must be kept in a cool pl ac e

.

and protected from light But it can not be kept in tightly stop
.

pered bottles because the containers would burst shoul d the

d ioxide decompose in them .

S olution o f hydrogen dioxide may be evaporated on a water

'

°
bath at a temperature not exceeding 6 0 C until reduced to one
, .
,

fif t h o f its original vol ume being thus rendered five times the
,

o fficial strength or made o f such strength that each volume o f

,

the concentrate d soluti on will yield fi fty volumes o f oxygen upon

decomposition o f the hydrogen dioxide it contains .

O ne per cent o f boroglycerin is said to retard the decompos i

tion o f th e solution I t should be kept in a cool dark pl ace
.
,
.

D e scri pt i on —
A
colorless odorless liquid slightly acidulou s in
, ,

taste and producing a peculiar sensation and soapy froth in the

mouth R eaction acid owing to the free acid left in the l iqu id
.
,

to preserve it The dioxide is liable to decomposition when the

.

solution i s rapidly heat ed to a temperature above 6 0 C °

.

H YD R O G EN S UL PH I D E .

H 28 : 3 4 .

When hydrogen sulphide is required for laboratory Operations ,

as in the preparation o f hydrobromic o r hydriodic acid it may ,

be produced as follows
Put any convenient and suitabl e quantity o f ferrous sulphide
’
in small fragments into a Kipp s apparatu s ( Fig and add .

diluted sulphuric acid o r diluted hydrochloric acid as requi red

, , .

The ferrous sulphide i s first covered with water in the apparatus ,

and the dilute aci d then added as may be necessary .

 6
3 4 I ODI NE .

I OD I N E .

I OD U M .

5 .

Commercial iodine is easily resublimed S mall quantiti es may .

be resublimed in a d ish heated in a sand bath the sublimate bein g -

collected in an inverted funnel which is placed over the contents

o f the dish .

R esublimed or purified iodine consists o f d ry br ittle shinin g , ,

purplish black crystals o f a strong characteristic odor and acrid

-

taste S oluble in alcohol

. .

Iodine imparts y ellowish brown or deep brown stains t o the

-

skin and to articles with which it com es in contact The stains and .

odor are pers istent M ortars a n d other apparatus stained w ith

.

iodine may be cleaned with potassium or sodium hydroxide a m ,

monia potassium iodide or sodium thiosulphate ; but the stains

,

on the hands and organic substances generally can not be thu s

removed .

Iodine must be kept in glass stoppered bottles -

.

Compou n d I od i n e S ol u ti on .

( L U GO L s
’
S OLU TI ON ) .

D issolve 5 Gm o f iodine an d 1 0 Gm o f potass ium iodide in 8 5

Gm o f distilled water .

Keep the solution in a glass st oppered bottle -

.

D e scri pti on —
A deep red solution of strong iodine odor
-
.

T i n c tu r e f
o I o di ne , U S P . . .

R educe 7 0 Gm o f iodine to coarse powder by tritu ration in a

mortar Trans fer it to a graduated glass stoppered bottl e o f
.
-

’
about one and one hal f l iters capacity R inse the morta r with
-
.

several success ive portions o f alcohol and pour these washings ,

into the bottle A dd enough additional alcohol to make the total

.

volume of the contents o f the bottle measure one liter S e t the .

bottle in a warm place A gitate it occasionally until the iodine

.

is dissolved .
3 66 1 RON .

This preparation contains sodium iodide ammonium

N ot e s .
,

iodide ethyl iodide sodium tetrathionate alcohol and water

, , ,
.

IR ON .

F ERRU M .

P ow d e r e d I r on .

M etallic iron prepared by filing the m etal and triturating the

filings in steel mortars The iron used for this purpose may be
.

either c ast i ron wrought iron or steel Wrought iron is however

, , .
, ,

extremely di fficult to powder and cast iron contains rather too ,

much carbon .

D e scr i pt i on a nd Te s t s .
—
A
heavy gray impalpable powder , ,
.

S ol uble in dilute h ydrochlor i c acid without residue except traces

o f carbon The gas evolved when it is dis solved in H Cl should
.

have no odor o f H 5 ( absence o f s u lphu r )

2
T he solution .

oxidized with nitric aci d and compl etely precipitated with a m

monia shoul d not yield a blu e l iquid ( absence o f c oppe r ) It .

should be free from arsenic .

“
U se s
. Powdered iron ( ferrum p u l ve rat u m is used in med i
“ ”
c 1 n e I n the same w a y as reduced iron .

R e du ce d I r on .

Prepared by reducing basic ferric hydroxide or ferric oxide

to metallic iron by means o f hydrogen at a su fficiently high heat , .

Ferric hydroxide is prepared by precipitation from a solution o f

ferric sulphate by mean s o f ammonia in the u sual w a y and the ,

thoroughl y washed precipitate is dried This dried ferric h y d rox .

ide i s introduced into an iron tube and confined to the middle o f

that tube by m eans o f asbestos plugs The tube is placed in a .

furnace and the middle portion o f it containing the ba sic ferric ,

“ ”
hydroxide i s heated to a strong but not bright red heat Then
,
.

hydrogen obtained by the action o f zinc on sulphuric acid i s

, ,

passed throu gh the tube The hydrogen gas before it is passed

.
,

through the reduction tube is dried by pas sing it through strong

,
“ ”
sulphuric acid and then thro ugh a tube eighteen inches long
'

filled with fragm ents of calcium chloride The farther end o f the .
 I RON . 6
3 7

iron tube is connected by a cork with a bent tube dipping under

water ; and when the hydrogen is observed to pas s through the
water at about the rate that it bubbl es through the sulphuric acid ,

the furnace is to be allowed t o cool down to the temperature o f

”
the atmosphere a slow current o f hydrogen being still continued
,
.

R educed iron must be kept in small dry tightly stoppered , ,

-

bottles .

R e act i on . F e 20 3 + 3 H 2
2 2F e H
+3 20

N ot e s The thoroughly dried ferric hydroxide ( it i s rendered

.

partl y basic in dr y ing and soon becomes entirely converted into

,

ferric oxide when heated ) must be in fine powder This is placed .

i n an iron tube ( such as a gun barrel or a tube constructed e X ,

pressl y for thi s operation ) H y drogen i s then passed through

.

the tube over the basic ferric hydroxi de The hydrogen must be
-
.

pure and is there fore passed through solution o f lead acetate to

remove sulphu r through copper sulphate o r s ilver n itrate solution
,

to remove arsen ic and phosphorus and through concentrated sul ,

p h u r i c acid to remove moisture be fore it enters the iron tu be ,

.

When the gas has passed over the ferric hydroxide for a m inute
so that the tube i s filled with the gas heat is appl ied at the point ,

where the ferric hydroxide is placed and the temperature is grad ,

u a l l y raised A t about 3 50 C the ferric h vd rox i d e is reduced

.
°
.

°
to ferroso ferric oxide ; at about 5 0 0 C to ferrou s oxide ; and at
-
.

°
about 7 00 C to metallic iron I t is necessary there fore that
. .
, ,

the temperature should be su fficiently high for i f the product ,

should contain much ferrous oxide it will become sel f ign iting in -

contact with ai r O n the other hand i f heated too strongly the

.
, ,

iron particles cak e together and incompl ete reduction w ill be the
result The tube and its contents should therefore be heated t o
.
, ,

“ ” “
dull red heat not to a bright red heat
—
.

The heating must be continued until the ga s a fter passing

through the tube no longer deposits moi stu re on a glass plate or ‘

other suitabl e cold obj ect held nea r the end o f the reduction tube .

The reduction is then completed and the heat i s to be withdrawn ;

but the current o f hydrogen through the tube must be continued
until the tube and contents have cooled o ff for i f the reduced ,

i ron whil e still hot comes in contact with air it might ign ite and
, , ,

become oxidized again .

 I RON A CE T AT E .

'

D e scr i pt i on . very fine grayish black lustreless odorless

—
A ,
-
, ,

and tasteless powder The A m e r i c a l Pharmacopoeia re q u ires it

.

to contain at least 8 0 per cent o f metallic iron ; the B ritish Phar

m a c op oe i a 7 5 per cent .

I R O N ( F E R R I C ) A C E T A T E S OLU TI O N .

L I QUOR F ERR I A CE T A T I S .

A n a q ueou s solution o f ferric acetate ( F e ( C H 2 3 O2) 3

_
-
233 )
containing about 3 1 p e r cent o f the anhydrous salt correspondin g ,

to about per cent of iron .

S olu tion o f ferric sulphate

Glacial acetic acid
A mmonia water
D istilled water su fficient ,
.

To the ammonia water diluted with 3 0 0 parts o f col d water add ,

constantly stirring the solution o f ferric sulphate previously

,

diluted with 1 00 0 parts of col d water Pou r t he whol e on a wet .

/

muslin strainer allow the precipitate to drain then return it to

, ,

the vessel an d mix it intimately with 60 0 parts o f cold water ;

again drain it on the strainer and repeat the washing with succes
,

sive portions o f col d water until the washings are no longer a i

f e c t e d by S odium cobaltic nitrate test solution ( showing the -

removal o f ammonia an d its salts ) Trans fer the m ixture to a wet .

muslin strainer al low the precipitate to drain compl e tely and

, ,

press it folded in the strainer until its weight is reduced to 7 0

, ,

parts or l ess by expressing the water from it N ow add the .

pressed ferric h y droxide gradually to the glacial acetic acid in a

tared j ar provi ded w ith a glass stopper stirrin gthe mixture a fter ,

each addition until each p ortion added has been near ly dissolved
before another portion is added Finally when all o f the ferric .
,

h y droxide has been added and no more o f it dissolves add enough

, ,

di still ed wate r to make the product weigh 1 0 0 parts mix well , ,

allow the mixture to become clear by S ubsidence and decant the ,

clear solution or draw it off by me ans o f a syph on

, .
37 0 I RON A CE T A T E .

representing 5 per cent of its weight of metallic iron is more easily

obtained ( see German formula b elow ) .

The solution o f acetate of iron o f the A merican

D e s cr i pt i on —

Pharmacopoeia is a dark brown red cl ear liqu id of acetous odor -

, ,

sweetish acidulous mildly st y ptic taste and slightly acid reaction

-
, ,
.

S p w about
. . at
This preparation is about 5 0 per cent stronger than that o f the
German and S wiss pharmacop oeias both o f which contain a sol u ,

tion cor responding in strength to from to 5 per cent of metal lic

iron while the A merican preparation contains about 7 5 per cent
,
.

"

o f iron
The S olution of F e r r1 c A cetate of the B ritish Pharmacopoeia
contains onl y per cent o f metall ic iron Thus 1 0 0 0 parts by .

weight o f the A merican solution equals 4 5 4 5 parts o f the B ritis h

,

solution o f th e same name .

Ge r m a n O ffici a l F or m u l a ( E d . III ) .

[ The S wiss preparation i s the sam e ]

S olution o f ferric chloride , U S P . .

A mmonia water
A cetic acid U S P , . .

D istilled water su fficient ,

.

D ilutethe solution o f ferric chloride with 1 2 5 parts o f distilled

water and the ammonia water with 5 0 0 parts A dd the iron sol u
, .

tion S lowly and during constant stirring to the dilute ammonia

solution Wash the precipitate in the usual manner with col d
.

distilled wat er L et the precipitate drain and expres s as much o f

.

the water from it as possible by means o f strong pressu re .

Put the moist mas s o f ferric h ydroxide thus obtained into a

suitabl e vessel with the acetic acid and s et the m ixture aside in a ,

cool place S haking it frequently When solution has been e f

, .
.

f e c t e d or but a S light residue remains undissolved filter the

, ,

l iqui d an d ad d enough distilled water to make the specific weight

o f the product from to

Thi s solution represents from to 5 per c ent o f Fe It .

i s therefore about two thirds the strength o f the solution o f ferric

, ,
-

acetate o f th e U S P .
 I RON A CE T A T E .
37 1

I r on A c e ta t e T i n c tur e .

TI N CT URA F ERR I A CE T A T I S

S olution o f ferric acetate 86 ml

A cetic ether 45 ml
A lcohol 7 4 ml
'

M ix the alcohol and acetic ether ; then add the s ol u t i on o f ferric

acetate S lowly an d in small quantities at a time .

N ot e s . I f the ferric acetate is ad ded all at once heat is gen ,

crated whereb y acetic acid an d acetic ether are volatil ized and
, ,

the preparation i s liable to become unclear from basic ferric ace

tate.

M ust be kept in a well stoppered bottl e in a cool dark place , .

The Tinctura Ferri A cetici A e th e r e a o f the German Phar

“ ”

m a c op oe i a i s a mixture o f 8 parts o f the s olution o f acetate o f iron

( G P ),
1 part o f alcohol and 1 part o f acetic ether I t is .

nearly identical with the A merican tincture 1 8 8 0 ) as to the per

centa g e of i ron [ the A m erican tincture c orresponding to about
and the German to about o f metall ic iron ] .

The tincture o f ferric acetate was dropped from t he A merican

Pharmacopoeia in the revision of 1 890 ; but the solution o f ferric
acetate w a s reta ined .

B as h a m
’
s M i x tu r e .

[SOLU TI ON O F I RON AND A M M ON I U M A C E T A T E ]

Tincture o f ferric chloride

D iluted acetic aci d
S olution of ammonium acetate
A romatic el ixir
Glycerin
Water su ffi cient
,
.

Pour the solution o f ammonium acetate into a suitabl e container

and add to it successivel y the d iluted acetic acid tincture o f
, , ,

ferric chloride elixi r and gl y cerin and finally enough water to

, , , , ,

make the total product measure 1 l iter .

This preparation shoul d be prepared only as wanted .

3 7 2 I RON AL B U M I NA T E .

N ot e s The solution o f ammonium acetate used shoul d not be

.

alkaline The quantity prescribed o f diluted acetic aci d is su fh

.

cient to prevent any turbidity A s the tincture o f ferr 1 e chloride

.

is added the color changes to a decidedly red because o f the forma ~

tion o f ferric acetate The preparation should be perfectly cl ear

.
.

I R O N AL B U M I N A T E .

[ Ferrated A lbumin ] .

S olution o f ferr i c oxychloride ( containing

o f Fe ) 3 0 0 parts
D ried egg albumen 7 5 parts
S olution of sodium h y droxide ( containin g
about o f N aO H ) .

D istilled water of each su fficient ,

D ilute the solution o f ferric oxychloride with parts o f

water o f th e temperature o f 5 0 C °
.

D issolv e the egg albumen in parts o f d istilled water o f

the same temperature as be fore .

Pour the solution o f egg albumen slowly and with constant

stirring into the solution o f iron .

N e u t r a l i z e the m ixture care fully an d exactly with solution o f

sodium hydroxide .

The iron albuminate which will now be completely precipitated

, ,

i s to be washed w ith distil led water until the washings give no

further reaction for chloride ( With A g N O ) Collect the p re ci p 3 .

i ta t e on a cloth strainer let it drain well squeeze out as much o f

, ,

the water contained in it as can be pressed out o f it by gentle

° °
pressure S pread it on glass plates an d dry at from 40 to 5 0 C
.
, .

D e scri pt i on . brown scales or powder odorless o f feebly

—
R ed -
, ,

ferruginous taste forming a clear solution with water containing

,

about o f sodium hydroxide in solution It contains about .

2 0 % o f Fe .

S ol u ti on of A l bu m i n a te d I r on .

[ A fter the D a nish Pharmacop oei a ]

D ri ed egg albumen 10
Ferric chloride 60
Cinnamon water 1 00
A lcohol 5 0

D istilled water su ffici ent ,

.
374 I RON AR S E NAT E .

A dd care full y enough solution o f sodium hydroxide ( of

strength ) to render the liqu id perfectly neutral .

Wash the precipitated ferrated albumin with distilled water hav

ing the temperature o f 5 0 C until the washings no longer give
°
.

any reaction for ch loride .

Collect the precipitate on a strainer an d let it drain until its

weight is reduced to 4 0 0 parts .

Trans fer the ferrated albumin to a bottle add the solution o f ,

sodium hydroxide to it and mix well , .

Then add the alcohol an d cinnamon water previousl y mixed ,

and finally enough distilled water to make the total weight o f the
produc t 1 00 0 parts .

L et it stand until any sol id particles shall have subsided and

“

then decant the cle ar l iquid or filter the product i f necessary

,
.

I R O N AR S E N AT E .

F ERR I ARSE N AS .

Ferrous sulphate
°
S odium arsenate dried at , 1 49 C
S odium bicarbonate

D issolve the sodium arsenate in 2 0 0 parts o f boil ing distilled

water and the ferrous sulphate in 2 4 0 parts of boil ing water ; add
,

the solution of the iron salt to that o f the arsenate then add the
sodium bicarbonate previously d issolved in 1 2 0 parts o f hot
water S tir well Collect the precipitate on a wetted mu sl in
. .

strainer an d wash it with water until the washings ceas e to be

a ffected by test solution o f barium chloride Press out the water .

from th e washed precipitate folded in strong l inen in a screw, ,

press and dry the product on porou s bricks in a warm a ir cham

,

ber at a temperature not exceeding 4 0 C °

.

N ot e s The reaction 1 5 analogous to that occurring in the

.

process o f preparing the precipitated ferroso ferric ph osphate -

.

Th e precipitate is ferroso ferric arsenate o f variable composition

-
,

and color .

D e scri p ti on —
A
green to greenish blue odorl es s and tastel ess -
,

powder insolubl e in water and alcohol

,
.
 I RON B EN Z OA TE .
37 5

I R O N B EN Z OA T E .

F ERR I B E N Z OA S .

To a solution o f ferric chloride add ammonia water gradually

as long as no precipitate is formed Then add a solution o f a m .

m on i u m benzoate until precipitation is completed Collect the .

precipitate wash it with a limited amount of col d water let it

, ,

drain somewhat press out the remaining water as far as p ra ct i

,

cable an d then dry the product without th e ai d of heat

, .

A n oth e r M e th od .

S odium benzoate
Ferric chloride
D istilled water su fficient ,
.

D i ssolve t h e sodium
benzoate in 2 5 parts o f distilled water an d ,

the ferric chloride in 4 0 parts o f distilled water .

Pour the solution o f ferric chloride slowly into the solution o f

sodium benzoate stirring constantly ,
.

Wash the precipitate well with distilled water l et it drain and , ,

dry it .

D e s cr i p t i The product i s a ( brownish ) fl esh colored odor

on .
— -
,
~

less an d t asteless powder S paringly solubl e in fixed oils . .

IR ON BR O M ID E .

F ERR I B RO M I DU M .

F e B r 2=2 1 6 .

Ferrou s bromide in water solution i s obtained when iron and

bromine react upon each other in water the iron being used in ,

excess The solution is bright g reen Ferrous bromide in the

. .

sol id state can not be kept nor does a water solution keep with
-
,
-

out sugar .

S yr u p of B r om i d e Of I r on .

A p
s yr u oi
f f
s sometimes
e r r ou sused which contains
br om i d e ,

1 0 per cent o f the bromide keeps well and may be prepared as , ,

follows
 I RON B ROM I D E .

I ron in the form o f wire cut into small p ieces Gm

‘

, , .
3 0
B rom in e 7 5 Gm
S ugar in coarse powder , 6 0 0 Gm
D istilled water su ffici ent ,
.

I ntroduce the iron into a flask add 2 00 ml o f distilled water , ,

and a fterward the bromine S hake the m ixture occasionally until

.
,

the reaction ceases and the sol ution has acquired a green color and
has lost the odor o f bromine Place th e sugar in a porcelain dish .

and filter the solution o f bromi de of iron into the sugar R ins e .

the flask and i ron wire with 90 ml of distilled water and pa ss the ,

washings through the filter into the sugar S tir the mixture with .

a glass rod heat it to the boiling point on a sand bath and having
,
-

, ,

filtered the syrup through paper into a tared bottle add enough ,

distilled water to ni ake the product weigh 1 0 0 0 Gm L astly .

,

S hake the bottl e which shoul d be completely filled s ecurely stop

, ,

pered an d kept in a place accessibl e to da y light

,
.

N ot e s The bromine must be added cautiously as the reaction

.
,

is sometimes viol e nt When too v 1 olent the chemical action can

.
,

be controlled by keeping the flask in cold water .

IR ON S A CCH A R A T E D CA R B O N AT E .

F ERR I C AR B ONA S S A CC H A R A T U S .

Ferrous sulphate
S odium bicarbonate
S ugar in fine powder su fficient
, ,
.

D issolve the ferrous sulphate in 2 0 0 parts o f boiling distilled

water and the sodium bicarbonate i n 5 0 0 parts o f distill ed water
,
°
o f th e temperature o f about 4 0 to 5 0 C Filter the solut ions °
.

separately Put the bicarbonate solution into a flask capable o f

.

hol ding 1 0 0 0 parts o f water ; then add the hot solution o f ferrous
sulphate agitating the m ixtu re w ell and when the e ff ervescence
, ,

has subs ided fill the flask at once with boili ng distilled water ,

cork it to exclude ai r and set it aside for two hours Then r e

,
'
.

move the m ot her l iquor by means o f a s iphon and again fill the ,

flask with boiling distilled water S hake it well l et it s ettle onc e , ,

more and repeat the washing in the same manner until the wash
,

water pr o duces but littl e turbidit y with test solution o f barium

 I RON CAR B ONA T E .

M as s o f Ca r bon a te o f I r on .

[ PI LL O F C AR B ONA T E O F I RO N . V ALLE T ’
S M AS S

Ferrous sulphate
S odium carbonate
Clarified hone y
S ugar in coars e powder ,

S yrup distilled water each su ffi cient

, , .

D issolve the sulphate o f i ron a nd the carbonate o f sodium sep

a ra t e l y each in two hundred parts o f boiling distill ed water and
, , ,

having added twenty fi ve parts o f s y rup to the solution o f the iron

—

S alt filter both solutions

,
M i x when cold in a bottle j ust large .
,

enough to hold the mixture or add enough distilled w a t e r t ofill

'

it cork the bottle well an d set it as ide that the carbonate o f iron
, ,

may settle Pour off the supernatant l iqui d and having mixed
.
, ,

syrup and distilled water in the proportion o f one part o f s y rup

to sixteen parts o f water wash the precipitate with the mixture ,

until the washings no l onger have a saline taste D rain the p r e c i p .

i t a t e on a flannel cloth and express as much o f the water as ,

possibl e L astly mix the precipitate immediately with the honey

.
,

and sugar and by means o f a water bath evaporate the m ixtu re

, ,
-
, ,

constantly stirring until reduced to one hu ndred parts ,

.

N ot e s .The reaction is given under the title S ubcarbonate of ,

I ron Compare this process w ith that for saccharated carbonate

.

o f iron The ferrous sulphate must be in crystals in no degree c i

.

fl or e s c e d S odium bicarbonate may be used here as well as in

.

the preceding preparation i nstead o f the normal carbonate ; 7 5

parts o f bicarbonate shoul d be substituted for the 1 1 0 parts o f
carbonate I f bicarbonate is used the solution o f it must be made
.

not with b oiling water but w ith water o f a temperature not ex

c e e di n g 5 0 C The use o f hot solutions r e n d e ts the precipitate
°
.

more dense which is o f material advantage in th e p reparation o f

,

saccharated ferrous carbonate and V a l l e t s m a s s where expedi ’

tious washing is necessary .

D e scri pti on . A
so ft dark grayish brown mass having a sweet
—
,
-
, ,

a fterwards ferruginous taste ,

.
 I RO N C H LOR I DE
1 .
3 79

I R O N ( F E R R I C ) CH LO R I D E .

F ERR I CH L OR I D U M ( RU B RU M ) .

F e Cl 3 + 6 H 20 2 2 70 2 . .

I ron in the form o f fine bright wire and

, , ,

cut into s mall pieces 1 5 parts

Hydrochloric acid ,

N itric acid ,

D istilled water each a suff i cient quantity

, ,
.

Put the i ron into a flask capable o f hold ing two or three hun
d red parts o f water A dd 5 4 parts o f h y drochloric acid diluted
.

with 2 5 parts o f distilled water .

L et the mixture stand in a warm place until e ff ervescence has

nearly ceased Then heat it to the boiling point and continue the
.

boiling for two or three minutes .

L et the liquid cool somewhat an d then filter it whil e still hot , ,

through paper ; an d hav i ng rinsed the flask and undissolved iron

,

with a little hot distilled water pass the rinsings also thro ugh the ,

filter .

A dd 2 8 parts o f hydrochloric acid to the filtrate ; add thi s mix

ture a l ittl e at a time to 8 parts o f n itric acid contained in a
, ,

capacious porcelain d ish gently warmed waiting a fter each addi

, ,

tion until the copious evolution o f red n itrous vapors subsides

be fore a dding more When all o f the iron sol ution has been
.

added to the nitric acid and active e ffervescence has ceased heat
, ,

the dish an d contents by means o f a sand bath until the l iqui d is -

free from nitrous odor .

Then test a few drops of the l iquid d iluted with water with , ,

freshly p repared potassium ferric y ani de test solution S houl d

- -
.

thi s reagent produce a blue precipitate or a bl ue color add a littl e ,

more nitric aci d drop by d rop to the hot solution o f ferric chlorid e
, ,

in the porcelain dish as long as any further evolution o f red

,

vapors i s observed Th e solution i s then tested as be fore and

.
,

when the test solution o f potas sium ferric y anide no longer pro
-

duces a decidedly blue color showing that only a trace o f ferrous

,

chloride remains in the l iqu id no more nitric acid must be added ,

.

[ S houl d an excess o f nitric acid be found to have been added ,

the exces s mu st be expell ed by heating the l iqu id until all odor

o f nitric aci d has cease d ]
3 8 0 I RON C H LOR I DE .

Then add 5 parts o f hydrochloric aci d and enough distilled

water to make the whole weigh 6 0 parts .

S e t the dish aside covered with glass in a cool place until a

, , ,

solid cry stalline mass is formed of the contents .

R emove the crystalline mas s break it into pieces and keep the , ,

product in glass stoppered bottles protected from light

—
, .

R e a ct i ons . First ,
2F e +4 H Cl z z F e C12 + 2H then ,
6 F e C12 + _

6 H C1+ 2 H N n 3 F e 2 C16 +4
H zO +
2N O .

N ot e s .
The iron is readily di ssolved by the h yd roc h l or 1c a c 1 d
- ,

especially in the beginning ; as the solution becomes charged with

ferrous chloride however the action is slower and it is a d van
, ,

t a g e ou s to promote it by the ai d o f heat In order that the density .

o f the solution o f ferrous chloride may not be so great as to retard

the chemical acti on, the Ph a rm a c O p oe 1a directs that the h y dro
chloric acid be diluted before the iron is added The evoluti on o f .

h y drogen may cease be fore all the H Cl is decomposed by the iron

at the ordinary temperature but when th e l iqu id i s brought to ,
_

the boiling point the acid is completely satu rated .

A s the amount o f hydrochloric aci d saturated with iron to form

ferrou s chloride determines the strength of th e finished solution [

'

and th e amounts o f hydrochloric and n itric acids required to

raise that ferrou s chlorid e to ferric chloride it is important that ,

the whol e quantity o f hydrochloric aci d first used be compl etely

saturat ed .

S ome f erric chloride is formed be fore th e acid is satu rated ,

especially i f the iron was rusty ; but a fter boiling the liquid with
the excess of iron present the solution contains ferrous salt only .

The solution o f ferrous chloride is then to be treated with

hydrochloric an d n itric acids to convert it into ferric salt When .

the solution is concentrated this may be accompl ished at l ittl e

above ordinar y room temperature When the solution is dilute .
,

on the other hand a temperature near the boiling point is required

,

to complete the reaction A good rul e is to evaporate the solution

.

of ferrous chlori de until it has about sp w and a fter adding . .

,

the a d d i t i on a l q u a n t i ty o f h y drochloric aci d prescribed t o add

‘
,

this solution slowly a littl e at a time to the nitric acid I f all o f

, ,
.

th e solution o f ferrou s chloride i s added at once the reaction is ,

too violent the red fumes being evolved so copi ously and suddenly
,
3 8 2 I RON C H LOR I DE .

the vessel this di fficulty may b e avoided by gentle warmin g

, ,

whereby the cake i s loosened .

The product ought to be dried over sulphuric acid or ove r

quick lime
-
.

The ferric chloride is used chiefly for p reparin g aqueou s and

alcohol ic solutions .

D e s cri pt i on .
—
O range yellow crystalline mas ses or pieces , ,
h av
ing a faint odor o f hydrochloric aci d ( sometimes odorless when
quite a strongly styptic taste D el iquescent i n moist .

air Freely solubl e in water and in alcohol

. .

F e rr a t e d A m m oni u m Ch l or i d e .

[ F LORE S M AR TI S ] .

Ferric chloride
A mmonium chloride
D iluted hydrochloric aci d
D istilled water .

D iss olvefilter and evaporate the filtrate over a water bath

, ,
-
,

during constant stirring to drynes s ,

.

Put the dry product at once in a glass stoppered bottl e and

keep it protected from l ight .

A n orange y ellow deliquescent powder which is not a chemi

, ,

cal compound but a m echanical mixture o f the two chlorides .

It contains about 2 per cent o f F e .

N ot e s The S wiss Pharmacopoeia orders 7 7 parts o f solution o f

.

ferric chlori de ( U S P ) to 6 0 0 parts o f ammonium chloride

. . .
,

with 3 3 0 parts o f water and without any hydrochloric aci d ; this

,

solution to be evaporated to dr y ness .

The German Pharmacopoeia orders about 7 parts o f solutio n of

ferric chloride ( U S P ) and 3 2 parts o f H N Cl
. . .
4 .

I r on
( F e rri c
) Ch l or i de S ol u ti on .

L I QUOR F ERR I C H L OR I D I ; U . 8 .

A n aqueous solution o f ferric chloride containing ,

per
cent o f the anhydrous salt [ F e Cl corresponding to 3
z

per cent o f the cr y stall ized chloride or

to about 1 3 per cent o f metallic iron and containing also some ,
 I RON C H LOR I DE . 8
3 3

free hydrochloric aci d [ about per cent o f H Cl equivalent to ,

5 per cent o f the o fficial hydrochloric acid ] .

The o fficial solution o f ferric chloride is prepared fr om iron ,

hydrochloric acid nitri c acid an d water a s described under the

, ,

titl e o f I ron Chloride The quantities o f th e materials required

.

to make one hundred parts o f the finished solution are

I ron in th e for m o f fin e bright w ire cut

, ,

into small pieces

Hyd rochloric acid
N itric acid .

D istilled water each su ffi cient

, , .

The i ron i s put into a flask capabl e o f hol ding at least twic e the
volume o f the finished product t o be made ; 5 4 parts o f hydro
c hl or 1c a c 1 d and 2 5 parts o f distilled water are added ; the com

p l e t e saturation o f the acid is insured by the ai d o f heat an d the ,

ferrous chlorid e i s converted into ferric chloride by mean s o f 2 8

parts o f hydrochloric acid and 8 parts o f n itric acid precisely as ,

described under the titl e o f ferric chloride The solution is .

tested an d when it no longer contains any ferrou s salt ( or when it

,

contains o nly traces o f ferrous chloride ) and the excess o f nitric ,

acid has be en d issipated by heat s o that no nitrous o dor is r e

t a i n e d by the liquid the last 5 parts o f hydrochlori c aci d i s added
,

together with enough di stilled water to make the whole weigh

1 0 0 parts ( instead o f only 6 0 pa rt s as prescribed in the formula

for making solid cr y stall in e ferric chloride ) .

N ot e s The reactions and the several steps o f the process are

.
, ,

explained under t h e titl e Ferric Chloride , .

A solution o f ferric chloride cannot be permanent without the

presence o f free h ydrochloric acid In th e absence o f a su fficient .

quantity o f H Cl a basic ferric chloride is formed which p r e c i p i

, ,

tates To redissolve this yel low basic salt requires more hydro
.

chloric acid than it takes to prevent its formation Continued .

heating results in th e l oss o f H Cl an d the formation o f yellow

oxychloride ; i f however su ffi cient H Cl i s present no precipitate
, , ,

is form ed but the solution upon being heated becomes darker in

,

color a ferric chloride w ith 5 molecules o f water being formed

,
.

A fter standing some time however the darkened sol ution resumes
, ,

i ts original color and then contain s the chloride with 1 2 mol e

,

cul es o f water Weak solutions are more readily altered and

.
,
 8
3 4 I RON C H LOR I DE .

when darkened by heating do not resume a l ighter color on stand

in g .

The solution o f ferric chloride often contains l ess iron than

the pharmacopoeial standard o f strength r equires This may be .

the result o f the employment o f h y d roc hl or 1 c a c 1 d not of the full

o fficial stren gt h or o f the inco mplete Saturation o f the aci d with
,

iron .

The preparation i s frequently foun d to be contaminated w ith

nitric acid or to contain some ferrous chloride ; it can not con
,

tain both ferrous salt and free nitric aci d except for a ver y brie f
period during the process o f preparation and then only traces o f
,

each The p resence o f a tr a ce o f ferrous chloride can not be

.

considered as a very serious de fect for the solution is used

,

almost exclus ively for the purpose o f preparing the tinctu re o f

chloride o f iron which unavoidably contains a large amount o f
f e r r ou s s a l t formed by the reducing action o f the alcohol upon
'

the ferric chlori de .

But the presence of free nitric acid i s more obj ectionabl e .

Hence it is better to u se a trifle less nitric aci d than is n e c e s s a r y t o o

completely remove all traces o f ferrous salt than to use a trifle too
,

much so as to leave an excess o f that acid becaus e the ex p ulsion

,

o f the excess o f n itric acid by heating t he l iqu id i s almost 1m p os

sibl e without the great risk o f caus ing the formation o f basic
f e rric chlo ride by oxidation a corresponding amount of hydro
,

chloric acid ( formed from the decomposing f e r r1 c chloride ) being

evolved fro m the hot li quid .

S unl ight sl owl y decomposes ferric chl oride ( soli d as well as in

solution ) into ferrou s chloride and chlorine In the presence .

o f organic substances such as alcohol and other reducing agents

, ,

t h i s r e d u c t i on i s much more rapid .

S olution o f ferric chloride may al so be prepared by dissolving

ferric hydroxide in h y drochloric acid ; but a strong solution can
not be made in that way because undiluted h y drochloric aci d is
o f only 3 2 per cent stren gth and recentl y precipitated ferric h v
d r ox i d e contains much water wh i ch woul d further dilute the solu
tion thus formed I f the o fficial h y drochloric acid be us ed and a
.
,

ferric h y droxi de fr e e fr om w a te r w ere employed to form th e solu

tion o f ferric chloride according t o the equation
3 8 6 I RON C H LOR I DE .

oe i a has the w and ml of it contains

co
p ( 1 8 98 )
s p 1 0 0 . .

gram s o f iron ; in other words 1 4 2 grams o f the solution Contains ,

2 2 5 grams o f iron which corresponds to

.
, per cent of metal
“
lic iron Thus 8 2 0 gram s o f the B ritish strong S olution o f fer
.

ric chloride exactly equals 1 00 0 grams o f the A merican solu “

”
tion o f ferric chloride B ut the B ritish Pharmacopoeia al so con
.

“ ”
tains a weaker preparation called solution o f ferric chloride
( the E nglish titl e being i dentical with that o f the A merican prep
aration ) which is made by mixing 1 volume o f the strong
,

solutio n o f ferric chloride with 3 volumes of d istilled water and ,

therefore contains an amount o f ferric chloride corresponding

,

to pe r cent o f metall ic iron Thus 2 55 2 grams o f the British .

solution o f ferric chloride equals grams o f the A merican

sol ution of ferric chloride .

The B ritish s tr ong s ol u ti on of f e rr i c c hl or i d e contains about

“

4 6 per cent o f anhydrou s ferric chloride corresponding to ,

“
per cent o f crystallized ferric chloride The B ritish solution .

”
o f ferric chloride contains about per cent o f anh y drou s
ferric chloride corresponding to about ,
per cent o f the crys
t a ll i z e d salt
The solution o f ferric chlori de o f the Ph a r m a c opoe i a of th e
N e th e r l a n d s i s prepared by dissolving 3 parts o f ferric chlorid e
in 1 part of water It is described as containin g . to per
cent o f Fe and having th e s p w
,
to . .

The soluti on o f ferric chlori de o f the A merica n

D e scr i p t i on .
—

Pharmacopoeia is a reddish brown liquid having but a faint odor -

( an d that the odor o f h y drochloric acid onl y) It has a strongly .

styptic ferruginous taste and an aci d reaction S p w . . .

°
at 1 5

M e th od a f te r th e S w i s s P h ar m a c opoe i a

I ron fine bright wire cut in small

,
In , ,

pieces
Hydrochloric acid 3 2 % o f H Cl )
D istilled water su fficient , .

Put the i ro n and hydrochloric acid in a su itable vessel o f glass

or porcelain in a warm place When e ff ervescence has ceased
'
.

heat the liquid at the b oiling point for a few minutes Filter the .

solution .
 I RON C H LOR I DE . 8
3 7

Conduct a current of washed chlorine into the solution until

the l iquid no longer produces a blue precipitate with test solution -

o f potassium ferricyanide
-
.

Then evaporate the solution until reduced to five times the

weight o f the iron dissolved cover it and set it aside in a cool ,

place to crystallize D ry the crystall ine mass over sulphuric

.

aci d ( or over lime ) and dissolve the ferric chloride thus dried
, , ,
'

in an e q u a l w e i g h t o f distilled water .

Thi s solution contains about 5 0 per cent o f crystallized ferric

chlori de corresponding to about 1 0 per cent o f metallic iron .

N ot e s . T o ascerta in the amount o f iron d issolved in the hy

acid the undissolved portion o f the metal must be col
d r oc h l o r i c ,

l e c t e d and weighed an d its weight deducted from the quantity

originally put into the acid .

The solut i on o f ferrous chloride may i f most convenient be , ,

put into a series o f Woul ff bottl es connected with each other and
with the wash bottle through which the chlorine gas i s pas sed
-

from the generator O nly the solution in the last Woul ff bottle
.

need be tested w ith the solution o f potass ium ferricyanide -

.

I t is well also to c onnect the last Woul ff bottl e with another

, ,

bottl e containin g sodium carbonate solution in order to fix th e

excess o f chlorine passing beyond the last Woul ff bottle so as
to preven t its escape into the room .

The Pharmacopoeia o f the N etherlands al so directs the us e , ,

“ ”
o f chlorine to oxidize the ferrous chloride to ferric .

It will be seen that by thi s process we first make crystall ized

ferric chloride and t h e n m a k e the solution out o f that finished
,
‘

chlori de It would therefore be as well to d ivide the working

.
, ,

formula accordingl y into t w o giving one formula for the prep —

aration o f the dried cr y stall ized ferric chloride and a separate ,

one for the preparation o f the solution .

I r on ( F e rr i c
) Ch l or i d e T i n c tu r e .

TI N CT URA F ERR I CH L OR I D I .

The o fficial tincture o f chloride o f iron is a h y droalcoholic s o

l u t i on o f ferric chloride c on t a m m g about
”
per c ent o f the anhydrous salt corresponding to per cent ,
3 8 8 I RON C H LOR I DE .

o f crystalline ferric chloride ( F or to abou t

per cent o f metallic iron .

[ It shoul d be understood however that the o fficial preparation

, ,

contains not only ferric chloride alcohol and water but also a ,
‘

large proportion o f ferrou s compound together with aldehyd e

and chlorinated ethereal compounds formed by reaction betwee n
the alcohol and the ferric chlorid e ]
I t is prepared as follows :
S olution o f ferric chloride 2 50 volumes
A lcohol su fficient to make
,
the prod
u c t 1 00 0 volumes .

M ixthe l i q u i d s a n d let the mixture stand in a closely c ov

, . ,

ered vessel at least three months ; then t rans fer it to glas s stop
,
-

”
pered bottl es and keep it protected from l ight
,
.

N ot e s We are in formed that the obj ect o f l etting the mixture

.

“
o f alcohol and solution o f ferric chloride stand for at least thre e
” “
months is the formation o f certain chlorinated ether com
po und s
S everal writers attribute the formation o f the ethereal com
pounds to the reaction of the free hydrochloric acid ( contained i n
the solution o f the ferric chloride ) upon the alcohol ; but this can
not be true because a l iquid containin g only per cent o f H Cl
does not react upon alcohol at all .

The ethereal products are formed by reaction between the ferric

chloride and the alcohol and the principal reactions are probably
,

the following :

F e C13 + 3 C2H 5 O H Z Fe ( OH ) 3
—
C H
3 2 5 Cl , and

The ferric h y droxide formed by the reaction first stated is not

at once precipitated It remain s dissolved in th e liqu id forming
.

a solubl e compound with the undecomposed portion o f the ferric

“ ”
chl ori de B ut a ba sic ferric chloride or oxychloride o f iron
.
-

'
is finally th rown down .

That aldehyde and ethyl chloride are both contain ed in a tinc

ture o f ferric chloride may be at on ce di scovered even by the
sense o f smell .
390 I RON C H LOR I DE .

aldehyde and ethereal compounds . I t ha s a st y ptic ferruginous

°
taste and an acid reaction S p w . . . at 1 5

T i n c tu r e: P e r r i Ch l or a ti A e th e r e d

o f the German Pharmacopoeia i s prepared as follows

S olut i on o f ferric chloride ( G P ) . . I part

E ther I part
A lcohol 7 parts

M ix the liquids put the m ixture in a bottle of white glas s

,

and set it in full sunl ight until whol ly decolorized Then put the .

bottle in a shaded place and remove the stopper occas ionally to

,

admit ai r until the liqui d acquires a yellow color

,
.

N ot e s . L ight causes reaction between the ferric chloride and

alcohol resulting in the formation o f ferrous chlori de aldehyde
, ,

and hydrochloric acid and also ethyl chloride and water When
,
.

the liqu id is now put in a shaded place and the stopper o f the
bottl e removed from time to time the ferrou s chloride is oxidized ,

by the ai r and some bas ic ferric chloride i s formed which colors

the solution yellow A part o f t h e aldehyde i s at the same time
.

Oxidized to acetic acid perhaps partly by the aid o f s ome free

,

chlorine formed while the l iquid w a s exposed t o light .

The fini shed ethereal tincture o f chloride o f i ron therefore , ,

contains alcohol ferric chloride ferrous chloride ethyl chlori de

, , , ,

aldehyde acetic acid and bas ic ferric chloride

, ,
.

IR ON ( F E R R OU S ) CH LO R I D E .

F ERR I C H L OR I D U M I R I DE )
(V .

F e Cl 2 4 H 20
.
2 1 98 . 8 .

I ron wire I part

H y drochloric acid 4 parts
D istilled water 2 parts

D is solve the iron in the aci d and water previously mixed ; ,

when e ff ervescence has ceased h eat to boiling L et settl e de , .

,

cant wash the un dissolved iron with a l ittle water add ing the
, ,

washings to th e decanted l iquor filter while hot and crystallize , , .

 I RO N CIT RA T E .
39 1

R emove the crystal s from the mother liquor drain them in a ,

funnel and put them at once in a bottle

,
.

R e ac ti on . F e 2 + 4 H Cl z z F e Cl 2 + 2H 2
.

D e s cr i p t i on .
—
L arge blu ish green transparent crystal s
,
-
, . O dor
l ess Taste astringent ferruginous R eadily soluble in water and
.
,
.

in gl y cerin .

O xidizes on exposure to ai r an d can not be e ffectively pro ,

t e c t e d against oxidation except by submerg i ng the cr y stals in

some liquid in which the chloride is insoluble .

I R O N ( F E R R I C ) CI T R A T E .

F ERR I CIT RA S .

E vaporate any convenient quantity o f the solution o f ferric '

citrate over a water bath at a temperature not exceeding 60 C

-
°
.

to the consistence O f syrup and spread it on glas s plates to dry ,

in scal es .

Keep it in well stoppered bottles in a cool dark place ,

.

D e s cri p t i on Thin transparent garnet red scales odorles s o f

—
, ,
-
, ,

slightly ferruginous and only slightly acidulous taste Freely .

soluble in water ; quickly in hot water Insolubl e in alcohol I t . .

gradually loses its ready sol ubility in water an d more rapidly ,

when exposed to l ight The percentage o f iron is from 1 9 to .

but it varies ; and the percentage o f moisture retained by

the scales is al so variabl e The preparation nearly corresponds
to F e C6 H O 7 3 H O but m
.

s a y contain less iron and more water

.
2 ,

than that formula indicates I t i s therefore not a definite chem i .

, ,

cal compound .

Ge r r ncm O ffi ci a l M e th od .

o f ferric chloride U
S olution , . S . P
A mmonia water
Citric acid
D istilled water su ffi cient , .

D ilute the solution o f ferric chloride with 1 0 0 parts o f dis

tilled water and the ammonia water with 7 5 parts o f distill ed
,

water Pou r the iron solution slowly and du ring uninterrupted

.
39 2 I RON CIT RA T E .

stirring into the dilute ammon i a solution Wash the precipitate .

well with cold dis tilled water in the usual way .

_

D issolve the citric acid in 3 5 parts o f distilled water A dd the .

ferric hydroxide to the citric aci d solution in a porcelain d ish ,

a n d heat the mixture at not over 5 0 C stirring frequently until

°
.
, ,

the solution is saturated or the ferric hydroxide nearly all dis

solved .

°
Filter the solution evaporate i t at not over 50 C to the con
,
.

sistence of syrup and scale the product in the usual way ( see
,

other formulas for scale salts ) .

A mm oh i o F -
e rri c Ci tr a te .

S ol ution
o f ferric citrate
A mmonia water
M ix and evaporate the mixtu re over a water ba th at not over —

6 0 C to the consistence o f thick syrup ; spread this on glass

°
.

plates and let it dry in scales .

Keep the product in a well stoppered bottl e in a cool dark place , , .

N ot e s For making thi s preparation some formulas prescribe

.

that three parts o f citric acid dissolved i n water be saturated

with ferric hydroxide as described in the notes under S olution o f
Ferric Citrate and that one part o f citric acid saturated with
, ,

ammonia be a fterwards added an d the solution evap orated to

, ,

form scales .

I n the O fficial for mula o f A merica the proportions p rescribed

o f the material s are : 1 00 volumes o f solution o f ferric citrate
and 4 0 volumes o f ammonia water which proportions correspond ,

to 3 parts and I part by weight .

D e scr i p t i on
Thin transparent garnet red scales ; odorless ;
.
—
, ,
-

taste sl ightly saline and faintly ferruginous Completely and .

quickly solubl e in water Insol uble in alcohol . .

A n ot h e r M e th od .

[ A fter the S wiss Pharmacopoei a ]

S olution of ferric chloride U S P , . .

Citric aci d
A mmonia water .

D istilled water o f each su ffi cient, .

3 94 I RON CIT RA T E .

parts o f solution o f ferric sulphate m ay be pressed until the press

cake weighs l ess than 6 5 part s ]
Put the citric acid in a porcelain dish and add to it about one
hal f its weight ( 1 5 parts ) o f distilled water Place the dish .

over a water bath and keep its contents at a temperatur e not

-

exceeding A dd the press cake of ferric hydroxide in small ,

portions at a time stirring well and allowing each portion to

, ,

dis solve before adding another When about three fourths o f .

the ferric hydroxide has been added raise the temperature o f the ,

contents of the dish to an d when all o f the ferric hydroxide

has been added let the temperature be increased to and con
t i n u e h eating and stirring for about fi fteen m inutes taking care ,

not to allow the temperature to ris e above Filter the solu

tion and evaporate it at a temperature not e xceeding OO until it O

weighs 1 0 0 parts .

Keep the product in well closed bottles in a cool place and pro
t e c t e d from light .

R e act i on s .

Fe ( S O 4 ) 3 l
—
H 4N ) 5 0 4 ; then
2

Fe O H ) 3 4 — H 3 C6 H 5 O 7 : F e C6 H 5 O 7 — l 3 H zO -
.

N ot e s . The pharmacop oeial directions do not require that the

water shoul d be squeezed out O f the magm a o f ferric hydroxide ,

nor that the hydroxide shall be added gradually to the citric aci d
mixed with a littl e water The Pharmacopoeia instead directs that
.

the drained magma be at once m ixed with the citric aci d and
the mixture heated at 6 0 until the precipitate ( the hydroxide )
°

i s dissolved It is better however to proceed as here described

.
, , ,

adding gradual ly the ferric h y droxide deprived o f as much water ,

as can be pressed out o f it and raising the temperature to 6 0 only

,
°

at the end By proceed ing in this manner the saturation of the

.

citric acid will be e ffected without exposing the ferric hydroxide

or the solution o f ferric citrate to that high temperature any longer
than is unavoi dable and the concentration o f the sol ution to the
,

required standar d requ ires but l ittle evaporation .

Ferric hydroxide is easily decomposed and rendered insolubl e ,

or d i ffi c u l t ly solubl e by heat But a higher heat than the tempera

,
.
~

ture o f the room is necessar y to e ffect the solution o f the ferric

 I RON CIT RA T E .
395

hydroxide in the citric acid solution and especiall y so when sat

,

u ra t i on is approached .

I f I ml o f ammonia water o f ten per cent ( H 3 N ) strength be

added to the citric acid and water be fore the ferric h ydroxide is
added the solution o f the latter is greatly hastened an d thi s small
,

quantity o f ammonia shoul d not be obj ected to amounting to only ,

1 Gm o f H 3 N in each l iter o f finished product .

A small a m ou ht o f the ferric hydroxide remains undissolved ,

and is filtered away before the solution is evapo rated to 1 0 0 Gm .

This undissolved hydroxi de is usually ba sic owin g to the expos

u re o f the normal hydroxide to heat .

E xam inations mad e o f many samples o f solution o f ferric cit

rate and o f the ferric citrate in scal es show that the percentage
o f I ron i n these preparations i s quite variabl e This is due to .

the varying degree o f care observed in their manu facture and ,

especial ly to the conversion o f a greater or les s portion o f the

ferric hydroxide into insolubl e meta hydroxide It i s intended
-
.

that the citric acid shall be saturated with ferric hydrox ide but .

the fact that a portion o f the hydroxide remains undissolved at

the en d doe s not indicate saturation i f the undissolved portio n
cons ists o f bas ic ferric hydroxide for that is insoluble Hence i t .

i s necessary in order to obtain as nearly uni form results as pra e

t i ca bl e to a dopt all the precautions described in the working d i
,

rections given in the foregoing formula .

The Pharmacopoeia states that the solution is o f a strength

corresponding to about 7 5 per cent o f metall ic iron Thi s is a
. .

minimum o f i ron When well made the solution must contain

.

about per cent o f normal ferric citrate that being the pro
,

portion o f ferric citrate formed by the quantity o f citric acid em

ployed A ssum ing that the citric acid i s all neutral ized so as to
.

form normal ferric citrate the finished preparation contains about

,

8 per cent o f i ron . O ne hundred grams o f the solution shoul d ,

upon evaporation yiel d about

,
per cent o f scaled ferric cit
rate ; bu t the yiel d depends in part upon how far the solution i s
evaporated be fore it is put on the glass plates to be dried an d the ,

temperature at which the scal ing is e ffected or in other words , , ,

the amount o f moisture retained by the scaled salt I f the scal ed .

salt correspond to F e C6 H O 7 3 H O the y ield from 1 0 0 Gm o f

5
.
2 ,

solution can not be over Gm .

39 6 I RON C IT RAT E .

The solution o f ferric citrate o f t h e A merican

D e scri pt i on .
—

Pharmacopoe ia is dark brown an d has a sl igh tly

ferruginous and only faintly aci d taste I ts reaction on test paper .
-

is acid The s p w is not less than

. at . .

I R O N CI T R A T E WI TH Q U I N I N E .

F ERR I E T QU I N I N AE C IT RA S ; U . s .

Ferric citrate 22 parts

Q uinine dried at ,
1 00
°
C until it ceases
.

to l ose weight 3 parts

D issolve the ferric citrate in 3 0 parts o f distilled water in a '

porcelain dish over a w ater bath at not over 6 0 C A dd the -

°
.

alkaloid and stir constantl y until dis solved E vaporate at the .

temperature named until the liqui d i s reduced to the consistence

o f syrup and spread it on glass plates to dry in scales
, .

Keep the product in well stoppered bottl es in a cool dark , ,

place .

N ot e s This th e O fficial citrate o f iron and qu inine o f the

.
,

U nited S tates i s reddish brown and only sl owly though per

, ,

f e c tl y water soluble
, The most commonly employed citrate o f
.

iron and quinin e however is that prepared with the ad dition Of

, ,

ammonia by which the preparation is not only rendered more

,

rea dily sol ubl e but changed also in color being greenish yellow ,
.

The quinine shoul d be finely divided and ought to be tritur ,

ated first with five parts o f water and then with a portion o f cold
solution o f the citrate o f iron being a fterwards well m ixed with ,

the whol e be fore the digestion begins O therwise it may run .

together in lumps wh ich a fterwards are very di fficult to dis

, , ,

solve .

I n this as in all other scale salts o f iron it is necessary that no

, ,

considerabl e excess of free citric aci d shoul d be contained in the

preparation for then the salt will not form scales but adheres
, ,

like a varnis h to the glas s plates .

“
Q uinine dried at 1 0 0 C until it ceas es t o lose weight is0
.
, ,

monoh y drated quinine ( C H N O I I O ) T he dryin g at this

QO M z z z .

temperatu re i s directed for the pur p os e o f insurin g uni formity .

 I RON C IT RA T E .

o f water Wash the ferric h y droxide thoroughly and press out

.
,

the mo isture from it D issolve the citric acid in 2 5 parts o f dis

.

tilled water warm the solution over a water bath at not abov e
,
-

40
0
C ( 1 04
. an d add during constant stirrin g the ferric
°

, ,

hydroxide in small portions at a time until th e citric acid is sat

u r at e d .Then add the quinine in the manner prescribed in th e
“
working formula for the preparation o f the I ron and Q uinine
Citrate o f the A merican Pharmacopoeia .

D es cr i pt i on .
—
S imilar to th e preparation o f the A merican Phar
m a cop oe i a .

It contains about 1 4 pe r cent o f quinine .

The N orwegian and D ani sh Pharmacopoe ias require from 10

to 1 2 per cent o f qu inine .

S ol u bl e Ci tr a te o f I r on a n d Q u i ni n e .

F ERR I E T QU I N I N AE C IT RA S S OL U B I L I S ; U . S .

Ferric citrate
Q uinine dried at 1 0 0 C to a constant
,
°
.

weight
Citric acid
A mmonia water .

D istilled wat er each su fficient , .

Heat 1 6 0 ml o f distilled water in a porcelain dish over a water

bath to a temperature not exceeding 6 0 C and add th e ferric °
.
,

c i trate ,
stirring until the scal e salt is d issol ved Triturate the -
.

quinine and the citric aci d w ith 2 0 ml o f distilled water add this ,

to the sol ution o f ferric citrate in the porcelain dish and stir con ,

s t a n t l y until al l i s d issolved N ow add gradually and with con .

stant stirring about 5 0 ml O f ammonia water or a su fficient quan ,

tity to render the solution greeni sh yellow waiting a fter each -

,

addition O f ammonia until the precipitated quin ine shall have r e

dissolved before another portion O f the ammonia water i s added .

E vaporate the greenish yellow solution over a water bath at a -

,

temperature not exceeding 6 0 C to a s y rupy consistence and °

.

spread it on plates o f glass o r porcelain to dry in scales .

Keep the product in well stoppered bottles protected from

‘ -

light .

D e scri pt i on —
Thin transparent scales o f a greenish golden
,
 I RON C IT RA T E .
3 99

yellow c olor ; Odorless ; taste bitter mildly ferruginous Com , .

p l e t e l y and quickly soluble in water O nly partially solubl e in .

alcohol D arkens on exposure to light Hygroscop ic in damp

. .

air.

It contains 1 2 per cent o f monohydrated quinine .

B r i ti s h P re pa r a ti on .

S olution o f normal ferric sulphate U S 3 2 8 ml ,

. .

S ulphate o f quin ine 4 0 Gm

.

D iluted sulphuric acid 6 0 ml

Citric acid 1 2 3 Gm
A mmonia water distilled water each su fficient
, , .

M ix 3 20 ml o f ammonia water w ith 1 6 0 0 ml o f cold water ; add

to this the solution O f ferric sulphate also previously diluted with ,

1 6 0 0 ml o f co d water stirring constantly and briskly

l , L et the .

mixture stand for two hou rs stirring it occasionally ; th en trans

,

fer it to a wetted musl in strainer and when thoroughly drained , ,

wash the hydroxide w ith water until the washings ceas e to give a
precipitate with barium chloride .

M i x the quin ine sulphate with 3 2 0 ml o f water add the di ,

luted s ulphuric acid and when th e salt i s dissolved precipitate

, , ,

the quinine with a slight exces s o f ammonia water Collect the .

pre cipitate on a filter and wash it with 1 0 0 0 ml o f distilled water

,
.

D issolve the citric acid in 1 2 5 ml o f distilled water heated on ,

a water bath add the ferric h y droxide previously well d rained ;

-
,

sti r them together and when the hydroxide has dissolved add the
, , ,

precipitated quinine continuing the stirring until the alkaloi d

,

has also d is solved L et the m ixtu re cool A d d cautiously a

. .
,

littl e at a time 6 0 ml o f ammonia water previ ou sly diluted with

,

80 ml o f distilled water stirring bri skly and allowing the quinine

, ,

which separates with each addition o f ammonia to re dissolve be -

fore adding another portion Filter the solution evaporate i t to

.
,

the con sistence o f a thin s y rup and spread it on glass plates to ,

°
dry in scal es at not over 4 0 C .

N ot e s The product is in greenish gol den yellow scales some

.
,

what hygroscopic and read ily sol ubl e in water It contains abou t
,
.

1 6 per cent o f quinin e .

40 0 I RON C IT RAT E .

S ol u ti on o f Ci tr a te of I r on a n d Q u i n ine .

A mmonio ferric citrate -

Q uinine dried at ,
1 00
°
C until it ceases
.

to lose weight
Citric acid
A lcohol
D issolve the citrate o f iron and ammonium in 2 0 0 parts of
distilled water in a tared porcelain dish ; heat the solution over
,

a wate r bath to 6 0 C add the citric aci d and when this has
—
o
.
, , ,

dissolved add the alkaloid previously triturated to a homogene

,

ous m i xture with a cool ed portion o f the liquid and continu e ,

stirring unti l a perfect solution results E vaporate to 1 60 par t s .

,

let cool add the al cohol and finally 1 0 parts o f distill ed water
, ,
.

S hould be kept in a wel l stoppered bottle in a cool dark place , ,

.

D e scrl p t i on .
—
A
dark greenish yellow to yellowish brown - -

l iquid O dorless Taste l ike that o f citrate o f iron and qu inine

. . .

R eaction slightly acid Corresponds to about 50 per cent Of .

soluble citrate of iron and quinine .

IR ON CI T R A T E WI TH S T R Y CH N I N E .

F ERR I E T S T R Y CH N I N A E C IT RA S .

Citrate o f iron and ammonium

S tr y chnine
Citric a c i d

D issolve the ammonio ferric citrate in 1 00 parts o f d istilled -

water ; and the alkaloi d together with the citric acid in 2 0 p arts , ,

o f distill ed water M i x E vaporate the mixture by water bath

. .
-

°
at not over 6 0 C to a syrupy l iquid an d spread this on glass
.
,

plates to dry in scales .

'

Keep the product in well stoppered bottles in a cool dark , ,

place .

D e scri pt i on
Transparent garn e t red scales del iquescent on
—
,
-
,

exposure to air Odorles s having a bitter and sl ightly ferruginous

, ,

taste and a sl ightly aci d reaction R e adily and wholly soluble i n

, .

water .
4 0 2 I RON N IT RAT E .

than twice as much iron it uses only 3 3 per cent more nitric acid .

H ence t h e B r i t i s h preparation contains both ferrous and ferric

n itrate while the A merican preparation contains only ferric n i
,

trate .

Th e B ri ti s h F or m u l a ( 1 8 98 )
18 as follows
I ron
N itric acid ( 7 0 % o f H N O 3 ) , 90 ml or ,
.

D istilled water .

the n itric acid w ith 3 20 ml o f distilled water D issolve

D ilute .

the iron in the m ixture being careful to moderate the reaction

, ,

should it become too V iolent by the addition of a l ittl e more dis

,
'
till ed water F i l t e r A dd enough d istilled water to produce 6 0 0
. .

ml o f the solution ( or Gm ) .

This solution has the s p W . .

IR ON OX Y CH LO R I D E S OLU TI O N .

L I QUOR F ERR I O X Y C H L OR I D I .

The followin g process i s a fter the S wiss Pharmacopoeia ( 1 89 3 )

S olution o f ferric chloride U S , .

A mmonia water
H y drochloric aci d
D istilled water su fficient
,
.

Warm the solution of ferric chloride to about 3 0 C D ilut e °

.

3 0 0 parts o f ammonia water with 3 0 0 parts of water A d d the .

ammoniacal l iquid slowly and with constant stirring to the solu

tion o f ferric chloride Then dilute the mixture with 1 00 0 parts
.

o f distilled water .

D ilute 1 00 parts o f ammonia water w ith 2 0 0 0 parts o f distilled

water .
3

N ow pour the i ron mixture and the diluted ammonia s imul ,

t an e ou s l y sl owly and with uninterrupted stirring into 8 00 0 parts

, , ,

o f di stille d water .

Wash the precipitate by the a ff usion and decantation o f distill ed

water until the washings no longer give any reaction for chloride .

Collect the washed precipitate on a strainer and express the

 I RON O X Y C H LOR I DE .
40 3

water from it by strong pres su re until the press cake is reduced to

a weight not exceeding 4 00 parts .

Trans fer thi s to a bottle add the hydrochloric acid and al so , ,

enough distill ed water to make the total wei g ht o f the m ixture

1 0 0 0 parts .

L et the mixture stand shakin g it occasional ly until the soli d

, ,

matter has dissolved .

Filter the solution .

The finished product should have the s p w . .

Keep the product in a dark place or in amber colored bottles ,

-
.

D e scri p ti on —
A
clear brown red liquid containing an amount -
,

o f ferric oxychloride correspondin g to about 3 5 per cent o f Fe . .

I t shoul d yiel d 5 per cent o f ferric oxide on precipitation with

ammonia in excess and ignition o f the precipitate in the u sual way .

D i alys e d S ol u ti on o f I r on.

L I QUOR F ERR I D I A L Y S ATU S .

S oluti on o f ferric chloride

A mmonia water
D istilled water su ffi cient ,
.

M ix 86 ml of the sol ution o f ferric chlori de with 5 0 0 ml o f

c ol d distill ed water Pou r the mixture slowly and with constant
.

stirring into the ammon ia water previously diluted with 4 00 ml

o f cold distill ed water Wash the precipitate with col d d istilled
.

water first by decantation and a fterwards on a wetted muslin

strainer until the washings cease to be a ff ected by test s ol u t i on of -
.

s ilver nitrate aci dulated with nitric acid L et drain and then .
,

press out from the magma as much as possible o f t h e moisture it

holds .

A dd t h e ferric hydroxide to th e remainder o f the solution o f

ferric ch loride stir wel l and s et aside until no more ferric h y
, ,

d rox i d e d issolves .

D ecant the l iqu id from the und issolved po rtion place it in a ,

covered dialyser and wash it by dialysis until the washings are

,

n early tasteless
‘
.

Then dilute th e solution in the dialyser until it measu res nearly

3 7 5 ml and has a s p g r o f
, . .
40 4 I RON P E P T O N A T E .

Keep the product in tightly closed bottles and protected a g ainst

light .

N ot e s When 1 0 Gm o f this sol ution is treated with ammonia

.

water in excess the precipitate , when washed dried and ignited

, , , ,

should weigh Gm A drop o f the sol ution dilu ted w ith

.
,

water shoul d yield n o precipitate with test solution o f silver

,
-

nitrate acidulated with nitri c acid

‘

.
.

Th i s I S the s o called dialysed iron

“
-
It w ill be observed that .

the product is not the dialysed portion but th e res idue a fter the ,

dialys is It contains a highly basic ferric oxychloride

. .

i pt i
D e scr A dark reddish brown liquid ; Odorless and o f a
on — -
,

m ild non styptic taste

,
-
.

I R O N P E PTO N AT E .

F ERRU M PE PT O N A T U M .

S olution o f oxychloride o f iron ( conta i n

ing per cent o f Fe )
D ried egg albumen
H y drochloric acid ( 2 5 70 o f H Cl )
Pepsin
D istilled water su fficient ,
.

D issolve the egg albumen in 20 0 0 parts o f distilled w ater to ,

which have been p reviously added the pepsin together with 3 0

parts o f the hydrochloric acid L et this mixture stand stirrin g .
,

or shaking it occas ionally for a period o f 1 2 hours in a place ,

°
where the temperature i s about 4 0 C Then let the solution cool .

to 20 C filter or strain it and carefully neutral ize it with a very

°
.
, ,

weak solution o f sodium hydroxide S houl d a precipitate be .

formed filter the liquid

,
.

D ilute the solution of ferric oxychloride with 2 00 0 parts o f

distilled water and add this solution to the solution o f digested
,

egg albumen M i x well . .

N eutral ize the mixture carefull y with a very weak solution o f

sodium h y droxi de stirring well ,
.

Wash the precipitated iron peptonate with distilled water as

lon g as the washin g s give a pr e ci pi ta te with silv e r n itrate solu
40 6 I RON T ART R AT E .

I R O N A M M O N I U M TAR TR A TE .

F ERR I E T A M M ON II TA R TRA S .
’

F e rr y l —
A mmonium Tartrate ) .

S olutiono f normal ferric sulphate 90 parts

Tartaric acid 1 8 parts
A mmonia water 7 2 p arts
A mmonia water distilled water each su fficient
, , .

M ix the ammonia water with 1 8 0 parts o f cold water ; add

gradually and with constant stirrin g the solution o f tersulphate
, ,

o f iron previously d i l uted with 900 parts o f col d water .

Pour the mixture on a wetted musl in stra i ner allow the magma ,

to drain and then return it to the precipitation ves sel and m ix it

,

well with 1 0 0 0 parts o f col d water D rain it again on the strainer .

,

and repeat the operation once or O ftener until the washin g s onl y , ,

give a sl ight clou dines s with barium chloride solution Then .

allow it to drain thoroughly D issolve one hal f o f the tartari c .

-

acid in 4 5 parts of distilled water neutral ize the acid exactly with ,

ammonia water then ad d the remainder o f the tartaric acid and

, ,

d issolve it by the aid of heat Keep the solution o f ammonium .

bitartrate hot but not above 60 C over a water bath and add
,
°
.
,
-
,

to it with constant stirring the ferric hydr oxide in s mall portions

, , ,

at a ti me until no more will dissolve F ilter the solution while

,
.

hot evaporate it at not over 6 0 C to the consistence o f syrup

,
°
.
,

and spread it on glass plates to dry in scal es .

Keep the product in amber colored bottles tightly corked and -

, ,

put in a cool dark place ,

.

N ot e s The remarks under I ron and Potassium Tartrate a p

.

l
p y i n a general way t o thi s process as well The ammonium .

bitartrate is H 4 N H C H 0 by which the ferric hydroxide is dis

4 4 6 ,

solved i n a manner analogous to the solution e ff ected by digesting

the hydroxide with potassium bitartrate in making the tartrate o f
iron and potassium .

D e scr i pt i on
Transparent garnet red to brown red scales
—
,
- -
,

somewhat l ighter and clearer in color than the tartrate o f i ron and
potassium O dorless Taste sweetish slightly ferruginous Very
. .
, .
 I RON T ART RA T E .
407

soluble in water Insoluble in alcohol Produces more clear and

. .

permanent sol ution s than potassium iron tartrate .

I R O N P O TA S S I U M T A R T R A T E .

F ERR I E T PO T A S S I I T A R T R A S .

( F e r r y l -
Potass ium Tartrat e ) .

S olution o f normal ferric sulphate

Potassium bitartrate
D istilled water .

A mmon ia water su fficient , .

M ix 10 parts o f ammonia water w ith 2 0 parts o f col d water ;

add gradually and w ith con stant stirring the solution o f t e r s u l
, ,

phate o f i ron previously diluted with 1 0 0 parts o f col d water

, .

Pour the mixture on a w e t muslin strainer allow the magma to ,

drain an d then return it to the precipitation ves sel an d m ix it w ell

,

with 1 0 0 parts o f col d water D rain it again on the strainer and .

,

repeat t h is operation once or twice as may be n ecessary until , ,

'

the washings produce but a slight cloudines s with test soluti on o f -

barium chloride L et the ma gm a be well drained ; then forcibly

.

press ou t O f it as much o f the water as possible A dd it in small .

portions at a time to a m ixture O f the distilled water an d the p ot a s

sium bitartrate heated over a water bath at not over 60 C
,
—
°
.
,

stirring constantly until all the ferric hydroxide has been added
and dissolved Filter wh il e hot and set the filtrate aside in a cool
.
,

dark place for twenty four hours then stir it well with a p orcelain
-

or glas s stirrer until any precipitate which may have formed in

“

the liqui d is evenly distributed through it Then cautiou sly add .

j ust enough ammonia water to dissolve this precipitate filter and , ,

evaporate the solution in a porcelain d ish to the consistence of

thick syrup and spread it on glass plates to dry in scales
, .

Keep the product in well corked amber bottl es i n a dark place ,

.

R e ac ti on . Ferric hydroxide is first prepared from the ferric sul

phate :

F e z S O4 ) 3 6
-
H
3( 4 N S
)2 4O .

The ferric hydroxide i s then dissolved by the potassium tartrate ,

forming s everal compounds one o f which i s perhaps ,

40 8 I RON T ARTR AT E .

H
3 ZO ,
—

while another I S probabl y made in this w ay

B ut the tartrate o f iron and potassium probably is not a definite

double salt ; the pharmacopoeial products are all variable as to the
proportion o f iron .

N ot e s Whether prepared from solution of tersulphate o f iron

.

or from solution O f chloride o f iron the ferric hydroxide must be ,

care fully precipitated from col d dilute solutions an d wel l washed

, ,
.

When made from chlori de it i s more readil y washed cl ean The .

h y dro xide does not d issolve rapi dl y in the l iquid or the soluble tar ,

trat é Of I ron an d potassium is but slowl y formed from the ferric

h yd foxi d e and the potassium bitartrate S everal hours are required
'

t o com
"
plete the solution In view of the fact that ferric .

hy droxide i s so liable to become basic and insoluble when

subj ected to heat it is best to add the ferric hydroxide,

in portions to regulate the h eat carefully an d to stir

,

constantly The succes s o f the whol e proces s d e p e n d s t o a great

.
‘

extent upon the character o f the ferric hydroxi de and upon the pre
cautions described i n the foregoing The addition o f ammonia .

is intended to r ender the product readily water soluble w ithout

residue The Pharmacopoeia does not direct that the sol ution
.

shoul d be filtered but this is necessary to Obtain a good product

,
.

D e scri p t i on —
T ra fis p a r e n t
garnet red or brown red scales odor - —
,

less taste sweetish slightly ferru ginous Very soluble in water ;

, ,
.

insoluble i n alcohol

[ in p ure M a l a te f
o I r on .

Iro n wire cut ,

20 Gm
Crab apples nearl y ripe , 5 0 0 Gm

Pare the appl es beat them into a pulp and express the j uice
, , .

A dd the iron mix well set the m i xture in a warm place for ten
, ,

days or until all signs o f e ff ervescence ceas e stirring frequently

, ,
.

R eplace from time to time the water lost by evaporation Heat .

0
the m ixture on a water bath at 7 0 C for s ix hours replacing —
.
,

water lost by evaporation A dd 1 00 ml o f warm water express .

, ,
410 I RON HYD RO X I DE .

throughout the reaction that for this purpose the cyani de s hou l d
,

be added to t h e chloride and not vi c e v e r s a a n d t h at some ferric ,

'

chloride shoul d remain undecompos ed at t h e end O therwis e the .

product will be contam inated with more potass ium salt than when
the directions given are observed U nder any circumstances there .

will be a slight amount o f potas sium compound in the product .

A ny attempt to wash out all the potassium salt will resul t in the
formation o f ferric oxide which remains in the preparation
, .

The precipitate is a voluminous ma gm a which is diffi cult to

wash as it settles very slowly Washing on a filter is i m p rac t i
, .

cabl e becaus e the precipitate completely cl oses the pores o f the

,

paper .

The presence o f a l ittle free H Cl i n the liqu id ( which w ill be

insured by u sing t h e solution o f ferric chloride o f the U S P ) . . .

considerably facilitates the washing .

I R O N ( F E R R I C ) H Y D R OX I D E .

F ERR I H Y D R OX I D U M .

Pe ( O H )3
—
_ : I O7 .

S olution o f normal ferric sulphate ( 5 0 Gm ,

or )
A mmonia water ( 4 0 Gm or ) ,

Water su ffi cient
,
.

D il ute the ammonia water w ith 1 0 0 ml o f col d water in a pre

’
c i p i t a t i on vessel o f about one liter s capacity D ilut e the solution .

of ferric sulphate with 5 00 ml of cold water and pour this into ,

the dilute ammonia slowly and du ring constant stirring .

Wash the precipitated ferric hydroxide with col d water first by

-

a ff usion and decantation and afterwards on a wetted muslin

,

strainer until the washings are tastel ess Then l et the magma
,
.

drain return it to the precipitation vessel and m ix it well with as

, ,

much col d water as the vessel will hol d or abou t one liter L et , .

settle decant the supernatant liquid and aga in trans fer the magma
, ,

to the wette d strainer and allow it to drain Continue the wash .

ing in this manner until the wash water is no longer a ffected by

test solution o f barium chloride
- .

[ When the ferric hydroxide i s to be u sed as an antidote for

 I RON HY DROX I DE .
41 I

a rsenic the whol e process must be hastened an d the washing need

, ,

not be carried farther than to remove the mother l iquor T o e ffect .

thi s the precipitate is al lowed to drain until most o f the l iqui d has
run off and the strainer is then gathered up so as to enclose the
,

magm a which is then forcibly p ress ed with the hands until no

,

more liqui d can be s queezed out a fter wh ich enou g h water i s ,

added to the hydroxide to make the wei ght o f the whole product
equal to twice the weight o f the solution o f ferric sulphate us e d ]

R e act i on . F e2 S O4 ) 3 ( H 4
N ) 25 0 4
.

N ot e s and c ol d sol ution s a re necessary The diluted

. D i l u te .

solution o f ferric sulphate shoul d be poured slowly or in a i rfl é ll

m
,

stream into the d iluted ammonia water during c on s ta

,
rr i ng ,

as d irected When the whole o f the I ron solution has been a dded
.
,

the m ixture shoul d still ha ve a decidedly ammoniacal Odor ; a s

'

the ammonia gas is di ff used through the stratum o f ai r above t h e

surface o f t h e l iquid that air mu st be fanned or blown away before
,

the Odor of the liquid itsel f can be ascertained .

There are several ferric hydroxi des di ffering from each other in ,

the proportio ns o f H O they conta i n in color and in their solubility

’

, ,

in acids Th e product intended by the Pharmacopoeia i s F e ( O H ) 3

.

another ferric hydroxide is F e O ( O H ) 4 ; an d dried ferric h y d rox

z

ide is O F e ( O H ) The more bas ic it i s and the less water it

.
,

contains the less readily soluble is it A s Obtained by the O ffi cial

,
.

pr ocess all the necessary precautions being observed the product

, ,

is dark reddish brown an d readily soluble in citric aci d and in

-
,

glacial acetic acid When yellowish brown br Ow n grayish

.
-
, ,

brown or clay colored it i s bas ic insolubl e and unfit f or the uses

,
-
, ,

for which it is intended in pha rmacy .

The solution of ferric sulphate mu st contain th e full a m ount o f

ferric sulphate an d be free from ferrous salt in order that the
,

quantity o f ferric hydroxide obtained from it may be definite ;

the importance o f this will be readily understood from the fact
that the proportions o f the material s prescribed in several working
formulas for ferric salts are calculated with re ference to th e
amount o f ferric hydroxide theoretically yielded by the solution
o f ferric sulphate .

In summer it is best to u se ice for cool ing the dilute solutions

previou s to the precipitation The chemical reaction generates .

heat an d i f th e solution s are al ready warm the temperature o f

,
4 1 2 I RON HY DROX I DE .

the mixture is l iable to rise su fficiently high to cause the formation

o f light colored m eta hydroxide B ut the l iquids must not be ice
- —
.

cold .

The o fficial solution of ferric sulphate containing per cent ,

o f F e ( S O 4 ) 3 yields per cent o f ferric hydroxide The

‘

2 , . .

offi cial solution O f ferric chloride containing per c ent o f ,

F e Cl yi elds about per cent o f F e ( O H ) 3

’

3 , .

S houl d the quantity o f ammonia used be insuffi cient or should ,

it be added to the ferric sulphate instead o f vi ce ve rs a basic ferric ,

salts will be formed I f the H 3 N is added to the i ron solution a

.

dark red brown solution containing ferric salt i s obtained at first

-
,

and no f erric hydroxide is thrown down until more amm onia is

a dded .

Ferric hyd roxi de may al so be precipitated from ferric chloride

or f erric n itrate and soda may be u sed as a precip itant instead o f
'
,

ammonia .

I f solution o f ferric chloride is u sed the hydroxi de formed is

more easily washed free from the ammon ium salts I f ferric n i .

trate is u sed the product i s soluble in an excess o f potassium car

,

bonate ( S tahl s tincture ) ’

.

Ferric hydroxide precipitated w ith soda instead o f ammonia is

lighter in color and extremely di ffi cult to wash fre e from sodium
salt.

Ferric hydroxide forms very solubl e compounds with sugar ,

and with glycerin It is also soluble in solutions o f ferric salts

.
,

as in solution o f ferric chloride The precipitation o f ferric h y

‘

d r ox i d e from s olutions o f ferric salts by means of alkalies is

prevented by the presence o f citric acid tartaric aci d s u gar g ly , , ,

cerin and certain other or g anic substances

,
.

When mo i st it is a dark red brown ma gm a i n

D e scr i pt i on — -
,

soluble i n water but soluble in citric tartaric acetic hydrochloric

, , , , ,

sulphuric and nitric acids When dried it is a reddish brown

, .
-

amorphous powder l es s readily soluble in acids than the moi s t

,

hydroxide .

U se s For th e preparation o f ferric acetate citrate tartrate

.
, , ,

n itrate etc A lso as an antidote for arsenic with which it form s

, .
,

insolubl e arsenate
 I RON HYP O PH O S P HIT E .

M agnesia 28 Gm
D istilled water 5 0
2 Gm

wel l and keep this mixture in another bottle

M ix .

When required for use mix equal volumes of the two liquids
and shake well .

I R O N ( F E R R I C ) H Y P O PH O S PHIT E .

F ERR I H Y PO P H O S P H I S .

—
25 I .

14 (4 3 S ulphate o f i ron an d ammonium .

3 0 parts
S odium hypo phosphite 20 parts

D is solve each salt in I 5 0 parts o f water and filter the solutions , .

A dd the solution o f the i ron a l um to that of the sodium h yp oph os

‘

p hi t e stirring
,
constantl y S e t aside for a few hours .Trans fer .

the precipitate to a wetted filter or muslin strainer drain i t tho r ,

oughly and wash it w ith I 5 0 parts o f cold d istilled water D rain

,
.
,

press out as much as possible of the moisture from the magma ,

and dry the product between blotting paper with the aid o f gentle
heat protecting the preparation as far as practicabl e from th e air
, .

R e act i on . 2 F eH 4N S O4 —

I 2H O
; )+ 6 N a PO ,
H 2. H zO )

2F e P0 2H 2 ) 37l ‘ ‘

( 4
H N )2 5 0 4 + 3 N 8 2 5 0 fi
4 + 39 H a

N ot e s The quantity o f water used i s necessarily l imited to

.
,

prevent loss because ferric hypophosphite is not quite insolubl e

,

in water and i f the washing should be done with the large quan
,

tities o f water requ ired to thoroughly remove the sulphates o f the

mother l iquor from the bulky ma gm a o f hypophosphite consider ,

abl e loss must follow i f not the disappearance o f the entire

,

product The precipitate must there fore be care fully freed from
.
, ,

all mother l iquor that can be removed by draining it before it i s

washed and the quantity o f water prescribed for washing it
,

shoul d not be exceed ed .

Ferric hypophosphite is solubl e in a strong hot solution o f ,

citrates o f potassium and sodium .

D e scr i pt i on A gra y ish powder odorles s and al most tasteless

—
, ,
 I RON I OD ID E .
415

slightly soluble in water readily soluble in acetic acid and in

, ,

solutions o f potassium citrate or o f sod ium citrate .

IR ON ( F E R R OU S ) I O D I D E .

F ERR I I OD I D U M .

FeI 2
:
309 .

I ron w i re cut
, 6
parts
Iodine 1 7 parts
D istilled water 20 parts

D igest in a flask at a moderate heat until all Odor o f iodine has

ceased and a green solution has been Obtained Filter the solu .

tion and evaporate the filtrate as rapidly as poss ible in a pol ished
i r on d i s h until a trial drop sol idifies on cooling Then pou r the
‘

l iqui d out on a porcelai nsl ab and as soon as it has hardened break

,

it into p i eces while still warm and put it into small d ry warm , , ,

bOtt l e s which must be at once tightly stoppered

,
.

For reaction and notes see S yrup o f Ferrous Iod ide .

D e s cri pti on
Ferrous iodide is a crystall ine sol id which in
—
, ,

mass appears nearl y black In solution it is green But the prod

, . .

~
u e t easily decomposes and it i s for that reason scarcely employed
,

“ ” “
except in the form o f saccharated iodide o f iron or as syrup ,
”
o f ferrous iodi de .

S a c c h ar a te d F e r r ou s I od i d e .

F ERR I I OD I D U M S A CC H ARA T U M .

I ron in the form o f fine bright w ire cut

, , ,

into small pieces -

R educed iron
Iodine
D istilled water .

D ry milk sugar o f each s u ffi cre nt

, , .

M ix the iron wire iodine an d 20 parts o f di stilled water in a

,

flask and shake them together occasionally until the reaction

,

ceases and the l iqu id has acquired a green color and lost the odo r
,

o f iodine Warm the flask and contents i f necessary to com

.
, ,

p l e t e the reaction Filter the l iquid

. through a small white paper
4 16 I RON I OD I DE .

filter previousl y wetted with distilled water into a porcelain dish ,

‘

containing about 4 0 parts o f powdered milk suga r R inse the .

flask and the undissolved iron wi re with a l ittl e distilled water ,

and pass the rinsings through the same filter as before used into
the porcelain dish .

M i x the contents o f the dish by stirrin g w ith a glass rod or

porcelain spatula E vaporate the water from the mixture by
.

water bath heat stirring frequently until a dry mass remains

—
, ,
.

T rans fer the dry residue while still hot to a cl ean bright iron ,

mortar heated by placing it in boiling water and then wiped d ry ,

powder it add the reduced iron an d enough powdered milk suga r

,

to make the weight o f the total product 1 0 0 parts and triturate ,

these ingredients together until intimately mixed and reduced to a

fine powder .

Trans fer the powder at once to small warm per fectly dry bot , ,

tles which shoul d be filled and tightly stoppered

, ,
.

N ot e s . the reaction and remarks giv en under the titl e o f

S ee
S yrup o f Ferrous Iodide .

The ferrou s iodide contained in this preparation is protected

from decompos ition by the milk sugar and the reduced iron I t .

shoul d c ontain at least 2 0 per cent o f ferrous iodide .

D e scri pt i on el low ish white grayish

—
A white or greeni sh :
y
— -
.
, ,

gray powder ; odorless ; h y groscopic ; having a sweeti sh ,

f e r ru g i
nous taste S oluble in 7 parts o f water at 1 5
.
°

S yr u p o f F e rr ou s I odi d e .

S Y RU P U S F ERR I I OD I D I .

A syrupy l iquid containing 10 per cent o f ferrou s io dide ( F e l z,

I ron in the form o f fine wire and cut into

, ,

small pieces
Iodine
S ugar in coars e powder
,

D istilled water su fficient ,

.

Introduce the iron into a flask add 2 0 0 ml o f distilled water , ,

and a fterward the iodine S hake the mixture oc ca s i on a l l v until

.
,

the reaction ceases and the solution has acquired a green color and
418 I RON I OD I DE .

bottles but with much less risk in glas s stoppered bottles E x

,
'
-
.

p o s u r e to light seems to decolorize the preparation even after the ,

green color has changed to a pal e yellowish But in order to best .

preserve a bright green s y rup o f ferrous iodide from change it

shoul d be kept in a sha ded place .

L ong exposure to light almost completel y decolorizes the prep

aration and the sugar in th e syrup becomes to a great extent i n
,

verted ( J H L ong )
. . .

U nless the bottle containing the syrup is filled the surface o f ,

the preparation soon becomes yellow or yellowish brown from -

oxidation by contact with the air above it H ence the direction .

that t h e bottl e shal l be filled .

When this preparation becomes slightly discolored yellowish —

green but not yell ow or yellow ish brown the bright green co l or - —

can usually be restored by heating it to nea r the boiling point in a

flask by means of a water bath —
.

S training does not su ffice to make the product cl ear It must .

be filtered through white fi lt e r paper -

.

A s the preparation is prone to discoloration by decompositio n ,

assuming a y ellowish brown color from free iodine variou s means

-
,

have been suggested to prevent this change It was at one t im e .

proposed to place a piece o f polished iron for exampl e a nail —

,

filed until bright over its whol e surface i n the syrup ; but thi s is —

wors e than useless A nother and more success ful plan was to
.

add tartaric or citr c aci d in the proportion o f about 1 part in 5 0 0

i
,
.

A l l such additions are however unnecessary as the preparation

, , ,

w ill keep wel l i f properly made and put into clean glas s stop ,
-

pered bottles in the manner indicated above .

D e scri p t i on —
M
ust be perfectly cl ear pale green odorl ess with , ,

a sweet strongly ferruginous taste R eaction neutral S p w . . . .

about at
The size o f the container should be determined by the rate at
which the preparation is dispensed in the pharmacy It shoul d .

not be so large that the contents m ay not be entirely consumed

in a few weeks Bottles holding 5 0 0 Gm are as large as should
.

be used a nd bottles containing 1 0 0 Gm are not too small when

,

the demand for the preparation is l imited .

The same preparation ( containing 1 0 per cent o f ferrous iodide )

is contained in all other pharmacopoeias .
 I RON LA CT AT E .
4 9
1

Gly ce r i te o f F e r r ou s I od i d e .

I odine 8 3 Gm
I ron wire 25 Gm
D i stilled water 1 5 0 ml
Glycerin 300 ml

D igest the iron w ire an d iodine together in the water con ,

the l iquid has acquired a bright green

'

t a i n e d in a flask until ,

color and lost all odor

,
o f iodine Filter the solution into the
.

glycerin m ix well and

, ,
evaporate the mixture unt il it weighs
5 00 Gm .

N ot e s This glycerite keeps indefinitely mixes clear with

.
,

water ,alcohol and syrup and i s exactl y twice the strengt h ( in

, ,

ferrous iodide ) o f the Pharmacopoeial syrup o f iodide o f iron

(U s )
. .

I R O N ( F E R R OU S ) LA C T A T E .

F ERR I LA CT A S .

z as
-
.

Whey
M ilk sugar
S odium bicarbonate
Ferrous sulphate
The white o f two eggs .

D iluted sulphuric acid .

Water .

A d d the milk sugar to one liter o f the cl ear whey obtained from
spontane ou sly sou red skimmed milk in a cyl indrical vessel of ,

about two cubic decimeters capacity L et the mixture stand in .

°
a place where the temperature is maintained at between 3 0 and
A fter fermentation has commenced ( within a day or two )
and th e l iqu id is sou r from lactic acid ne utral ize with a portion ,

O f the sodium bicarbonate R epeat th is neutral ization e ve r v d a y

.

or two adding each tim e enough sodium bicarbonate to com

,

p l e t e l y neutral ize the lactic acid formed .

When the mixtu re n o longer acquires a decidedly aci d reaction

with in three or four days a fter n eutral ization an d when about ,

6 0 Gm o f sodium carbonate has been consumed add enough d i ,

4 2 0 I RO N LA CT AT E .

luted sulphuric aci d to render the liquid distinctly acid Then .

add the whites o f two eggs M i x thoroughly . .

N ow heat the mixture to boiling Filter the hot l iquid . .

E vaporate the filtrate to about 2 50 ml .

D issolve the f e r r ou s s u l p h at e in 8 0 ml o f hot distilled water ,

and filter A dd this solution while hot to the hot solution o f s o

.

d i u m lactate R emove from the hot m ixture the brown fl oc c u l e n t

.

precipit ate formed passing the l iqu id through a flannel strainer

, .

S e t the hot colature asi de in a col d place for two days Collect .

the crystallized ferrous lactate on a strainer L et the crystalline .

mass be well drained Wash it with a littl e col d distilled water

.
,

an d a fterwards with a l ittle al cohol Pres s the moist lactate be .

tween blotting paper changing the paper s everal times D ry the

,
.

product well w ith th e aid o f moderate heat .

Keep the product in small tightly closed bottles in a cool dry ,

place .

R e act i ons .

C1 2H 22 0 11+
H 2 O Z
4 H C3
H 5 O3 ;
the n

and ,
fi n a ll v ,

N ot e s The whey contains 4 to 5 per cent o f milk sugar and

.
-
,

this , together with that added y ields lactic acid as shown above
, ,
.

U nless this aci d is neutral ized from time to t ime the lactic ,

fermentation which ordinaril y continues for a week may change

, ,

to v i nous and acetic fermentation The production o f alcohol and .

acetic acid might al so follow i f the temperature of the liq uid is

°
below 2 0 C .

C1 2H 22
0 1 1 + H 20 2
4 C2 H 5 0 H + 4 C0 2 °

S hould t he temper a ture be allowed to exceed 4 0 C or an i n °

.
,

s u ffi c i e n t quantity of milk su gar be used butyric a c i d w ill be

—
,

formed .

To arrest further fermentation the liquid i s heated to the boil ,

ing point which at the same time coagulates and facilitates the
, ,
4 2 2 I R O N OLEAT E .

Y ellowish green cr y stalline masses or a greenis h

D e s cr i p t i on .
—
,

white powder nearly inodorous having a sweetish ferruginou s

, ,

taste and a slightl y acid reaction S oluble in 4 0 parts o f water

,
.

at 1 5 C and in 1 2 parts of boiling water : Freely soluble w ith

°
.
,

a green col or in solutions o f alkali C itrates N early I nsolubl e in .

'

alcohol .

I R O N ( F E R R I C ) OLEA T E .

F ERR I OLEA S .

F e ( C1 8 H 3 3 O 2) 3
2 8 99

S olution
of normal ferric sulphate
White casti le soap in fine powder ,

D ilute the solution o f ferric sulphate with m 1 of water ,

and dissolve the soap in 2 5 0 0 ml o f hot water M i x the solutions

,
. .

Wash the precipitated oleate twice with hot water usin g about ,

ten l iters each time .

R e act i on .

F e 2 5 0 4 ) 3 +6 N 3 C1 8 H 33 0 2
2 2F e C
( 18 H 33O2 3 +3 N a 2S O 4 '

N ot e sThe y ield is about 1 2 0 Gm

. .

Ferrou s oleate can al so be made by d ouble decomposition from “

ferrous sulphate and soap but the g reenish ferrous oleate soon ,

oxi dizes .

D e scri p t i on
Ferric oleate is a dark red plaster like solid
.
— -
.

S oluble in oleic aci d and in fixed oils .

I R O N ( F E R R OU S ) OXALA T E .

F ERR I OX A L A S .

F e CzO 4 H zO .
: 1 62 .

Ferrous sulphate
O xalic aci d 0
A mmon i a water
D i s s ol ve t h e oxal ic acid in the ammonia water diluted with
l

ml o f water ; and the ferrous sulphate in ml o f hot

 I RON OXALA T E . 23

water ; filter the solutions and then m ix them Wash the pre ,
.

c i p i t a t e by decantation and a fterwards on a filter until the wash

ings are tasteless D ry the product between bibulous paper with

.
,

the aid o f gentle heat .

R e act i on .

F e S O4 + H 4N ) 25 0 4 .

N ot e s . oxalate can also be made by the proces s o fficial

F errous
I n the U S P o f 1 8 7 0 which prescribed ferrous sulphate d is
. . .
,

solved i n water to be added t o a solution o f oxal ic acid When .

this process is followed ferrous oxalate and f ree sulphuric aci d

are formed the precipitate separates slowly and a cons iderable
, ,

loss results from the fact that the oxalate i s not insoluble in the
sulphuric acid By neutralizing n early all o f the oxalic aci d with
.

ammon ia using a sl ight excess o f oxalic acid and mixing the

, ,

solution o f ferrous sulphate with the aci d solution o f ammonium

oxalate the precipitate falls at once an d no los s o f product is
, ,

sustained I f a perf ectly neutral solution o f ammonium Oxalate

.

is u sed the product will have a dull reddish yellow color

, .

To obtain a bright y ellow ferrous oxalate the mother l iquor in

which the precipitate is formed must be deci dedly acid .

D e scr i pt i on A l ight yellow crystalline powder ; odorl es s ;

.
— -

nearly tastel ess N early insolubl e in water an d insoluble in alco

.
,

hol.

I R O N ( FER R I C ) O X I D E .

F ERR I OX I D U M .

F e 20 3 2 1 60 .

Heat dried ferric hydroxide strongly until it ceases to los e

weight .

2F e ( O H ) 3
: F e zO 3 —
H
3 20

S even parts o f dry ferric hydroxide will yiel d rather more than
five parts o f oxide It i s brown red .
-
.

A n o th e r M e t h od .

H eat ferrous oxalate until completel y decomposed .

 I RON OX I DE .

The product obtained from ferrous oxalate is e x t re m e l y fi n e l y .

divided and there fore so ft an d o f a rich dark brown color T his ,

-
.

is used by j ewellers to pol ish gold .

M ag n e t i c Ox i d e o f I r on .

F e, O4 —
2 32 .

o f ferric sulphate U S
S olution , .

Ferrous sulphate
A mmonia water ( 1 0 70 o f H 3 N )
Water .

D issolve the ferrous sulphate in two l iters o f water and filter .

A dd the solution o f ferric sulphate .

D ilute the ammon ia water with one liter o f water .

Pour the iron sol ution gradually into the dil uted ammo nia
water stirring well
, .

S e t the mixture as ide to settle D ecant the supernatant l iquid .

from the precipitate Then add enough water to make the whole
.

mixture measure about three l iters .

Boil this mixture about fi fteen minutes or until the brown ,

ferroso ferric hydroxide i s changed to the nearly black ferroso

-

ferric oxide .

Wash the precipitate first by a ffusion and decantation o f hot,

water and a fterwards on a filter until the washings cease to give

, ,

a precipitate with test solution o f barium chlori de Then dry the

-
.

product with the aid of heat .

R e a ct i on .

Fe ,
S O4 ) 3 -
F e S O4 —
8H 4N OH

H 4N ) S O, —
4H , O .

D e s cr i pt i on .
—
A fine heavy brownish black odorl ess and taste
, ,
-
,

less powder .
4 6
2 I RON P H O S P H A T E .

D issolve the ferrous sulphate and the sodium phosphate each

in 3 00 parts o f boiling water filter and allow the solutions to cool , ,
o °
to about 40 to 5 0 C ( 1 0 4 to 1 2 2
° °
D issolve the so dium .

acetate in 5 0 parts o f warm water A dd the solution o f f errous sul .

phate to the solution o f sod ium phosphate and lastly add the solu ,

tion o f sodium acetate M i x well A s soon as the p r e c i p i . .

tate has subs ided decant the mother l iquor Wash the precipitate
,
.
,

either by decantation or on a musl in strainer with hot water , ,

until the washings cease to give a precipitate with solution o f

°
barium chloride D ry the product at not over 5 0 C ( 1 2 2
. .
°

R e act i on .

PO , ) , + 2 N a, S O4 H , S O, .

Th e sulphur i c a c i d then reacts w ith the sodium acetate form ,

ing free acetic acid in which the phosphate o f iron i s but ,

sparingly soluble an d the precipitated ferrous phosphate is par

,

t i a l l y oxidized .

N ot e s . U nles s sodium bicarbonate sodium acetate or sodium , ,

phosphate in excess be added a portion o f the ferroso ferric phos ,

-

phate remains in solution in the free acid formed by the reaction ,

and loss ensues By n eutral iz ing the free sulphuric aci d wi t h

.

sodium bicarbonate which does not aff ect th e precipitate alread y

,

formed all of the phosphate o f iron i s thrown down When first

,
.

formed the precipitate i s gra y ish white or bluish gra y ; it soon - -

becomes grayish blue and shoul d retain this color until washed
-
,

and dri ed The color m a y be eas ily spoiled however by too high
.
, ,

heat or by too long exposure to the action of the mother liquor

, ,

or to the air during the proc es s o f washing and drying I nstead .

o f bluish the color may become greeni sh gray T h e su rest way -

.

to obtain a handsom e grayish blue product i s to empl oy sodium -

acetate a s directed in the foregoing formula A fter drying the

,
.
,

product mu s t be powdered and si fted D ried at a high h eat the .

,

preparation forms ver y hard lumps ; but i f dried by moderate heat

it may be easily rubbed through a fine sieve without u s ing much
force .

This pro duct is the Ferri Ph os p h a s o f th e British Pharmaco

p os ia and o f the U S P o f 1 8 7 0 . . . .

It shoul d contain at least 4 7 per cent o f ferr ous phosphate It .

may also contain some ferric oxide .

 I RON P H O S P H A T E .
42 7

De scr i pti on .
—
A fine grayish blue odorles s tasteless insoluble
,
-
, , ,

powd e r .

IR ON PH O S PH A T E S YR U P .

S Y RU P U S F ERR I P H OS PH A T I S .

Precipitated ferrous sulphate

S od ium phosphate
S odium bicarbonate
Phosphoric acid 5 o % )
S ugar

D issolve the ferrous sulphate in about 3 0 0 ml o f boiling water ,

and the sodium phosphate in a s imilar quantity o f cold water ;

mix the solutions ; add the sodium carbonate previously dissolved
in 1 0 0 ml o f water and a fter stirring well trans fer the precip itate
, , ,

to a musl in filter an d wash it with distilled w a ter until the filtrate

ceases to be a ff ected by test solution o f barium chlori de M i x the .

washed an d drained precipitate in a mortar with the phosphoric

acid A s soon as the phosphate is dissolved filter the solution into
.

“
,

a bottle add 40 0 ml o f distill ed water and the sugar and shake

,
'

until dissolved without the ai d o f heat L astly add su ffi cient

,
.
,

d istilled water to make the final product measure 66 0 ml .

N ot e s The product contains about I Gm o f anh y drous phos

.

phate o f iron in one imperial fl u i d ra ch m I f th e .

quantity Obtained by the above formula be diluted with 3 0 ml o f

s imple syrup the preparation will then contain I Gm to each 4 ml
,
.

A n oth e r M e th od .

I ron wire poli shed cut

, ,

Phosphoric acid ( 5 o % )
D istilled water
S impl e syrup

Put the iron wire acid and water into a flask being careful that
, , ,

the metal is completely covered by the liquid ; insert a loose plug

o f cotton in the neck o f the flask an d set it asi de for two or three
,

da y s When the iron is dissolved filter the l iquid add the s y rup
.
, , ,

and lastly enough distilled water to make the final product m eas
u re 8 20 ml .
4 8
2 I RON P H O S PH A T E .

N ot eThis preparation is identical with that o f the B ritish

.

Pharmacopoeia .

D e scri pt i on —
. A clear nearly colorless thick syrup o f acid and
, ,

ferruginous taste .

I R O N ( F E R R I C ) P H O S PH A T E ; P R E CI PI T A T E D .

F ERR I P H OS PH A S PR A E CI PI T A T U S .

S olution O f normal ferric sulphate

S odium phosphate
S odium ace tate

D ilute the solution o f ferric sulphate with 40 0 0 ml o f water ;

add the sodium acetate and dissolve D iss olve the sodium phos
,
.

phate in 40 0 0 ml o f water and filter i f necessary Pou r the solu

, , .

tion O f ferric sulphate and sodium acetate gradually into th at o f

the sodium phosphate stirring wel l Wash the precip itate with
,
.

warm water until the washings are free from sulphate Collect .

and d ry the precipitate with the ai d o f gentl e heat .

R e act i on .

+3 ( N a I OH , O)

N ot e s . I t will be seen from the equation that the sodium ace

tate is added simply to prevent the formation o f free sulphuric
acid wh ich woul d occasion loss o f ferric ph osphate which is
, ,

soluble in that acid but insolubl e in acetic acid .

The precipitate is white or cream colored and very voluminous -

.

O n this account it is di fficult to wash When the quantity oper .

ated upon admits o f it the washing shoul d be e ff ected by m ixing

,

the precipitate with warm water in a tall vessel allowing it to ,

settle dra wing O ff the clear supernatant l iquid by means o f a

,

siphon and then trans ferring the magma to a wetted muslin

,

s trainer where it may be l eft to drain thoroughly

,
This operation .

is to be repeated i f necessary .
 I RON PH O S PH AT E .

S y r up f
o th e Ph os ph a te s f
o I r on, Q u i ni n e , an d S try c hni ne .

S oluble ferric p hosphate

Q uinine sulphate
S trychnine
Phosphoric acid
Gl y cerin
Water
S yrup .

Heat the soluble ferric phosphate with the water in a porcelain ,

capsule until it is dissolved Then a dd the phosphoric acid the

,
.
,

quinine sulphate and the strychnine and stir until solution is e f

, , ,

fe cte d . Filter t h e liquid into the gl y cerin contained in a grad ,

u a t e d bottl e add enough syrup to make up the volume to one l iter

,

and mix thoroughly L astly s t ra i n i f necessary

’

.
.
, ,

D e scri p t i on . clear pale green s y rup ; odorl ess ; of b itter

—
A ,
-
,

acid taste . The preparation shows a bluish flu orescence .

A m m ni o F e rri c
o -
Ci tr o P h os ph a t e
-
.

[ S oluble Phosphate o f I ron with Citrate o f A mmonium ] .

A dd the washed precipitated ferric phosphate obtai ned by the

formula given on p from 6 6 ml o f solution O f normal ferric
.

sulphate and 4 5 Gm o f sodium phosphate to 6 0 ml o f d i ammon ,

-

ium h y drogen citrate prepared by the formula given under the

head of A mmonium Citrate Heat the m ixture by means o f a .

water bath for three hours stirring occasionally taking care not
—
, ,

t o a l l ow the temperature to exceed 6 0

t C E va p o rate the solution °
.

to the consistence of syrup spread it on plates of glass and d rv

‘

, ,

it in scales .

N ot e s The ferric phosphate i s added in slight excess in order

.

to perfectly saturate the solution w ith it .

I f 6 0 ml o f solution o f di sodium h y drogen C itrate be used i n

- -

stead o f the citrate o f ammonium the product will be the Pharma ,

”
c op oei a l solubl e
“
phos p hate o f i ron .
 I RON PY RO PH O S PH A T E .
43 1

I R O N ( F E R R I C ) P Y R O PH O S PH A T E ; P R E CI PI T A T E D .

F ERR I PY R O P H O S P H A S P R A E C I PI T A T U S .

F 6 4 ( P20 7 )3 =7 4 6
S olution o f normal ferric sulphate 5 00 ml
S od ium pyrophosphate 3 2 0 Gm

D ilute the solution o f ferric sulphate with 3 500 ml O f water and ,

dissolve the pyrophosphate o f sodium in 40 0 0 ml o f hot water .

Filter the li quids Pou r the solution o f ferric sulphate slowly int o
. .

that o f the p y rophosphate stirring well Wash the precipitate

, .

with warm water on a wetted muslin strainer until the washings

are free from sulphate D ry the product by the aid o f g entl e
.

heat.

R e ac t i on . 2F e, S O, ) P, O 7 ) 3 -
6N a, SO

N ot e sThe solutions mu st be col d when m ixed and the iron

.
,

solution must be added very slowly to that of the sodium salt w ith ,

constant a n d br i s k stirring The precipitate is very light and

’
.

bulky and hence quite di fficult to wash

, .

D e scri pt i on white or cream colored

.
—
A -
,
odor les s and tastel ess
powder Insoluble in water S oluble in
. . dilute metaphosphor i c
acid but in s oluble in dilute or t hophosphoric acid [ D i ff erence from
.

the phosphate

I r on ( F e r ri c ) Py r oph os ph a te ; S ol u bl e .

F ERR I PY R O PH O S P H A S S OL U B I L I S .

[ S odio -
F erric Citro -
Pvrop h o s p h a t e .
]
Ferric citrate 5 parts
S odium pe p h o s p h a t e 5 parts

D issolve the citrate in 1 0 parts o f distilled water heated on a

water bath add the pyrophosphate and continue the heating with
-
, ,

constant stirring until the pyrophosphate of sodium is dissolved -

and the solution tu rn s green E vaporate at a temperature not .

exceeding 60 C ( 1 4 0 F ) until the solution has the consistence

°
.
°
.

o f thick s y rup ; spread it on glass plates and dry it in scales , .

43 2 I RON PY RO PH O S PH A T E .

N ot e s . S odium
citrate has been substituted for ammonium
citrate for the preparation o f pyrophosphate o f iron by the Phar
m a c op oe i a on the ground that the ammonio ferric salt became
,
—

insoluble through loss o f ammonia and because it either darkened ,

or becam e opaque by age The sodio ferric p e p h os p h a t e h ow .

—
,

ever is also liable to be come impaired by age an d exposure to

,

light The preparation is di ffi cult to scal e satis factorily I n small

. .

quantities it may be best scal ed in the cold Pe p h o s p h a te o f .

iron shoul d be carefully protected against light It is best pre .

served in amber colored bottles tightly corked and kept in a dry , , ,

cool dark place

, .

S ol u bl e f e r r i c py r oph os ph a te w i th a mm oni u m ci tr a te may be

prepared by adding the precipitated ferric pyrophosphate obtained
fr om 5 0 0 ml O f sol ution o f normal ferric sulphate and 3 2 0 Gm o f
sodium pyrophosphate to 4 60 ml o f the s oluti on o f di ammonium —

hydrogen citrate and digesting at n ot over 60 C for three hours °

.
,

o r until no more o f the ferric pyrophosphate dis s o lves The solu .

tion is then filtered evaporated and the preparation scaled

, ,
.

T hin transparent green scal es ; odorless ; taste a

D e scri pt i on .
—
, ,

l ittle acidulous slightly saline Freely soluble in water I nsol

, . .

ubl e in alcohol .

A n o th e r M e t h od .

[ A fter the S wis s Pharmacopoei a ]

S odium p y rophosphate
S olution o f ferric chloride ,
U . S . P
Citric aci d
A mmonia water ,

D istilled water o f each suffi cient,

.

D issolve the sodium pe p h o s p h a t e in 5 0 0 parts o f d istilled

water .

D ilute th e solution o f ferric chlori de with 80 0 parts o f distilled

vva t e r .

Pour the iron solution a l ittl e at a time into the solution o f

sodium pyrophosphate stirring uninterruptedly , .

Wash the precipitate thoroughly in the u sual w ay .

D i ssolve the citric acid in 5 0 parts o f distill ed water with

enough ammonia water to render the solution slightly alkal ine .
434 I RO N S A C C H ARA T E .

have redissolved be fore adding the next portion o f the alkal i Ca r ‘

bonate .

When finally all o f the sodium carbonate solution has been

added the precipitate i s to be washed by the a ffusion and decan
,

t a t i on o f distilled water until the washings when d iluted w ith 5 ,

volumes O f water no longer give a n y precipitate with silver n itrate

,

test solution but only ren dered opalescent by it

—
.

Trans fer the magma to a cloth strainer and let it drain E x .

press as much o f the water from the dra ined ma gma as practicable
by moderate pressure .

Put the still w e t sol id mass into a porcelain dish and add 50 0
parts o f sugar together with the solution o f sodium hydroxide
,

and mix well .

Heat the m i x t i1 re over a water bath until a cl ear solution is -

formed .

E vaporate the liquid by the water bath heat during constant ,

-
,

stirring to d ryness and powder the residue

, ,
.

A dd enough sugar to make the total weight o f the product 1 0 0 0

parts and reduce it to a medium fine powder .

N ot e s The product i s a water soluble ferric sodio saccharate

. .

1 4 5 parts o f crystalline ferric chloride may be u sed instead o f

2 3 0 parts o f the O fficial ( U S P ) solution . . . .

When the sodium carbonate solution is added to the solution of

ferric chloride e ff ervescence takes place from the C O l iberated ,

an d the precipitate at first formed consisting o f ferric h y droxide , ,

redissolves in the solution O f ferric chloride But when more than

‘

one hal f O f the sodium carbonate solution has been added and
-

much sodium Chlori de is accordingly contained in th e liquid the ,

precipitate formed afterwards redissolves no longer .

D e s cri p t i onred brown powder having a sweet and sli ghtly

—
. A -

ferruginous taste O ne part of it dissolved in 2 0 parts o f boiling

.

water forms a perfectly cl ear red brown solution having a feebly -

alkaline react i on It Contains from to 3 per cent of Fe

. .

A n oth e r M e t h od .

S o lution o f ferric Chloride

D istilled water cold ,

S ugar granulated
,

M ake a solution . .
 I RON S U B CAR B ONA T E .
435
'

A dd to thi s s ol u t i on ,
gradu all y and with constant stirring 400 ,

parts o f solution o f sodium hydroxi de o f 1 5 per cent stren gth .

L et the mixtu re stan d a few hou rs ( until it becomes clear ) .

Then add 5 0 0 0 parts o f boil ing water .

The precipitate which is now formed is then washed by the a f

f us ion and d ecantation o f distilled water until the washings have
but a feebly alkal ine reaction and begin to be colored .

Trans fer the well drained precipitate to a porcelain d ish and

-

add 900 parts o f powdered sugar mix well and dry the m i xture , ,

over a water bath stirrin g constantly A dd enough powder ed

-
,
.

sugar to the dry res idue to make the total weight o f the product
1 0 0 0 parts .

N ot e s It i s recommended that the diluted ferric chlori de solu

.

tion an d the sodium hydroxide solution shall both be c old whe n

m ixed The boi l i ng water afterward s added makes the precipitate
.

denser an d easier to wash When about one hal f o f the alkal i

.
-

solution has been added a precipitate i s form ed but thi s gradually ,

rediss olves as the remainder o f the alkal i is added and the liquid
becomes cl ear on s tand ing a few hours The boil ing water i s then .

added .

S accharated iron should make a clear solution in 5 parts o f

distilled water .

S i r u pu s F e rr i O x y d a ti

o f the German Pharmacopoeia i s a syrup made out o f equal pa rts

o f saccharated iron distilled water and simpl e syrup I t contains
, , .

or represents 1 p e r ce nt o f its weight o f Fe .

IR O N S U B CAR BO N ATE .

F ERR I S U B CA R B O N A S .

Ferrous sulphate 8 parts

S odium carbonate 9 pa rts

D issolve th esalts each in 4 0 parts o f boil ing water filter and

, , ,

pour th e solution o f i ron sulphate into that o f the sodium car

bonate with constant stirring Wash the precipitate with cold
,
.

water first by decantation an d a fterwards on a mu slin strainer

, .

until the washings c ease to b e precipitated by test solution of

43 6 I RON S U B CAR B ONA T E .

barium chloride . T hen drain and , d ry t h e ,

precipitate without
heat .

R e act i on . The ferrous

carbonate oxidizes as explained in the note , .

N ot e s TO
insure that the sod ium carbonate is in exces s over the
.

ferrous sulphate which is neces sary to insure complete double de

,

composition add the solution o f the iron salt to the solution o f

, .
‘

sodium carbonate The solutions should be hot in order that the

.

ferrous carbonate formed may be heavy and also to prevent the ,

formation o f solubl e bicarbonate When cold solutions are used .

a portion o f the precipitate which i s at first nearly white soon , ,

decomposes losin a po rtion o f its carbon ic acid which combines

,
g
,

with another portion o f ferrous carbonat e and hol ds it in solution

as bicarbonate A fter a time this too decomposes the carbonic
.
, , ,

acid being liberated and ferric hydroxide is formed by the ah

sorption of oxygen from the ai r When hot solutions a re used the .

carbonic acid is rapidly expelled and the perfect precipitation o f

the iron compound not retarded O wing to gradual oxidation the .

precipitate rap idly Changes color in contact with the air passing ,

through various shades o f gray green blue ol ive brown and , , , , ,

red The gray green blue an d ol ive are du e to ferroso ferric h y

.
, ,
-

d r ox i d e whil e the brown and red are caus ed by ferric hydroxide

,
.

Finally the precipitate becomes almost compl etely ferric D ried

,
.

at high heat the preparation is more red and les s readily solub l e ,

in hydrochloric acid .

The ferric hydroxide generall y rises to the surface o f the mixed

l iquids an d during the washing of the precipitate the surface o f
,

the magma becomes covered with it whil e the interior continues ,

bluish gray or gre en The washing i s best e ff ected with boiling

-
.

water and on a muslin filter The pores o f the fi l t e r paper be

,
.
-

come rapidly closed by yellowish red ferric hydroxide -

.

D ried at ordinary temperatures the preparation is olive brown -

with a reddi sh tint re taining a small amount o f ferrous carbonate

, ,

and i s easily powdered D ried with the aid o f considerable heat .

the produ ct is brown red and cakes together in hard lump s which —
, ,
.
are not so readil y powdered .

D e s cr i p t i on .
—
A red or brown red odorless tasteless insoluble-
, , ,

powder .
43 8 I RO N S UL PH AT E .

the cry stals as rapidly as poss ible and at once bottl e the product
in a dry container to be tightly closed .

N ot e s The crystal s must have a bluish green and not a yellow

.
-

i sh green color and they must be perfectly clear The ferric sul
-
,
.

phate and other ferric compounds contained in the green vitriol

a re removed partly by the boiling and filtration and partly in the ,

crystall ization when the ferric sulphate present remains in the

mother liquor .

Gr a n u l a t e d F e rr ou i S ul ph a t e .

Ferrous sulphate 1 00 Gm
Boiling distilled water 1 00 ml

D iluted sulp huric acid 5 ml

A lcohol 2 5 ml

D issolve the ferrous sulphate in the water add the acid and , ,

filter the solution whil e hot E vaporate at once in a tared por e e

.

lain dish over a sand bath until the weight o f the liquid i s reduced
-

t o I 5 0 Gm Then cool it quickly stirring uninterruptedly

,
.

Trans fer the liquid and crystals to a glas s funnel loosely stopped
with absorbent cotton and when the liquid has passed O ff pou r
, , ,

t h e alcohol over the mass o f crystals in the funnel When the .

alcohol has pas sed through trans fer the crystal s to bibulous
,

paper and d r y them quickly at the ordinary temperature and

trans fer the dry product at once to well stoppered bottles -
.

Pr e ci pi ta te d F e r r o us S u lph a te .

I ron wire
S ulphuric aci d
D istilled water
A lcohol
A dd the sulphuric acid gradually to the water st i rr i ng well ,
.

A dd the iron to the warm m ixtu re When e ff ervescence has

.

nearly ceased heat the mixture at the boil ing point for about ten
minutes Filter while hot A dd a small quantity o f sulphuric
. .

acid to t he filtrate Then pour the solution into the alcohol stir
.
,

ring constantly .

Collect the precipitated crystall ine ferrous sulphate on a filter ,

trans fer it to bibulous paper and d r y it quickl y at the ordinary

,
 I RON S UL PH A T E .
4 39

room temperatu re stirring th e c rystals o ften an d changing the

,

paper once or twice to facilitate rapid drying .

When thoroughly dry put the product in dry bottles to be well ,

corked or stoppered .

N ot e s I ron i s used in excess and the acid i s saturated with it

. .

Free sulphuric aci d i s a dded to the solution becaus e the salt crys
t a l l i z e s best from an aci d solution .

Ferrou s sulphate is insoluble in alcohol but ferric sulphate i s ,

soluble Hence any ferric sulphate present wil l remain in the

.

alcoholic liqui d .

The crystal s wet with alcohol instead o f water dry rapidly and
are moreover surrounded by an atmosphere o f alcohol vapor i n
stead O f air so that the p roces s o f dr y ing i s accomplished with far
,

less danger o f oxidation .

T u r bi d a te d F e r r ons S ul ph a t e .

Ferrous sulphate 1 00 parts

D istilled water 1 0 0 parts
D iluted sulphu ric aci d 5 parts
A lcoho l 2 5 parts

D issolve the ferrous sulphate in the water heated to the boiling ,

point add the ac id and filter the hot solution E vaporate the
, , .

filtrate in a tared porcelain dish over a sand bath until the weight -

o f the contents is reduced to 1 5 0 parts and then cool it quickly ,

stirrin g constantly Trans fer the wet salt mass to a glass funnel
.

the throat o f which i s loosely closed with a plug o f absorbent cot

ton and when th e product has well drained pour the alcohol upon
,

it When the alcohol has passed through it spread the crystall ine
.

salt upon bibulous paper dry it quickly at the ordinary tempera ,

ture and trans fer it at once to perfectly dry bottles and clos e these
,

tightly .

The product is a pale bluish green crystalline pow der I ts offi -

.

c i a l title ( U S
“ ”
P 1 8 90 ) i s Granulated Ferrous S ulphate
. . .
.
.

Ferrous sulphate forms large Clear t ransparent

D e scr i p t i on .
—
, , ,

bluish green crys tals or a crystall in e granular salt ; odorl ess ; tas t e
’

-
,

saline styptic ferruginous E fflor e s c e n t in d ry ai r O n exposure

, ,
. .

it becomes first whitish on the sur face then yellowish brownish or , ,

reddish from ferric compounds S olubl e in parts o f water a t .

and in part o f boiling water Insolubl e in alcohol . .

44 0 I RON S UL PH A T E .

I R O N ( F E R R OU S ) S U L PH A T E . DR I ED .

F ERR I S UL PH A S E X S I C CA T U S .

A pproximately F e H 5 0 5 22 1 7 0 .

Crystallized ferrous m on om e t a sulphate contains 6 molecule s —

o f water When moderately h eated it dissolves in its water o f

.

°
cr y stal lization ; between 3 3 C and 90 C the salt loses that water .
°
. .

A t 2 80 C partial decomposition o f t he sulphate is l iable to take

°
.

place .

In exs iccating ferrous sulphate liqu efaction o f th e salt by , , ,

solution in its water o f crystall ization must be avoided i f a l ight ,

colored product u noxidized an d free from hard particles is to be

, .

Obtained The ferrous sulphate should be pure ; an d granulated

.
,

precipitated or reduced to coarse powder I t m a y then be spread

,
.

out in a thin layer on paper and be placed in a drying room where

the temperature i s about 4 0 C The dr y ing may al so be e ff ected
°
.

by the heat o f the sun until thoroughl y e ffl ore s c e d or convert ed ,

into a white powder O ccasional stirring is requ ired S houl d

. .

the temperature exceed 5 0 C the salt partly dissolves in its water

°
.

o f crystallization and the l iqui d penetrates the paper D el f plates .

may be used instead o f paper or porcelain or iron dishes ,

.

I f the salt is allowed to become so hot as to dis solve in its water

o f cr y stallization it w ill oxidize more rapidly and becomes dis
, ,

colored A fter having e fflor e s c e d however it will no longer

.
, ,

liquefy even at water bath heat or higher temperatures

-
, .

I f water bath heat i s u sed in finishing the exsiccation several

-
,

days heating will be necessary to expel the last portions o f the

’

sixth molecul e o f water ; but an almost wh ite product m a y readily

be obtained amounting to about 6 4 to 6 5 per cent o f the cr y stal
,

li z e d salt without prolonging the heating over water bath

,
-

beyond a few hours the powder being well stirred during the
,

process
To get rid of th e remainder o f t h e water it is neces sar y to raise
the heat to about 1 2 0 to 1 5 0 C continuing the heat until the
° 0
.
,

product ceases to lose weight This prolonged exposure inevi .

tabl y resul t s in a dark colored product -

.

To avoid decomposition and discoloration the Pha rmacopoeia

no longer requires the product to be abs olute F e H S O but allows , 5 ,

some moisture in it .
442 I RO N S U B S UL PH A T E .

S ol u ti on o f B as i c F er r i c S u lph a te .

( M S olution
’
on s e l s .
)
A n aqueous solution containin g about per cent of
basic ferric sulphate o f varying chemical comp os ition con ,

s isting perhaps principally o f a compound repres ented by the

formula F The proportion o f iron compound
in the solution corresponds to about per cent of metallic iron .

It is prepared as follows :

Ferrous sulphate
S ulphuric acid ,

N itric acid ,

D istilled water each su fficient, , .

A dd the sulphuric acid gradually parts o f d istilled water to 1 0 0

in a roomy porcelain dish pou ring the acid slowly and in a thin
,

stream into the water stirring constantly with a glass rod Heat
,
.

the mixture to a temperature o f nearly 1 0 0 C ; add I 5 parts o f 0

.

n itric acid and mix well .

D ivide the coarsely powde red ferrous sulphate into four equal
portions and add t hese portions one at a time to the hot l iquid
, , , ,

waiting a fter each addition until e ff ervescence has nearly ceased .

When all the ferrous sulphate has been a dded an d has dis ,

solved add a few drops o f nitric acid a n d i f this causes a further

, , , '

evolution Of red fumes continu e to a d d more n itric acid a few ,

drops at a time until it no longer causes n itrous vapors to be

,

evolved .

Then boil the solution until it assumes a ruby red color and is -

free from nitrous odor .

L astly add enough distilled water to make the total product

weigh 200 parts .

Filter i f necessary .

Keep the product in g lass stoppered bottles in a moderately -

warm place ( not below 22 protected from light °

.

R e act i on .

1 2 F e H ,S O 5 6 H , O.
-
3 , S O,
H —
H
4 N O3

N ot e s . S ee the notes under th e title o f S olution o f Ferric

 I RO N T ER S UL PH A T E .
44 3

S ulphate .ote that the only di ff erence between the formulas

N
for the preparation o f solution o f normal ferric sulphate and the
solution o f basic ferric sulphate respectively is that about twice , ,

as much sulphuric aci d is employed in proportion to the ferrou s

s ulphate to make the normal ferric sulphate as i s prescribed for
makin g the subsulphate .

T he quantity o f ni t r i c a c i d prescribed is a l ittle scant .

S olution of bas ic ferric sulphate sometimes crystall izes and

forms a semi sol id whitish mass i f kept in a room t oo cold
-
,
. .

S hould thi s happen the mas s may be easily liquefied again by

,

warmin g it I f kept in a suffi ciently warm place as d irected it

.
, ,

does not crystallize .

This solution is also called solution o f subsulphate o f iron .

D e scri pt i on .
—
A
clear dark red brown l i quid ; almost Odorless ; -

taste strongly styptic acid S p w about ,

at 1 5
. . .
°

O n slowly mixin g 2 volumes of the solution with 1 volume o f

concentrated sulphuric acid in a beaker a semi solid white mass
, ,
-

w ill separate on standing ( di fference from te rs u lph a te ) .

I R O N ( FER R I C ) S UL PH A T E S O L U TI O N .

L I QUOR F ERR I T E R S U L PH A T I S .

( S olution of T e r s u l ph at e o f Iron ) .

A n aqueou s solution o f normal ferric sulphate

containing about per cent o f that salt correspondin g ,

about 8 per cent o f metallic iron .

Ferrous sulphate
S ulphuric aci d
N itric aci d
D istilled water each su ffi cient , ,
.

A dd the sulphuric acid gradually with constant sti rring to an d

2 00 mill iliters o f distill ed water in a capacious porcelain dish ;

heat the m ixture to 1 00 C ; then add 44 Gm o f nitric acid and

°
.
,

mix well .

D ivide the ferrous sulphate coarsely powdered into fou r equal , ,

portions and add these portion s one at a time to the hot liquid
, , , ,
44 4 I RO N T ER S U L PH A T E .

waiting a fter each addition until e ffervescence has nearly ceased .

When all the ferrous sulphate has been added an d has dissolved ,

add a few drops o f nitric acid and i f this caus es a fu rther e vol u , ,

tion o f red fumes continu e to add more nitric acid a few drops
, ,

at a time until it no longer causes red fumes to be evolved

, .

Then boil the solution until it assumes a reddish brown color -

and i s free from nitrous odor .

L astly add e n ou g h d i s t i l l e d water to make the whole product

'

weigh Gm F ilter i f necessar y .

,
.

R e acti on .

:
3F e, S O4 ) 3 + I I H ,O —
2N O .

N ot e s . The fe r fou s sulphate used m u s t be in clear crystals and '

dry ; or in other words it must be dry but not in any degree

, ,

e ffl o r e s c e d I f granulated precip itated or t u rbi d a t e d ferrou s sul

.
,

phate is used it need not be powdered at all .

The oxidation o f ferrous sulphate t o ferri c sulphate by nitric

acid takes place much below 1 0 0 C ( 2 1 2 Water bath °
.
°
-

heat is there fore su fficient for this purpose “ The process i s

, , ,

however hastened by the application o f a somewhat higher de

,

gree o f heat .

To oxidize all the ferrous sal t is not di fficult a su ffi cient amount ,

o f n itric aci d being used B ut the preparation must be free from

.

nitric acid when finished an d it is di fficult to expel the excess ,

which is almost alwa y s a dded in order to c omplete the Oxidation .

Hence gr eat care shou be taken not to us e more n itric acid than
,
‘

is necessary .

But the presence o f a trace o f nitric acid is l ess obj ectionable

in th is preparation than the presence o f ferrou s salt .

When the ferrous salt is being raised to ferric by means o f

the nitric and sulphuric acids a ver y dark brown or almost black ,
—

compound is formed by the ferric salt with the nitrogen oxide .

Hence the liquid grows nearl y black at times an d the evolution

of nitrous vapors is at the same time temporaril y arrested But .

when the heat i s then increased a sudden and copious evolution

“ ”
o f red fu mes results when the dark colored compound is de
composed and the l iqu id at once becomes lighter in color S hould
,
.

more ferrou s sulphate be added be fore that decomp os i tion has

taken place and while the solution i s still dark or should the ,
44 6 I RO N A L U M .

Heat the iron solutio nto the boil ing point ; add the ammonium
sulphate and when this has dissolved add the acid S tir well
, , , . .

S e t the m ixture as ide in a well covered vess el in a cool place for , ,

a day or t wo R emove the crystal s from the mother liquor wash

.
,

them h a s t i ly w i t h a little cold water dry them at once by press in g

‘

them gently between blotting paper and put them without delay , , ,

in a bottle which must be tightly stoppered and kept in a c ool

,

place .

The cr y stal s shoul d be clean w ell developed and o f a hand , ,

some violet color .

R e acti on .

Fe , S O, ) 3 + ( H 4N ) S04) 1 2H , O .

N ot e s The sulphuric acid is a dded because go od crystals are

.
,

best obtained when a slight excess of aci d is pres ent I f there .

is a deficiency o f acid the crystals will be brownish unclear or , ,

very pale .

The col or o f the crystal s o f i ron alum varies materially ; it is

sometimes bluish or purpl ish sometimes violet and sometimes , ,

a pale rose color Crystals which ar e purplish violet may become

.

almost devoi d o f color up on recrystall ization from a water solu -

tion u nl ess the soluti on is rendered decidedly acid by the addition

o f H S O4
, .

[ Crystal s o f common alum g row in a saturated soluti on o f iron

alum L arge clear well defined crystal s can thus be made which
.
~

, ,

have a colorles s center envel oped in a beauti fully col ored exterior .

This is an interesting e xperiment for students to mak e ]

D e scri pti on .
—
A
viol et colored salt resembl ing alum in crystal ,

line form insolubl e in alcoh ol readily soluble in water giving a

, , ,

brown solution .

R e cry s ta l l i z e d I r on A l um .

Iron alum when e ffl ore s c e d discolored or otherwise unsi g htly

, , , ,

may be recrystal lize d as follows :

I ron alum 1 00 parts
Water 3 0 0 parts
D iluted sulphuric acid 10 parts
D issolvethe salt in the acidified water with the ai d o f heat ,

filter the solution and cr y stallize in the usual w a y ,

.
 I RO N S U L P H ID E .
4 47

I R O N ( F E R R OU S ) S U L PH I D E .

F ERR I S U L PH I D U M .

F e S : 88 .

M etall ic iron in the form o f wi re filings , ,

turn ings or s craps 7 parts

'

S ulphur 4 part s

Heat together in an earthenware crucible until fused .

R e act i on . Fe + S z F eS .

D e s cr i pt i on
Heavy black lustreless Odorless pieces or
—
, , ,

masses readily sol ubl e in hydrochloric acid with copiou s e vol u

,

tion o f hydrogen sulphide .

I R O N TA N N AT E .

F ERR I TA N N A S .

S olut i onof ferric acetate

Tannic acid
D istilled water su fficient , .

M ix the solution o f acetate o f iron with 3 5 parts o f distilled

‘

water and dissolve the tannin in 7 5 parts o f d istilled water

,
.

Filter the liqu ids .

A dd the tannin solution slowly t o the iron solution stirring ,

constantly .

Wash the precipitate and dry it .

D e scri pt i on .
—
An odorless and tastel ess in soluble black powder ,
.

I R O N ( F E R R I C ) VA L ER A T E .

F ERR I V ALER I ANA S .

3 59 .

S odium valerate
S olution o f ferric chloride U S ,
.

D istilled water .

D issolve the sod ium val erat e in 60 parts o f dist il led wat er and
44 8 I RON VALERAT E .

filter M i x the solution O f ferric chloride with 1 00 parts o f dis

.

till ed water A dd the iron solution gradually to the solution o f

.

sodium valerate stirring well taking care to discontinue the a d

, ,

dition of ferric chloride as soon as it no longer causes precipitation .

Collect t h e precipitate on a filter and wash it qu ickly with col d

distilled water until the washings are tastel ess D r y the product .

on blotting paper frequently changed and without the aid o f heat .

Keep the product in small tightly clos ed bottles in a cool dark , ,

place .

R e a ct i on .

F e C13 + 3 N a C 5
H , O,
=F e C 5 H O ) 3 + 3 N a Cl
, , .

D e s cri p t i on .
—
A
brick red or redd ish brown powder having -
,

an odor o f val eric acid D ecompos ed by boilin g water S oluble

. .

in alcohol .

LEA D A C E T A T E .

PL U M B I A CE TA S .

( S ug ar o f L ead .
)

M ix the l itharge acid and water in a porcelain dish S tir w ell

,
. .

L et stand a day Then heat over a water b ath until the oxide
.
-

is dissolved Filter E vaporate until a pellicle forms an d then

. .
,

set aside to cool and cry stallize adding first i f n eces sar y a l ittl e , , ,

more acetic acid to impart to the solution a decidedly acid r e a c

tion Collect the cr y stals drain and d ry them i m m e d i a t e l v put
.
, ,

the produ ct in dry bottles clos e these tightly and keep them in , ,

a cool place .

R e a ct i o
n

N ot e s . acetic acid dissolves the lead oxide w ithout the

T he
ai d o f heat i f su fficient tim e is allowed But the solution is .
4 50 LEAD A CE T A T E .

tin g paper changing the paper several times and as soon as moist
, ,

until the salt is dry .

M oist lead acetate rapi dly absorbs carbonic acid from the air ,

i f exposed and forms insoluble carbonate The sur face o f the

, .

crystals becomes white when covered with carbonate .

T he salt al so easily loses water of crystallization .

L ead acetate must there fore be quite dry before it is bottl ed the ,

containers must be dry quite filled tightly closed and put in a

, , ,

cool p lace .

Pu r i fi ca ti on .

Co mmercial sugar o f lead may be purified by r e c r y s t a ll i z a

-

tion .

D issolve 60pa rts o f sugar O f lead in 8 0 parts o f hot di stilled

water add 1 part o f acetic acid filter the solution let it cool
, , , ,

and when cold collect the crystals E vaporate the mother liquor
, ,
.
—

to obtain further crops o f crystal s and continue this as long a s ,

a pure product i s obtained .

Collect and dry the product as indicated in the notes above .

D e scri p t i on Colorless clear crystal s o f a faintly acetous odor

—
.
, , ,

and sweetish astringent finally nauseou s metallic taste E f

, ,
.

fl or e s c e n t B ecomes whiti sh on exposu re to ai r both from loss

.

o f water o f crystallization and by the formation o f carbonate du e

to the absorption o f carbon dioxi de from the a ir .

S olubl e in parts o f water and in 2 1 parts o f alcohol at , ,

15
0
in 1 5 parts o f boiling water and in 1 part o f boiling alcohol
. .

A t 40 it loses its water o f crystallization which amounts t o

°
,

per cent ; but it loses a portion o f its water even at I 5 on °

exposure .

A solution o f 1 0 per cent stren gth i f made with distilled water ,

which has j ust been boil ed to expel air and carbon dioxide mu st ,

be almost i f not quite clear

R e cr ys ta l l i z e d L e a d A ce ta te .

1 00 parts
2 0 0 pa r ts

5 parts

D issolve
the sugar o f lead in the water by the aid o f heat ad d ,

the acetic acid mix well filter and set th e solution a side to
, , ,
 L EAD C AR B ONA T E .
45 1

crystallize at rest Collect and drain the cr y stal s press them

.
,

gently between cloths or bibulous paper dry rapidly in cold ai r , ,

and keep the pr od uct in tightly closed bottles .

T ur bi d a te d L e ad A ce ta te .

S ugar o f lead . .
30 parts
Boiling distill ed water 3 0 parts
A cetic acid 1 part

D issolve filter evaporate over a water bath to one hal f Cool

, ,
- -
.

the solution qu ickly stirring frequently Coll ect drain and dry
, .
, ,

the crystal s at the ordinary room temperature a s qu ickly as pos

s ible with the ai d o f bibulous white paper frequently changed ,
.

Put the product at once in dry bottles close these tightly and keep , ,

them in a cool place .

L EA D C A R B O N A T E .

PL U M B I C AR B ONA S .

Prepared by acting on sheet l ead with acetic acid moisture

and carbonic aci d gas until the lead is consumed or covered with
,

a thick coat o f w h i te l e a d which is then removed ground w ith

, ,

w ater washed an d dried O r carbonic oxide is conducted

,
.
,

through solution o f subacetate o f lead the precipitate being the ,

p roduct while the remaining liquor containing normal lead ace

,

tate is again conve rted i nto solution o f subacetate o f lea d by

maceration with l evigated litharge .

W hi te l e a d is a basic carbonate as may be s een from the ,

formula given above .

The same lead carbonate i s also obtained when lead n itrate or

n ormal lead acetate is decomposed by sodium carbonate :

L ead nitrate 10 parts

S odium carbonate 9 part s

D issolve the l ead nitrate and th e sodium carbonate each in 1 0 0

parts o f water and filter the solutions separately Pou r the lea d
,
.

salt solution into the sodium carbonate solution stirring con ,

s t a nt l y
.
Wash the precipitate with hot water ; coll ect and dry it .
 LEAD CAR B ONA T E .

R e acti on .

3 Pb

: 2 PbCO , . Pb ( O H )

D e scr i pt i heavy wh ite p owder inso lubl e

on .
—
A , ,

solubl e with effervescence in acetic or nitric acid .

tasteles s .

LEA D CH R O M A T E .

PL U M B I C H ROMA S .

Ch r om e Y e l l ow
( .
)
L ead nitrate
Potassium dichromate
Water .

D issolve the lead salt i n 3 5 parts o f hot water filter and d ilute , ,

the solution with 3 0 parts o f col d water .

D iss olve the dichromate in 3 5 parts o f hot water filter and , ,

d ilute this filtrate with 6 5 parts O f col d water .

A dd the dichromate solution gradually to the lead nitrate solu

tion stirring well
, .

Wash the precipitate by a ff usion and decantation o f water s e v

eral times until the washings are free from nitrate Collect the .

lead chromate on a muslin strainer let it drain pres s out the , ,

most o f the remainder o f the water with the ai d o f a screw pres s ,

break the pres s cake into pieces and dry it upon glass plates with
the aid o f moderate heat .

R e a ct i on .

2 Pb N O, ) —
K , Cr , O 7 -
H ,O

2 PbCr O ,

N ot e s There should be as nearly compl ete decomposition o f

.

both factors as possibl e Hence it i s advisabl e not to add all o f th e

dichr omate solution to the whole quantity o f the l ead salt at once .

R eserve instead a small portion o f t h e solution o f lead nitrate ;

, ,
4 54 LEA D I OD I DE .

finely divided product When hot liqui ds are used a portion o f

.

the iodide is held in solution until the liquid i s cold separating ,

gradually in crystalline scales .

L ead iodide l s also soluble in cold water and thus there is ,

always a slight loss which is increased by washing Hence the

,
.

quantity o f water u sed for wash ing the precipitate should be

limited and the washing should be per formed on a filter instead o f
,

by d e c a n ta t i on
_
.

Th e l ead acetate solution mu st be added to the solution o f the

iodi de for it is necessary to have the latter present in exces s until
,

the liquids are mixed S houl d the orde r o f m ixing be reversed

.
,

or sh ould the lead acetate be in excess oxyiodide of lead is ,

formed .

O n the other hand i f the potassium iodi de is in too great

,

excess after all the lead acetate has been added loss will be oc ,

c a s i on e d by the formation o f soluble doubl e salts o f the iod ides

o f lead and potassium .

Potassium acetate also dissolves lead iodide .

To obtain a larger yiel d lead nitrate is used instead o f acetat e

, ,

the lead iodide being almost insoluble in a solution of potassium

nitrate The formula is then as follows :
.

S e c ond M e th od .

L ead nitrate
Potassium iodide
Water su fficient
, .

D issolve the lead n itrate in 8 parts o f col d water and the ,

potassium iodide in 3 parts o f col d water Filter the sol utions . .

A dd the lead soluti on to the solution o f potassium iodide wit h ,

stirring D ecant the mother liquor and throw it away Collect

. .

t h e precipitate on a filter and wash it with col d water D ry it .

between bibulou s paper .

Cry st al l i zat i on
I f a cr y stall ine product i s desired dissolve the
.
,

washed and still w e t precipitate by boiling it with two hundred

times its weight o f water filter and let the solution cool very
, ,

slowly T h e l ead iodi de obtained from 1 0 Gm of lead nitrate

.

woul d requ i re nearl y three liters of boil ing water for its s olution .

To obtain a small quantity o f cr y stall ized lead iodide as a speci

men boil the precipitate with 2 00 times its weight of w ater filter
, ,
 L EA D N IT R A T E .

455

whi le hot and set the filtrate aside to cool slowly

, . The undis
solved portion should be reserved separately .

R e ac t i on . Pb N O 3 —
Ph l , .

D e s cri p t i on —
A
heavy bright y ellow powder ,
- °

odorless an d
tasteless S oluble in
.
parts o f water at 1 5 and in about
2 0 0 parts o f boiling water .

LEA D N I T R AT E .

PL U M B I N IT RA S .

Pb N O,

L ead oxide in fine powder ,

Nitric acid ( 68 70 )
Water
'

Heat the oxide acid a n d w a t e r together in a porcelain dish

,

until the Oxide h a s dissolved ; filter th e solution ; acidi fy it by

adding about 0 5 0 part o f nitric acid ; evaporate and crystallize
.
.

R e a c t i on . PbO + 2 H N O , : Pb N O 3 —
H ,O .

N ot e s . I f copper be present in the lea d oxide the solution o f

lead nitrate will be bluish instead o f colorless I ron woul d make .

it yellowish Copper may be removed by precipitation on metal

.

lic lea d as described in the notes under p l u m bi acetas Iron i s .

rem o ved by repeated recrystall izations .

Cl ear crystals cannot be obtained unles s the solution o f lead

n itrate i s decidedly acid ; hence a fter saturatin g the nitric acid,

w ith lead oxide a small quantity o f free n itric acid mus t be

,

added to the solution before it i s set aside to cr y stallize .

The solution must also be saturated only at the room tempera

ture and the c rystal s formed by spontaneous evaporation o f the
,

col d solution .

In the absence o f free n itric acid the crystal s Obtained w il l be

white or opaque ; al so when formed by cool ing hot solutions .

The mother l iquor shoul d be evaporated for more crystal s

-
.

Commercial impure lead nitrate may be purifi ed by reer vstal -

l i z a t i on from a water solution acidified with n itric acid any cop ,

per or iron present being first removed as already described .

45 6 L E AD N IT RA T E .

Colorless trans parent cr y stals odorless sweeti sh

D e s cr i p ti on .
—
, , , ,

astringent taste finall y metall ic S oluble in 2 parts o f w ater at

, .

I 5 an d in
°
part o f boiling water Insoluble in alcohol R e . .

a ction acid .

'

Crys ta ll iz e d L e a d N i tr a te .

Crude l ead nitrate 10 part s

Water 20 parts
D i luted nitric acid 3 part s

D iss olve th e l ead n itrate in the wat er by t h e aid o f heat add ,

the acid filter the hot solution and s et it asi de to crystallize

, , .

Collect drain an d dry th e crystals and keep the product in a

, , ,

tightl y closed bot t le .

N ot e s The crystal s shoul d be perfectly colorless an d trans

.

parent I f unclear o r whitish they shoul d be redissolved and re

.

crystallized from a water solution a cidified with nitric acid as -

before .

LEA D OLEA T E .

PL U M B I OLEA S .

Pb
L ead acetate 1 00 Gm
White castile soap in fine powder ,
1 65 Gm

D issolve the lead acetate in ten l iters o f water ; i f decidedly

milky add to it gradually enough acetic acid to render the solu
, , ,

tion clear being careful to avoi d adding an excess o f th e acid

,
.

D is solve the soap in 2 5 0 0 ml o f hot water and add this solution

, ,

slowly to that o f the lead acetate Boil the mixture rej ect the .
,

mother liquor wash the precipitated oleate twice with boiling

,

water using ten l iters each time S eparate the water from the
,
.

product .

R e ac t i on .

Pb Czfi s o ) + 2 N 3 C H z 2 1s ss oz

Pb ( C 1 8 H 3 3 O ) 2

N ot e s . Prepared in this manner the l ead oleate i s a hard brit ,

458 L EA D OX ID E .

nitra t e should first be powdered the heat gradually increased and , ,

the powder stirred .

S houl d the res idue be partly yellow and partly red as it al ways ,

will be i f not thoroughly stirred or m ixed it is tritu rated until ,

o f per fectly uni form color .

Pure lead oxide i s compl etely soluble in solution o f normal ace

tate o f lead .

L EA D P E R OX I D E .

PL U M B I PE R O X I D U M .

PbO , : 238 .
5 .

L ead nitrate
Chlorinated lime
Water .

D is solve the l ead salt in 3 0 parts o f hot water T riturate the .

chlorinated l ime well with 6 0 parts o f col d water and strain A dd .

.

the chlorinated lime sol ution in po rtions to the hot lead salt solu
tion in a dish stirring well When about one hal f o f the solution
,
.
-

o f chlorinated lime has been added heat the mixture until t h e ,

l ight colored precipitate tu rn s dark brown Then filter about -

.

1 0 ml o f the l iquid and test it by addin g a l ittle o f the chlorinated

lime solution and warm i ng .

I f a precip itate is fo rmed add more chlorinated l ime solution ,

to the mixture in th e dish Test again from tim e to time in the .

same w a y until no further precipitation i s caused by the Chlorin

ated l ime Then heat the m ixture nearly to the boil ing point
.
,

stirrin g well L et s ettle an d wash the precipitate with boiling

.
,

water by decantation until the washings are tasteless or free

, ,

from chloride or nitrate Collect and dry the peroxide

. .

R e acti on .

D e scrl pt i on .
—
A heavy dark brown insolubl e powde r
,
-
, .
 LEAD T AN NA T E .
4 59

LEA D T A N N A T E .

PL U M B I T A N N A TU M .

L ead acetate
Tannic acid
D istilled water su ffi cient , .

D is solvethe l ead acetate an d the tannic aci d each separately , , ,

in ten times its weight o f distilled water A dd enough O f the .

tannin solution to the lead solution to precipitate the lead in the

form o f tannate di scontinuing the addition o f the tann ic aci d
,

whenever it ceases to produce further precipitation .

Wash the precipitate w ith distilled water until the washings

no longer give an acid reaction on test paper -
.

D ry the product with the a id o f g entl e heat .

D e scri pt i on .
-
A grayish yellow -
,
Odorl ess ,
tasteles s insoluble
powder .

The substantive noun ta n n at u m is used instead o f tann as t o

indicate that the composition is indefinite ,
.

GL TCE R I T E OF TA N N A T E OF LEA D .

O ak bark in coars e powder

,
I 75 Gm
Glycerin 35 Gm
S olution O f subacetate o f lead su fficient ,
.

Water su fficient
, .

Boil the bark with two l iters o f water for fi fteen minutes .

S train. To the colature ad d gradually solution o f subacetate o f

lead so long as a precipitate c On t i n u e s to be formed Collect t h e .

precipitate on a wetted muslin strainer and wash it with water

until the washings are t a steless L et drain an d pres s the magma .
,

between bibulous paper until enough o f the moisture has been

removed from it to reduce its weight to 6 5 Gm M i x this whil e .

still moist with the gl y cerin .

LEA D P LA S T E R .

E M P LA S T RU M PL U M B I .

[ D iachylon Plaster ] .

0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0

0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
46 0 L EAD P LA S T ER .

M ix the lead oxide previously passed through a N O 8 0 sieve

, .
,

intimately with about one hal f o f th e olive oil by trituration -

, ,

and add the mixture to the remainder o f the oil contained in a

bright copper kettle o f a capacity equal to at least four times the
bulk O f the ingredients Then add 1 0 parts o f boiling water and .
,

boil the whole together over a fire constantly stirring with a , ,

wooden spatula until a small portion when droppe d into cold

, ,

water is found to be pliable and tenaciou s F rom time to time

,
.

add a little water to replace that lost by evaporation When the .

mixture in the kettl e has acquired a w h i t i s h color and is per ‘

f e c t l y h omogeneous trans fer it to a vessel containing warm

,

water and as soon as the mass has su fficiently cooled knead it

, ,

well with the wa ter so as to remove the glycerin renewing the ,

water from tim e to time as long as it may be necessary Finally ,

.

d ivide the mass into rolls o f suitable size .

D e scri pt i on .
—
A yellowish white tenacious plaster -
,
.

A n oth e r M e th od ( G P . .
)
0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0

0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0

0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0

M ix the oil and lard by melting them together A dd the lead .

oxide previously s ifted and then well mixed with 20 parts water .

Boil the m ixture stirring well and uninterruptedly w ith a wooden

,

spatula A dd from time to tim e about 3 parts of hot w ater to r e

.

place that lost by evaporation Continu e the boiling until the .

plaster is fo rmed and all red color has disappeared .

S e e also directions I n the method first described .

N ot e s . L ead plaster made with ol ive oil alone ( without lard )

i s so fter than that made with oli ve oil and lard because the ,

former plaster contains principal ly lead oleate with but l ittle

stear ate while the latter contains a greater proportion o f stearate
,
.

The const ituents o f the l ead plaster a r e oleate palmitate stearate , ,

and a ra c h a t e o f lead .

The lead oxide does not react readily with oil or fat except at a
very high temperature and in the presence o f water In the .

absence o f water a plaster can be made but onl y at so high a

4 6 2 LEAD S U B A CE T A T E .

equivalent to about per cent o f which is

the composition assigned to th e basic lead acetate contained in
this solution by the definition g iven in the A merican Pharma
c op oei a
]

L ead acetate
L ead oxide in fine powder
,

D istilled water .

Heat 7 0 parts o f distilled w a t e r t o boiling D issolve the lead .

acetate in the hot water Trans fer the solution to a bottl e A dd

.
.

the prev i ously si fted lead oxide in small portions shaking well
, ,

an d frequently a fter each addition t o prevent the oxide from

caking toget h er an d waiting a fter each addition until th e portion
,

adde d has been dissolved before adding another portion When .

all o f the lead oxide has been added and dissolved add enough ,

distill ed water to make the total product weigh 1 00 parts and ,

filter the solution through paper in a well covered funnel .

Keep the product in well stoppered bottles —

.

R e a ct i on .

+ 2H , O .

N ot e s . The lead acetate must be in good condit i on i e in —

. .
,

transparent cr y stals conta i n i ng the full amount o f water o f crys

t a ll i za t i on and free from carbonate The l ead oxide al so must be
.

free from carbonate and from minium an d other impurities U n .

less these conditions are observed the solution can not have the
required strength for l ead carbonate and m in ium are not soluble
,

in a solution o f lead acetate For the same reason the distilled

.

water should be boiled to expel carbon dioxide A fter making the .

sol ution o f l ead acetate with the hot water it i s not neces sary to ,

longer maintain the high temperature It i s u sually directed that

.

the solution o f acetate be boiled with the oxide ; but the lead oxide
d issolves as well even in a cold solution .

S everal basic l ead acetates are known di ff ering as to their sol

,

u bili t y as
yve l l as their percentage o f lead A ll are prepared by.

dissolving l ead oxide i n a solution o f l ead acetate the onl y di f ,

ference being the proportion o f oxide added D i fferent pha rma .

c op oe i a s moreover prescribe di ff erent proportion s o f water

, ,
The .

strength o f the soluti on obtained can not be reliabl y determined

 L EAD S U B A CE T A T E .
46 3

from the proportions o f the materials but will always be les s than ,

theory indicates for there is always an undissolved white po wder

,

remaining which cons ists O f carbonate

,
.

The molecular weights o f lead acetate and l ead oxi de

and are in the proportion o f I 7 to 1 0 ; parts o f lead
acetate and parts o f lead oxide form 5 6 5 parts of
which woul d make 2 2 6 0 parts o f solution o f 2 5
per cent strength ( that is 2 5 per cent o f ,
having
the molecular weight The exact quantity o f s olution
which shoul d be obtained from 1 7 parts o f lead acetate and 1 0
parts o f lead oxide woul d be 1 0 2 parts But only 10 0 parts o f .

solution are d irected to be prepared from 1 7 parts o f ace tate and

1 0 parts o f oxide
.
With such approximately pure material s as
.

may be obtained without any di ffi culty a product containing full y ,

2 5 per cent o f H O PbC, H , O 2 [ or re

s u l t s from the formula given .

The proportions ordered by the B ritish Pharmacopoeia a re 2 50

Gm o f lead acetate and 1 7 5 Gm o f l ead oxide to make ml
o f prod uct ( or Gm ) .

The Germa n Pharmacop oeia orders 3 parts o f lead acetate I ,

part o f lead oxide and 1 0 parts o f water

, .

The Pharmacopoeia o f N orway prescribes 1 7 parts o f lead ace

tate 5 parts o f lead oxid e and 7 8 parts o f water
, , .

Bottles containing solution o f subacetate o f lea d soon becom e

coated with lead carbonate which forms a white crust on their ,

s ides Thi s white crust i s most readily removed by n itric acid

. .

The preparation becomes whitish on dilution with water con

tainin g carbonic acid sulphates etc an d can be d iluted so as
, ,
.
,

to form a cl ear l iquid only with distilled water .

D e s cri p ti on .
—
A colorless solution with a sweetish taste and
alkaline reaction . S p gr about
. .

Gly c e r i te o f S u ba c e ta t e o f L e ad .

GL Y C E R I T U M PL U M B I S U B A CE T A T I S .

L ead acetate
L ead oxide in fine powder,

Glycerin
D istilled water
 6
4 4 L EAD S U B A CE T A T E .

M ix in a porcelain dish and boil the m ixture fi fteen minutes .

Filter and evaporate the filtrate to ml .

N ot e s This Solution will bea r dilution with distilled water

.
,

yielding a cl ear l iqu id It has about the same strength a s the

.

o fficial sol ution o f subacetate o f lead .

D il u te d S ol u ti on o f L ead S u ba c e ta te .

L I QUOR PL U M B I S U B A CE T A T I S D I LU T U S ; U . S .

A
( q u a S a t u r n i . L e ad Wa t e r ) .

M ix 3 0
ml o f solution o f l ead subacetate with 9 7 0 ml o f distilled
water previously boiled an d allowed to cool again
, .

LI TH I U M B E N Z OA T E .

LI TH I I B E N Z OA S .

L i C7 H 5 O , : 1 28 .

L ithium carbonate
Distilled water
Benzoic acid

Put the l ith ium carbonate and water into a porcelain dish placed
over a water bath warm gentl y and add the benzoic aci d gradu
-
, ,

ally When solution has been e ff ected filter the l iquid and e va p or
.

ate the filtrate until a moist crystalline mas s remains D ry the .

°
mass at a temperature o f about 3 0 C .

R e act i on .

—
CO , .

D e s cr i p ti onwhite cr y stall ine salt either Odorless or o f a

—
A ,

fa int benzoin odor an d cooling sweetish taste S oluble in 4 parts

,
.

°
o f water at 1 5 C and i n 1 2 parts o f alcohol ; and in
. parts
boiling water .
 466 L ITHI UM C IT RA T E .

toward the close o f the evaporation so as to Obtain a granulated

product .

D e scri pti on .
—
A
white granular powder ; odorless ; taste saline
, .

. R eadily soluble in water and in alcohol N eutral in reaction . .

L ITH I U M CIT R A T E .

'
LI TH I I C IT RA S .

L ithium carbonate
Citric aci d
D istilled water

D issolve ,
filter and evaporate to crystallization or until a gra n
, ,

ular salt remains D ry the product with the aid o f g entle heat
. .

Keep it in tightly closed bottles .

R eact i on .
— H
5 ,O

D e scri pt i on A
white c rystall ine or granular powder ; odorl ess ;
—
.

taste faintly alkaline cooling Hygroscopic in moist ai r S oluble

,
. .

in 2 parts o f water at and in one hal f its weight o f boiling -

w ater Insolubl e in alcohol and in ether

. .

E ff e rve s c e n t L i th i u m Ci tr a te .

L ithium carbonate
S odium bicarbonate
Citric acid
S ugar in fine powder a suffi cient quantity
, ,
.

T riturate the citric aci d with about 2 00 Gm o f sugar an d dry ,

the m i xture thoroughly Then incorporate w ith it by tritu ration

.
, ,

the lithiu m carbonate and sodium bicarbonate an d enough sugar ,

to make the product weigh I ooo Gm .

It may be granulated in the same w ay as e ff ervescent magnes

ium citrate .

Keep the powder in we ll stoppered bottles

’

-
.
 L ITHI U M I OD I DE .
46 7

D e s cri pt i on .
—
A
white coarsely granular powder readily sol
, ,

ubl e in water with e ff ervescence forming an aci dulous solution

, , .

LI TH I U M IOD ID E .

L I TH I I I OD I D U M .

L iI : 1 33 .
5 .

Prepared by doubl e decompos ition between calcium iodi de and

lithium carbonate which are heated together in water Ca I ,
,
.

L i CO ,
,
:2L i I Ca CO , It may also be made from iron iodine
— .
,

and l ithium carbonate in a manner similar to the process for pre

,

parin g l ithium bromide from iron bromine and l ithium carbonate ,

.

The solution is evaporated to dryness .

D e s cri pt i on .
—
A
white granula r salt ; odorless ; taste acrid bit ,

teris h ; del iquescent Freely solubl e in water alcohol and ether

.
, ,
.

LI THI U M PH O S PH A T E .

LI TH I I P H OS P H A S .

L i , H PO , _
—
_
I O3 .

L ithium chloride
S odium phosphate
Water .

D issolve the salts each in 1 5 0 parts o f water filter the solutions

, , ,

and pour the lithium chlori de solution into the other stirring well ,
.

Collect the precipitate on a filter and wash it with col d water .

R e act i on .

D e scri p ti on .
—
An insol uble white powder odorles s an d taste ,

less .

LIT H I U M S AL I C Y LA T E .

LI TH I I S A L I CY L A S .

L i C7 H 5 O , : 1 44 .

S al ic y lic
acid 75 parts
L ithium carbonate ,
0

D istill ed water o f each ,

s u ffi CI e n t .
46 8 L ITHI U M S AL I CY LA T E .

M ix the salic y l ic acid with 2 0 0 parts o f distilled water in a

porcelain dish an d heat gently over a water bath A dd the -
.

lithium carbonate gradually stirring well until the solution ob , ,

t a i n e d is n e a r ly neutral ized ( or bu t f e e bl v though distinctly aci d , ,

in reaction ) Filter the solution an d evaporate it to drynes s stir

.
, ,

ring constantly .

Keep i t in well stoppered bottles -

.

R e act i on .
-
CO , .

N ot e s . The quantity o f lithium carbonate required for 7 5 parts

o f sal icyl ic acid is about 2 0 parts The acid shoul d not be com .

p l e t e l y neutralized w ith l ith ium carbonate ; still less should the

solution be m a d e a t all alkaline for the salt would then soon be
~

come discolored The filter paper used must be white filter paper
.
,

entirely free from i ron ; otherwise the product will be reddish .

D e s cri p t i on white odorless powder having a sweetish

—
A , , ,

somewhat disagreeabl e taste D el iquescent on exposure . .

R eadily soluble i n water and in alcohol Its water solution .

-

sh oul d have a slightly acid reaction on litmus paper .

M A G N E S I U M A C E TA T E .

M A GN E S I I A CE T A S .

M agnesium carbonate 40 pa rts

A cetic acid 1 3 7 parts

D iss olve the carbonate in the acid with the usual precautions ,

to prevent overflowing on account o f the e ff ervescence Heat .

the liquid to expel carbon dioxide Filter E vaporate to drynes s . . .

D e s cri pt i on white amorphous gummy deliquescent salt

.
—
A , , ,
.

Freel y solubl e in water an d in alcohol .

M ust be kept in tightl y closed bottles .

f S ol u ti on o M ag n e s i u m A c e ta t e .

T his solution i s said to be an effective antiseptic :

A cetic acid
M agnesium carbonate
D istilled water su fficient ,
.
47 0 M A G NE S I U M C AR B O NA T E .

These di ff erences depend upon the methods employed in the

preparation o f the products The workin g formulas given in the .

B ritish Pharmacopoeia are as f ollows

L igh t M ag n e s i u m Car bona te .

M agnes i um sulphate 25 parts

S odium carbonate

each salt in 2 00 parts o f Cold distilled water filter and

D is solve , ,

mix the solutions c old Boil th e mixture i n a porcelain dish for

.

fi fteen m inutes T rans fer the precipitate to a wetted muslin

.

strainer and wash it with boiling distilled water until the wash
,

ings ceas e to give a precipitate with test solution o f barium

chlori de T hen l et the precipitate drain and dry it at not over
.
,
°
1 00 C .

H e a vy M ag n e s i u m Car bon a te .

M agnes ium sulphate 25 parts

S odium carbonate 3 0 parts

D issolve the salts each in 5 0 parts o f boil ing distilled water ;

,

filter an d mix th e two s olutions whil e h ot E vaporate the m ix

,
.

ture on a sand bath to per fect dryness D igest the residue for
-
.
'

hal f an hou r with 1 0 0 parts o f boil ing water collect the precipitate ,

on a wetted muslin strainer and wash it repeatedly with distilled

,

water until the Washings ceas e to give a prec ipitate with test solu
tion o f barium chloride D rain the product and d ry it at not over
.

°
1 00 C .

R e act i on .
4M gS O ,
—
4N a , CO , —
H
5 , O =
; O r perhaps 5 M g S O

+ CO , .

N ot e sIt will be seen that the d i ff erences in manipulati on are

.

the use o f more dilute and col d solution s in making the light
magnesiu m carbonate and the p recipitate is in that case s imply
,

heated for fi fteen minutes with the mother l iquor ; while in mak ,

ing the heavy magnesium carbonate the sol utions are four times ,

as concentrated and mixed while hot the m ixture being then

, ,
 M A G NE S I U M C AR B O NA T E .
47 1

evaporated to perfect dryness on a sand bath a fter which the -

,

residue is freed from sodium sulphate by di g estion and subsequent

washing with boiling water .

When the precipitate is form ed with col d sol utions it contains ,

rather less magnes ium than i f prepared with hot solutions When .

boiled in the liqu id for a short time carbo nic acid passes away ; in
preparing the light magnesium carbonate the heating shoul d be
d iscontinued a s soon as the evolution o f carbonic acid has com
m e n c e d When formed with hot concentrated solutions the m ix
.
, ,

ture being boiled down to dryness the precipitate contains l es s ,

carbonic acid when formed and loses more o f that acid a fterwards
,

when exposed to the stronger heat .

Comp os i t i on F r i t z s c h e Hager and Fluckiger state that the

.
,

composition o f m a gn e s i u m carbonate is
-
4H , O 2
.

the U S P g i ve s i t a s
. . . . the B ritish
-

Pharmacopoeia states it as being That

there is a difference in compos ition between light and heavy mag
n e s i u m carbonate may be regarded a s certain although the same ,

formula is given by the B ritish Pharmacopoeia for both L ight .

magnesium carbonate contains a greater proportion o f true carbon

ate ( M g CO ) and a correspondingly less proportion o f hydroxide
,

The quantity o f water in the product seem s also

to var y ,

D e scri p ti on .
—
L ight white friable masses or a light white
, , , ,

powder ; Odorless ; produces a sl ightly earthy feel in th e mouth .

Practically insoluble in pure water although it imparts to it a ,

slightly alkalin e reaction Insoluble in alcohol . .

The foregoing description appl ies to the l ight variety T he .

heavy carbonate is a powder only one third as bulky -

.

M A G N E S I U M CH L O R I D E ; C R U D E .

M A GN E S I I C H L OR I D U M CR U D U M .

M agn es ite in powder ,

Hydrochloric aci d ( 3 2 % o f H Cl )
M agnesium oxi de
Water
47 22 M A G NE S I U M C H LOR I DE .

M ix the magnesite with the water in a large porcelain dish ; ,

heat to about and add the acid in small portions at a time ,

stirring well and allowing the e ff ervescence to subside a fter each

addition be fore adding more When all o f the aci d has been .

a dded heat the liqu id to 90 for a few minutes N e u t ra l i z e per

°
.

f e c t l y with magn es ia A dd 5 0 parts o f water and m ix well Then

. .

add 5 parts o f chlorine water sti r well and keep the mi xture hot , ,

for about one hour Filter while hot E vaporate the filtrate until
. .

it h a s about sp w while still hot Then allo w it to cool

. . . .

Collect and drain the crystal s .

R e act i on . M g CO 3 + 2 H Cl Cl
g ,

N ot e s . The pr oduct contains some calcium chloride because

the magnesite contains calcium carbonate The solution o f m ag .

n e s i u m chloride shoul d not be allowed to boi l as the salt w oul d ,

then be l iabl e to decompose to some extent .

D es cr i p t i on
Colorles s deliquescent crystals soluble in l ess
—
, ,

than two third s o f their own weight o f cold water

-
.

Pu r e M ag n e s i u m Chl or i d e .

M ay be prepared by saturating pure hydr ochloric acid with

pu re magnes ium carbonate filtering the solution and evaporating
,

to crystallization .

M A GN E S I U M CI T R A T E .

M A GN E S I I C IT RA S .

M ei ( 6 50 7 ) e
C H aq .

I n the S wedish Pharmacopoeia occurs a magnesium citrate O f

the formul a indicated but mixed with an excess o f citr i c acid
,

amounting to about 9 per cent It is prepared as follows .

M agnesium carbonate in powder ,

Citri c aci d in fine powder

,
.

A lcohol
M ix the magnesium carbonate an d acid intimately by tritura
tion in a mortar and add the alcohol mixing the whole well s o
, ,
4 74 M A G NE S I U M C ITR A T E .

citrate contains 7 molecules o f water and requires 1 0 0 part s o f ,

water for its sol ution T he amorphous variety when in watery

.

solution gradually changes to the crystalline f orm passing

,
,

through the metamorphous form this alteration bein g u sually ,

compl eted in from three to five days .

The chan g es referred to are at l east partially prevented by the , ,

presence o f alkal i citrates -

.

E ff e r v e s c e n t M ag n e s i nm Ci tr a te .

M agn es ium carbonate

Citric acid
S odium bicarbonate
S ugar in fine powder
,

A lcohol ,

D istilled water .

M ix the magnesium carbonate intimately with 3 0 Gm o f c itric

aci d an d 4 m l o f distilled water s o as to form a thick paste D r y , .

this at a temperature not exceeding 3 0 C and reduce it to a fi ne °

.

powd e r Then mix it intimately with the sugar the sodium bi

.
,

carbonate and the remainder o f the citr i c acid previously reduced

,

to a very fine powder D ampen the powder with a suffi cient quan
.

tity o f alcohol so as to form a mass and rub it through a N o 6

, , .

tinned i ron S ieve Then dry it and reduce it to a coarse g ranular

-
.
, ,
'

powder .

Keep the product in well closed vessel s -

.

N ot e s By reference to the preceding notes under the title

.

M agnesium Citrate it will be seen that the first part o f the process ‘

has for its obj ect the formation o f acid magnes ium citrate .

This is then dried powdered an d mixed with powdered sugar

, , ,

sodium bicarbonate and citric acid The citric aci d must be finely .

powdered I t i s neces sary that these ingredients shoul d be very

.

thoroughly mixed before the alcohol i s added and onl y enough ,

alcohol to dampen the mixture should be u sed The small amount .

o f water contained in th e normal magn esium citrate and in the

alcohol i s su fficient to cement the particles o f powder together
into l ittle granules and the coarse powder is run through a N o
,
.

6 siev e t o make it more uni form A s a brass sieve would be a t .

tacked by the compound a tinned iron s ieve i s directed to be em,

ployed The sodium bicarbonate is not decomposed by the citric

.
 M A G NE S I U M C IT RA T E .
47 5

acid in the dry mixture and hence the preparatio n when dissolved
, , ,

in water y ields an e ffervescing drink

, .

D e scri p t i on .
—
A
white coarsely granular mixtu re del iquescent , ,

on exposure to air inodorous having a m il dly acidulous taste and , ,

aci d reaction S oluble with copious e ffer vescence in two parts

.
, ,

o f water nearly insoluble in alcohol The aqueous solution con .

tains sodium magnes i um citrate som e free carbon ic acid citric

-
, ,

a cid and sugar

, .

S ol u ti on f
o M ag n e s i u m Ci tr a te .

Contains M g H C6 H 5 O 7 .

M
agnes ium carbonate
Citric aci d
S yrup o f citric acid
Potassium bicarbonate

D issolve the citric acid in 1 2 0 ml o f water add the ma gn es ium ,

carbonate and stir until dissolved Filter th e solution into a

,
,
.

stron g bottl e o f the capacity o f 3 60 ml and contain ing the syrup , .

Then add enough water previously boiled and filtered to nearly , ,

fill the bottl e d rop into it the potassium bicarbonate and imme
, ,

d i a t e l y insert the cork s ecuring it with twine L astly shake the

, .
,

mixture occa sionally until the potassium bicarbonate i s di ssolved .

R e a cti on . M
4 g CO 3
M g( O H .
) H C H O
+5 3 6 5 7 2 M
5 g H C6
H 5
07

+ 6 H 20 + 4 C0 2 .

N ot e s . A c id magnesium citrate which i s contained in this prep ,

aration does not yiel d any deposit o f magnes ium salt such as i s
“

formed a fter about three days in solutions o f normal ma gnesium

citrate A s calcium citrate is insolubl e in water the magnesium
.
,

carbonate and the water used ought perhaps to be free from lime .

A cid calcium citrate is however solubl e to a limited extent It , , .

i s d irected in the P harmacopoeial working formula that the water

“ ”
added la st shall b e previously boiled and filtered A s this pre .

caution has for its obj ect the removal o f a n y lime present the ,

same treatment shoul d be applied to the whol e o f the water u sed ,

i f it be intended that the preparation shall be free fr om calcium

salt for all o f the calcium citrate formed from the calcium car
,
47 6 M A G NE S I U M C IT RA T E .

bonate present in the water will dissolve in the excess o f citric

“ ”
acid used unless the water employed is qu ite hard in which
, ,

case it is unfit for use .

The water as well as all other ma t erials u sed S houl d be perfectly

pure Impure materials lead to the formation sooner or ater
.
1
, ,

o f slimy deposits in the product .

Heat materially hastens the solution of the acid and the mag
n e s i u m carbonate an d with the qu antity o f citric acid taken no
,

harm will result i f th e water in which th e acid i s dissolved be hot ,

and th e heat continued until the magnesium carbonate h a s dis

solved The sol ution shoul d then be filtered and all owed to be
.
,

come q uite c ol d before th e other ingredients are added The cl ear ’

syrup should be first put in the bottle ; then the filtered acid solu
tion o f magnesium citrate care fully added so as not to mix it w ith
the layer o f syrup covering the bottom o f the bottle ; then the
bottl e shoul d be n e a r ly filled With water and the potassium bicar ,

bonate in large clear cr y stals dropped in a fter which the cork

, , , ,

is at on c e d r i ve n into the n e c k o f t h e bottle

'

.
.

The bottles used for thi s preparation are made strong enoug h
to bea r the pressure caused by the car bonic aci d liberated from
the potassium bicarbonate by the citric acid They must n e c e s .

s a r i l y be o f S uch size as to be nearly fill ed by the solution when

fin ished and o f proper strength The corks used must be about .

I % inches long and o f the finest qual ity as large as the y can pos
, ,

s i bl y be used and soaked in hot water s o as t o be so ft an d elastic

,

when inserted ; t h e soaked corks ought to be fitted t o the n ecks of

the bottles when the latter have been cleaned but while still empty , ,

and shoul d be so large that after u sing the cork presser they , ,

can be driven in by one or two smart blows with a mallet cl osing ,

the bottles perfectl y The wire or twine used to tie the corks down
.
-

securely must be properl y attached to the necks o f the bottles be

forehand leaving a loop on one S ide long enough to reach to the
,

center o f the top of the cork and the two ends on the opposite s ide
, ,

so that as soon as the cork has been driven in rather more than
one hal f its l ength it can be at once tied ove r
-
,
.

The quantit y of potas siu m bicarbonate u sed h as been a dvan

t a g e ou s l y i nc reased to Gm so that the solution may be well ,

charged with carbonic aci d The bottl es shoul d be laid on their

.

S ides in a cool place taking care not to S hake the contents so as

,

to mix the syrup with the l ighter w atery solution The potassium .
 47 8 M A G NE S I U M O X ID E .

and then dropped into diluted sulphuric acid gives but a ve ry ,

slight e ff ervescence .

R e act i on . when strongly heated

i s decomposed into 5 M g O + 6 H 2O + 4 CO z .

N ot e s The magnesium carbonate being very li ght a g reat dea l

.

of it ris es from the dish l ike dust and i s scattered about .

In O perating upon larger quantities a bright clean i ron pot ,

may be u sed placed immediately over the fire and heated gradually
,

to dull redness .

I f heated too strongly or too long th e magnesia becomes de a d

burnt s o that it does not b ecome hydrated and form a g elat
” “ ”

i n ou s mass o f hydr oxide when m ixed with water This failure o f .

the oxide to react with water results whenever the carbonate is

heated until all o f it i s completely decomposed so that no e ff e rve s
cence whatever occurs when the product is tested with diluted
sulphuric acid O n the other hand the product may i f not heated
.
, ,

long enough contain much basic anhydrous carbonate although

‘

it gelatinizes with water ; in such a case it does not retain the

property o f becoming converted into gelatinous hydroxide A .

s l i g h t e ff ervescence with diluted sulphuric acid 1 5 therefore allow , ,

able but considerable e ff ervescence with diluted acid shoul d con

,

d e m n the product .

M agnesium oxide may als o be made in a crucible packed nearly ,

full o f magn es ium carbonate with the ai d o f a pestle the crucibl e ,

being covered and heated in an oven or furnace first moderately ,

and finally to dull redness for about an hour a fter which the con ,

tents may be tested and then heated again i f necessary B ut this

,
.

procedure is more ri sky as the product is very liabl e t o become

,

”
dead burnt in this w ay s ince it can not be so frequently tested
-
,
.

'
to prevent it .

M agnesia must be kept in small filled tightly c orked bottl es , ,

-
,

the corks dipped in melted para ffin to e ff ectively exclude air so as

to prevent the absorption o f CO and the consequent formation o f 2

carbonate Containers capable o f holding about 5 0 Gm o f mag

.

n e s i a are p e rhaps the most su itabl e in size .

Te st When I Gm of magn esia

. light ma gnesia is thor
oughly stirred with 1 5 ml o f water in a beaker and the mixture
allowed to stand in the beaker for an hour a semi translucent ,
-
 M A G NE S I U M OX ID E .
4 79

gelatinous mas s o f magnesium hydr oxide S houl d be formed which ,

is firm enough to remain in the beaker when the latter is inverted .

A magnes ia which do es not poss ess the qual ity to thus form
h ydroxide is not to be used medicinally being in ferior , .

D e s cri pt i on white very light and extremely fine powder ;

.
—
A ,

Odorless and tastel ess but producing in the mouth the s ensation
,

u sually produced by dry absorbent tasteless earthy S ubstances

, , , .

I nsoluble in alcohol and practically insoluble in water although

, ,

when moistened it exhibits a slightly alkal ine reaction on litmus

paper .

L ight magnesia is about three times as bulky weight for ,

wei g ht as heavy magnesia

,
“ ”
.

H e a vy M ag n e s i a .

M A G NE S I A P ONDERO S A .

( H eavy M agnesium O xide ) .

M g O : 4o . 2 .

A white very fine powder about three times as dense a s the

, ,

light magnesia but otherwise o f similar physical properti es It

,
.

al so con forms to the reactions and tests given by the Pha rmaco
“ ”
p oe i a for M agn esia but does not,
form a gelatinous hydro x ide
with water or does so only with great di fficulty
,
.

M A GN E S I UM S AL I C Y L A T E .

M A GN E S I I S A L I CY L A S .

M g ( C7 H 5 0 3 ) 2 4 H 20 °
2
37 0 2 ° °

S al ic y lic
aci d
D istilled w ater
M a gn esium carbonate su fficient , .

M ix the sal icylic acid and distilled water in a large porcelain

dish and heat the mixture over a water bath A dd 5 part s o f -
.

magnesium carbonate to the hot liquid sti r wel l an d continue , ,

heating until e ffervescence ceases .

Test a filtered portion o f the l iqu id on litmus paper and i f the ,

 M A G NE S I U M S AL I CY LA T E

reaction i s acid add more magnesium carbonate enough to render ,

the reaction o f the liquid almost entirely neutral .

When the l iquid S hall be almost or quite neutral to test paper -

,

l et it cool filter and then add enough salicyl ic aci d to render the
, ,

reaction distinctly acid .

Filter again and evaporate to crystallization

, .

N ot e s .In order to obtain a product which will keep well and

produce a clear solution with water it i s necessary to render the ,

liqu id aci d from an exces s O f salicylic acid before evaporatin g to

crystall ization .

The magnes ium carbonate employed shoul d be free from iron i n

order to insure a perfec tly colorl ess product .

A s a supersaturated solution may be easily formed it is n e ce s

sary to determine th e right degree o f con centration o f the li quid
by repeated trials during the process o f evaporation .

The fine crystalline powder deposited whil e the l iquid is stirred

during the process o f cool ing i s to be collected the crystals care
, ,

fully freed from adhering mother liquor an d dried -

,
.

A dditional crops o f cr y stals may be Obtained by evaporati on o f

th e mother liquor but the crystals thus Obtained are usually more
-
,

or les s co l ored ( reddish ) .

D e scri pti on Colorl ess crystal s permanent in the ai r Odorles s

.
-
, , ,

o f sweetish bitterish taste S olubl e in 1 0 parts o f water forming

-
.
,

a clear solution which has a d istinctly ac id reaction S olubl e in .

alcohol .

M AGN E S IUM S UL PH A T E .

M A GN E S I I S UL P H A S .

( E psom S alt ) .

M agnesite in powder ,

S ulphuric acid of H zS O 4 )
Wat r
e
M ix the magnesite in a porcelain dish with 4 0 parts
o f water Then add about 2 parts o f the sulphuric
.

acid an d sti r
,
When e ffervescence has ceas ed add another
.
48 2 M A GNE S I U M S UL PH IT E .

M A GN ES I U M S UL PHI T E .

M A GN E S I I S U L PH I S .

M gS O3 6 H .
2
. O _

By saturating either magnesium carbonate or magnesium oxide ,

suspended in water with sulphurou s oxide the crystall ine product

, ,

being drained and dried .

D e s cri pti on . A
wh ite c rystalline p owder ; Odorl ess taste bit
—
,

terish ; somewhat sulphurou s S oluble in 2 0 parts o f water . .

M ust be kept in tightly stoppered bottles as it oxid izes on e x

-
,

p o s u r e to air .

M A GN E S I U M TA R T R A T E .

M A GN E S I I TA R TR A S .

M g C4 H 4 O 6 = I 7 2 2

Tartaric aci d
M agnes i um carbonate

D issolve the aci d in 2 0 parts O f distilled water keep the sol ution ,

hot over a water bath and add gradually the magnesium carbon
-
,

ate until a neutral salt i s Obtained E vaporate to dryness and .

,

powder the residue .

D e scr i pt i on .
—
A white powder which i s practically insoluble in
cold water .

M A N GA N E S E C A R B O N A T E .

M A N G AN I C AR B O NA S .

M n CO 3 Z I I5 .

M a nganous S ulphate
S odium bi carbonate

D issolve the bicarbonate in 200 parts Of boilin g water ; add the

 M A N G AN E S E DI OX I DE .
48 3

sulphate previously dissolved in 1 0 0 parts o f boilin g water and

sweetened w ith 5 parts o f su gar Wash the precipitate with boil
.

ing water containing about 4 per cent O f s ugar When the wash .

ings give but a s light turbid ity with test solution o f barium
chloride press the water out o f the ma gm a and dry it as rapidly
, ,

as practicable with the ai d o f moderate heat

,
.

D e scri pt i on A
dirty white powder with a reddish tinge
.
—
. I t is
insoluble in water but dissolves in dilute acids
, .

M AN GA N E S E D IOX ID E .

M AN GAN I D I O X I D U M .

( B lack O xide o f M anganese ) .

M n0 2
=8 7 .

Pure manganes e dioxide i s not obtainable T he best grades o f .

pyrolusite or brownstone contain about 90 per cent o f M n O The z

.

impurities in native black oxide o f manganese are ferric oxide ,

silica barium carbonate calcium carbonate alumina etc T he

, , , , .

A me rican Pharmacopoeia requires the manganese dioxide to con

ta in not less than 66 per cent o f M n O S ince this is the cas e z
.

“ ”
the O fficial title S houl d not be manganese dioxide but native ,

black oxide o f manganese .

In the emplo y ment of the native mineral its variabl e composi

tion m ust be taken into account In the trade the pyrol usite .

occurs both whole an d powdered The whole mineral can not .

be adulterated ; but the powdered is frequently mixed with coal ‘

etc.

E xtremely fine powder is n ecessary for some purposes ; but for

the preparation o f chlorine from hydrochloric acid a coars ely
powdered or crushed pyrolu site i s the best .

T he Pharmacop oeia describes it as a he avy gra y ish black more ,

-
,

or less gritty powder without odor or taste Insolubl e in water

,
. .

alcohol o r any other S impl e solvent N ot a ffected by col d sul

,
.

p h u r i c or hydroch l oric acid .

4 84 M A N G ANE S E C H LOR I DE

M A N GA N E S E CH L O R I D E .

M AN G AN I C H L OR I D U M .

T he aci d liquid containing manganese chloride which remains '

'

in t he flask or other generato r when chlorine gas is prepared from

hydrochloric acid and manganese dioxid e can be used to make
manganous chlorid e as follows .

E vap orate the liquid to dryness an d continue the heat as lon gas
acid vapors pass o ff Boil the residue with water for about ten
.

minutes Filter the solution Preci pitate manganous carbonate

. .

from about one e i ghth o f the filtrate with an exces s o f sodium

-

carbonate solution ; wash the precipitate and then add it t o the

'

other seven eighths O f the filtrate Boil for about hal f an h our
“

-
.
,

adding more wat er i f required Filter e vaporate and crystallize .

, ,
.

The preparation may be readily made from manganous sulphate

and barium chloride .

D e s cri pt i on .
—
Pale red deliquescent crystal s solubl e in alcohol
, ,

as well as water .

M AN GA N E S E I O D I D E S Y R U P .

S Y RU P U S M AN GAN I I OD I D I .

M anganous sulphate
Potassium iodide .
5 0 Gm
S ugar 280 Gm
S imple syrup distilled ,
w at e i , each su fficient .

D issolve each o f the salts in 5 0 ml o f w ater mixed Wi th

1 0 ml o f s impl e syrup M i x the solutions and shak e well
. Cool .

the mixture to about 1 O C ( 5 0

‘
Filter rinsin g the p re
°
.
,

c i p i t a t e on the filter with a l ittle sweetened w ater letting the ,

filtrate and washings run into a bottle containing the su gar .

S hake until d issolved and then a dd enough distill e d water to

,

make the total product measure 4 00 milliliter s .

M ust be protected from l ight .

 M AN GA N E S E S UL P H A T E .

M A N GA N OU S S UL PH A T E .

M A N GA N I

M nS O 4 4 H 2O 223
—
.
: .

anganese dioxide
M .

Concentrated sulphuric acid .

S odium carb onat e

Water .

M i X th e ~
finely powder e d manga nese di oxi de with a s ufficient
quantity of strong sulphuric acid to f or m a very so ft paste Heat .

this m ixture in a porcelain dish strongly on a sand ba t h s t i r , ,

-
,
‘

ring constantly until dry Then t rans f er the dry mass t o a

,
.

Battersea crucible and keep it at a red heat f Or about an hou r .

L et c ool L eech out the salt with hot water fi lter the solution
.
, .

S e t aside seven eighths o f this solution —

T o the remaining .

eighth add a solution o f sodium carbonate I part o f carbonate in

I O parts o f water ) as long as a precipitate fall s Wash this pre .

c i p i t a t e d manganous carbonate by decantation until the washings

are free from sulphate .

Then add the washed magma o f manganous carbonate to the

reserved portion of the solution o f m anganous sulphate m 1 x ,

well and heat the mixtu re in a porcelain dish to boiling

, .

Fil t er an d evaporate t h e filtrate to cr y stall ization

, .

Collect drain and dry the cr y stal s

, ,
.

Bottle th e product at once as soon as the cr y stals are dry to

the touch .

R e ac t i on . 2M nO z + 2H z
S O 4
2 2M nS O 4 + 2H O + O

N ot e s The solution o f manganous sulphate obtained from one

.
’

kilo o f manganese dioxi de may be evaporated to about 90 3

Cc and then set asid e in a shallow dish over sulphuric
. ,

aci d in a desiccator when a soli d cake o f crystal s will

, ,

be O btained in a few days at the ordinary room tem ,

.

p e r a t u r e Thes e
. crystals however contain 5 molecul
,
es o f ,

water The Pharmacopoeia orders a salt with 4 molecules o f

.

water and thi s can be Obtained by red issolving the manganou s

,

sulphate obtained as describe d in an equal weight o f water and

letting this soluti on stand in a dish at 3 0 until crystall ization
°
 MA N GANE S E S U L P H ATE . 8
4 7

takes place A t a very low temp e rature the salt cr y stallizes with
.

7 molecules of water .

When the cr y stal s are drained they should be covered with a

damp piece o f cloth to prevent e ffior e s c e n c e .

The Obj ect o f adding manganous carbonate to the solution o f

manganous s ulphate i s the precipitation an d removal o f any iron
b
,

which may still r e m a i n a ft e r the ignition which decompo s es n e a r l v

all o f the iron sulphate without decompos ing the manganese salt .

D e scr i p t i onPal e rose colored or colorless ; transparent crys

— -
,

tal s ; Odorless ; taste slightly bi tter astringent E ffl ore s c e n t in d ry ,

.

air S olubl e in
. p art O f w ater at and in I part o f boilin g
‘

water Insolubl e I n alcohol

. .

M ER CUR Y P U R I FI E D .

H YD RAR GY RU M P UR I PI CA T U M .

H gZ Z OO .

parts 10
0 o
'
o o o o o o o o o o o o o o o o o o o o o o o o o o I part
5 parts

Put the metal with the acid and water in a porcelain dish and
l et them remain together during four days stirring the contents ,

frequently and strongly Then pour o ff th e acid l iquid and wash

.
,

the metal first with water and finally with distilled water until
, ,

the washings no longer g ive an acid reaction on litmu s paper .

D ry the mercur y by pouring it through a co n e made o f white

filter paper or blotting paper and having an aperture at the apex
barely large enough to admit a p in so that the metal passes ,

thr o ugh in a thin stream .

N ot e s Common mercur y us ually contain s one or more o f the

.

metal s lead tin copper antimon y arsenic bismuth S uch impure

, , , , , ,
.

merc ur y sometimes presents a dul l su rface D rops o f m ercury .

containing l ead do not retain thei r globular form When made

to roll about on white paper but leave streaks or traces and m ay
'

even form l ittl e tail like proj ections

-
.

N itric aci d attacks the t i n a n t i m on y an d some o f the other

'

,
'

metal s before it attacks the mercury and removes them l eaving ,

488 P UR IFI ED M ER CUR Y .

the mercury purer than before and su fficientl y pure for the prep ,

aration o f th e mercury compounds to be employed for pharma

c e u t i c a l purposes .

M ercury boils at C (U S and the most e ff ective . . .

method o f purification o f commercial m ercury is distillati on .

M ercury should present a perfectly bright sur face but it may ,

present a dark colored film or patches on the surface i f contam

i n a t e d with dust dirt moist u re or th e oxides O f the foreign
, , ,

metal s present To restore its brightnes s it i s only neces sary

.

to run the metal through a paper cone as before described ; but

i f other metals are present the mercur y becomes dull and dirty
again from metallic oxi des floating on its sur face .

M E R C U R I C B E N Z OA T E .

H Y D R A R GY R I B E N Z OA S .

Hg C6 H 5 C0 2 ) 2 3
44 2

Freshly precipitated mercuric oxi de from 2 7 parts o f m ercuric -

chloride is m ixed w ith 2 2 5 parts o f artificial benzoic acid ( from

.

toluol ) and the m ixture d igested at a temperature near the boil

ing point ( at full water bath heat ) until the yellow color o f the
-

mer curic oxide has given place to the yellowish white c olor o f -

the mercuric benzoate formed The product forms voluminous .

masses floating in the li quid .

L et the l iqu id cool to 5 0 C trans fer the whole mixtu re to a

°
.
,

cloth strainer or a paper filter according t o the quantit y operated ,

upon and wash the benzoate with water O f the temperatu re o f

,

o
from 5 0 to 6 0 C
°
.

D issolve the salt in boil ing water an d l et the solution cool so .

that the pr oduct may be Obtained in crystals D ry these at from .

4 0 to 5 0 C
°
.

D e s cri p t i on M ercuric benzoate thu s prepared is in c olorless

—
,

gl istening crystal needles of a somewhat metall ic taste Gives an

, .

acid reaction on moist blue litmu s paper N early insolubl e in .

Col d water but freel y solubl e in boiling water

,
R eadily soluble .

in a water solution of sodium chloride and this solution has been ,

u sed for h y podermatic inj ection S oluble in alcohol but with .

partial decomposition It contains a bout . per cent o f Hg .

49 0 M ER C UR I C C H LOR I DE .

N ot e s The materials must be thoroughly dry and reduced to

.

very fine powder The manganese dioxide shoul d be strongl y

.

heated a fter havin g been powdered and before it is m ixed wi t h

the other substances .

*
O n a small scale the sam e apparatus as described in the notes
under the head o f H y d ra rgyri Ch l or i d u m M ite may be employed .

O r a retort may be used having the neck cut off rather short so
as to leave a wide open i ng T he retort should be buried in the dry
.

sand up to the neck H eat i s then applied gradual ly I f the ma

. .

t e r i a l s were not perfectly dry water vapor will be formed and it is ,

then necessary to heat gently at first until the moisture shall have
been expelled and even the neck o f the retort should be warmed
,

su fficiently to insure the expul sion o f all water vapor The iro n .

dish employed for the sand bath is th en heated more and more
—

strongly until subl imation is e ffected the end o f the neck o f ,

the retort being capped with a w ide mouthed bottle The heat is -
.

continued until th e sublimation i s completed care being taken ,

.

not to perm it the neck o f the retort to become choked up To .

wards the close o f the proces s the heat is raised almost to the
fusing point O f the mercuric chloride in order to obtain a sub
limate o f more deci dedly developed crystalline structure The .

retort i s finally allowed to cool slowly a fter which the sublimate ,

may be readily removed from the s hort neck .

In order to obviate the danger o f inhal ing any vapor o f mer

curi e chloride it i s necessary that the whol e operation be carried
out in a hood with a good d raught The product must not be .

carel essly handled being extremely poi sonous I f it is desired

,
.

to powder corrosive subl imate it shoul d be kept dampened with

,

alcohol durin g the process o f trituration to prevent the rising o f ,

dust .

S hould the mercuric sulphate emplo y ed contain any mercurous

sulphate a corresponding quantity o f mercurous chloride must
be produced To prevent thi s the manganese dioxide is a dded
. .

The rationale o f its action is sh own in the following equation

Wi thout the addition o f manganese dioxide it i s scarcel y pos

sible to obtain a corros ive sublimate that does not contain calomel
 M ER CUR I C C H LO R I DE .
49 1

to such an extent as to produce a very unclear solution in water .

B ut the sublimed mercuric chloride may be dissolved in diluted

a lcohol and crystallized from the filtered solution .

A n oth e r M e th od .

M ercuric oxide
Hydrochloric acid ( 3 2 % of H Cl )
D istilled water

Heat together until the oxide is completely dis solved Filter .

the hot solution and evaporate it to drynes s Crystallize the

,
.

product .

R e act i on . H gO + 2 H C l g C12
H
+ 2 O

N ot e s The product Obtained by thi s m ethod may be subl imed

.
;

to Obta in it in the form o f crystal s or cr y stalline m a sses or it

may be crystall ized in needles from a solution made with war m
,

d iluted alcohol or with water , .

S olutions O f mercuric chloride for certain purposes may be

~

readily made o f definite stren gt h from mercuric oxide h y dro ,

chloric aci d and water in such proportions as may be required .

T he hydroch l oric acid is prescribed in sl ight excess .

D e scr i p t i onHeavy transparent colorl ess odorless cr y stal s or

—
, , ,

cr y stalline masses havin g an acrid nauseous pers istent metallic

, , , ,

taste It i s extrem ely poisonou s an d should there fore not be

.
, , ,

tasted except in the most cautious manner .

O btained by subl imation on e large scale or heated at or n ear ,

its fusing point ( about and then very slowly Cooled it ,

forms large transparent colorles s crystals When crystallized

, ,
.

from solutions it is Obtained in the form of long needl es which

are somewhat opaque S olubl e in 1 6 parts o f water and in
.
,

3 parts o f alcohol at in 2 parts,

o f boiling water and in ,

parts o f boiling alcohol ; al so in 4 parts o f ether an d in 1 4 parts ,

o f glycerin ;
M ercuric chloride dissolves so sl owly in water that in making
s ol utions o f it the most advantageou s procedure i s to emplo y
powdered chloride and hot water .
492
.
M ER CUR I C C H LORA M I DE .

M E R C U R I C CH LO R A M I D E .

HY DRAR GY RU M A M M ON I A T U M .

( M e r c ura m m on i u m Chloride A mmoniated . M ercury . White

Precipitate ) .

H zN H g C12 25 1 4 .

M ercuric chloride I O parts

A mmonia water d 1 s t i l l e d water each su fficient
, , .

D isso lve
the chloride in 2 0 0 parts O f warm distilled water ;
filter an d allow to cool Pour the filtrate gradually and d u r m g
.
‘

constant stirring i nt O 5 parts of ammonia water tak ing care that ,

the ammonia shall rema i n 1n exces s when al l o f the mercuric

chloride has been added Collect the precipitate at once on a filter
.

'
,

drain a s much as possi ble and then wash it t w i c e e a c h tim e

, ,

with a mixture O f 2 0 parts o f distilled water and I part

o f ammonia water Finally dry the precipitat e between filter
.
,

paper in a dark place at a temperature not exceeding 3 0 C .

°
.

( 8 6 F )
°
.

R e acti on .

N ot e s When a solution O f mercuric chloride is poured into

.

ammonia water the latter being in exces s throughout the o ff i ci al

, ,

ammoniated me rcury is formed .

When h owever the order O f mixing the liquids i s reversed

, , ,

the ammonia water being added to the mercuric chloride or when ,

the mercuric chloride i s p r e s e n t i n excess over the pr opor

tion o f a m
~

moni a u sed the product will be or will contain

, , ,

i n st ead o f H 2N H g Cl The is .
,

however converted into the o fficial m e r c u ra m m on i u m chl oride

, .

when al l owed to remain in contact with an exces s o f a m monia for

some time .

S ome pharmacop oeias order the addition o f the ammonia to

the solution of mercuric chloride ; others includin g ours direct , ,

the opposite order o f mixing .

M e rc u r a m m on i u m chlori de i s per fectly white A g rayish . .

color indicates that the solution o f mercuric chlorid e wa s not

filtered before adding it to the ammonia whereby the cal omel , ,
494 M ER C UR I C C Y AN I DE .

T riturate I part o f this ferrocyanide o f iron with parts o f 2

mercuric oxide until thoroughly mixed Put the m ixture in a .

porcelain dish add 2 0 parts of water and heat upon a water bath
, ,
-

for one hour stirring frequently and replacing the water lost by
,

evaporation Then boil the mixture until the blue color d i s ap

.

pears S houl d a blue color still remain a fter boil ing the mix
.

ture for ten m inutes add a l ittle more mercuric oxide and c on
,

t i n u e boi lin g until the color o f the insolubl e matter becomes black .

Filter the liquid Boil the black precipitate with about I O

.

parts o f water filter and add this liquid to the other filtrate
, , .

S upersaturate the united filtrates w ith hydrocyan ic acid u sing ,

enough t o impart a permanent odor o f that acid to the liquid .

N ow filter the solution and evaporate to crystall ization .

Collect the crystals in a funnel let drain an d then d ry them , ,

on a filter paper with the aid of moderate heat .

E vaporate the mother liquor to obtain additional crystal s in —

the usual way .

R i
e a ct on s .

K F Cl Fe ( F e CyG) 1 2 K C1 ; and then

First , 3 4 F e ( )6
Cy — l—
1 4 e 3
:
3 +

F e 4 ( F e Cy 6 ) 3 + 9 H g O —
H
9 Q O

—
_

9 H g Cy2
—
3 F e ( O H ) 2
.
4F e ( O H )3 .

N ot e s The precipitated iron ferrocyanide contains potassium

.

compound and the wash water i s acidulated with hydrochloric

aci d to remove that compound I n order to render the p re c i p i .

tate more dense to facilitate th e otherwise extremely di ffi cult

,

washing boiling water is repeatedly employed The washing is

,
.

compl eted with pure water to remove th e hydrochloric aci d as

w ell as the last traces O f potassium chloride To facil itate the .

drying o f the ferrocyanide the water i s forcibly pressed out ,

“ ”
and the finely d ivided prussian blue is then spread out thinly
over the bottom and inner sides O f a large porcelain dish and
moderate heat u sed .

To make the mercuric cyanide from ferrocyanide o f iron the ,

latter mus t be recentl y precipitated and o f th e right composition .

“ ”
Hence the commercial prussian bl ue can not be success fully
emplo y ed .

The solution o f mercuric cyanide obtained by boiling ferro

 M ER C UR I C C Y AN I DE .
49 5

cyanide of iron with mercuric oxide contains some basic salt

“
( o x y cyanide o f
-
and it i s there fore neces sar y to , ,

acidulate this solution with hydrocyanic acid S ome iron usually .

precipitates on this addition o f hydrocyanic acid .

T h e hydroc y anic aci d required for this purpose may be made

from potassium cyani de A su ffi cient quantity for the product.

obtained from 60 parts o f potassium ferrocyanide will be pro

d u c e d by 4 parts O f potass ium cyanide which may be dissolved in
8 0 parts o f diluted alcohol and mixed with parts o f tartaric
acid a fter which the m ix ture is allowed to stand for one hour an d
then filtered .

A n oth e r M e th od .

Potassium c y anide
Tartaric acid
M ercuric oxide
D iluted alcohol
Water .

D issolve the potassium cyanide in the diluted alcohol A d d .

the powdered tartaric aci d and shake well L et the mixture .

stand one hou r shaking occasionally Filter in a covered fun

, .

nel into a bottle A d d the mercuric oxide to the filtrate and let
.
‘

stand shaking frequently until the odor o f hydrocyanic acid

, ,

has n early ceas ed and the mercu ric oxide has dissolved E va p or .

ate the filtered solution to crystallization a fter first adding some ,

more hydrocyanic acid .

R e a ct i on s .

First K Cy + H
, 2 C4
H 4 O e
z K H C4
H 4 O G+
H Cy ; then

H g O + 2 H Cy z H g Cy 2+ H 2Cl

N ot e s . S houl d
the solution o f m ercuric cyani de be basic it
deposits m ercuric oxide on evaporation It is therefore meces .
,
.

sary to have the h y drocyanic acid in excess It is best to dis solve .

the mercuric oxide and then add enough h y drocyanic aci d to

impart its odor to the liquid ( S e e notes under preceding .

formula ) .

i pt i on
D e s cr —
Colorless or white crystals ; odorles s ; O f bitter
metallic taste . I t is e xtr e mely poi s onous and there fore shoul d , , ,
496 M ER CURI C C Y AN I DE .

not be tasted exc ept in a diluted condition and with the utmost
caution .

It is darkened by exposure to light and must therefore be kept , ,

in dark amber colored bottles or in a dark place

-
.

S oluble at I 5 in parts of water and in I 5 parts o f alcohol ;

0
,

in 3 parts of boiling water and in 6 parts o f boiling alcohol .

M E R C U RI C I O D I D E .

H Y D R A R GY R I I OD I D U M RU B RU M .

( R e d I odi de o f M ercury ) .

H gI z
=4 5 s
M ercury
Iodine
A lcohol .

Triturate the iodine in a glazed porcelain mortar ( or in a gla ss

mortar ) with 2 parts o f alcohol A dd the mercury Continue . .

the trituration until a uni form scarlet red powder has been oh
t a i n e d adding a littl e more al cohol from time to time as may
,

be necessary to keep the mixture moist until the chemical r e ac

tion shall have been accomplished as fa r as practicable .

R e a ct i on . H g+ I z
—
_
H gl z.

N ot e sA pure mercuric iodide is not obtained by this method

.

for the react i on 1 5 not complete The alcohol is added to pre.

vent the vaporization of any o f the iodine by the heat generated

by the reaction the alcohol being evaporated instead o f the iodine
,

ahd the temperature thereby reduced .

This method is not recommended but i s included in this man ,

ual o nly as an illu stration o f the preparation of chemical p rod

u c t s by dry trituration .

The product obtained from 4 parts o f mercury and 5 parts o f

iodine may be put in a fl ask with 1 6 0 parts of alcohol and dis
solved by boil ing ; the hot solution may then be poured into a
beaker and allo wed to cool s lowly in Ord e r to Obt ain the mercu ric
i odide in crystals .
498 M ER CUR I C I OD I DE .

B eing soluble in 1 5 parts o f boil ing alcohol the mercuric iodide ,

may be easily cr y stallized from a hot alcoholic solution .

D e s cri pt i on . A
scarl et red heav y Odorles s and tasteless pow
— -
, ,

der A morphous i f made by triturating mercur y and io d ine to

.

gether or by cold precipitation ; c ry St a ll i n e i f made by precipita

,

tion with hot solutions B rilliant although small crystal s can be

.
, ,

obtained from a hot alcohol ic solution .

S oluble in 1 3 0 parts o f alcohol at and in 1 5 parts O f boiling

alcohol S olubl e also in soluti ons o f potassium iodi de mercuric
.
,

chloride and sodium thiosulphate respectively

, , .

B e comes yellow when heated to about but turn s scarlet

again on cool ing It fuses at about 2 3 8 to a dark yellow l iqu i d
.
°
-

which form s a mass o f minute y e ll ow c ry s t a l s on cool ing but ,

thes e crystals turn red again a fter a time ( or at once i f triturated ) ,

.

M E R CU R I C N I T R AT E S OLU TI O N .

L I QUOR H Y D R A R GY R I N I TRA TI S .

A liquid containing about per cent of mercuric nitrate

60
together with about I I per cent o f free nitric
acid .

R e d mercuric oxide 8 parts

N itric ac id 9 parts
D istilled water 3 parts

M ix the acid and water and dissolve the oxide in the m ixture .

Keep th e solution in glass stoppered bot tles -

.

R e ac ti on . H gO + 2 H N O 3

D e s cr i p t i onclear Colorl ess heavy corrosive liquid strongl y

.
—
A , , , ,

acid in its reaction and having an Odor of n itric acid The s p w

,
. . .

is about at 1 5 C °
.

B r i ti s h S ol u ti on f
o M e r curi c N i tr a te .

The liquor h y d r a r g y r i n i t ra t i s a c i du s o f the British Pharma

c o oe i a is prepared as follows
p
Dd e r c u r y
N itric a c i d
D istilled water
 M ER C UR I C N IT RA T E .
4 99

M ix the aci d and water in a flas k D i ssolve the mercu r y in the .

mixture without the aid o f heat Then boil gently for fifteen .

minutes or until a drop o f the l iqu id no longer gives a n y pre

,

c i p i t a t e in dilute hydrochloric acid L et it cool and preserve the

.
,

solution which should wei g h about

, Gm in a stoppered bot ,

tl e awa y from the light .

R e a ct i on .

N i tr a t e of M e r c u ry O i n tm e n t .

UN G UEN T U M H Y D R A R GY R I N I TRA T I S .

( Citrine O intment ) .

M ercury 14 parts
N itric acid 35 parts
Lard O il 1 5 2 parts
“

Heat the lard O i l in a porcelain d ish to a temperature o f 1 0 0 C 0

.

remove the dish from th e source o f heat ; gradually add to the o i l

1 4 parts o f nitric acid and when the e ffervescence caused by t h
, ,
'

reaction begins to subside heat the dish again to 6 0 until the

,
°

reaction is completed and e ffervescence has ceased Then allow .

°
the mixtu re to cool down to about 4 0 C .

D issolve the mercury in 2 1 parts o f nitric acid with the aid of

su fficient heat to prevent the solution from cr y stallizing and add ,

this l iquid to the warm mixture made o f lard oil and nitric acid
as above described S tir well an d then l et the mixture stand
.
,

until cold a fter which it must be again mixed thoroughly in a

,
.

porcelain mortar or dish with a pestle o f the same material ,

using a spatula o f horn wood or porcelain to remove the ointment

, ,

from the mortar and pestle .

N ot e s The reactions occu rring when fat i s treated w ith strong

.

n itric acid are not wel l known ; however th e lard O i l is acted U pon ,

with more or les s energy according to the temperature an d the ,

ol ein i s converted by oxidation at the expense o f the nitric acid

into elaidin wh ich is a firm er fat having a fusing point o f about
, ,

3 2
°
C. It is necessar y that the nitric aci d used should be o f full
strength in order that this reaction m ay be completed be fo re the
solution o f mercuric nitrate is added I f the temperature i s per .

f e c t l y controlled the acid used o f ful l stren gth and the reaction
, ,
5 0 0 M ER CUR I C N IT RA T E .

thoroughly completed before the nitrate of mercury is added the ,

product will be a han dsome firm lemon yellow o intment I f the

, , .

heat is too high the mercury n itrate will be decomposed and the
,

product rendered brown or gray from mercury oxide and reduced

,

metal .

I n m i x m g the m e r c u r 1 c n 1 t r a t e solution with the oxidized fat it ,

is necessa ry to stir wel l with a porcelain spatula or glass rod

"

until nearl y cold in order t o thoroughly incorporate the h e avv

,

l iquid which might ot h e r w 1 s e s ettle to the bottom o f the capsule .

The solution o f mercuric nitrate to be a dded t o the ointment

may be advantageously made by dissolving mercuric oxide ( i n
stead of the metal ) in nitric aci d .

M E R C U R I C OLEA T E .

H Y D R A R GY R I OLEA S .

Hg C1 8 H 33 0 2)

M ercuric oxide .

N itric acid s p gr ) . .

S olution o f potassium oleate

M ix the oxide the acid and 20 0 ml o f distilled water in a

, , ,

beaker or an evaporating dish and heat the mi xture until the ,

Oxide dissolves adding a few drops more o f nitric acid i f n e c e s

, ,

s a ry .D ilute the solution o f mercuric nitrate thus formed wit h

three liters O f water A dd ml o f solution of potassium
.

oleate ( prepared as described un der that title ) Warm the m ix .

ture and wash the separated mercuric oleate twice with warm
d istilled water u sing about one liter each time S ubj ect the
,
.

oleate to a low temperature in a mortar and then press out o f it ,

all the water by means o f a pestle .

R e acti on .

H g ( N Os )

N ot e s . Mercu ric chloride cannot be empl o y ed in place o f the

n itrate nor can sodium ol eate be used instead of the potassium
,

oleate as the washing then becomes very di ffi cult

,
.
5 0 2 M ER C UR I C OX I DE .

to dryness T O the residue add another 8 parts O f mercury and

.
,

triturate in a mortar until metallic globul es are no longer vi s i ble ,

and the m ixture appears to be uni form Heat th is mixture in a .

porcelain dish over a sand bath stirring frequently until acid -

, ,

vapors are no longer evolved .

R e act i on s .

First ,
H
3 g + 8 H N O 3
: —
l
—
2N O .

S econd ,

Third; H g2 ( N O 3 ) 2 , when heated decomposes int o ,

2H g O l N —
zO 4
-
.

N ot e s The n itrate is decomposed by heat red fumes ( nitrogen

.
,

tetroxide ) being evolved When all the nitrate has been thus .

decomposed the acid vapors cease and th e resi due is mercuric

, ,

oxide Care must be taken to continue the heating until not a

.

trace o f n itrate rema i ns M ercuric oxide when strongly heated

.

becomes very dark but the red color returns on cool ing I f the
,
.

heat is too high ( over 3 6 0 C ) the oxide decomposes into its °

.

elements which m a y be d iscovered by holding a p iece o f fi l t e r

,

paper over the heated mass when metallic m ercury wil l condens e ,

on the paper .

It is sometimes directed to digest the residue a fter cooling with ,

distilled water to which a l ittl e solution o f soda has been a dded ,

the Obj ect being to remove any remaining n itrate In this cas e .

the oxide must a fterwards be thoroughly washed an d dried at a ,

gentl e heat .

D e scri pt i on A brick red inso lubl e pow der

—
M ust not p r o
-
,
.

duce red v apors when heated It i s completely soluble in H Cl . ,

producing H g Cl z .

A n o th e r M e th od .

A finely divi ded red mercuric oxide m a y be obtained by heating

the y ellow ( precipitated ) mercuric Oxide until it becomes red
on coolin g and corresponds to the pharmacopoeial i dentit y tests
,
.
 M ER C UR I C OX I DE .
5 3
0

M E R C U R I C OX I D E Y ELLO W .

H Y D R A R GY R I OX I D U M F LA V U M .

[ Precipitated M ercuric O xid e ]

H gO z 21 6 .

M ercuric chloride
S odium hydroxide .

D istilled water , su fficient .

D issolve the powdered mercuric chloride in 3 l iters o f hot dis

tilled water and filter the solution
, .

D issolve th e sodium hydroxide in 5 0 0 ml distilled water .

Pour the solution o f mercuric chloride when col d slowly and , ,

i n a small stream or a littl e at a time into th ES O

,
ftiti On o f sodium,

h y droxide stirring briskly and uninterruptedly

,
.

A llow the mixture to stand for an hour stirring frequently , .

D ecant the S u p e r n at a nt l i q u i d f f omfl i e precipitate and wash

' a

the latter by a ff usion and decantation o f cold distilled water

-
.

Collect the pr e cipitate on a strainer or a paper filter and con

t i n u e the wash ing with warm d istilled water until a portion o f
the washings when poured over a little test solution O f mercuric -

chloride no longer produces a yellowish turbidity at t h e point of

contact O f the two liquids .

Then allow the p recipitate to drain and dry it between sheets ,

o f white blotting paper in a dark place at a temperature not ex

, ,

ce e d in
g 30 C
°
.

Keep the product in well stoppered bottles in a dark plac e -

.

’
L
R e act i on .

N ot e s .Th e mercuric chloride 1 5 used in the form o f powder

and hot water is to be used to dissolve it in o rder to save time .

But the solution o f mercuric chloride must be col d when poured

into the solution o f sodium hyd roxide The use of very hot s o .

lutions in making precipitated mercuric oxide would yi el d a prod

u e t consisting partl y o f the red variety The u se o f a too high
heat in wash ing and drying yello wOxide o f mercury is to be
.

avoided for the same reason A n over heated freshl y p re c i p i .

-
5 4
0 M ER C UR I C OX I DE .

tate d m ercuric Oxi de has a more reddish color than the product
not exposed to a too high temperature and the reddish p r e c i p i
,

t a t e d oxide does not readil y form mercuric oxalate when treated

w ith a strong solution of oxal ic aci d as described in the Pharma
c op oe i a .

A s mercuric chloride i s l iable to contain calomel the omission ,

of the filtration might result in th e d iscoloration o f the product

by the mercurous oxide formed by that calom el .

The sodium hydroxide used shoul d contain at l east 90 per cent

o f N a O H and must be free from carbonate The presence o f
, .

“
sodium carbonate in the soda used woul d cause the formation o f
mercur i c carbonate which is dark brown and usuall y fall s a fter
,

the orange yellow mercuric Oxide has subsided and thus forms a
thin la y er over the oxide .

D ilute solutions are emplo y ed becau se the use o f a strong solu

tion O f m ercuric chloride might ea s il y lead to the formation O f
“
oxy chloride O f mercur y having a brown or brick red color -
.

There are two such ox yc hl or i d e s one o f them so dark brown as to

,

appear nearl y black and the other brown red or —

brick red—
In order to prevent the formation
O f either o f these ox y c h l o r i d e s it is necessary that the m ercuric

Oxide formed shoul d not be permitted to come in contact with the

mercuric chloride Hence the mercuric chloride must be com
.

p l e t e l y decomposed as fast as it is ad ded to the solution o f s o

d i u m h y droxide This result is insured by ( 1 ) making the solu

.

tion o f mercuric chloride very dilute whil e the solution o f sodium

hydroxide i s les s diluted ; ( 2 ) add ing the solution of the mer
c u r i c chloride to the solution o f sodium h y droxide instead O f ,

vi c e v e r s o ; 3) adding the mercur y solution very gradually ;

'

(4 ) stirring constantly and briskl y while mi x ing the sol utions ;

and using a lar ger amount o f sodium hydroxide than required
by theor y according to the chemical equation so that the alkali ,

shall be in excess from beginning to end .

S houl d the solution o f sodium h y droxide be poured into that o f

the mercuric chloride the mercuric oxide then formed would at
,

once ( and throughout the process o f mixing the sol utions ) come
into contact with the mercuric chloride and woul d then form ox y
,

chloride which would be evidenced by the dark dirty col or of the

, ,

precipitate .

S hould mercuric carbonate or any oxychloride be formed caus ,

50 6 M ER CUR Y P E PT ONA T E .

3 . D issolve 1 part o f sodium chloride in 5 0 parts o f distilled

,

vva t e r .

Pour solution I slowly and with constant stirring into solution

2 . L et the mixture stand an hour Collect the precipitate on a .

filter and let it drain well Trans fer the precipitate to a porcelain .

dish add solution 3 and stir well until solution results Then
, .

add enough distill ed water to make the whole product weigh 1 0 0

parts F ilter . .

Keep it in small completely filled an d well stoppered bottles

.
,
-

in a cool dark place , .

D e s cr ip t i on —
A yellowish acid l iquid o f disagreeable metallic
,

taste .

M ER CUR I C S AL I C Y LA T E .

H Y D R A R GY R I S A L I CY L A S .

H g C7 H 4 0 3 =3 3 6

M ercuric chloride
S olution o f s o dium h y droxide
S alic y lic
acid
D istilled water su fficient , .

issolve the mercuric chloride in 5 4 0 parts o f hot distilled

D , ,

water filter the solution and let it cool to the ordinary room tem
, ,

p e r a t u r e .

D ilute the sodium h y droxi de solution with 5 0 parts o f distilled

water .

Pour the cold solution o f mercuric chloride gradually and dur

ing uninterrupted stirring into the solution o f sodium hydroxide .

Wash the precipitate by decantation and finally on a paper filter

with distil l ed water until the washings give no further reaction
for chloride .

Collect the precipitate and put it in a flask with enough d istilled

water to form a thin m ixture when shaken Then add the salic y lic .

aci d shake again so that the mixture m ay be made as nearl y uni

,

form as pr acticabl e and then heat the flask on a water bath ,

-
,

shaking the flask frequently .

When the yel low color o f the mercuric oxide has given place to
the pur e white color of the mercuric sal icylate which is the finely ,
 M ER C UR I C S AL I CY LA T E .
5 7
0

divided insolubl e matter now contained in the l iquid remove the ,

flask from the water bath —

.

Wash the m ercuric salicylate with hot water until the washings '

no longer give an acid reaction on test paper T h e n c ol l e c t the -

.

product on a paper filter l et it d rain well a n d dry it at first at a

, , ,

°
moderate heat and finally at 1 00 C .

N ot e s The sal icyli c acid is used in slight excess and forms

.

mercu ric sal icylate with the freshly precipitated mercuric oxide .

The exces s O f salicylic acid is then washed out .

D e s cri pt i on —
A
white amorphous Odorles s and tasteles s pow
, ,

der almost insoluble in water and in alcohol

,
.

M ercuric salicylate is not decompos ed by carbonic acid or by ,

tartaric lactic or acetic acid nor by sodium hydroxide sol ution

, ,
.

When the salt is dissolved in a solution o f sodium h y d rox i d e i n

such proportion that one molecule o f N a O H i s present for each
molecul e o f H g C7 H 4 O 3 a doubl e salt is formed which crystallizes
,

out o f the solution .

M ER CUR I C S UL PH A T E .

H Y D R A R GY R I S UL P H A S .

H gS O , : 296 .

M ercu ry
S ulphuric aci d

Heat them together in a porcelain capsule , stirring constantly ,

until the metal disappears and a dry white salt remains .

R e act i on . H g + 2 H zS O , = H g S O 4 —
S O 2 + 2 H 2O .

N ot e s . M
ercury is insolubl e in cold sulphuric acid .

M ercuric sulphate is u sed in the preparation o f calomel corro ,

s ive subl imate and bas ic mercuric sulphate

,

It m ay also be made a s described in the next paragraph with

, ,

the aid o f nitric acid when less sulphuric acid will be required
, .

D e s cr i p t i on
heavy white crystalline powder which d e c om
.
—
A
poses on the addition o f water y ielding y ellow subsulphate o r , ,
 M ER C UR I C S U L PH A T E .

B as i c M c
e r uric S ul
ph a t e .

H Y D R A R GY R I S U B S U L PH A S F LAV U S .

[ Y ellow S ubsulphate of M ercur y . Turpeth M ineral ] .

M ercury
S ulphuric acid
N itric acid
D istilled water , su fficient .

Put the mercury in a roomy flask add the sulphuric acid pre , ,

vi ou s l y m ixed with 1 5 ml o f distilled water and then the nitric ,

acid previously mi x e d with 2 5 ml o f distilled water D igest the

, .

mixture at a gentl e heat until red fumes cease to be given O ff .

Trans fer the mixture to a porcelain dish and heat it on a sand bath -
,

under a hood or in the open ai r with frequent stirring until a , ,

dry white salt remains This white salt is normal mercuric sul
, .

'

phate Powder this and throw it in small portions at a time into

.
, ,

2 l iters O f boil ing distilled water stirring constantly Havin g ,

.

added al l o f the mercuric sulphate boil the m ixture ten minutes , ,

all ow it to s ettle decant the liquid trans fer the precipitate to a

, ,

filter wash it with hot distilled water until the washings ceas e to
,

give an acid reaction on test paper and finally dry the product in -
,

a moderately warm place .

R e act i on .

Then the mercuric sulphate i s spl it up by water into a basic salt

which precipitates a nd an acid salt which remains in solution
, ,

the result varying somewhat according to the quantity o f water

used and its temperature .

N ot e s . M
ercuric sulphate can be made from mercury and sul
p h u r i c acid without the use o f nitric aci d ; when th e latter is added ,

however the reaction is more easily accompl ished

,
.

Basic mercuric sulphate can also be made by gradually addin g a

sol ution of mercuric nitrate to a solution o f sodium sulphate the ,

latter salt to be in exces s .

D e scri p t i on heavy lemon yellow powder odorless an d

.
-
A ,
-
,

nearly tasteless very sl ightl y soluble in water insoluble in alc oh ol

, ,
5 10 M ER C UR I C S UL PHI DE .

the black s ulphide was made provided the mortar is large enough , .

It should be kept warm by placing it in warm water .

The yield will be about 1 0 0 parts .

Cr u d e M e r cu r i c S ul p h i d e ( M i x e d w i t h S ul ph u r
) .

( ZE t hi op s M i n e r a l i s .
)
I part
1 part

Triturate them together in a glass mortar ( or in a glazed por

c e l a i n mortar ) until a uni form black powder shall have been ob

t a i n e d in which no globules o f mercury are visible under a lens o f

ten d iameters mag i fying power
n
.

R e act i on . H g+ S z H g S

N ot e s . A s the atomic weight o f mercury is

and that o f 2 00 ,

sulphur only 3 2 it follows that this product cons i sts o f about 3

,

parts O f mercuric sulphide and 2 parts o f sulphu r It is an old .

preparation formerly employed in veterinary medicine and i s ,

included in this book simpl y as an illustration o f chemical com

bination between d ry sol ids triturated together .

The trituration must be continued at least two hours under

strong pressure This necessarily causes the formation o f shining
.

black scales which mus t finally be reduced to powder by gentl er

”
,

trituration and by s i fting the product through a fine sieve .

The mortar and pestle are at the end o f the tritu ration covered
with a black coating o f mercuric sulph ide wh ich is not easily r e
.

moved i i the mortar u sed be on e made o f wedgew oo d ware or

other porous material S trong nitric acid and powdered glass or
.

white sand may be triturated together in the mortar to remove the

stain .

M E R C U R OU S CH LO R I D E .

H Y D R A R GY R I CH L OR I D U M M IT E .

( Calomel . M il d M ercurous Chloride ) .

H g Cl : 23

M ercuric sulphate
M ercur y
S odium chloride dri ed ,

Boil ing distilled water suffi cient , .

 C ALO M E L .
5 I 1

oisten the m ercuric sulphate w ith some o f the water ; add the
M
mercury ; triturat e until metallic globul es are no longer visible ;
add the sod ium chloride and mix the whol e thoroughly by long
continued trituration S ublime by a suitable apparatus Wash
. .

the subl imate with boiling distilled water until the washings cease
'

to be darkened by a drop o f ammonium hydrosulphide D ry it at .

°
not over 1 0 0 C .

R e act i on . H gS O4 +n n S O4 ; then , n S O4 l — —
2 N a Cl :

2H g Cl + N azS O 4 .

N ot e s . O n a small scal e the sublimation may be e ff ected in

bottles o f about 2 0 0 Cc capacity These bottles shoul d be thin
. .

bottomed an d o f uni form thickness and should have rather wide ,

mouths D uring the pr oc es s O f sublimation the mouths of the

.

bottles may be closed loosely with chalk stoppers The m ixed .

powder to be subj ected to sublimation must be thoroughly dried

before it is put into the bottl es Flasks or retorts may al so be .

used The bottles flasks or retorts are heated by means o f a

.
, ,

sand bath The y should be onl y about one fourth filled and buried
-
.
-

into the sand su ffi ciently deeply to bring the l evel o f the contents
o f the subl iming vessel below the level o f the san d surround ing
it The heat must be applied ca utio usly being moderate at first
.
, ,

then gradually increased until the cal omel has all been sublimed .

S ubl imed calomel is yellowish white when prepared in small -

quantities and in the w a y here described When manu factured .

on a large scale the vap or is rapidly condensed in large cham

,

bers into which steam is inj ected and the product is then n e a rl v ,

or qu ite white and more finely d ivided .

The sublimate obtained in operating with small amounts i s

crystall ine and must be triturated with warm water a long time
( levigated ) until reduced to an extremely fine ( impalpable ) pow
der The warm water u sed for th is purpose is to be frequently
.

changed in order that the mercuric chloride may be eff ectuall y r e

moved from the calomel .

The heat must n ot be too h igh for then a portion o f the calomel
i s decomposed into mercury and mercuric chloride .

Th e sublimate formed in vessel s heated in a sand bath is de -

posited immediately above the level O f the sand as well as higher

up To remove the sublimate it i s necessar y to break the vessel
.
5 1 2 C ALOM EL .

containin g it Great care should be exercised in doing this so

.

that no fragments o f gl ass become mixed with the product I f .

necessary to d etach the crust from the glass while the sublimate
is still warm it is best to moisten it a little ; but a fter a f e w days
,

the crust can be readily removed without bein g moistened .

A l l subl imed calomel however made is contaminated w ith , ,

mercuric chl oride so that calomel free from corrosive sublimate

,

can be Obtained only by levigating the sublimed or precipitated

calomel until pu re E lutriation may be advantageously combined
.

with the l evigation When the water with which the calomel is
.

l evigated ceases to become darkened by ammonium hydrosulphide

or to be rendered uncl ear on the addition O f ammonia and when ,

the wet calomel fails to produce a dark dull spot on pol ished steel ,

a fter five m inutes cbn ta c t with it the product i s free fr om mercuric

’

é hl or i d e .

A n oth e r M e th od .

M ercuric chlori de
M ercury
A lcohol .

Triturate the m ercuric chloride and mercury together in a por

c e l a i n mortar until all m eta lic globules have disappeared keeping
l ,

the mixture moistened all the time w ith some alcohol to prevent
the poisonou s dust from ris ing When no more mercury globul es .

a re vis i ble the mixture is gray Put the gra y mixture still damp .
,

from the alcohol used in a porcelain dish and heat it moderately

,

upon a sand bath with constant stirring until the moisture

—
, , ,

mercuric chl oride and mercur y have been expelled leaving a

, ,

yellowish white nearly pure calomel which will be the case when
-
,

a white subl imate is formed on the bottom of a flask or bottle held

’

immediately above the contents O f the dish when strongly heated .

This part o f the process must be performed u nder a hood with a

goo d dra ft or in any manner insuring the removal o f the poison
,

ous vapors which pass O ff The calomel mixture thus thoroughly .

,

dri ed and partiall y freed from mercuric chloride is then put in ,

bottl es flas ks or retorts an d subl imed as described in the notes

, , ,

under the preceding process .

D e scri pt i on heavy white impalpable powder ; Odorless and

—
A , ,

tasteless .
B ecomes y ellowish white on being triturated under -
5 4
1 C ALO M EL .

weight O f distill ed water and add to thi s solution 5 per cent o f

,
i

its weight of hydrochloric acid Then pour the sodium chloride .

solution gradually into the mercury solution stirring con stantly , .

Wash t h e precipitate with col d distilled water by aff usion and ,

decantation un til the washings no longer give an acid reaction on

,

test paper
-
.

D ry the product at a temperature not exceeding 40 C °

.

R e act i on s . and sub

sequ ently H gN O3 + N a Cl g Cl + N a N O 3 .

N ot e s It i s necessary that the mercury solution should Contain

.

enough n itric acid to remain clear when diluted with its own vol
ume of water and it is to be tested to make sure O f that fact befo e
,
,
r

the solution o f sodium chloride is added because i f the mercury ,

solution shoul d contain too l ittl e nitric acid the precipitate formed
upon dilution with water is a basic me rcurous nitrate and this
would then be precipitated by the solution of sodium chloride
“

together with the calomel B ut i f the solution o f mercurous n i

.

trate will bear dilution with its own volume o f water without
becoming turbid it may sa fely be m ixed with more than its own
,

volume of so dium chloride solution gradually added without any , ,

danger o f the precipitation o f basic mercurous nitrate together

with the mercurous chloride .

The large dilution o f the liqui ds is necessary to prevent t h e for

mation o f mercuric salts by the nitric acid .

Precipitated calomel is much bulkier than sublimed calomel and ,

is extremel y finel y divided

It shoul d b e tested for nitrate from which it must be quite ,

free .

A n o th e r M e t h od .

D issolve part o f mercuric chloride in 5 0 parts o f d istilled

1

water Keep the solution at a temperature o f from 7 0 to 8 0 C

.
° °
.
,

and conduct into it a current o f washed sulphu r dioxide ( prepared

from s odium bisulphite and diluted sulphuric aci d as described
under the title o f sulphurous acid until saturat ed with it L et ,
.

the l iqui d cool Wash the precipitated cal omel upon a filter with
.

distilled water D ry the product with the ai d O f gentle heat

. .

R e ac t i on . 2H g C12 + S O z+
2 H z
O : 2 H g Cl —
H zS O 4 + 2 H CL
 M ER C UR I U S S OL U B I L I S .
5I5

D e s cr i p t i on S e e sublimed calomel
.
—
The only di ff erences be .

tween subl imed calomel a n d p re c i p i ta t e d calomel is that the latter

is lighter ( bulkier ) being finer and less l iable to contain crystal s
, ,

( visible under the microscope only ) , .

M e r cu r i u s S ol u bi l i s H a h n e m a n ni .

[ N itras amido -
h y d ra r g y r i Cu s cum h y d ra r gy ro ; D anish Ph .
]
M ercu rous nitrate
N itric acid
A mmonia water
A lcohol
D istilled wat er su fficient
,
.

D is solve
the mercurou s n itrate in a cold mixture o f the nitric
acid with 1 8 00 parts o f distilled water Pour this solution slowly .

into a mixture o f the ammonia water and alcohol stirring con ,

s t a n tl y .

[ The m ixture thus Obtained shoul d have a feebly acid reacti on ] .

Collect the precipitate on a fi lter l et it drain an d wash it with a , ,

small quan ti ty o f alcohol D r y it in a dark place and without the

.

a id of heat .

M ust be protected from the light .

heavy dead black fine powder odorl es s taste

D e s cri p t i on .
—
A , , , ,

l ess insoluble i n water and in alcohol Heated t o a h igh tempera

, .

tu re it decomposes giving off n itrous vapors and l eaves no fixed

, ,

resi due Heated with sodium hydroxi de solution it gives off am

.

monia S hould be compl etely s olubl e in nitric acid

. .

M E R C U R OU S I O D I D E .

H Y D R A GY R I I OD I D U M F LAV U M .

Y ellow Iodide o f M ercury .

H gI :
3 2 6 .
5 .

ercury
M
Iodine
A lcohol .

T riturate the iodine in a gl azed porcelain mortar ( or in a glass

 5 1 6 M ER CUROU S I OD ID E .

mortar ) with three parts o f al cohol A dd the mercury Con . .

~

f inue the trituration until all globules o f mercury have disappeared

and the mixtu re when nearly dry has acquired a greenish yellow
, ,
-

color D uring the trituration add more alcohol from time to

.
, ,

time as may be necessary to keep the m ixture c onstantl y moist

, .

When the reaction i s at a n end as indicated by the disappear .

a nce o f mercury globules and by the development o f a greeni sh

yel low color add enough alcohol to reduce the whol e to a th in mix
,

ture l iquid enough t o be poured into a bottle U se su ffi cient addi

,
.

t i on a l small portions O f alcohol to rins e the mortar well and to

-

trans fer all o f th e wet powder to the same bottle .

Cork the bottle and set it aside in a dark but moderately warm
place for a day shaking it occasionally d u r i ri g that period Then
,
.

let the heavy powder subside completely pour o ff the alcohol from ,

the soli d matter and add instead o f the alcohol thus decanted , ,

about 5 0 parts o f pure alcohol warm th e bottl e shake w ell and , , ,

again set it aside well corked for a day or two , ,

.

D ecant again and i f necessary repeat once more the washing

, , ,

o f the mercurou s iodi de with another portion o f warmalcohol .

Finally shake the bottl e well trans fer i ts contents t o a white ,

paper filter and continue washing the product on the filter with
,

warm alcohol until the washings are no longer darkened by hydro

gen sulphide or by a weak solution o f sulphu rated potassa .

When t h e w a s h i n g shall have been compl eted as described dry

, ,

the product between wh ite bl otting paper in a dark place at a

temperature not exceeding

Keep the product in a wel l closed bottl e and protected from -

l ight .

R e act i on . H g+ I —
H gI .

N ot e s The reaction between th e two elements causes much

.

h eat . The alcohol a dded be fo re and during the trituration is

evaporated by this h eat and thus keeps the temperature down s o,

as to prevent the loss o f iodine by vaporization which would be ,

'
s u s t a i n e d w e r e the material s triturated together in a d r y state .

But the reaction i s not complete The product O btained by this .

method contains mercury and mercuric iodide as well as mercurou s

iodide The mercury cannot be removed and its presence gives
.
,

the mercu ro us iodide a greenish hue Pure mercurous iodide is .

5 18 M ER C UROU S I OD I DE .

solution o f potassium iodide into that o f the mercurous nitr ate _

,

with constant stirring allow the precipitate to s ubs ide decant ,

,

the supernatant liqui d and trans fer the precipitate together with
, ,

the remainder o f the liquid to a filter When the precipitate has , .

drained wash it with distilled water until the washings no longer

,

have an acid reaction upon l itmus paper and a fterwards wash it ,

w ith alcohol as long as the clear colorless washings give any

, ,

color with hydrogen sulphide test solution L astly d ry the -

.
,

p roduct in a dark place between sheets o f bibulous paper at a , ,

temperature not exceeding 4 0 C °

.

Keep it in dark amber c olored bo ttl es with th e least possibl e

,
-
,

exposu re to light .

R e act i on s H : 4H N O : H N O H O N O ; and , then

3 g + 3 g 3+
2
- —
.
3 z ,

H gN O3 —
KI :
—
H gI —
KN O 3 .

N ot e s . The preparation o f mercu rous nitrate is described else

where Instead o f adding the m ercu ry nitrate to the potassiu m
.

iodide which woul d cause the precipitation of some bas ic mer

,

eurou s nitrate with the mercurous iodide it is necessary that the ,

u sual order o f mixing the reagents be reversed in this case ;

hence the formula d irects that the soluti on o f potassium
iodide be added to the solution o f mercurous n itrate The p r e c i p .

i t a t e d m e r c u rou s i od i d e is l ight yellow It shoul d be protected

‘

against ligh t throughout the process o f p reparation as well as

a fterwards The mercuric iodide which is formed w ith th e mer
.

c u r ou s i o dide O wing to the presence o f mercuric nitrate and nitric

,

aci d with the mercurous nitrate is washed out with alcohol ,

.

Instead o f weighing o ff 4 0 Gm o f the mercurous ni t rate as above

directed the whole O f the crystall ized salt may be taken and the
,

amount o f potassium iodide etc adj usted in accordance with the ,

.
,

proportions given ab ove .

D e s cr i p t i on A
bright yellow amorphous Odorless tasteless
—
, , , ,

insoluble heavy powder D arkens on exposure to l ight d e c om

,
.
*

posing into m ercuric iodide and mercury .

M ade by t riturating mercu ry and iod ine or mercu ry and mer ,

c u r i c iodide together the preparation i s invar iably yellowish

, ,

green because the reaction is not complete so that t h e product

contains mercuric as well as mercurous iodide and mercury .
 M ER C UR OU S N 1 I RA T E .

M E R C U R OU S N I TR A TE .

H Y D R A R GY R O S U S N IT RA S .

H g N O 3 H 20 . _ — 2 80 .

A dd a cold mixtur e o f parts o f nitric acid an d 2 0 parts o f

3 0

d istill ed water to 5 5 parts o f mercury in a flask L et the mixture , .

stand in a dark place agitating it occasionally until reaction ceas es

, ,

and but littl e o f the metal remains undissolved Collect in a glass .

funnel the crystal s o f mercurou s n itrate wh ich have been formed

'

in the col d liquid and allow them to drain Then place the crys
,
.
,

tals on white blotting paper and dry t h e m i n a dark place '

.

R e act i on
”

N ot e s . The m ercur y nitrate remaining in the mother l iquid

shoul d be recovered as wel l as the undissolved mercu ry The r .
e

t i on a l e o f the proces s is the formation o f normal mercurous nitrate

in solution in a mixture O f nitric acid and water employing s o ,

small a qu antity o f liqu id that the greater part o f the salt crystal
l izes out .

By digestion o f an excess O f mercury with the acid and water ,

or with the acid sol ution O f mercurous nitrate a basic m ercurou s ,

salt woul d s oon be formed which separates in pal e yellow cr y stals

,

or powder A n experienced operator may employ digestion and

.

continue it until basic mercurous nitrate begins to depos i t a fter ,

which the solution shoul d be decanted a little nitric aci d added to ,

“

it and the clear l iqu id set aside in a col d place that crystals may be
,

I
formed .

M ercur y dis solves in n itr 1 e acid with greater or less rapidity a c

cording to the temperature and the degree o f concentration o f the
acid When strong nitric acid i s u sed the solution wil l co ntain
.

mercuric nitrate which however i s reduced to mercurous nitrate

, , ,

by digestion w ith more m ercury .

By dissolving mercu ry in col d dilute nitric acid mercurous ,

nitrate is obtained .

The acid should be present l n excess because otherwise basic ,

salts are formed which are insolubl e in the liqu id .

N orm al mercurous n itrate m a y be obtained from the solution in

colorles s plates which can be dissolved in a smal l quantity o f
5 2 0 M ER CURO U S N IT RA T E .

water but which decompos e i f much water is added an acid mer

, ,

eurous nitrate remaining in solution whilst a yellow basic mer

eurou s nitrate precipitates .

A dilute solution of mercurous nitrate can therefore not be made

without an excess o f nitric acid .

D e scr i pt i on
Colorless crystal s which partiall y e ffl or e s c e on
.
—
,

exposure to air and when heated first fuse and then volatilize
, , ,

without res idue S oluble w ithout decomp os ition in a small quan

.

tit y o f warm water ; easily solubl e in d iluted nitric acid A larger .

proportion o f water decomposes the salt caus ing the formation o f ,

a l i g h t y e llOw basic mercurou s nitrate

‘

Te st s . A s olution o f the salt in water strongly aci dulated with

nitric acid g ives a black precipitate w ith sol ution o f sodium h y
d r ox i d e and a white precipitate with hydrochloric acid
,
.

When five hundred milligrams o f the salt is triturated with two

hundred and fi fty m illigrams o f sodium chloride an d water is
added the filtrate Obtained from this m ixture i s darkened on the
,

addition o f hydrogen sulphide but should not give a p re c 1p 1t a t e

,

with that reagent ( absence o f mercuric nitrate ) .

M E R C U R OU S OX I D E .

H Y D R A R GY R I OX I D U M N I GRU M .

n Oz 416 .

Prepared by macerating freshl y precipitated mercurous chlori de

with solution o f potass ium h y droxide in excess The thoroughly .

washed an d still moist mercurous chloride is gradually added to

the soluti on o f potassa w ith diligent stirring ; the whole i s well
,

shaken an d then set asi de in a dark place until the black mercurous
,

oxi de has settled This is then washed with cold distill ed water
.
,

coll ected and dried between folds o f blotting pape r in a cool dark
, ,

place .

M u st be kept well protected from the light .

A bout 1 2 parts o f precipitated calomel and 2 4 parts o f soluti on ,

o f pot assium hydroxide o f .

specific weight will be required to ,

prepare 1 0 parts of mercurous oxide .

S olution o f sodium hydr oxide may be used instead o f the solu

tion o f potassium hydroxide .
 O X Y GE N .

Fuse the sodium carbonate in its own water o f crystallization

add the potassium chlorate ; m ix well ; evaporate to dryness and
“

powder the mass M i x this powder intimately with the powdered

.

manganese dioxide Put the m ixture in a suitable flask provided

.

with delivery tube an d sa fety tube and hea t the contents over
-

a B unsen burner The g enerator or flask shoul d be connected

.

with a wash bottle cont aining water

-
.

The reaction is : 2 K Cl O 3 z 2 K Cl — l 3Oz

v—
.

N ot e sThe manganese dioxide causes the potassium chlorate

.

to decompose more quietl y and at a low er temperature than woul d ,

be the case when the chlorate is heated alone The sodium car .
,

bonate also facilitates the regularity o f the decomposition o f the

chlorate and prevents the formation o f gaseou s chlorine oxides
which are liable to contaminate the oxygen A s a further p r e ca u .

tion the gas i s washed by pass ing it through water .

The manganese dioxide must be free from carb on ( powdered

coal ) and organic matter and the materials perfectly dry ,
.

The retort Fig 1 2 0 p 1 8 4 may be u sed

,
.
,
.
,
.

O ne kilogram o f K Cl O should furnish abo ut 2 40 liters o f 3

oxygen .

O ne cubic decimeter o f ox ygen at 0 C bar 7 6 0 mm weighs

—
°
.
,
.
,

about Gm so that 1 Gm o f oxygen under those conditions

,

occupies the volume o f about 699 cubic centimeters -

.

PH O S PH O R U S .

Phosphorus for medicinal and pharmaceutical uses shoul d be

w h i te
. It i s p r e s e rve d in glass stop p ered bottle s filled with water -
,

which shoul d be put in a place where there is no danger that they

may be broken .

P h os ph or a te d O i l .

OLEU M P H O S P H OR A T U M ; U . S .

Introduce about 1 0 0 Gm of almond O il into a flask and heat it

°
for fifteen m inutes over a sand bath at a temperature o f 2 5 0 C -
.

A llow it to cool to abo ut 6 0 C a nd then filter it Put 90 °

.
,
.

Gm o f this filtered O i l into a dry an d tared bottl e o f about

1 2 0 Cc Capacity A dd I Gm o f phosphorus previously well
.
'
 P H O S P H O R AT E D O I L .
5 3
2

dried by gently touching it with white blottin g paper Close .

the bottle with a glas s stopper and heat i t in a water bath .

-

until the phosphorus melts Then shake until the phosphorus

.

has dissolved allow it to cool and add enough ether to make the
, ,

total conte n ts o f th e bottle weigh 1 0 0 Gm S hake again . .

Keep the product in glass stoppered bottles o f about 3 0 Cc

-

capacity completely fill ed and put in a coo l and dark place

, ,
.

N ot e s . Keeping the O il o f almond at the high temperature

prescribed for fi fteen minutes expel s moisture and air from it ,

and al so causes the separatio n o f some organic matters which ,

depos it in the form o f a fl occ u l e n t sediment on cool ing and are

then filtered out The oil thus prepared is nearly colorl ess
. .

The phosphorus used should be clean translucent pieces ,

.

T he ether used should be o f the o ffi cial strength ; ordinary com

m e r c i a l ether would render the preparation unclear
.
.

A t a too low temperat ure the phosphorus crystalliz es out ; this

shoul d be care fully guarded against and when it occurs it shoul d
,

not escape observation The separated phosphorus may be readily

.

redissolved by gently warm ing and shaking .

The preparation is not phosphorescent in the dark .

P LA T I N U M . CH LO R I D E .

C H LORO P LA TI N I C A CI D .

D issolve platinum scraps in a mixture O f 1 part o f stron g n itric

acid and 5 parts of strong hydrochloric a c 1 d E vaporate to dry .

ness D issolve the residu e in hot water adding a littl e h y dro

.
,

chloric acid A dd an exces s of sodium hydroxide solution Boil

. .

the mixtu re for about an hour adding a few drops o f alcohol

, .

R edissolve the precipitate in hydrochloric acid filter and add a , ,

hot saturated solution o f ammonium chloride as long as it causes

precipitation o f ammonium pl atinum chloride ( or ammonium
-

chloroplatinate ) Collect the yellow precipitate and wash it with

.

col d and very dilute hydr ochloric acid Then dry it in a por .

c e l a i n dish or on glass Heat it in a porcelain crucible until r e

.

duc e d . When no more ammonia or chlorine is evolved dissolve ,

the metal again in a m ixture o f strong hydrochloric and n itric

5 4
2 C H LORO P LA TI N I C A CID .

aci ds in the same proportions as before evaporate to dr y ne ss

, , ,

addin g hydrochloric acid from time to time until all nitric acid
shall have been expelled R edissolve the residue in hydrochloric
.

acid and evaporate to crystallization .

N ot e s The Obj ect o f treating the first solution with sodium

.

hydr oxide at boiling heat i s to reduce a n y iri dium tetrachlori de

present to trichl oride which afterwards forms a solubl e double
,

salt with ammonium chloride when the ammonium c hl or op l at i n

—

ate is precipitated The alcohol added during the treatment with

.

N a O H i s to decompose any sodium hyp ochlorite formed .

The evaporation to crystallization may be advanta g eously com

p l e t e d over concentrated sulphuric acid or l ime in a desiccator .

Chloroplatinic aci d i s a yell o w deliqu escent salt

D e s cr i pt i on —
.
,

s ol uble in alcohol as well as in water It is cons idered as formed .

by the direct union of platinum tetrachloride an d hydrochloric

acid .

P O TA S S I U M A C E TA T E .

PO T A S S I I A CE T A S .

K C2 H 3 0 2 2 98 .

A cetic acid
Potassium bicarbonate

A dd the potassium bicarbonate graduall y to the aci d ; filter ;

evaporate over a sand bath to dry ness s t i r r 1 n g constantly adding
-
, ,
'

a l ittle acetic aci d i f neces sary to keep it in decided excess to the

end .

M ust be kept in tightly corked bottles .

R e acti on .

N ot e sTheoretically the proportions given in the fore goin g

.

formul a leave the aceti c acid slightly in excess but this excess ,
.

o f acid will be driven O ff during the evaporation and more must ,

be added from time to time as m a y be required in order to main

tain a slightly acid reacti on .

The temperature during the evaporation shoul d be 1 2 0 to

°

°
1 40 C .
5 2 6 P O T A S S I U M A N TI M ONA T E .

I f the mixture O f the antimony and potassium nitrate a fter ,

detonation shoul d be heated to so high a temperature that t h e

,

mass undergoes fusi on the product is not the same being water
, ,

soluble .

The composition is uncertain .

D e scri pti on —
A white or but slightly yellowish powder ins ol ,

uble in water .
[ I f the antimony was free from iron the product
i s whit e ]

P O TA S S I U M A R S E N IT E S OLU TI O N .

LI QUOR PO T A S S I I A R S E N I TI S .

[ L iquor A rs e ni cal i s Fowler s S olution

’
. .
]
A rsenou s oxide in ,
fi n e p ow d e r
'

Potassium bicarbonate
Compound tincture of lavender
D istilled water su fficient , .

Bo il the arsen ous oxide and potass ium bicarbonate with 1 0 0

ml o f distill ed water until solution has been e ff ected Th en add .

enough d istill ed water to make the solution when c old meas , ,

u re 9 7 0 ml and lastly add the comp oun d spirit o f lavender

, , ,
.

Filter through paper .

R e act i on .

N ot e s Prior to the revision o f 1 8 90 the Pharmac opoeia o f the

.

U nited S tates contained a working formula for this preparation

wh ich called for only one hal f as much potas sium bicarbonate -

as i s necessary The proportions were in oth er words equal

.
, ,

parts o f arsenous oxide and potassium bicarbonate The com .

plaints frequ ently made that arsenic separated from Fowler s s o ’

l u t i on on standing may have been due to that error I f 1 2 Gm o f . .

K O H be used instead o f the 2 0 Gm o f K H CO 3 the arsenous

oxide dissolves much more rapidly and the final result is the
same It i s necessary that the compound tincture of lavender
.

be added last in order to obtain a clear solution .

De scri pt i on —
A clear liquid havin g a reddish color
,
an d an
 P O T A S S I U M B EN Z OA T E .

5 7
2

aromatic odor derived from t h e compound tincture o f lavender .

It has an alkaline reaction on l i tmus paper .

P O TA S S I U M B E N Z OA TE .

PO T A S S I I B E N Z OA S .

K C7 H 5 0 2 3 H Z O .
: 214 .

Potassium bicarbonate 82 parts

Benzoic acid . . 1 00 pa rts
D istilled water 5 0 0 parts

D issolve , neutral ize filter and eva p orate to drynes s or to crys

, ,

t a ll i z a t i on .

White Od orless , , or Of faint benzoin odor ; sweetish ; readily

soluble .

P O TA S S I U M B I CA R B O N A T E .

PO T A S S I I B I CA R B O N A S .

KH CO 3 Z I OO .

Prepared by treating potass ium carbonate w ith carbonic acid

gas The gas i s either conducted into a concentrated solution
.

o f the carbonate or over the moist salt To facil itate the abs orp
,
.

tion o f carbonic aci d the potash is m ixed with powdered charcoal

The m
.

oist mas s is exposed to the action o f the carbonic acid gas

until a test portion in solution no longer precipitates a solution
o f magn esium sulp hate .

°
The black mass i s mixed with wate r heated to about 7 0 or .
,

8 0 C the solution i s filtered while warm to remove the charcoal

°
.
,

an d the sil ica which has been precipitated by the carbonic acid ,

an d the filtrate is set aside in a cool place to crystall ize The crys .

tal s are carefully washed to remove adhering mother l iquor which ,

contains normal carbonate a little bicar bonate chloride and sul , , ,

phate o f potassium .

i pt i on A white salt crystall ine and solubl e in

D e scr .
—
parts , , ,

o f water Insoluble in alcohol When absolutely pure th e r e a c

. .

tion is neutral or only very slightly alkaline By heat it i s con .

verted into the monocarb on at e wit h l os s of CO 2 D i ssolved i n .

5 2 8 P O T A S S I U M BI CAR B ONA T E .

water it loses carbonic acid even at ordinary tempera tures but ,

rapi dly and to complete conversi on into normal carbonate above

°

5 0 C In the dry state it does not readily part w ith any of its
.

carbonic acid until at 1 00 C °

.

P O TA S S I U M B I TA R T R A T E .

PO T A S S I I B I TA R TR A S .

K H C4 H 4 0 6 2 1 88 .

I n the manu facture o f w ine a large amount o f impure potassium .

bitartrate is deposited from the g rape juice during the second

fermentation the s alt being thrown out o f sol ution by the alcohol
,

formed Thick crusts are formed in th e vats over the bottom

.
,

and sides The bitartrate formed on the bottom contains more

.

“ ” “
calcium salt than that on the s ides The argols or crude tar .

”
tar must be p owdered redissolved in boiling water freed from
, ,

coloring matter by the additi on o f clay which carries it do w n ,

in settling The solution is then clarified with albumen strained

.
, ,

and allowed to deposit crystals The crystals forming on the .

s ides are again l ess impure than those on the bottom Thei r rela .

tive freedom from calcium salt is indicated by their cl earnes s or

opacity the milky opaqu e cr y stal s being more contaminated with
,

calcium tartrate .

This purified argols or refined tartar is further purified by r c

d u c i n g it to fine powder and digesting this with pure h y drochloric
acid diluted with distill ed water The calcium tartrate is then .

decomposed by the h y drochloric acid forming calcium chloride ,

and free tartaric acid both of which are washed out The mix
,
.

tu re is now allowed to cool s o that most O f the potassium bitar ,

trate dissolved in the water may deposit again a fter which th e ,

“ ”
cream o f tartar i s washed with cold water until the washings
c ease to give any reaction for chlorides and then dried A small ,
.

percentage o f bitartrate is lost by solution in the water with which

it is treated .

'

D e s cri p t fonColorl ess or slightly opaque crystals or a w h i t e

.
—

po wder havi ng no odor but an agreeabl e acidulous taste ,

.

S oluble i n 2 0 1 parts o f water at but in parts of boilin g

water .
 B ORAX T AR T AR .

To powder the product fine is both di fficult and disadvantage

ous ; it should only be reduced to a very coarse powder in a warm ,

mortar and then at once put into warm dry bottles which must be
, ,

tightly corked .

D e s cr i pt i on
“

.
—
A
coarse white powder dry very deliquescent
, , , ,

soluble in its own weight o f cold water but insoluble in alcohol , .

I t has a pleasant acidulous taste .

P o t as s i u m B or o T a r tr a t e
-
.

Potassium bitartrate
Boric aci d
Boiling water

Heat together with constant stirring until diss olved .

and e vaporate to dry ness .

Powder the residue .

D e scr i p t i on A
white powder having an agreeable a c i d u l Ou s
—

taste It is not deliquescent S ol ubl e in twice its wei ght o f

.
.

water : insoluble in alcohol .

P O TA S S I U M BR O M ATE .

PO T A S S I I B ROM A S '

KB r O 3 -
I 67 .

B romine
Potass ium hydroxide
Water

D issolve th e potassium h y droxide in the water in a hal f liter -

flask A dd the bromme ver y gradually keeping the fla sk in c ol d

. .

water and shaking well a fter each addition o f bromine The .

solution a fter all o f the bromine has been added shoul d be neutral
, ,
'

and colorless I f y ellow or red add more potassium h y droxide

.

until sl ightl y alkaline and let stand until colorless a fter which
.
,
“

neutralize carefully with h y drobromic acid Filter the liqu id .

and set it aside in a cold place for some hours Collect the c rys .

tals o f bromate which have separated drain them well R edis ,

.

solve the salt i n three times its w e i g h t o f boiling distilled water '

,
 P O T A S S I U M B RO M A T E .

53 1

filter the solution and s et it in a cool place When col d put it

, .
,

in an ice water bath Collect drain and dry the crystal s

-
.
, .

The res iduar y solutions contain potass ium bromide which

shoul d be recovered in the usual way

R e act i on .

D e s c ri p
ti White or colorless crysta ls O dorles s Tas t e
on .
—
. .

salin e S oluble in 1 4 parts o f water at

. in about 3 parts at
and in about 2 parts o f b oil ing water .

P O TA S S I U M BR OM ID E .

PO T A S S I I B RO M I DU M .

KB r z l 19 .

I ron wire cut ,

B romine
Potassium bicarbonate
D istill ed water .

Put the i ron together with 40 parts o f d istilled water in a flask .

A dd 9 parts o f bromine in small portions at a time s haking the , ,

flask a fter each addition H eat the flask and contents i f meces .

sary t o cause the reaction to be compl eted i e until all odor —

. .
,

o f brom ine ceases and a green s olution o f ferrous bromide results .

Filter the solution A dd the remainder of the brom ine to th e

, .

filtrate and shake well .

Put the potassium bicarbonate in a porcelain dish with 5 0 parts

O f distilled water he a t until e ffervescence ceases an d then raise
, ,

the heat to boil ing .

A dd slowly to the boiling solution o f potassium carbonate t h e

solution o f bromide o f i ron Boil the mixture for fifteen min .

utes The solution shoul d now have a sl ightly alkal in e reaction

. . .

I f not add more potas sium carbonate or bicarbonate until the

,

reaction is alkal ine .

L et the precipitate subside Filter the solution Wash the . .

precipitate on th e fil t e r with hot distilled water and add the wash

ings to the filtrate E vaporate the solution to the requisite degree
.

of concentration and set it aside to cr y stall i ze D rain the cry s .

53 2 P O T A S S I U M B ROM I DE .

tals in a funnel Then spread the salt upon bibulous paper and
.

dry it with the aid o f moderate heat .

A dditional crystal s may be obtained from the mother liquor in -

the usual way .

Instead o f crystallizing the salt the solution may be evaporat e d

to dryness and the bromide g ranulated .

R e act i on .

F e +2 B r z =F e B r then 3 Fe B r + B rz 2
z F e B r2 . 2 F e B r3 ;

an d , finally ,
F e B r2 . 2 F e B r3 -
K
4 2CO 3
—
8 K B r + F e O F e zO 3 .
—
4 CO z .

N ot e s . Ferroso ferric bromide gives better results than fer

-

rou s bromid e because the iron is more readil y and completely pre
c i p i t a t e d in the form o f ferros o ferie oxi de -
.

Potassium bromide crystal lizes best from a sl ightly alkaline

solution B ut i f the salt i s to be recovered in a granular condi
.

tion by evaporation to dryness with constant stirring then the ,

solution should be neutral It i s however necessary to render .

, ,

the solution faintly alkal ine for the purpose o f precipitating a l l

the iron The liqu id can a fterwards be made neutral again by
.

adding enough hydrobromic acid wh ich for this purpose may , , ,

well be made from potassium bromide and tartaric acid .

To improve the appearance o f potas s ium bromide the crystals

may a fter dr y ing be heated for a few minutes at a temperature
, ,

o f 8 0 to °

S e c on d M e th od .

S olutiono f potass ium h y droxide 2 50 parts

B romine about ,
20 parts
W oo d charcoal in fine powder ,
10 parts
Boiling distilled water 1 5 0 parts

Put the solution o f h y droxide in a flask ; add the bromine

gradually with constant agitation until the l iquid has acquired
, ,

a perman entl y brown color E vaporate to dryness ; powder the .

r es idue and m ix it well with the charc oal Throw the mixture .

into a red hot iron crucibl e and when reduced to a state o f fus ion , ,

pour out the contents let cool dis solve it in the boiling water , , ,
5 34 P O T A S S I U M CAR B ONA T E .

from the solution by boiling it down to dry nes s The residue is .

then purified by heating it strongl y in a furnace until all organic

matters have been destr oyed Calcined potash is the result ; it .

contains 5 0 to 8 0 per cent o f potass ium carbonate and is con ,

t a m i n a t e d with sulphate chloride etc By converting this crude

, ,
.

potassium carbonate into bi carbonate most o f the impurities are ,

removed and a nearl y pure normal carbonate can then be pre

,

pared from the bicarbonate .

Formerly pure p ot a s s i u m c a rbon at e was prepared by strongly

, _

heating ( detonating ) potass ium bitartrate w ith hal f its weight o f

potass ium nitrate .

A t S ta s s fu r th potassium carbonate i s pr epared as follows

,

A solution o f magnesium sulphate ( k i e s e r i te ) i s mixed wit h a

solution o f crude potassium chloride both of the material s being ,

taken from the S ta s s f u r t h mines ; a double salt o f sulphate o f p o

'

t a s s i u m and magnesium is then formed together with a double

chloride ( c ar na l l i te ) 3 K Cl + 2 M g S O 4 K M g ( S O ) K M g Cl 3 z
2 4 2
—
.

The double sulphate i s boil ed with m ore potassium chloride which ,

results in the formation O f potass ium sulphate and carnall ite The .

carnall ite decompos es slowl y in water so that the magnesium

chloride can be separated and t h e potass ium chloride i s then
,

u sed over again as before

The potassium sulphate i s then turned into carbonate by a proces s

analogous to L eblanc s m ethod for manu facturing soda The
’
.

resulting product contains 9 2 to 9 3 per cent o f potass iu m car

bonate 2 or 3 per cent o f s odium carbonate 2 per cent o f p ot a s
, ,

s ium chloride and I to 2 per cent o f potassium sulphate

,
.

Crude potash may be partly purified by dissolving it in twice

its weight o f water l etting it stand two days decanting filtering
, , ,

through linen an d evaporating the clear l iqui d in a cl ean 1 ron

,

vessel until a pellicl e begins to form on the su rface The liquid .

is then put in a stone pot and set aside for a week in order that ,

sulphates chlori des etc may cr y stall ize out The solution is
, .

,
.
, .

then filtered and boiled d own to dryness in an i ron pot stirring ,

constantly at the cl ose so as to obtain a dry granular product ,

.

Pure potas sium carbonate for pharmaceutical an d m e d icinal

uses is most readily obtained by heating potassium bic arbonat e
 P O T A S S I U M CAR B ONA T E .

53 5

until the residue is entirely soluble in twice its weight of water ,

or until it has lost from 3 0 to 3 1 per cent o f its weight .

B eing very deliquescent potassium carbonate must be kept in ,

tightl y closed vessels .

P r e pa r a t i on o f P o tas s i u m Ca r bon a t e fr om B i car bon a t e .

Potassium bicarbona t e any des ired quantity , .

Put the salt into a porcelain d ish cover it well with distilled ,

water heat gradually and continue the heat until e ffervescence

,

c e ases an d the l iquid boils Then evaporate to drynes s stirring

.
,

constantly Put the product at once into a per fectly dry bottl e
.

and clos e this tightl y .

R e ac t i on .

N ot es obtain a per fect product the potassium bicarbonate

. TO
used must be perfectl y clean and pure I f it makes an uncl ear .

sol ution in water the bicarbonate sh oul d all be dissolved in about

,

five or s ix times its weight o f water an d the solution filtered

be fore it i s heated to decompose it into normal carbonate water ,

and carbon d ioxide .

The product must be per fectl y d ry and white .

Potassium carbonate suffi ciently pure to fulfill

D es cr i p t i on —
,

th e requ irements o f the Pharmacopoeia is a white granular ,

powder odorless o f strongly alkal ine taste It is very d e l i q u e s

, ,
.

cent S olubl e i n
. parts o f water at and in part O f
boil ing water Insol uble in alcohol
. .

P O TA S S I U M C H LO R A T E .

POT A S S I I C H LORA S .

KCl O 3 :
Formerly prepared by satu rating a solution o f potas sium h y
d rox i d e or carbonate with chlorine whereby hy p ochlorite and
,

chloride o f potassium were formed the hypochlorite being a fter

,

wards d ecomposed by heat into chloride and chlorate

and then ,

3 K Cl O z K C l O 3 +
2 K CL
53 6 P O T A S S I U M C H LORA T E .

The chlorate being much l es s soluble than the chloride is

.

readily separated by cr y stallization from the solution .

L i e bi g s method now used cons ists in treating a m ixture o f

’

, ,

calcium h y droxide and potas sium chloride with chlorine when ,

calcium chlorate 1 5 formed Then the calcium chlorate and p ota s .

sium chloride interact to form potass ium chlorate and calcium

chloride The product 1 s readil y crystallized out from the li quid
.

and purified by recry stallization .

T u r bi d a te d P o tas s i u m Ch l or a te .

K C1O 3 2 1 22 .
4 .

Potassium chlorate
Boiling distilled water

D issolve and filter S tir the filtrate constantly until cold Col
.
.

lect the crystal s on a filter let drain and then dry the pr o duct , , .

N ot e s Commercial potass ium chlorate usually contains p o

.

t a s s i u m chloride and calcium chloride These impurities are .

much more readily water soluble than potass i um chlorate H ence -

.

the t u rbi d a t i on o f the salt results also in purification for the ,

chlorides remain in the mother liquor .

°
When cooled to 1 5 C t h e mother l iquor still retains about .

6 per cent o f its weight o f chlorate o r 3 0 per cent o f the amount ,

o f salt operated upon This must be recovered as far as prae

.

t i c abl e which can be e ffected by evaporating the mother l iquor

,
-

by water bath heat to about one third its bulk stirring until cold
- -

, ,

”
and collecting draining and drying the secon d cr op o f small
,

crystal s in the same manner as the first .

i
D e scri pt on Potassium chlorate consi sts o f colorl ess crystal s
.
—
,
'

or a gl istening white cr y stalline powder Odorless of a cooling

, , ,

sal ine taste S oluble in . parts o f water at I 5 in abo ut 3

parts o f water at and in parts o f b oiling water N early .

insoluble in alcohol E xplos ive with certain readil y Oxidized sub

.

stances esp ecially when heated with them or mixed with redue
, ,

ing agents by trituration or by concuss ion A powerful ox i d i z ,

.

ing agent .
53 8 P O T A S S I U M CIT RA T E .

P O TA S S I U M CIT R A T E .

PO T A S S I I C IT RA S .

Potassium bicarbonate 10 parts

Citric acid . .
7 parts

C rush the citric acid and the bicarbonate separately ; add the ,

latter gradually t o 5 0 parts o f boil ing water an d when e ff e rve s

.

cence ceases add the citric acid a s mall port 1 on at a time until , ,

the l iqu id 1 s n e u t ra l to l itmus paper or but faintly alkaline Fil

v

,
.

ter and evaporate to drynes s stirring constantl y a f ter a pell icl e

,
. ,

has commenced to form so that t h e product may be granular ,

.

R e act i on .

or ,

N ot e s The temperature must not be too high toward the close

.

o f the evaporation as citric aci d and citrates are d e composed at a

,

high heat .

The product should be perfectly white and must be entirely ,

dry before it is bottled .

i pt i on White transparent crystals or a white granular

D e s cr —
,

powder ; odorl ess and o f a pure sal ine cooling taste H y g r o

, ,
.

scopic S olubl e in
. part o f water at and freely solubl e in
boilin g water S paringly soluble in alcohol N eutral to l itmus
. .

paper .

P otas s i u m Ci tra te S ol u ti on .

L I QUOR P OT A S S I I CI T R A T I S .

Citric acid 6 parts

Pota ssium bicarbonate 8 parts

D issolve each in 4 0 parts o f col d water Filter the solutions .

separately and wash the filters with enou gh water to Obtain in

,
,

eac h cas e 50 parts of filtrate M i x the two solutions and when

,
.
, ,
 P O T A S S I U M CIT RA T E .

5 39

e ff ervescence has nearly ceased put the product in a bottl e and ,

cork it tightly .

S houl d be freshly prepared whenever requi red for use .

N ot e sIt is intended that col d water shoul d be used an d that

.
,

the preparation should retain in solution as much o f the carbonic

acid as may be soluble in that volume of the watery liquid A n .

excess o f citric acid is purposely employed in order that the

preparation may have a slightly acidulous taste .

D e scri pt i on .
—
A
clear colorless liqu id o f pure , , , m il d l v saline
taste and slightly acid reaction .

E ff e r v e s ce n t P ota s s i u m Ci tr a te .

Cit ric acid . 63 Gm

Potassium bicarbonate 9 0 Gm
S ugar .
4 7 Gm

Powder t h e i n g r e d i e n t s separately and m i x them thoroughly

'

in a warm mortar D ry the resulting uni form paste rapidly at

.
,

a temperature not e x c e e d i n g 1 2 0 C and when it i s perfectly dry

o
°
.
, , ,

reduce it to a powder of the desired degree o f fineness .

Keep the product in well stoppered bottles -

.

N ot e s . A partial reaction ens ues when the ingredients are trit

u rat e dtogether in a warm ( not h ot ) mortar on account o f th e ,

water always contained in the citric acid and the liberation of a ,

portion o f water formed by the reaction renders the m ixture some

what pasty a t the moderate heat employed When the m ixture .

is dis solved in water a complete reacti on takes place and normal

potassium citrate is formed :

P otas s i u m B or o Ci tr a te -
.

Citric aci d 1 0 Gm

Boric acid 9 Gm
Potassium carbona te I 5 Gm

Water 6 0 ml
D issolve and evaporate to dr y ness stirring constantl y
.
,
.

D es cr i pt i on —
A per fectly white salt readily formin g a ,

solution in water .
5 4 0 P O T A S S I U M CY ANA T E .

P O TA S S I U M .
C YA N A T E .

PO T A S S I I CY A N A S .

K CN O Z S I .

A nhydrou s potass ium ferrocyanide

D ry potass ium dichromate
A lcohol
M eth y l alcohol

M elt the p otas sium dichromate and while it is still warm , , ,

mix it with the powdered anh y d ro u s potassium ferrocyanide .

Put t h e m i x tu r e a small spoon ful at a time into a large iron dish

‘

, ,

heated over a gas stove stirring w ith an iron spatula a fter each
,

addition so that ea ch portion o f powder added i s converted into

a black mass takin g care not to rais e the temperature so high that
,

the mass fuses .

Powder the black mass whil e still warm Then put it m a flask .

and heat it in a water bath for ten minutes with a mixture o f the
-

two alcohols shaking the contents frequently an d well

, .

D ecant the clear soluti on through a pleated fil ter into a beaker

placed in crushed ice .

S e t the flask containing the undissolved black resi due in ice

water w ithout delay .

A fter the crystals have deposited in the beaker pour the mother ,

l iquor back over the black mass in the flask .

R epeat the extractions o f the cyanate from the residue i f nec

essary .

D rain the cr y stals wash them w ith strong ether and dry them
,

i n va c u o over sulphu ric acid .

N ot e s . To make anh y drous p ota s s 1 u m ferrocyanide heat the ,

crushed commercial salt in an iron dish slowly until completely

e ffl oresced or until no yellow unchanged salt remains in the i n
,

t e r i or o f any piece Then powder it whil e still warm and c om

.

p l e t e the drying by heating the powder spread out in a thin layer

on a hot iron plate or dish for two or three hours .

When the mixed salts are heated to a black mass there should
be no evolution o f ammonia and there will be none i f the material s
were fi r s t t h orOu gh l y dried .

The yiel d is about parts The product is ver y unstab l e

. .

D ecomposed by water .
5 4 2 P O T A S S I U M D I C H ROM A T E .

P O TA S S I U M D I CH R O M ATE .

PO T A S S I I D I CH R OM A S .

K 2 Cr 2O 7 —
2 94 .

[ Potassium B ichromate ] .

Chromite ,
in powder
Potassium carbonate
L ime
Potassium sulphate
S ulphuric
”
acid .

Water .

D is solve the potassium carbonate in 3 parts o f water .

S lake the l ime in a large porcelain dish with about two thirds -

of the solution o f potass ium carbonate Then add the remainder .

o f that solution and mix the whole well E vaporate the mixture .

to dr y nes s Heat the residue to 1 50 and stir it until reduced to

.
°

powder M i x this with the powdered chromite

. .

Heat the d ry m ixture to a bright red heat for three or four

hou rs in free contact with air stirri ng frequently ,
.

L et the mass c ool p owder it and m ix the powder with 20

, ,

parts o f water stirring well : S train the solution a n d evaporate

,

the colature until crystal s begin to form .

D issolve the potass ium sulphate in 1 part o f boiling water and ,

add this solution gradually to the concentrated solution of eb r o

mate so long as precipitation o f calcium sulphate is produced
,

by it Then filter while hot

. .

To the hot y ellow filtrate add sulphuric acid diluted with twice
its volume o f water until the l iquid is strongly acid L et the .

liqu id coo l Collect the crystalline precipitate on an asbestos or

.

glass wool filter or on a bed o f broken glas s in a funnel Puri fy

,
.

the salt by recr y stallization .

D rain the crystals of dichromate and dry them with the aid
o f m oderate heat .

R e act i on .

8 CO z ; and 4Cr F e O 2 , l
—

8 H 2O ; then Ca CrO + K 4 z S O 4
z K 2Cr O 4 + Ca S O and , finally ,

2 K 2 Cr O 4 + H 2S O 4 s Cr zO 7 + K Z S O 4 + H zO
 P O T A S S I U M D I C H RO M A T E .
5 43

N ot e s . T he chromite consists mainly o f

but also con Cr zF e O 4
tains silicates When ign ited with the potash and lime it forms
.

ferric oxide the chromates o f potassium and calcium and p ot a s

, ,

s ium sil icate The ign ition m ay be per formed in a mu ffle furnace
.
,

or more advantageously in a reverbatory furnace using the

, , ,

oxidation flame .

The l ime is us ed in l arge excess to keep the mass porou s when

ignited and a portion o f it forms chromate so that the amount
,

o f potassium carbonate required is lessened The chromates are .

leeched out O f the mas s with water and the potassium sulphate ,

is added to Convert the calcium chromate into potassium chromate ,

calcium sulphate being precipitated The liqui d containing the .

chromates is yellow .

When sulphuric acid is added t o the solution o f potassium

chromate the color o f the liqu id i s at once changed from yellow
to orange red and a s the potassium dichromate now formed
, ,

i s much less solubl e in water than the chromate a large propor ,

tion of the dichromate cr y stal lizes out on coolin g The quantity .

o f water prescribed i s adj u sted with this vi ew .

The first crop thus obtained i s nearly free from potas sium
sulphate and may be purified by one r e c rystallization .

The mother l iquo r can be concentrated by evaporation an d

more cr y stal s obtained but the secon d and subsequent crops o f ,

dichromate are di fficult to puri fy because they are so largely con

t a m i n a t e d with potassium sulphate .

B eauti ful crystals o f potas sium dichromate can be eas ily ob

t a i n e d by recrystall izing it from a solution o f 1 part o f the

salt in 1 0 parts o f water allowing the filtered solution to e va p o ,

rate spontaneously .

T u r bid a t e d potassium dichromate may be convenientl y pre

pared from a solution o f I part O f the salt in 5 parts o f boiling
vva t e r .

The mother l iquors obtained in recr y stall izing and in t u rbi d a t

ing the d ichromate yield all o f the salt they c ontain on evaporation ,

to dryness .

D e sc ri pt i on —
L arge clear transparent orange red cr y stals ;
, , ,
-

odorl ess ; taste bitter metallic S oluble in 1 0 parts o f water at

, ,
.

an d in parts o f boil ing water Insoluble in alcohol . .

The water solution turns blue litmus p aper red

-
.
5 44 P O T A S S I U M C H ROM A T E .

P O T A S S I U M CH R O M A T E .

PO T A S S I I C H ROM A S .

K 2 CI O 4 2
‘

1 94 .
5 .

Potassium dichromate
Pot a s s 1 u m carbonate
Wa ter .

Put the potas sium dichr omate in a porcelain dish with 3 0 parts
of water Heat to about . A d d the potass ium carb onate in ,

small portion s at a time stirring well When all o f the carbonate

,
.

has been added h ea t the liqui d to boiling add 2 0 parts o f water , .

filter an d evap orate to crystall izati on D rain and dry the crys
,
.

tals with the ai d o f moderate heat .

R ec over the remainder o f the salt from the mother liquor in

the usual way .

R e act i on . K 2 CrzO 7 + K2 CO a

Y ellow translucent crystals

D e scr i p t i on —
. S oluble in about 1 .
5
parts o f water at

P O T A S S I UM F E R R I C Y A N I D E .

POT A S S I I F E R R I CY A N I D U M .

Potassium ferrocyanide 1 00 parts

L ead dioxide .

Water .

D issolve the ferroc y anide in 1 5 0 parts o f water with the aid o f ,

heat in a flask capable o f hol ding about 6 0 0 parts o f water

,
.

Pass a c u r r e n t o f carbon dioxide into the sol ution heated to

the boiling point A dd 1 0 parts o f lead dioxide to the hot
.

solution a nd stir well B oil for an hou r or longer passing a

,
.
,

stream o f carbon dioxide into the l iqui d during that time .

S houl d the precipitated lead carbonate cau se too viol ent bump
ing remove it by filtering the hot l iquid through a mu sl in fi l ter ,
5 4 6 P O T A S S I U M F ERRO CY AN I DE .

R e crys ta l l i z e d P otas s i u m F e r r ocy a ni d e .

Y ellow prussiate o f potash

Water

D issolve
with the aid of heat Filter Crystall iz e at rest by . .

spontaneous evaporation .

Very large crystals can be obtained Turn the crystals n ow .

and then to permit thei r development in all directions .

D e s cr i p t i on —
L arge soft transparent light yellow cry stals
, , ,
—
,

odorl ess o f mil d sal ine taste S oluble in 4 parts of water at

, .

and in 2 parts o f boiling water Insolubl e in alcohol The water . .

solution i s neutr al to litmus paper .

P O T A S S I U M H Y D R OX I D E .

PO T A S S I I H Y D R OX I D U M .

Potassa .

KO s o .

.
A strong soluti on O f potassium hydroxide prepared as de ,

scribed below m a y be evaporated to drynes s and the residu e

, ,

purified w ith alcohol .

When 1m p u re potas sium hydroxide i s dissolved in alcohol any ,

carbonate sulphate and the greater portion o f a n y chloride pres

, ,

ent remain undissolved and m a y thus be removed The alcohol

, .

may then be distilled off from the clear decanted solution and , ,

the remaining mass is dried and fu sed in a silver capsule A l .

though the solution is brown from the action o f the alkali upon
the organic substances 1 n the alcohol the fused potas sium h y d rox ,

ide will still be white T O prevent the formation o f carbonate

.
,

a little boiled distill ed water i s added from time to time to the

,

alcoholic solution during its evaporation .

N ot e s Potass i um hydroxide must be kept in bottles o f hard

.

glass as i t attacks so ft glass Green glass free from lead is best

,
. .

Glass stoppers in bottles containing potass ium hydroxide or its

solution are acted upon by the alkali an d Often becom so firml y
, , e

fastened to the n eck that they cannot be removed To prevent this .

a little petrolatum may be rubbed upon the stopper be fore ins e rtin g
 P O T A S S I U M H Y DROX I DE .
5 47
'

it This also e ff ectually excludes air an d thus p rot e c ts

’

.
, t h e p ota s
s ium hydroxide from moisture and carbonic acid .

D e scri pt i on D ry
white translucent hard brittle Odorless
.
—
, , , , , ,

very acrid caustic corrosive rapi dly deliquescent when exposed

, , ,
.

S oluble at 1 5 in hal f its weight o f water and in twice its weight

°

of alcohol Freely soluble in boilin g water and in boiling alcohol

. .

Intens ely alkali ne .

Potas s i u m H y dr ox i d e S ol u ti on .

L I QUOR PO T A S S I I H Y D R OX I D I .

S olution o f Potassa .

A n aqueous solution containing about 5 p er cent o f potassium

.

hydroxide ( K O H ,

Potass ium bicarbonate

L ime
D ist il led water su fficient ,
.

D issolve
the potassium bicarbonate in 400 ml o f distilled water ,

heat the s olution until e ff ervescence ceas es and then raise it to ,

boiling S lake the l ime and make it into a smooth mixture with
.

400 ml o f distilled water and heat it to boil ing Then gradually

‘

.
,

add the first l iquid to the second and continue the boil ing for ten
.

m inutes R emove the heat cover the vessel tightly and when
.
, , ,

the contents are cold add enough distilled water to make the ,

whole weigh Gm L astly strain through l inen or remove .

, ,

the clear s olution a fter subsidence o f the precipitate by means o f

, ,

a s yphon .

S ol ution o f potass ium hydroxide should be kept in well stop

pered bottles .

R The potassium bi carbonate is first converted into

e act i on .

normal carbonate by boil ing the solution Then K CO g + .

, 2

The potassium bicarbo n ate i s used in preference to

N ot e s .

monocarbonate because bicarbonate i s readily obtained n early

,

pure whereas carbonate usual ly contains various impurities The

,
.

l ime is used in considerable excess but no l ime will be contained ,

 54 8 P O T A S S I U M HYDROX I DE .

in the finished solution o f p otassium hydroxide , as calcium hy

d rox i d e is insoluble in that liquid Theoretically 1 part o f lime is .

su fficient to causticize parts o f potassium bicarbonate when

the process is conducted a s prescribed in the O fficial f ormula which ,

is the one given above I t would be a deci ded improvement up on

.

this process to first wash the calcium hydroxide throwing away ,

the first portion O f water used as in the proces s for mak ing l ime
water ; this removes dust salts etc A n unnecessarily large ex , ,
.

c ess o f l im e is disadvantageous in that the calcium h y droxide

settles more sl owly than the carbonate .

Potass ium carbonate may be causticized by calcium hyd roxide

without the aid O f heat but the calcium carbonate then formed
,

is very l ight settl es slowly and retains much l iqu id By using hot
, , .

solutions as directed by the Pharmacopoeia a much more dense

, ,

calcium carbonate is formed wh ich settles rapidly so that the ,

soluti on can be separated with les s waste .

N ot less than 8 parts and preferably 1 2 parts o f water should

,

be taken for each part O f normal potassium carbonate u sed The .

proc es s o f the U S Pharmacopoeia employs about 1 0 5 parts for

. .
,

9 0 parts o f bicarbonate corresponds t o about 77 parts o f

carbonate and the water used is 8 0 0 parts I f a more c on c e n
,
.

t rat e d sol ution is used the decompos ition will be incomplete The .

reaction i s complete when the liqu id no longer e ff ervesces with

d ilute acid a n d d oe s not cause a turbidnes s when dro pped into
,

clear l ime water .

S olution o f potass ium hydroxide can w ell be evaporated in a

clean bright iron pot down t o about
,
specific weight without
danger o f attacking the iron A stronger solution however .
, ,

would attack the metal In any event a solution o f pot assium

.

h y droxide shoul d not be allowed t o remain long in contact with

iron and whenever such a solution i s to be concentrated in an
,

iron vessel the e va p ora t 1 on shoul d be hastened as much as

,
~

possible .

S training or filtering t h e solution is l iabl e t o caus e its d i s c ol

oration It is therefore best to l et it stand long enough to be
.
, ,

come clear by subsidence and then to draw off the clear liquid
'
by m e a n s o f a glass s y phon .

The glass stoppered bottles used t o contain it should be made

-

o f green glas s free from l ead and the stoppers rubbed with ,

petrolatum .
 O T A S S I U M H Y P O PH O S PH IT E
P .

P O TA S S I U M H Y PO PH O S PH I T E .

PO T A S S I I H Y PO P H O S PH I S

KP O H 2 2
: 1 04 .

Calcium hypophosphite
Potass ium carbonate
‘

D i s s ol v esalt separatel y in 7 parts o f b oiling water M i x

e ac h .

the solutions Filter off the calcium carbonate and evaporate the
.
,

filtrate to dryness over a water bath stirring constantly so as

,
-
,

to Obtain a granular product .

N ot e s The temperature during the evaporation shoul d not

.

°
exceed 8 5 C as hypophosphites are prone to decompose with
.
, .

violent e x p l o s i on w h e n heated to nearly 1 0 0 C or"higher

.
°
.
,
.

The product may be freed from potassium c a rbonate and other .

impurities by dissolvi n g it in ten times its weight o f alcohol fi l t e r ,

ing evaporating the s oluti on t o the consistence o f t hick syrup

, ,

and setting this aside to solidi fy into a cr y stall ine mass .

R e act i on . Ca P O 2 H ) 2 2
—
K 2 CO 3 : Ca CO 3 —
2 K PO zH 2 .

D e s cri p t i on . A
white granula r s a lt e a s i l y soluble in water and
—
, , ,

weak alcohol It may be obtained in crystall ine form from the

.

aqueou s solution .

P O TA S S I U M H Y PO T H I O S U L PH I T E .

P O TA S S A S U L PH U R A T A .

S ulphurated Potas s a .

( L iver o f S ulphur ) .

S ubl imedsulphur
Potass ium carbonate

M ix by t r i t u r a t 1on Heat the m ixtu re gradually in a c overed

.

crucible which shoul d be only hal f fil l e d until the mass ceases

,
—
,

to swel l and is completely melted Then pour the molten mass .

upon a cold stone or glass slab and when it has become hard , ,
“
 S UL P H URAT E D P O T A S S A .
55 1

and nearl y cold break it into pieces and keep it in a dry bottl e
,

o f hard glass which must be tightly closed .

R e a cti on When the prop ortions o f the materials are as here

.

given the reaction is frequently represented as 4 K CO l TO S

, 2 3
— — :

3 K
z S S2+ K S O + 4 CO
z but the following
4 i s probably the prin
c i p a l reaction : T he
composition o f the product depends much upon the temperature
which should not be t oo high It i s quite probabl e that sulphur .

i s soluble in fused potassium sulphide ( K S ) as wel l a s in a Q

water solution o f it The proportion o f sulphur used is in some

.

formulas greater and in others l es s ; yet the product is in each

case physicall y homogeneous When a solution o f sulphurated .

potassa U S P is mixed with a solution o f copper sulphate

, . . .
,

the reaction between them i s : Cu S O + K S Cu S + K S O 4 + S 4 2 3

z
2
.

F rom the fact that only one third o f the sulphur contained in -

the s u lp h u ra t e d p ot a s s a forms Cu S in this case it i s obvious that ,

the sulphu r is not all o f one kind In other words the sulphur in .

sulphu rated potassa made by fusing sulphur and potas sium car
bonate together i s partl y positive a n d partly negative a s woul d ,

be the case in K S S 2 2
.

N ot e s The potassium carbonate and the sulphur must both be

.

quite d ry The y should be finely powdered and well m ixed in

.

order to O btain a uni form product It is wel l to pass the pow .

dered m ixture thr ou g h a s ieve o f about 60 0 meshes to the square

centimeter .

A covered iron dish will answer well for the fusion and a ,

moderate heat ( from 1 5 0 to 2 5 0 C ) shoul d be used The mas s ° °

. .

shoul d be occa sionall y stirr ed .

The heat should not be higher than i s nec e s sary to fusion w ith
out turning the mixture into a thin l iquid .

When the evolution o f carbon dioxide ceases and the whol e ,

mas s fuses quietly and compl etely a sampl e should be taken out ,

and put into about twice its weight o f water ; when it dis solves
entirely w i th ou t s e pa r a ti on of s u lph u r the fused mass is allowed
, ,

to cool somewhat and is then poured upon a slab ( or into an

,

Oiled iron d ish ) and covered well ( with a bell glas s or an inverted
,

dish ) to exclude air and moisture until nearly cold It i s then ,

.

broken and immediately trans ferred to a dry container .

D e scri pt i on .
—
L iver brown pieces having a bitter alkal i n e taste
55 2 P O T A S S I U M I ODA T E .

and an odor o f hydrogen sulphide Hygroscopic ; soluble in twic e .

its weight o f water at 1 5 C leaving a s mall res idue A lcohol °

.
, .

dissolves the potassium sulphide leaving the sulphate and thio ,

sulphate .

P O TA S S I U M I O D A T E .

PO T A S S I I I ODA S .

KI O 3
: 2 I3 .
5 .

Potassium permanganate
Potassium i od ide
Water ,

A lcohol ,

A cetic A cid .

D issolve the permanganate in 5 0 parts o f hot water add the ,

iodide dissolved in 2 parts o f water heat the m ixture over a

‘

water bath for about twenty minutes or hal f an hou r adding

-
,

alcohol drop by drop at the en d until the liqu id is decolorized ,

and then filter Wash the precipitated p ota s s i u m m a g a n i t e on the

.

filt er and add the washings to the filtrate To the filtrate add .

enough acetic acid to render the reaction on test paper distinctly -

acid E vaporate the liqui d to about 1 5 parts ; l et it cool ; separate

. .

the crystals from the m other liquor wash the product with alcohol -
,

and dry it .

R e act i on . KI l - —
KZ M nZO 5

N ot e sThe acidification with acetic acid is neces sary to prevent

.

the product from having an alkal ine reaction due to adhering

alkali which it is extremely diffi cult to wash away
,
.

D e scr i p t i onwhite granular cr y stall ine salt o f perfectly

—
A , ,

neutral reaction to test paper -

.

P O TA S S I U M I O D I D E .

POTA S S I I OD I D U M .

KI : I 65 5 . .

S olution o f potassium hydroxide ml

Iodine 1 00 Gm .
, or su ffi cient
Wood charcoal in fine powder ,
. I 5 Gm
Boil ing distilled water su fficient ,
.
5 54 P O T A S S I U M I O DID E .

S e c on d M e th od .

Iron wire cut ,

Iodine
Potass ium bicarbonate
D istilled water su ffi cient ,
.

D igest the ir on and 1 5 parts o f the iodine with 5 0 parts o f

water in a flask until al l odor o f iodine ceases and a green solution
o f ferrous iodide results Filter this and in the filtrate dissolve .
,

the remainder o f the iodine .

Put the potassium bicarbonate into a dish with 8 0 parts of dis

tilled w ater h eat until e ff ervescence ceases and then raise the
, ,

heat to b oiling A dd slowly t o this boiling hot solution the fil t

.

ered solution o f th e iodides or iron Boil the mixture fo r fi fteen .

minutes ( I f
. all the iron has not been precipitated from the so
l u t i on add a little more potassium bicarbonate )
,
Filter e va por .
,

ate and crystallize

, .

R e ac t i on . then 3 F 1 é
1
2+ 2
2 F e 1 2
2 Pe 1 finall y

Fel 2 2F e I 3
.

N ot e s . A s seen from the equation a solution

iodide ,
Of
‘

f e r rou s
i s first made This can be at once treated with potassium car
.

bonate to obtain the p otass ium iod ide

F e 1 2 + K 2 CO 3 2 2 KI + e CO 3
F .

B ut in this case t h e iron i s separated wit h greater di fficulty .

,

being first thrown down as fer rous carbonate wh ich at once

.
,

begins to lose c arbonic acid and at the same ti me oxid izes so , .

th at the precipitate gradually changes from l ight gray to blu e ,

y ell owi sh br o w n a n d finally to brown ferric hydroxi de F e ( O H ) 3

, ,
.

A ll o f the i ron does not separate at once however so that during

,
, ,

the sub se quent evapor ati on o f the filtered solut i on o f iodide o f .

potass ium a consi derable quanti t y o f fl oc c u l e n t deposit o f ferri c

h y droxide makes its appearan ce and must be filtered out .

This d i ffi cul ty may be remedied to a g re at e x t e n t by c onvert ,

ing the fer rous iodide int o ferrico fe rrou s iodide by adding the
.
-
,

req uired additional quantity o f iodine The precipitate will then . .

,

after the boil ing be black magnetic oxide of i ron which i s very
-
, ,

dense and therefore more easi ly separated than ferric hydroxi de

, ,
.
 PO TAS S I U M I OD ID E .
555

When the s olution o f iodide o f iron has all been added to the
hot solu tion o f p otass ium carbonate the l iquid shoul d have a
.

neutral or faintly alkaline reaction S houl d it instead be acid .

,

add more potassium b icarbonate I f too alkal ine add some h y .

d r i od i c aci d prepared from tartaric acid and KI .

T hi r d M e th od .

R ed p hosphorus
Iodine
Potassium carbonate .

D istilled water suffi cient , .

Put t h e p h os p h o ru s in a porcelain dish with 3 5 parts o f d is

tilled water and warm the l iquid over a wat er bath to about -

C A dd the iodine a l ittl e at a time stirring gently until

.
, ,

the liquid becomes permanently colored .

D ecant the clear solution fr om the residue wash the latter with ,

a l ittle distilled water and add the washings to the decanted

,

solution .

A d d eno ugh calcium hydroxide mixed with water milk o f

l ime to impart a slightly alkaline reaction to the l iquid .

Filter the sol ution an d add the potassium carbonate d iss olved
,

in 1 0 parts O f water stirring wel l

,
.

D ecant the liquid from the precipitate wash the latter with ,

som e distilled water add the wash ings to th e d ecanted solution

, ,

and filter the liqu id .

E vaporate the solution to c rystall ization .

R e act i on s . The first reactions result in the formati on of PI

and PI 5 .
_
Then PI 3 + 3 H 2O H 3 P0 3 + 3 H I ; and
2 :

H 3 PO s + I 2 + H 2O z H 3 PO 4 + 2 H L A t the same time this r e

action occurs : PI B + 4 H zO z H 3 PO 4 + 5 H L Hence two mole
cul es o f H g PO 4 and ten molecules o f H I are the final products .

When calcium hydroxide i s added the reactions are

and
—
2H O an d
 55 6 P OT A S S I U M I OD ID E .

When the calcium phosphate has been filtered out and the p o
t a s s i u m carbonate i s added t o the solution of Ca I 2 the reaction is

Ca I 2+ K2CO 3 2 2 KI + Ca CO 3 .

N ot e s The use o f red instead o f ordinary phosphorus lessens

.

the danger involved in this proces s But great care should be ex .

e r c i s e d lest the phosphorus iodides decompos e with violence .

A fter the addition o f the prescribed amount o f potass ium car

bonate to the solution o f calcium iodide t h e fi l t e re d l iquid should ,

be tested with a few drops o f potassium carbonate solution and , ,

i f furt her precipitation is caus ed thereby more potass ium car ,

bonate solution shoul d be cautiously added a little at a time , ,

stirring well until precipitation is no longer produced by it

, .

The final solution befor e evaporation should be o f a sl ightly

, ,

alkalin e reaction Instead o f evaporating to cr y stallization the

.

salt may be granulated .

D e scr i pt i on
Colorles s or white translucent cubical crystal s or
—

a granular crystalline powder with a faint iodine like Odor and ,

-

pungent saline bitterish taste S lightly hygroscopic S oluble

, , . .

at 1 5 in °
part o f water and in 1 8 parts o f alcohol ; in
part o f boiling water and in 6 parts o f boiling al cohol The
,
.

water solution has a neutral or only faintly alkal ine reaction on

—

test paper
-
.

P O TA S S I U M N ITR A TE .

POT A S S I I N IT RA S .

KN O 3 : 10 1 .

Potas sium chloride

S odium nitrate
Water .

M ixthe salts in a porcelain d ish with 1 2 parts o f water Heat .

at the boil ing point stirring well and without interruption for
,

several minutes Filter E vaporate the filtrate to 8 parts S h ould

. . .

any salt separate during the eva p oration heat the liquid to boil
ing and fi l t e f again L et the filt rate stand several hours Col
. .

l ect the cr y stals o f potassium nitrate and recrystalliz e several

times to remove adhering sodium chloride D ry the product per .

f e c t ly .
 "

55 8 P O T A S S I U M N I T RA T E .

parts o f the salt and ,

1 60 parts of alcohol o f 10 94; St rength
parts .

T u r bi d a te d P otas s i u m N i tr a te .

Potass ium nitrate

Boil ing w ater

D i ssolve , filter and stir until col d

,
. Collect drain, , an d d ry the
crystal s .

E vaporate the mother liquor nearly to dry ness stirring con -

,

s t a n t l y and dry the residue which shoul d be collected separately

, ,

or t u rbi d a t e d as before i f the quantity i s suffi cient to render i t

advantageous .

P O TA S S I UM O L EA T E .

S ft
o S oa p .

[ S apo M ollis . Green S oap . Pot as h S oa p ] -

L inseed oil
Potas s ium hydroxide
A lcohol
Water su fficient
,
.

Heat the oil in a deep porcelain dish on a water bath to a tem -

p e r a t u r e o f about 6 0 C D issolve the potassium

°
hydroxide in
.

4 5 0 ml o f water add the alcohol to the solution and then gradu

, ,

ally add this mixture t o the oil stirring constantly continuing , ,

the heat and stirring until the product becomes per fectly solubl e
in boil ing water without the separation o f oil y drops ( which may
be ascertained by tasting a small portion from time to time ) .

Then allo w the product to co ol and trans fer it to S u itable con

tai n e r s .

A soft brownish yellow sol id translucent in thin

D e s cri pt i on —
,
-
,

layers S houl d make an almost cl ear solution in 5 parts o f water

. .

S hould dissolve in 2 parts of hot alc ohol leaving not over 3 per ,

cent O f undissolved resi due .

 PO T A S S I U M OX ALA T E .
‘

5 59

P O TA S S I U M OXAL A T E ; N O R M AL .

PO T A S S I I OX A L A S .

K2 C2O 4 . 2 H O . .

O xalic acid 63 parts '

Potassium bica rb onate arts

“

1 00 p
D istilled water arts
‘

50 0 p

the oxal ic acid i n t h e water by the aid o f h e at ; then

'
D is solve
add the potass ium bicarb onate N eutral ize p e rfectly E vaporate . .

and crystallize .

R e a ct i on . 2 KH CO 3 + H 2 CzO 4 z K2CzO 4 l — —
2H 2
0 + 2 CO

D e scri pt i on —
T ransparent prisms or pyramids eas ily sol ubl e in ,

water .

A C I D P O TA S S I U M O XA LA T E .

K H C, O , . 2H z O

O xalic acid
Potassium bicarb onate
D istilled water

D issolve
the potassium bicarbonate in the water by the aid o f
heat boiling the liquid until e ff ervescence ceases ; then add the
,

oxal ic acid dissolve filter whil e hot a ri d set as ide to co ol and

, , ,

crystallize .

R e act i on s . 2 KH CO 3 : K CO l
2 s
— —
H Q O + CO °

then ,

D e s bri pt i dn .
—
O ccurs usually as anhydrou s prisms c ry stal ~

l i ze dwith one or two molecules o f water .

It is not readily sol ubl e in cold water .

5 6 0 P O T A S S I U M P ERM AN G ANAT E .

P O TA S S I U M P E R M A N GA N A T E .

PO T A S S I I PE R M A N GA N A S .

KM nO ,: 1 58 .

M anganese d ioxi de
Potassium h y droxide
Potassium chlorate
Water .

Heat the finely powdered manganese dioxide to a red heat .

L et it cool a gain Put the potassium hydroxide in a porcelain

.

dish add 1 0 0 parts o f water and then the potass ium chlorate
, ,
.

Heat until s ol u t i oh is e ff ected Then a dd the manganese dioxide . .

E vaporate the m ixture to a thick pasty mass stirring constantly ,

during the evaporation to make the mixture uni form Heat the .

paste to redness in an iron crucible or dish which should not be ,

more than hal f filled as the mas s swell s on heating When water .

vapors ceas e to escape an d th e mass bec omes dark green or brown

an d qu ite hard let i t c ool remove it from th e crucible or dish
,
.

, ,

and powder it M i x it w ith about 3 5 0 parts o f water boil the

.
,

mixture for an hou r passing a current o f carbon dioxide into ,

the boiling l iquid during that period The green color o f the .

l iquid i s changed to violet by thi s treatment and a brown p r e c i p i

tate is thrown down S e t the l iqu id as ide until the precipitate has
.

subsided Filter the solution through asbestos or glas s wool

. .

Wash the precipitate with a smal l quantit y o f hot water and add
the washings to the other filtrate E vaporate rapidl y until crys .

tals begin t o sepa rate Then allow the solution to cool in a well
.

covered ves sel Colle ct the crystal s E vaporate the mother

. .

li quor a fter adding a little hydrochloric or sulphuric acid to i t

, ,

an d again let crystal s be formed R ecrystall ize this s econd crop .

o f cr y stals before adding it to the first D ra in the crystal s by .

suction and dry them over sulphuric acid .

R e a ct i ons .

3 M nO 2 —
l
-
6 K O H l -
t he n ,

and
KO H l — —
CO z z K H CO 3 .
5 6 2 RO C H ELLE S AL T .

of tartar and continu e heating until all is dissolved S e t the

, .

solution aside for a day or two Then filter evaporate the filtrate .
,

to n ine parts or until a pellicle forms and then set it aside to crys
, ,

t a lli z e .

R e ac t i on .

2 KH C4 H 4 O G+ N a 2CO 3 : 2 K N a C4 H ,O6
—
H O + CO
N ot e s . A slight excess o f sodium carbonate is prescribed be ,

cause the salt crystallizes best from a slightly alkaline solution .

A ny excess o f s o dium carbonate will remain in the mother l iquor .

L arge crystal s are easil y Obtained The crystals shoul d be hastily .

rinsed with a l ittl e cold distilled water T he mother liquor is .

usually colored in or e so the far t her the evaporation is ca rried

,
.

( S e e also ,
Potassium Ta rtrat
,
e )
The d irection to allow the s oluti on to stand some time before
filtering and evaporating to cr y stall ization has for its obj ect the ,

deposition o f any calcium tartrate and carbonate .

The crystals must be dried w ithout the aid O f heat .

A fter s everal crystallizations the mother liquor bec omes col ,

-

ored It may be dec olorized with animal charcoal i f the quan

.

tity operated upon j ustifies it The tartaric aci d in the last .

mother liquor may be recovered in the form o f cream of tartar

—

by precipitation w ith hydrochl oric acid .

D e scr i pt i on Col orless transparent prisms or a white powder ;

.
—
, ,

odorless ; taste cool ing sal ine S lightly e fflor e s c e nt in warm d ry

,
.
,

a ir S oluble in
. parts o f water at and i n l ess than its own
weight of boiling water Practically insoluble in alcohol N e u . .

tral to l itmus paper .

P O TA S S I U M TH I O CY A N A T E .

PO T A S S I I T H I O CY A N A S .

( Potassium S ulphocy anate . R h od a n k a li u m .

)
K CN S ; 9 7 .

A nhydrous potassium ferroc yanide

Potassium carbonate
Washed sulphur
A lcohol .
 P O TA S S I U M THI O CY ANA T E .
563

M ix the thorou g hly dried and powdered s ol ids very intimatel y

by trituratin g them to g ether in a mortar Heat the mixture .

slowly until the mass fuses L et it cool E xtract the thiocyanate

. .

with hot alc ohol and coll ect the crystals which deposit on cooling .

E vaporate the mother liquor to obtain more -

.

N ot e sFor directions how to make the anhydrous potass ium

.

ferrocyanide see notes under potass ium cyanate .

D e scri pt i on white crystalline salt of bitter saline taste

—
A ,
.

R eadily water soluble -

.

P O TA S S I U M S UL PH A T E .

POT A S S I I S UL P H A S .

Kz S O ,

D ilutedsulphuric acid
Potassium bicarbonate

Place the acid in a porcelain dish and neutral ize i t with the
potassium bicarbonate gradually a dded stirring a fter each ad
, ,

dition until e ff ervescence has ceased be fore adding m ore Try .

th e solution with test paper and add more potassium bicarbonate

-
,

i f necessary to render the reaction quite neutral Filter the solu .

tion and evaporate to crystall ization .

R e act i on .

Colorl ess odorless crystals o f a som ewhat bitter

D e s cr i pt i on .
—
,

ish saline taste S oluble in . parts o f water at and in 4

parts of boiling water Insoluble in alcohol. .

P O TA S S I U M S UL PHIT E .

PO T A S S I I S U L PH I S .

KQ S O s . 2H zO
: 1 94 .

Prepared by passing sulphurou s oxi de into a s olution o f p o

t a s s i u m carbonate until all carboni c acid has been expelled and ,

then a ddin g another equal quantity o f potassium carbonate T he .

 6
5 4 P O T A S S I U M S UL PH IT E .

solution is then evaporated to crystallization S e e S odium S u l

“

p h i t e .

D e s cr i pti on
Col orles s crystals or powder readily solubl e in
—
,

water and but slightly in alcohol

, D ecomposed by acids yielding .

5 0 2 without deposit o f sulphu r .

P O TA S S I U M TAR TR ATE .

POT A S S I I TA R TR A S .

K2C4 H , O 6 H zO z 4 7 o .

Potassium bicarbonate
Cream of tartar .

D istilled water .

D issolve the potassium bicarb onate in 5 0 pa rts o f water w ith

the ai d o f su fficient heat to cause e ff ervescence R a i s e t h e tem .

p e r a t u r e o f the liqui d to the boiling point A dd the cream o f .

tartar in small portions at a time stirring well until all h as dis ,

solved leaving the liqu id faintly alkaline in its reaction on test

,

paper Filter E vaporate th e filtrate until s igns o f c ry s t a lli za

. .

tion appear Then set the dish aside for three or f our days in
.

a col d place Collect the crystal s in a funnel an d let them be

.

well drained .

E vaporate th e mother liquor over a water bath to one th ird o f - -

its volume and again set aside to cr y stall ize .

D ry the crystals by moderate heat .

Keep the product in a tightly closed bottle .

R e act i on .

N ot e s S hould t h e reaction O f the s ol u t i on n ot be faintly alka

.
'

line ,
make it s o by the addition o f more o f the carbonate or the
t artrate a s may be required The salt crystall izes best from a .

slightly alkal ine solution .

When colorl es s crystal s can no longer be Obtained fr om the

mother l iquor dilute the l iquid with an equal volume o f water
-
, ,

filter an d add hydrochloric acid as lon g as any precipitate is

,
5 6 6 ,
S I LV ER .

dish until it fuses Continue heatin g until the fused salt

c e l a i n. .

be g i ns to turn black L et it cool D iss olve the mass in I 5 0

. .

parts o f water and filter the solution A dd ammonia water stir .

,

ring well until the l iquid acquires a decided ammoniacal Odor

, .

M ake a forty per cent solution o f sodium bisulphite in water

and filter A dd a su fficient quantity o f this s olution to the a m
.

m on i a ca l s ilver sol ution to reduce the cupric salt in the latter t o

the cuprous state, This may be known to have been accomplished
when a sample o f the blue liquid becomes decolorized on heating it .

L et the li qui d stand in a cold place until m ost o f the s ilver has
c rystall ized out which it does slowly Collect the crystal s wash
,
.
,

them with c ol d distill ed water and then cover them with strong
ammonia water a n d let stand for a few hours Wash a g a i n w it h .

distilled water an d then dry .

To recover the remainder o f the s ilver f r om the mother l iqu or

heat it at from 60 to 7 0 until all o f the metal has precipitated
° °
,

an d wash and dry this precipitate in the same way as the other .

S I LV ER CH LO R I D E .

AR GEN TI C H L OR I D U M .

A g Cl= 1 4 3 4 . .

S ilve r nitrate
S odium chloride
D istilled water .

D issolve the s ilver nitrate in 2 00 parts o f distilled water and ,

the sodium chloride in 1 0 0 parts Filter both s olutions Heat . .

the sodium chloride solution to boil ing A d d the s ilver s olution .

to that o f the sodium chloride stirring well Wash the p r e c i p i , .

t a t e d silv er chloride w ith b o iling distilled water until the wash

ings are perfectly tastel es s D ry the product with the aid o f .

moderate heat .

Keep it in dark amber colored bottles —

.

R e a ct i on ?

D e s cri p ti on .
— white heavy insoluble Odorless and tasteless
A , , ,

owder R eadily solubl e in ammonia water D arkened by light

p
. .
.
 S I LV ER C Y AN I DE .
567

S IL V E R CYA N I D E .

AR G EN TI CY A N I D U M .

A g Cs 34 .

S ilver nitrate
Potassium c y an ide
D istill ed water .

D iss olve the s ilver n itrate in 5 0 0 parts and the potassium cyanide
in 20 0 parts o f distilled water A dd the sol ution of potassium .

c y anide to the solution o f silver nitrate gradually and stir well , ,

.

Wash the precipitate with distill ed water and dry it w ith the aid ,

o f moderate heat Keep it well protected against light

. .

R e a ct i on . A g N O 3 + K Cy z A g Cy + K N O 3 .

N ot e s The solution of s ilver n itrate might advanta g eously be

.

acidulated with nitric aci d .

D e s cr i pt i onr
heavy white Odorles s and tasteles s powder
—
A , , .

Insoluble in water or alcohol D arkens on exposure to li ght . .

S I LV E R I OD ID E .

AR G EN TI I OD I D U M .

A gI : 234 .
5 .

S ilver nitrate
Potass ium i od 1 d e

D issolve the salts separately each in a bout 1 2 parts o f dis ,

'

tilled water Pour the sol ution o f si lver nitrate graduall y and
.

with constant stirring into the solution o f the iodide Collect the .

precipitate on a filter wash it well with distilled water an d dry

, ,

it between bibulous paper .

The product i s to be kept in w ell cl osed bottles and protected

from light .

R e ac t i on . A gN O 3 + Kl g I K
+ N O3 .

D e scri pt i on —
he avy l ight yellowish powder ; odorl es s and
A ,
-

tasteless . Insolubl e 111 w at er and a l cohol .

 S I LV ER N IT RA T E .

S I LV E R N I TR AT E .

A R G E N TI N IT RA S .

A gN O 3 I I 7 O .

S ilver 3 0 parts
N itric aci d ( containing 68 % of H N OS ) 35 parts
D istilled water 5 0 parts

A dd the n itric acid an d the water to the metal in a flask and ,

heat gently until d issolved D ecant the cl ear l iquid into a por
.

c e l a i n capsule evap orate, and s e t aside to crystallize L et the

,
.

crystal s drain in a glass funnel and d ry them by exposure to the ,

hot a ir carefully avoiding contac with organic matter

, t .

Keep i t in an amber colored bottl e , with glas s stopper

.
.

R e ac t i on .

N ot e s
I f coin is used it should be well cl eaned w ith hot soda
.

solution before it is dissolved in the acid .

The metal dissolves rapidly at first and with considerable ,

evolution o f heat A fterwards however the reaction i s slower

.
, ,

as the s olution be comes more concentrated To prevent loss by .

spurting the neck O f the flask may be covered by a watch cry stal
,
-
.

‘
When large quantities are operated upon the flask may be set
in a warm place and left for several days The clear liqu id is .

then decanted from the resi due and the latter i s washed the , ,

filtered washings being added to the other solution I t i s best .

to have the metal present in excess so that a smal l quantity of it

remains undissolved By thi s precaution vap ors o f n itric aci d are
.

avoided in the subsequent evaporation .

To re move copper i f present the solution is evaporated to dry

, ,

n ess and the mas s fused m a thin porcelain capsule ( M eissen

dish ) over a sand bath keeping the salt fused two o r three hours
-
,

until a small quantit y o f it when removed from th e dish dis

.

, .

solved i n water and the solution filtered is not turned blue by

, ,

ammonia w ater A ll o f the copper nitrate which was present has

.

now been reduced to cupric oxide The mas s is then p ou red into .

a clean polished i ron dish or mortar and allowed to cool ; it can ,

not be allowed to co ol in the porcelain dish for that w ill burst .

57 0 S I LV ER N IT RA T E .

D e s cr i p t i on .
—
A
heavy opaque solid usuall y o f a grayish color ; ,

fracture granular crystalline .

A bout 9 5 per cent o f t h e mass i s readily soluble in water The .

remainin g 5 per cent consisting o f chloride is n ot It i s not So

, ,
.

quickly soluble as the pure salt .

D i l u te d S i lve r N i tr a te .

S ilver nitrate
Pot a s s 1 u m n 1 t ra t e

Fu se the salts together in a porcelain d ish over a sand bath at -

as low a temperature as poss ible stirring constantly until the ,

mass flows quietly Then cast the melted mass in suitabl e moul ds ]
.

N ot e s . S ilver
nitrate alone when fused an d moulded into pen ,

cils is too brittle and it happens frequ ently that a less energetic
, ,

caustic than the pure silver salt i s desired Hence the pharma .

c op oe i a s prescribe m ixtures o f s ilver nitrate and potassium nitrate ,

and some pharmacopoeias contain two such mixtures one c onsist —

ing o f equal parts and another o f one part s ilver nitrate and two
,

parts of potassium nitrate The Pharmacop oeia o f the U nited .

S tates prescribes equal parts in the S ixth R evision but

orders the more diluted kind in the S eventh R evision

D e s cri pt i on hard solid finely crystalline and readil y

.
—
A , ,

soluble in water It has a metallic taste and cau stic properties

.

similar to the pure nitrate .

M ixtures o f silver nitrate an d potas sium n itrate in other pro

portions are also o ffered by manu facturers o f chemicals and d is ,

t i ng u i s h e d from each other by numbers .

S i lve r N i tr a te w i th L e ad .

This caustic in pencils is made by fusing together 1 5 parts o f

lead nitrate and 8 5 parts o f s ilver nitrate moulding the mixture ,

into sticks of the usual form It is recommended as preferable .

to other s ilver nitrate caustics on account of its greater toughness

and softness It can be sharpened to a point with the kni fe like
.
'

a lead pencil .
 S I LV ER OLEA T E .
57 1

S I LV E R OLEA T E .

AR G EN TI OLEA S .

A g C1 8 H 330 2
2 8
3 9 ‘

Crystallized s ilver nitrate . 25 Gm

White castile s oap in fine powder , 4 5 Gm

D issolve the s ilver n itrate in m 1 o f cold distilled water

and the soap in 5 00 ml o f hot water A d d the soap solution v e rv .

slowly and with brisk stirring to th e S ilver solution Collect the .

oleate drai n it and wash it several times with cold distilled water
, , .

D ry it w ithout the aid of heat protecting it from exposure to,

light or dust .

R e act i on . A g N O 3 + N a C1 8 H 33 O z
z A C
g 1 8
H 33
O z l
—
N
—
a N O , .

N ot e s . S ilver
oleate i s very s ensitive to l ight heat and contact , ,

with dust impu re air etc When first formed it i s nearl y white
, ,
.
,

but cannot be kept so unless it is prepared at night or in a dark

room D ecomposition may be t o a great extent prevented by sur
.

round ing and covering with yell o w paper the funnel in which the
oleate is washed I f properly precipitated it is finely granular
.
,

and it should be dried by the use o f white blotting paper f r e ,

quently changed I f carefully protected the product will be o f

.

a l ight purplish white col or .

The product is about 5 6 Gm containing per cent of s ilver

,

oxide It shoul d be kept in smal l amb e r glass stoppered bottles

.
,

wrapped in yellow paper .

S I LV ER OX I D E .

AR G EN TI OX I D U M .

A g 20 2 23 2 .

S ilver nitrate 2 parts

D istilled water 4 0 parts
S olution o f potassium hydroxide I 3 parts

D issolve the silver n itrate in the water To this solution add .

solution o f potassa so long as any precipitate is pr od uced by it .

57 2 S I L VER oxI D E .

Wash the precip itate with distill ed water until t h e washings are .

nearly tasteless D ry the product and keep it well protected from

.

the light .

R e act i on .

N ot e s . Instead of potassium hydroxide a correspondin g

am ount of calcium hydroxide may be us ed T he pr oportions r e .

qu i red are then I part o f s ilver nitrate dis solved in 2 0 parts o f

water and I 3 5 parts o f satur ated solution o f calcium hydroxide
,

( lime water ) .

S ilver oxide eas ily parts with its oxygen and hence must not ,

be brought in contact with readily oxidizable substances as ex ,

plosion may result M oderate heat als o decompos es it With

. .

ammonia it forms a violently explosive compound known as

“
fulminate o f s ilver ”
Great care is accordin g ly necessary in
.

handling th is preparation I t shoul d be kept in a well closed .

-

bot t l e a n d in a cool place .

D e scri p t i on heav y dark brown nearly black powder ; odor

.
—
A ,
-
, ,

less ; taste metallic N early insol uble in water to which it never

.
,

the less imparts an alkaline reaction

,
.

S OD IUM A C E TA T E .

S OD I I A CE T A S .

Na C H 2 3 0 2 3
. H 2
0 : 1 36 .

L ead acetate
S odium carbonate
A cetic acid su ffi cient ,
.

D issolve the salts each in s ixty parts o f water ; filter and add
, ,

the solution o f l ead acetate to that of the sodium carbonate stir ,

ring briskly S e t aside t o s ettle D ecant the supernatant l iquid ;

. .

wash the precipitate with a littl e cold distilled water and add the
wash ings to the decanted sol ution Filter A dd enough acetic . .

acid to the filtrate to render it distinctly acid to l itmu s paper ;

then evaporat e it to 2 5 parts and set it aside to cool and crystall ize,
.

C oncentrate the mother l iquor by evap oration and crystallize ,

again .

M ust be kept i n tightly corked bottles .

5 74 S OD I U M A CE T A T E .

their odor comes out on neutral izing the acid The acetate “

"

should then be careful ly heated to complete fus ion at a temper a

ture o f about 3 00 ( and not exceeding °
for hal f an hour
when the empyreum a tic substances w ill be decomposed The salt .

is then recrystallized .

D e s cri p t i on .
—
Colorl es s
transparent crystal s ; odorless ; tas t e ,

sal ine cool ing E ffl ore s c e nt in warm dry air S oluble in I 4

,
. .
\
.

parts o f water and in 3 0 parts o f alcoh ol at I 5 in hal f its °

weight o f b oiling water and in twice its weight o f bo ilin g alcohol ,

.

The salt becomes l iqu id at and anhydrous at I t de

composes a t 3 1 5 C Its water solution turns red litmus
°
.
-

paper blue but shoul d not redden p h e nol p h t al e i n paper

,
I f it .

reddens p h e nol p h t al e i n it probably contains sodium carbonate .

S OD IUM AR S E N AT E .

s oon ARSEN AS .

A rsenous oxide
S odium n 1 t r a t e
D ried sodium carb onate

Powder thes e substances an d mix them intimately by tritura

tion Heat the mixture in a large covered clay c ruc ible at a
. .

red heat until e ff ervescence has ceased and complete fusion takes ,

place L et the fused mass solidi fy on a porcelain surface and

.
, ,

while still warm put it into 8 5 parts o f bo i ling distilled water and
, ,

stir until dissolved Filter while hot and s e t as id e t o crystallize

.
,
.

Collect drain and dry the crystals and keep them in a tightly
, , ,

corked bottle .

R e act i on .

and ,

H O N a zH A s O 4 7 H zO )
N a4 A s z
O l — I 5 z 2
— : -
7
.

N ot e s The res idue a fter the process o f heating the mixture

.

i s sodium pyroarsenate which is converted into ort h oa r s e n at e by ,

water .
 S OD I U M AR S ENA T E .
575

When crystallized at a low temperature sodium arsenate h a s

1 2 molecules o f water o f crystall ization ; at ordinary temperature

it usually crystallizes w ith 7 H zO in dry ai r it e ffior e s c e s losing ,

C an d °

5 H2O ; the last o f the water is driven o ff at about 1 49 .

,

when heated to redness it becomes converted into pyroarsenate ,

which how e ver when dissolved in water becomes immediately

, ,

converted back int o arsenate .

D e s cr i pt i on
Colorless transparent od orl es s crystals o f m ild
.
—
, , ,

alkaline taste ( very poisonous ) H ygroscopic in moist air . .

S oluble in 4 parts o f water at and freely soluble in boiling

water Ver y sparingly soluble in c ol d alcohol ; s oluble in 6 0
.

parts o f boiling alcohol .

S ol u ti on o f S od i u m A r s e n a te ; U . S .

S odium arsenate dried at , 1 49

°
C I part
D istilled water 99 parts

N ot e s . O wing to the variabl e amount o f water o f c ry s t a l l i za

tion found in the sodium arsenate of commerce the Pharma

c op oe i a d ire c ts that the salt shoul d be heated at 1 4 9 C 30 0 F ) °
. .

until deprived o f all its water o f cr y stallization be fore it is

weighed out and used in making the o ffi cial solution S e e pre
, .

ceding paragraph .

S OD IUM B E N Z OA T E .

S OD I I B E N Z OA S .

N a C7 H 5 O z=I 44 .

B enzoic acid 40 parts

S odium bicarbonate . 28 parts
Boiling water 80 parts
M ix the be zoi c acid w ith the hot water sti r well neutral ize , ,

perfectly by adding the sodium bicarbonate being careful to oh ,

serve the reaction on litmu s paper after e ff ervescence has ceased .

F ilter E vaporate to 5 5 parts ; remove it from the source o f heat

.

and stir until col d D uring the evaporation it is necessary to

.

scrape down the benzoate from the sides o f the capsule .

R e act i on . 2H C7 H fi O z f N
— —
az CO —
_
2 N a C7 H 5 O Q+
H O + CO , .
576 S OD I U M B EN Z OA T E .

D e s cr i p ti on . A
white semi crystalline or amorphous powder
—
,
-
,

effl orescent on exposure to ai r odorless or having a faint odor ,

O f benzoin o f a sweetly astringent taste free fro m bitterness and

, ,

having a neutral reaction S oluble in parts o f water and in .

,

4 5 parts o f alcohol at 1 5 C
°
in parts o f boiling water and in .
,

2 0 parts o f boiling alcohol :

S OD IUM B I CA R B O N AT E .

S OB I I B I CA R B O N A S .

N a H CO 3 =84 .

Prepared by saturating a solution o f s od ium carbonate with

carbon i c acid gas or by conductin g carbonic acid gas for several
,

days into closed chambers filled with crystallized sodium car

bonate The liberated water o f crystallization retains in solution
.

the chloride and s ulphate which may have been present in the
carb onate .

It may also be prepared as follows

S tronger ammonia water ( 2 8 % o f H 3N ) . 2 50 Gm

S odium chloride 2 50 Gm
Water ,

Carbon dioxide .

Put the ammonia solution in a flask o f 2 0 0 0 Cc capacity A dd

“

. .

one liter o f water Pass carbon dioxide into the mixture until
.

satu rated keeping the flask coo l by means o f a stream o f cold

,

vva t e r .

D issolve the s odi um chloride in 8 0 0 Gm o f water at A dd

'
to this the col d solution of ammonium bicarbonate stirring well , ,

and continuing the addition so long as a precipitate i s formed .

When no further precipitation results from the addit i on of more

o f the solution o f ammon i um bicarbonate collect the precipitated ,

sodium bicarbonate wash it with some cold water on a funnel and

, ,

dry it .

R e a ct i onS then H N H C0 3 +
’

'
.

N a Cl z N a H CO 3 + H 4 N CL

N ot e s . A mmonium bicarbonate i s not freely solubl e in water .

57 8 S OD I U M BI S UL PHIT E .

S OD IUM B I S UL PH IT E .

S OD I I B I S U L PH I S .

N aH S O 3 _
-
1 04 .

Prepared by saturating a solution o f sodium carbonate with

sulphur dioxide and evaporating the solution to drynes s .

M ust be kept in small entirely fill ed tightl y clos ed bottles in a

, ,
-
,

cool place .

D e scri pt i on .
—
O paque crystal s or a white granular powder , ,

emitting a sulphurous odor ; taste disagreeable sulphurous O x i ,

.

dized by contact with air to sulphat e giving o ff sulphur dioxide ,

.

S ol ubl e at I 5 i n 4 parts o f water and in 7 2 parts o f alcohol ; in

°
'

about 2 parts o f boiling w ater and in 4 9 parts o f boiling alcohol .

Its water soluti on exhibits an acid reaction on l itmus paper

-
.

S OD IUM B I TA R T R A T E .

S OD I I B I TA R TR A S .

'

N a H C4 H 4 O 6 H 2O .
:
-
I
9 o .

Tartaric acid 20 parts

S odium carbonate 19 parts
D issolve one hal f o f the acid in 5 0 parts o f distilled water neu
-
,

t ra li z e with the sodium carbonate and filter D issolve the other .

hal f of th e tartaric acid in 5 0 parts o f distilled water and filter .

M i x the two liquids S e t the mixture aside in a cool place for a

.

day or two ; then collect and dry the precipitated crystalline salt .

D e s cri p t i on .
—
A
white crystall ine p owder or colorless cr y stal s ;
, ,

odorles s ; acid taste S paringly soluble in col d water I nsoluble

. .

in alcohol .

S OD IUM BR OM ID E .

S OD I I B ROM I DU M .

N a B r= 1 0 3 .

I ron wire cut ,

B romine
S odium carbonate
D istilled water su fficient ,
.
 S OD I U M B ROM I DE .
57 9

D igest the i ron and 1 8 parts o f bromine with 5 0 parts o f water

in a flask until all odor of bromine has ceased and the l iquid be ,

comes green Filter add the remainder o f the bromine to the

.
,

filtrate and let it dissolve

,
.

D issolve the sodium carbonate in 1 0 0 parts o f boiling distilled

water and add the solution o f bromide of i ron B oil for fi fteen
,
.

minutes filter and evaporate the filtrate to dryness during con

, ,

stant stirring .

N ot e s The reactions are analogou s to those occurri n g in the

.

preparation o f potassium bromide from bromide o f iron an d p ot a s

s ium carbonate .

The sodium bromide ma y also be made from bromine and solu

tion o f sodium hydroxide as potass i um bromide is prepared from
,

bromine and solution of potassium hydroxi de .

S e e also no t es under Potassium B rom i de .

Where the sal t is deposited from hot concentrated solutions the

crystal s are anhydrous and cubical while hydrated monocl inic ,

crystals are deposited by sl ow evaporation o f cold solutions .

D e scri pt i on Colorless or white crystals or a white granular

.
—
,

salt ; odorl ess taste sal ine slightly bitter S om ewhat hygroscopic
,
. .

S olubl e at 1 5 in parts o f water and in 1 3 parts o f alcohol ; in

hal f its weight of boiling water and in 1 1 parts o f boiling alcohol
,
.

The water solution should be neutral or only faintly alkal ine to

-

test paper
-
.

S OD IUM CAR B O N AT E .

S OD I I C AR B O NA S .

N a zCO 3 10H 2 O z 286 .

By far the greater portion o f s a l s od a e or cru de sodium car ,

bonate consumed at this time is prepared by the s o called L e

,
-

bl au c s m e th od
’
A m ixture of sodium sulphate chalk and coal
.
,

is stron g ly heated in a reverberatory furnace ; the mas s i s then

l eached out with water the solution concentrated and the car
, ,

bonate collected as it separates from the hot liquid The product

,
.

contains carbonate sulphide h y drate sulphate and hyposulphite

, , , ,
5 8 0 S OD I U M AR B ONA T E
C .

o f sodium The res idue obtained by evaporating the first solution

.

to dryness is called s od a as h o f whi ch several hundred mill ion —

,

pounds are annually imported int o the U nited S tates The crude .

sodium carbonate i s purified by r e crystall ization -

.

A t N atrona Pa n e a r Pi tt s bu rg large quantities o f soda are

,
.
,
‘

made from cr y ol i te a mineral composed o f the fluorides o f sodium

,

and aluminum A m ixture o f powdered cr y olite and chalk is i g

.

n i t e d in a furnace the first reaction being : 6 N a F l A 12F l 6

, .

The fused mass i s p o w

dered and the sodium aluminate l eached out by water A stream .

o f carbonic oxide is conducted through the solution of sodium

aluminate which produces sodium carbonate and aluminium h y
,

drate : 0
.

A third method consists in treating a solution o f sodium chloride

with N H 3 an d a fterwards with CO ; the ammonium bicarbonate 2

gives w ith the N a Cl sodium bicarbonate and N H C1 The s o

, , 4 .

d i u m bicarbonate is then converted in to carbonate by heat a fter ,

which the product is di ssolved and crystallized .

Both the ammonia process an d the cryol ite process yiel d purer
products than the s od ium carbonate made by L eblanc s process ’
.

U se s . Vast quantities o f sal sod ae are us ed in the art s and man

u fa c t u r e s and in the household economy In pharmacy it i s us ed .

in the preparation o f various carbonates and for the production ,

o f sodium comp ounds .

Commercial sodium carbo n ate

Pu ri fi cat i on . sal sod ae may
be purified by recrystallization as follows ,

0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0

0
M ix and heat to 8 0 until the soda ash is dis solved Filter . .

E vaporate the filtrate t o a density o f 5 L et the liqui d slowly .

cool to about Collect the crystals drain and dry them and , , ,

place the m in a dry bottl e .

A dditional crops of cr y stals are to be recovered from the mother

liquor on evaporation .

N ot e s . To prevent the formation o f lumps the soda ash in ,

 S OD I U M C AR B ONA T E .

D r i e d S od i u m Ca r bon a te .

N a z CO 2H 2 O .

E xpose crystallized sodium carbonate in small fragments or

crystals for several days to a temperature not exceeding 2 5
, ,
°

until completely e ffl ore s c e d ; then d r y it at not over 4 5 until r e °

d uc e d to one hal f the weight o f the crystallized salt originally

-

taken .

Trit urate the product in a mortar until a un i form powder i s

obtained and keep this in well closed bottles —
.

N ot e s Crystall ized s o dium carbonate contains 1 0 molecules o f

.

water o f cr y stalli za tion When exposed to the ai r it e ffl or e s c e s

.
,

and in the course o f one or more weeks ac cording to the tempera ,

ture and drynes s o f the air it loses about 4 0 per cent o f i t s weight
,
'

A t 4 5 C it loses all but 2 m olecules o f its water o f crystallization

°
. .

[ A t 9 0 to°
1 0 0 C it becomes anh
0
y drou
. s ]
A t about 3 2 5 crystallized sodium carbonate di ssolves i n i t s
°
’

water o f crystallization Thi s aqueous fusion should be av oided

”
.

in the preparation o f dried sodium carb onate because it renders the

subsequent completion o f the process more d i ffi cult It is there .
,

fore directed that the crystallized salt shall be e ffior e s c e d at from

,

° °
20 to 2 5 C be fore higher heat i s appl ied
. .

D e scri pti on .
-
A white amorphous powder
,
.

S OD IUM CH LO R A T E .

S OD I I C H LORA S .

N a C10 3 :

Prepared from calcium hydroxide and sodium chloride

chlorine or from chlorinated lime and sodium chloride
, ,

proc es s analogou s to that for preparing potassium chlorate .

It may also be made as follows

Tar taric acid 1 1 7 parts

S odium carbonate 1 1 0 parts

Potassium chlorate 9 6 parts

D isso l ve t h e acid and the carbonate 1 n .

. 1 000 parts o f hot w a ter .
 S OD I U M C H LORAT E . 8
5 3

To the hot solution add the potassium chlorate Potassium bitar .

trate separates and the solution contain s the sodium chlorate to

,

gether with some potassium bitartrate which deposits during the ,

evaporation to crystallization the last being gotten ri d o f by ,

crystallizing it out from the saturated solution of the sodium

chlorate .

D e scr i p t i on
Colorless transparent crystal s or a white crystal
—
,

l ine powder ; odorless ; taste saline cooling S oluble a t 1 5 in ,

.
°

parts o f water and in about 1 0 0 parts o f alc ohol ; in hal f its weight
,

o f boiling water and in 4 0 parts o f boil ing alcohol ; in 5 parts o f

gl y cerin The water solution i s neutral to test paper L ike p ot a s
.
- -
.

s ium chlorate the sodium chlorate must be handled with care a nd ,

not triturated with reducing agents or subj ected to concu ssion .

S OD IUM CH LO R I D E .

S O BTI C H L OR I D U M .

N a Cl : 5 8 4 . .

D ilutedhydrochloric acid
S odium carbonate

A dd the sodium carbonate gradually to the diluted aci d M ake .

the solution quite neutral to litmus paper Filter E vaporate to . .

dryness or to crystallization as
, ,
m a y be desired .

R e act i on . N a zCO g + 2H Cl z z N a Cl H O
+ g l CO T
— —

P u r i fi c a ti on o f Com m on S a l t .

Common salt
Water
L ime
Barium chloride ,

S odium carbonate ,

Hydrochloric acid .

D issolve the salt in the water S lake the lime m i x it with 1 00 .

,

ml o f water and add the mixture to the salt sol ution Heat to the
,
.

boiling p oint Filter A dd a solution o f barium chloride to the

. .

filtrate a s long as it cau ses precipitation Then add solution o f .

sod ium carbonate until all the calcium and barium shall have been
 8
5 4 S OD I U M C H LOR I DE .

separated Filter N e u t ra l i z e with hydrochloric aci d E vaporat e

. . .

to crystallization or granulation and dry the salt thoroughly ,

.

N ot e s Common salt contains magnesium and calcium salts

.

( chlori des and sulphates ) These are precipitated as described. .

D e scr i p t i on
Colorless crystals or a white granular crystalline
.
—
,

powder ; d ry ; odorless and O f purely sal ine taste N ot h yg ro

,
‘

scopic S oluble in
. parts o f water at and in parts at
1 00 A lmost insolubl e in alcoho l The water s olution is n eutral .
-

to l itmus paper .

K i s s i ng e n S a l t .

D ried sodium sulphate 9 0 parts

Precipita t ed calcium sulphate 5 0 parts
Potassium sulphate 1 1 parts
Ferrous sulphate 3 parts
S odium bicarbonate 1 70 parts
D ried magnesium sulphate 1 30 parts
S odium chloride parts
‘

40 0
Tartar i c a c i d 10 parts

M ix the separately powdered dry ingredients well .

S OD IUM CI T R A T E S OLU TI O N .

L I QUOR S OD I I CI T R A T I S .

A solution of normal sodium citrate o f which each milliliter

contains 0 .
5 0 Gm o f N a 3 C6 H 5 O7 is prepared as follow s

Citric acid 40 0 Gm
S odium bi carbonate 4 8 6 Gm

D is solve the s odium bicarbonate in 7 5 0 ml o f distill ed water by

the aid o f heat gradually add the citric acid and when e ff e rve s
, , ,

cence has ceas ed bring the l iquid to the boiling point I f the s o
,
.

l u t i on is not neutral to litmu s paper add more sod ium bicar ,

bonate ( or citric acid as the case may requ ire ) t o produce a

. ,

per fectl y neutral reaction Finally add enough distill ed water .

,

to make the whole measure 1 0 8 0 ml .

To make solution of di -
s od i u m -
hy d r og e n c i tr a t e , containing
5 8 6 S OD I U M E T H Y L S U L PH A T E .

D e s cr i pt i on
Colorles s laminar crystals somewhat
.
—
, e ffl or e s ce n t
°

readily soluble in water .

S ol u ti on f
o S od i u m E thy l a te ; B . P .

A n alcoholi c solution containing 18 per cent o f C2 H 5 O N a .

S odium ,clean and bright 1 Gm

A bsolute alcohol 20 ml

Cautiously dissolve the sodium in the alcohol in a flask kept

cool by flowing water .

R e act i on . 2 C2H 5
O H + N a z
z 2 C2H 5 O N a + H 2 .

The met al shoul d i f larger quantities be employed be

N ot e s .
, ,

a dded gradual ly The heat l iberated by the reaction i s great

.
,

and hence the liquid must be kept cold .

D e s cri p t i on —
A
colorless syrupy l iquid which becomes brown
on keeping . It must be freshly prepared when required .

Sp w. .

S OD IUM H Y D R OX I D E .

S OD I I H Y D R OX I D U M .

N aO H

Prepared by evaporating the solution o f sodium hydroxide to

dr y ness fusing the residue dissolving it in alc ohol which leaves
, , ,

carbonate und issolved after which the alcohol is distilled off from
,

the clear solution and the sodium hydroxide again fu sed .

This alkal i must be preserved in the same manner as potassium

hydroxide i n tightly closed bottl es o f hard green glass the
-
,

stoppers t o be rubbed with a l ittle petrolatum to prevent them

from being cemented into the n ecks o f the bottl es .

D e s cri p t i on white translucent , hard o f crystalline frac

.
-
D ry , , ,

ture odorless acrid ; caustic corrosive Hygroscopic but not

, , , .
,

deliquescen t becoming first moist a n d then converted into dry car

,

b onate on exposure to ai r S oluble in parts of water at .

and in part o f boil ing water Freely soluble in alcohol . .

S trongly alkaline .
 S O DI U M H Y D ROX ID E . 8
5 7

S OD I UM H Y D R OX I D E S OLUT I O N .

L I QUOR S OD I I H Y D R OX I D I .

[ L iquor S od ae ; U . S .
]
A n aqueou s solution containing 5 per cent o f sodium hydroxide .

N aO H :
40 .

S od ium carbonate
Calcium oxide
D istilled water su ffi cient , .

D is solve
the sodium ca rbonate in 4 0 parts o f boil ing d istilled
water S lake the lim e and make o f it a smooth m ixture with
.

4 0 parts o f distill ed water and heat this m ixture to boiling Then .

ad d gradually the sodium carbonate solution to the milk o f

.

l ime and boil the whole mixture for ten minutes R emove the
, .

heat co er th e vessel tightly and when the contents are cold

,
v
.
, , .

add enough distill e d water to make the whol e weigh 1 0 0 parts .

L astly strain the liqui d through linen or when the precipitate , ,

has subsided draw off the clear solution by means of a s yphon

,
.

R e act i on .

N ot e s The sodium carbonate emplo y ed must o f c ours e be the

.
, ,

crystallized salt not in any degree e fflore s c e d

,
.

The l ime might advantageousl y be washed free from dust and

salts be fore being used This is done as follows : S lake the 5 parts
. .

'

o f l ime with about 4 0 p a rt S o f water ; then add about 5 00 parts of

water and stir the m ixture occasionally during hal f an hour ; let
the calcium hydroxide subs ide decant the l iquid and throw this ,

away Then add 4 0 parts o f pure water heat to boiling and use
.
,

thi s l iqui d w ith the sol ution o f sodium carbonate as described

in the formula above given .

A cons iderable exces s o f lime i s u sed but as calcium hydroxide ,

is insoluble in a solution of sodium hydroxide no l ime will be

contained in the product A n unneces sarily large excess o f l ime .

is however obj ectionabl e because the superfluous calcium h y

, ,

d r ox i d e does not subside as readily a s the calcium carbonate .

I f cold liquids are used the calcium carbonate formed by the

reaction i s s o finely divided and l ight that it s u bs i d e s ve r y slo wl y
5 88 S O D I U M H Y DR OX I D E .

and the bulky precipitate retains much liqu id causing correspond

ing loss o f product .

M ore concentrated solutions can not be used becaus e the r e a c

tion will not then be complete It is completed when the liquid .

no longer e ff ervesces with dilute acid o r when it does not cause

turbidity when dropped into a clear solution o f calcium hydroxi de .

S olution o f sodium h y droxide i s usually clarified by subsi dence

and decantation but it may i f pre ferred be success fully filtered
, ,

through coarsely powdered and washed marble .

The strengt h of such a preparation as solution o f Sod ium hy

d rox i d e should not be fixed by the quantities an d proportions o f
the materials as i s done in the Pharmacop oeia from which the
fore g oing formula is borrowed ; it shoul d be t ested quantitatively
with volumetric solution o f sulphuric aci d and the strengt h a d
justed by dilution in accordance with the result In order to carry .

out this plan the quantity o f water used in the process may be
diminished ten per cent and the product diluted as required ; or
the amount o f water directed may be used and the product di
luted or concentrated by evaporation as may be f ound neces sary
, ,
.

S olution o f sodium hydroxide attacks organic matt r ener e

g e t i c a l l y and i s therefore di scolored by contact with organic sub

stances It also attacks ordinary flint glass s o that i f it be put
. ,

in gl ass stoppered bottles of that k ind o f glass the stoppers

-

usually become firmly fixed and can not be removed neces sitating ,

the breaking o f the bottles to get at t he contents The solution .

shoul d there fore be kept in bottles ma de o f green glass which

, ,

is not so easil y attacked by the alkal i and the stoppers should ,

be coated with a littl e para ffin or petrolatum .

The official sodium hydroxide solution i s a Clear

D e s cr i pt i on .
—
,

colorless and odorless liqu id having a very acri d and cau stic taste
, ,

a corrosive action on organic matter and a strongly alkalin e ,

reaction .

Its specific weight i s about an d the specific volume

V al u at i on To neutralize 20 Gm Of o fficial solution o f sodium

.

h y droxide shoul d requ ire 2 5 ml of normal sulphuric acid each ml ,

o f the test s Ol u t i on i n dicating per cent o f N a O H ; p h e nolp h t a

lein shoul d be u sed as indicator .

O ne ml o f normal sulphuric acid is the equival ent o f

Gm o f N a O H .
59 0 S OD I U M HYP O C H LOR IT E .

d ium formed an d the value o f the preparation woul d then be

,_

impaired by loss o f available chlorine O n the addition of acids .

the solution e ffervesces because carbon dioxide and Chlorine are

l iberated ; the CO 2 comes from the excess o f sodium carbonate .

The containers shoul d be closed with rubber stoppers or glas s

stoppers instead o f corks as the Chlorine destroys the latter , .

D e s cri pt i on pale gre enish clear liquid having a faint odor

.
—
A -
,

o f chlorine and an alkaline as well as salty and peculia r taste

, .

S p w about
. . Colors red litmus paper blue and then
bl eaches it O n the addition o f hydrochloric acid the liquid gives
.

o ff chlorine and carbon d ioxide .

S OD IUM H Y P O PH O S PH I T E .

S OD I I H Y PO P H OS P H I S .

N a PO 2H 2
. H gO : 1 06 .

Calcium hypophosphite
S o dium carbonate

D issolveeach salt in 6 0 parts o f boil ing water and mix the ,

solutions Filter out the calcium carbonate and evaporate the

.
,

solution over a water bath until a dry granular salt remains -

.
,

taking care that the temperature during the evaporation does not
exceed 8 5 C °
.

N ot e s . be purified by r e dissolving it in ten time s its

M ay -

weight of hot alcohol filtering and evaporating to dryness , , .

R e a ct i on . Ca ( 2 O2) 2
H P —
2 N aH 2
POz .

Pearly white or colorless crystals or a white

D e s cri p t i on .
—
,

granular powder ; odorless ; taste sal ine bitterish Hygroscopic ,

. .

S ol u bl e a t 1 5 in its own weight of water and in 3 0 parts o f

' °

alcohol ; in part o f boiling water and in its ow n weight o f

’

boiling alcohol I nsolubl e in ether The water solution is ne u

. .
-

tral to litmus paper .

 S OD I U M I OD I DE .

S OD I UM IOD ID E .

S OD I I I OD I D U M .

N aI :

- wire cut
ron ,

I odine
S odium carbonate
D istilled water s u fli c i e n t
,
.

D igest the iron and 1 5 parts o f the iodine with 5 0 parts o f

water in a flask until the odor o f iodine ceases and a green solu
tion o f ferrous iodide results Filter this and d issolve the r e
.
,

m a i n d e r o f the iodine in the filtrate D issolve the sodium car .

bonate in 80 parts of water heat to boiling then add the solution

, ,

o f iodides o f iron durin g constant stirring boil the mixture fifteen

minutes filter evaporate and crystall ize
,

, , ,
.

N ot e s The reactions are analogous to those taking place in

.

the process for preparing potassium iodide in a similar way S e e .

the notes under that titl e .

S od ium iodide may also be made from iodine and solution o f

sodium hydroxide a s potassium iodide i s prepared from iodine
,

and solution o f p otassium hydroxide .

D e s cr i pt i on
Colorles s crystal s or a white crystalline powder ;
—

odorless ; taste sal ine somewhat bitterish H yg r os c0 p i c D e

, . .

composes when exposed to the air forming s odium carbonate and ,

free iodine which discolors the product S oluble at 1 5 in .

°

part o f water and in about 3 parts o f alcohol ; in one third its -

weight o f boiling water and in parts o f boiling alcohol The .

water solution shoul d be neutral or only faintly alkal ine to test

-

paper .

S OD IUM N I TR ATE .

S OD I I N IT RA S .

N a N 0 3 =8 5 .

Crude sodium nitrate occurs native in Peru and Bolivia The .

native sodium saltpeter contains from 20 to 8 0 per cent o f s o

59 2 S OD I U M N IT R A T E .

d i um
nitrate most frequently y ielding 5 0 per cent It is freed
, .

from earth and other impurities by sol ution straining and crys , ,

t a l l i z a t i on .

It is purified in the same w a y as potass ium nitrate by r e ,

cr y stall ization and by washing w ith a cold saturated solution o f

pure sodium nitrate which removes chlorides present
, .

It can be prepared by the neutralization o f diluted nitric aci d

with sodium carbonate .

D e sc ri p t i on Colorles s transparent crys tals ; odorless ; taste

—

s al ine cool ing bitterish Hygroscopic S olubl e in

, , . par t s o f .

w a t e r a n d in 1 0 0 pa rts o f alcohol at
~
in part of boil ing
water and in 4 0 parts o f boiling alcohol The ater solution is
'
“

-
.

neut ral to l itmus paper .

S OD IUM N I T R IT E .

S OD I I N I TR I S .

N aN 0 2 : 69 .

Prepared by fus ing together sodium nitrate and sheet lead ,

keeping the two substances together at the temperature required

for fus ion until the lead oxidizes t o lead oxide at the expense o f
the sodium nitrate which i s thus reduced to sodium nitrite The .

nitrite is leached out from the c ooled mass with water and the
solution treated with carbo ndioxide to free it from lead a fter ,

which the liquid is filtered and evaporated t o crystallization .

D e scr i pt i on
Colorles s crystal s fused into white
—
m asses or
sticks ; odorles s ; taste mild saline H yg r os c 0 p i c ,
. . O xidizes in
ai r to nitrate S olubl e at 1 5 in
. parts o f water °
. Freely sol
uble in boil ing water S paringl y soluble i n alcoh ol
. . T he water
solution has an alkaline reaction on test paper -
.

S OD I UM N I TR O PR US S ID E .

S OD I I N I T R O PR U S S I D U M .

)
N a, F e ( CN NO . 2H zO :
3 00 .

Potassium ferrocyanide
N itric acid ( 6 9 % H N O 3 )
S odium carbonate anh y drous about , ,

Water .

R educe the ferrocyanide to fine powder . D ilute the nitric aci d

5 94 S O D A S OA P .

D issolve the sodium hydroxide in the water add the oil and ,

the alcohol and heat the m ixture gently in a porcelain dish over
, , ,

a water bath stirring constantly until s a p on i fic at i on is com

-
, ,

p l e t e
. d Then add 3 0 0 parts o f warm distilled water and mix w e ll .

M ake a solution of

S odium chloride
S odi um carbonate
D i stilled water

and filter it A dd this solution to the solution o f the soap and

.
,

mix thoroughly
Heat the m
.

ixture over the water bath stirring gentl y until the -

, ,

soap s eparates an d rises to the surface o f the liquid L et the dish .

and contents cool When cold separate the mother liquor from
.

the soap and rinse the soap with a littl e cold water Then
, .

squeeze the water out o f the soap by means of strong pressure ,

dry the mas s with the aid o f gentl e heat and powder the product , .

N ot e s The quantity o f s odium hydroxide prescribed is slightly

.

in excess o f the amount theoretically required A ll hard soaps .

cons ist mainly o f sodium oleate The best Castile soap a p .

p r
.
oa c h e s pure sod ium oleate su ffi cientl y for al l practical purposes
in pharmacy including the preparation o f other oleates by
,
“ ”
double decomposition N o soda soap shoul d be used for t h e
.

preparation o f other metall ic ol eates except a fter complete drying ;

h ence pow d e re d soap is to be used This is because the amount .

o f moistu re in pow dered soap can not vary a great deal :

The soap i s completely soluble in water although the solution is
not cl ear S oda soap is precipitated from its water solution by
.

sodium chloride in the manner described .

Tran sparent soap may be made by d issolving soda soap in

alcohol filtering the solution an d evaporating Castor oil soap
, ,
.

easily for m s a transparent soap .

M edicinal soda soaps are sometimes mad e from almond oil a nd ,

also from fresh ( unsalted ) butter .

 S O DI U M PH ENOL S UL PH ONA T E .
5 95

SO D I U M PH E N OL S U L PH O N A T E .

S OB I I PA R A P H E N OL S U L P H O N A S .

( S odium S ulphocarbolate .
)

Crystallized phe nol 10 pa rts

S ulphuric acid 12 part s
Barium carbonate 20 parts
S od ium carbonate 34 parts
A dd the phenol to the sulphu ric acid sti r and heat the mix , ,

ture at 5 5 C for several days A dd 2 0 0 parts o f water and stir

°
. .
,

well Then gradual ly add the barium carbonate and mix th e

.
,

whole intimately Filter Precipitate the filtrate exactly with

. .

the sodium carbonate previously d issolved in 1 0 0 parts o f water, .

A gain filter and evaporate to crystallization Puri fy the product

,
.

by r e crystallization until c olorless or but faintly pinkish

-
, .

Re act i on .

and then
B a ( C6 H 5 5 O 4 ) 5+ N a 2CO 3 z 2 N a C6 H 5
S O 4 l B a CO 3
— —
.

N ot e s . A ny excess of sulphuric acid present in the phenol sul -

phon ic acid is removed by the use o f an excess o f barium car

bonate whereby insolubl e barium sulphate is formed which is
, ,

filtered away .

D e scri pt i onColorless transparent rhombic prisms perm a

.
—
, , ,

nent in the ai r odorl ess or nearly so having a cooling saline

, , , ,

somewhat bitter taste and a neutral reacti on S ol uble in 5 parts , .

o f water and in 1 3 2 parts o f alcohol at 1 5 C ( 5 9 F ) in

,
°
.
°
.

part o f boiling water and in 1 0 parts o f boiling alcohol .

S OD IUM PH O S PH A T E .

S OD I I P H O S PH A S .

N a zH PO 4 . 1 2H 20 :
35 8 .

[ D i S
Hydrogen Phosphat e ]
odium- -

Bone ash in fine powder

-
,

S ulphuric acid
S od ium carbonate suffi c i ent ,
.
59 6 S OD I U M P H O S PH AT E .

Wash the bone ash with ten t imes its weight of boilin g water
-
.

D ecant and rej ect the water M i x the w e t mass with the acid .
,

set the mixture in a warm pl a ce for three days replacing the ,

water vaporized by the heat and stir occasionally Then add 1 0 ,

.

parts o f boiling water mix thoroughly trans fer the mixture to a

, ,

m uslin strainer and l et the liquid pass throu gh R eserve the

,
.

liqu id Trans fer the magma from the musl in to an earthenware

.

vessel add 1 0 parts o f boiling water stir well an d again strain

, , ,

the mixture through muslin adding th e colature to th at previously , .

reserved Continue washing the residue with boiling water until

.

the liqu id passes nearly tasteless M i x the several acid liquids .

and evaporate the mixture to 2 0 parts S e t thi s aside a few days . .

Filter Heat the fi ltrate to the boiling po int and gradually add to
.
,

it a solution o f sodium carbonate in hot Water until a filtered por ,

tion o f the now alkal ine liquid e ff ervesces when mixed with dil ute
sulphuric aci d D igest the mixtu re an hour or two and then
.
,

filter Wash out the remainin g sodium phosphate from the resi
.

due by means o f h ot water adding the washings to the filtrate ,

.

Then evaporate the m ixed l iquids to 1 0 parts an d set as ide to ,

crystal l ize .

Puri fy the product by re crystallization a fter dissolving it in —

twice its weight o f water R epeat the r e crystallization as many

.
-

times as m a y be necessary to obtain a clean product .

D ry the cr y stal s with as littl e exposure to the air as possible

“

to avoid e fflor e s c e n c e .

First the tri calcium p hosphate ( bone ash ) i s de

R e act i on .
- -

compos ed by the sulphuric acid yiel ding acid calcium phosphate

and calcium sulphate as follows.

Ca3 P0 4 ) P0 4 ) 2 —2 Ca S O , .

Then the acid phosphate of calcium is decomposed by the so

d i u m carbonate as follows :

N ot e s When the b one ash is treated with sulphuric aci d the

.
‘
-

mixture becomes hot U sually the powdered bone a Sh is not

.
-

washed previous to mixing it with th e sulphuric a Ci d and no h

water added until after the powder and aci d have first been thor
oughly m ixed I f organic matter be p resent in the bone as h sul
. - r

,
59 8 S O DI U M P H O S PH A T E .

all owed to stan d a few da y s in order that the calcium s ulphate held
'

in solution may be deposited I t is then filtered diluted with an

.
,

equal volume o f water and heated to the boiling point To the

,
.

hot liquid is now added h ot sodium carbonate solution as de

scribed .

The quantity o f s odium carbonate required will depen d upon

'

the completeness o f the decompos ition o f the bone ash and the —

lixiviation i n other words upon the amount o f acid calcium

—
,

phosphate contained in the liquor I f the w ork has been well .

done it will require about 1 0 0 parts or more o f sodium carbonate

,

to render alkal ine the aci d l iquor f rom 1 0 0 parts of bone ash -
.

Hot liqu ids are e m p l ove d in order that the calcium carbonate
formed may be heavy so as to separate as rapidly as poss ible
,
.

The sodium carbonate must be added gradually because o f the ,

e ff ervescence caused by the escaping carbonic oxide L itmus .

paper cannot be used t o ascertain when su ffi cient sodium car

bonate has been added becaus e sodium phosphate itsel f has an
,

alkaline reaction A fter the further addition o f sodium carbonate

.

has ceased to cause e ffervescence it is necessary to remove a small ,

portion o f the liquid filter it and test it by pou ring it into a small
, ,

amount o f dilute sulphuric acid when it s h ou l d e ff e rve s ce T he

,
‘

slight excess o f sodium carbonate added is necessary to insure

satis factory crystall ization of the sodium phosphate and the car ,

bonate remains in the mother liquo r .

When the l iqui d contains an excess o f sodium carbonate the ,

precipitated calcium carbonate is filtered out and washed on the

filter with a littl e hot water the wash ings being added to the
,
'

previou s filtrate E v ap ora t e t h e filtrate until reduced to ab out

.

three times the weight o f the sod ium carbonate consumed or ,

until a pell icle begins to form on the surface Then set it aside to .

crystallize .

The crystallization i s best e ff ected when an excess o f sodium

carbonate i s present and the solution is not too concentrated I t .

should not be hastened by evaporating down the solution too far ,

because the salt then crystallizes with only 7 instead o f 1 2 mole

cules o f water o f crystallization .

The pr oduct generall y requires purification by recrystall ization

to obtain a sodium phosphate which answers the description and
tests o f the Pharmacop oeia :
D e scri p t i on —
Col orl e s s t ra n s p a r e n t crystal s ha vi ng
,
'

a speci fic
 S O DI U M PH O S PH A T E .
5 99

gravit y o f They e ffl or e s c e readily an d when sl ightl y heated ,

melt in their water o f crystallization .

The salt is odorless and has a cool ing saline somewhat alka
, , ,

l ine taste E fflor e s c e n t

, . .

S oluble in parts o f water at and in parts o f boil ing

water Insoluble in alcohol The water solution i s alkal ine t o
. .
-

l itmu s paper but not to p h e n ol p h t a l e i n paper

, .

R e c r y s ta l l i z e d S od i u m P h os ph a t e .

S odium
carbonate I part
Commercial sodium phosphate 5 0 parts
Water 2 50 parts

D issolve the sod ium phosphate in the water with the aid o f
heat filter the solution put it in a crystallizer and set this aside
, ,

at perfect rest in a place free from dust that crystal s may form by
spontaneous evaporation o f the solvent at the or d i na rv ro om
te mperature .

S houl d crystallization be much delayed place a few clear crys

tal s o f pure sodium phosphate in the soluti on to start it .

Collect the crystals in the usual way drain them pres s them , ,

gently between cloths or bibulous paper d r y them hastily and , ,

at once put the product in dry bottles which must be ti g htly ,

closed and ke p t in a cool place .

D ri e d S odi u m Ph os pha te .

N azH PO 4 = 42
1 .

Heat crystallized sodium phosphate in porcel a in dish over a

water bath until it ceases to lose weight
-
, stirring the contents until
°
d ry Then heat the powder on a sand
.
-
bath at about 1 2 0 C for .

a few minutes Keep the product in a . tightly cl osed bottl e -

.

N ot e s Crystallized sodium phosphate contains 1 2 molecules

.

°
o f water o f cr y stallization When heated to 3 5 C it begins to . .

0
l ique fy but does not compl etely di ssolve until at about 4 0 C
,
.

I f then allowed to cool at once it sol idifies to a cake o f a radiated

cr y stall in e textu re .

When heated above 4 0 C the salt loses 5 molecules o f water °

. .

A t 1 00 C all the water o f crystall ization is finally expel led

°
.

”
and dried sod ium phosphate remains But as water bath heat .
-
60 0 S OD I U M P H O S PH A T E .

is not su fficient ( being less than 1 0 0 C ) to e ff ect this result ; the °

.

drying must be finished with the aid o f the sand bath -

.

”
E ffl or e s ce d sod ium phosphate formed by the gradual drying ,

o f the crystallized salt in dry warm air contains 4 7 per cent o f ,

“ ”
water or seven molecules and the dried sodium phosphate ( a n
, ,

h y drous ) gradually absorbs moisture when exposed to the air , ,

until converted into N a H PO 7 H O z 4

.
2 .

D e scri pt i on —
A white , a morphous powder .

S od i u m A m m on i u m P h os ph a te .

S OD I I E T A M M ON II P H OS P H A S .

[ M icrocosmic S alt .
]

S odiumphosph ate 5 parts

A mmonium phosphate 2 parts

D issolve the salts in 2 0 parts o f hot water add a little ammon ia ,

so a s to render the l iquid alkal ine to turmeric paper filter, and ,

set aside to crystallize

- .

The crystals e ffl or e s c e ; their solution has a Sl ightly alkaline

reaction .

The salt is u sed as a reagent in blow pipe analysis -

.

S O D I UM PY R O PH O S PH A T E .

S OD I I P Y R O P H OS PH A S .

N a 4 P2 O7 . I OH 2
0 : :
44 6 .

Prepared by heating sodium phosphate in an iron dish raising

the heat gradually until the salt fuses in its water o f c ry s t a l l i za
tion then fall s to powder as that water is expelled and finally
, ,

decomposes at a temperatu re o f 2 4 0 to 3 0 0 C being converted ° °

.
,

into normal sodium p y rophosphate The dry powd er is dissolved .

in a su fficient quantity o f boil ing water about five times its —

'
weight t h e solution is filtered w h i l e h ot and then set aside to
—
,

crystalliz e M ore crystal s are to be obtained from the mother

.

l iquor up on evaporation .

R e act i on . 2 N a 2H PO 4 : N a 4 PzO 7 —
H 20 .
60 2 S OD I U M S AL I CY LA T E .

dark colored when finish e d or a fter being kept a short time

-
.

E Ho ffman recommends preparing the salt by stirring 2 0 parts

.

of sodium bicarbo nate an d 3 3 parts of dialyzed sal icylic acid with

enough water to form a thick paste allowing the carbonic acid ,

time to escape and then evaporating to dryness

, .

T he pres ence o f iron ( even mere traces ) cau ses a reddish dis
coloration of the salt and solutions o f it Hence filter paper quite .

free from iron must be use d .

A crystall ized product may be o btained from a saturated alc o

holic solution The crystals should then be drained in a funnel
.

and dried in a porcelain dish with t h e aid o f moderate heat A n .

additional quantity o f salt may be recovered from the mother

l iquor on evaporat ion S hould the mother l iquor be colored it
.
-

may be decolorized by filtration t h rou gh a n i m a l charcoal unles s

’

the coloration is due to iron The salicylic acid contained in the .

last mother l iquor can be recovered by evaporating to dry nes s

-
,

redissolving the residue in water and precipitating by adding an

excess o f diluted sulphuric aci d .

D e s cn p t i on white amorphous or crystalline powder odor

.
—
A , ,

less s weetish sal i n e a fterwards acrid S oluble in

, , ,
part o f .

water and in 6 parts o f alcohol at

,
Ver y soluble in these sol
vents at their boiling points S oluble al so in glycerin Th e water
. .

solution shoul d have a slightly acid reaction on test paper -

.

S OD IUM S AN T O N I N AT E .

S OB I I S A N TON I N A S .

2 N a C1 5 n O , 7 H zO 6 98
—
. .

S antonin 10 Gm
S olution o f soda 35 Gm
Water 1 0 Gm

M ix d digest until
an diss o lved ; filter set in a cool place t o ,

cr y stall ize E vaporate the mother l iquor to recover more as long

.
-
,

as the crystals obtained are colorl ess .

Keep it in a tightly corked bottl e an d protected from the light

-
,
.

R ecover the rem ainder o f the S antonin from the last mother
 S OD I U M S AN T ON I NA T E . 60 3

liquor by acidulating with hydrochloric acid when it will sep ,

arate in crystall ine form .

A l bu m i n a te d S a n t on i na te o f S odi u m .

S antonin
S odium bicarbonate
D rysoluble albumen
Water

D igest together at 60 C until d issolved Filter °

. . . E vaporate
by gentl e heat S pread it on glass plates to dry
. .

B rilliant pearly scal es solubl e in water , .

S OD IUM S I L I CA T E S OLU TI O N .

L I QUOR S OD I I S I L I CA T I S .

( Water glass
-
. S oluble glas s . L iquid glass ) .

Containing 3 3 per cent o f a mixtu re o f sodium tri s il icate -

( N a z S3
i O ) and
7
sodium t e t r a s i l i c a t e ( N a S i O 9)
It must be free z 4
.

from caustic alkali .

When an intimate mixture o f one molecul e o f dried sodium

carbonate and fou r molecules o f s ilica are fused t ogether the ,

fused mass is water soluble and a solution having a s p w o f from

-
,
. .

to is emplo y ed for surgical dres sings I t is a syrupy .

,

colorless odorless l iqu id

,
.

S OD IUM S UL PH A T E .

S OD I I S UL PH A S .

'
[ Glauber s S alt .
]
O btained as a bye product in th e -
of hydrochloric m a n u fa c t u ne
acid from sodium chloride and sulphuric acid A lso in many .

other chemical processes .

T he crude Glauber s S alt may be purified as follows

’
60 4 S OD I U M S UL PH A T E .

C r ys ta l l i z e d S o d i u m S u lph a te .

Glauber s salt ’

Water
L ime ,

Chlorinated lime .

D issolve the salt in the water and the solution to the boilin g
point .

S lake a piece o f l ime and add water enough to form a thick , ,

“ ”
m ilky mixture ; O f this milk o f lim e add so much to the hot
'

solution o f Glauber s salt to render it alkaline to test paper S ti r

’
.

well .

M i x some chlorinated lime with enough water to form a thick ,

milky mixtu re ; o f this add a small quantity at a tim e to the solu

’
tion o f Glauber s salt until a filtered test sample no longer bec omes ‘

discolored by hydrogen sulphide after acidulation with hydro

chloric acid .

When free from iron filter the li quid an d evaporate the filtrate
, ,
'

until it has ac q uired the s p w 1 z 5 a t 4 0 C S et the solution

‘
°
. . . .

aside in a crystall izer at rest and let crys tall ization be e ffected in
, ,

the usual w ay D rain the crystals press them g entl y between

.
,

cloths or bi bu l ou s p a p e r until dry and at once place them in dry

'

bottles wh ich are to be tightly closed

P u r e S od i u m S u l ph a te may also be m
.
,

ade from diluted sul

p h u r i c acid and sodium carbonate .

D e scri pt i on —
L arge colorl ess transparent cryst als odorless ; o f
, , ,

°
somewhat bitter sal ine taste ,
. in air S oluble at 1 5
E ffl or e s c e n t .

in parts o f water ; at 3 4 °
in one fourth its weigh t o f water ;
—

at 1 00 in
°
part o f water . Ins oluble in alcohol N eutral . .

Ca r l s ba d S a l t .

D ried sodium sulphate

S odium bicarbonate
S odium chloride
Pota s s ium sulphate

M ix the pr eviously powdered dry salts .

[ Carlsbad water contains about 6 Gm o f salts to each liter ] .

60 6 S OD I U M S UL PHIT E .

I n both cases a bi s u l p hi t e
is first made and this is converted into ,

normal sulphite by the addition o f a quantity o f the alkal i equal

to the amount used in making the bisulphite .

T he salt must be kept in tightly cl osed bottles in a co ol place -

.

D e scri pt i onColorl ess prisms or powder resembling potassium

.
—
,

sulphite in most o f its properties O dorl ess . .

It has a cooling saline s ulphurous taste S oluble in 4 parts

, , .

o f wa ter at I 5 and in °
part o f boil ing water S paringly sol .

uble in alcohol .

S OD IUM TAR TR ATE .

S OD I I T A R TRA S .

T artaric acid
S odium carbonate
D istilled water .

D issolve the sodium carbonate in the wate r A dd the tartari c .

aci d gradually stirring a fter each addition until dissolved Filter

,
.
,

evaporate an d crystallize or evaporate the filtrate t o dryness to ,

obtain a granular product .

R e act i on . N a zCO 3 — I
N ot e s . parts o f sodium bicarbonate may be used inste a d
1 48 of

2 5 1 parts o f normal sodium carbonate .

D e scri pt i onColorless transparent c rystals ; odorless ; o f cool

.
—
,

ing mildly saline taste S olubl e in 5 parts o f water at

,
. In
soluble 1 n alcohol N eutral to litmus paper . .

S OD IUM T E T R A B O R A TE .

S OD I I T E T R A B OR A S .

0
[ S odium Pyroborate ] Borate . S odium .

Borax occurs native in Pers ia Thibet an d other western A siatic , ,

countries and in large deposits in Cal i fornia and N evada either

, ,

alone or with othe r borates M ost o f the borax now used is made .
 B ORA X . 60 7

from crude boric aci d by fusion with dried sodium carb onate ,

solution in water and cry stallization , .

D e scr i pt i on
Colorless transparent crystals or white powder
.
—
, ,

inodorous having a sweetish alkal ine taste S lightly e fflor e s c e nt

, ,
.

in warm dry air S oluble in 1 6 parts of water at 1 5 C and in

, .
°
.

one hal f its ow n weight o f boiling water Ins oluble in alcohol

-
. .

S olubl e in 1 part o f glycerin at 8 0 C

°
.

Crys ta l l i ze d S odi u m T e tr a bor a te .

Borax 1 part
Water 1 6 parts

D is solve the borax in the water by the aid o f heat filter the ,

solution and crystall ize the salt by spontaneous evaporation o f the

,

solvent in t h e u s u a l way .

T u r bi d a te d B ora x .

Borax 1 part
B oil ing water 2 parts

filter and cool the solution rapidl y constantly st i rring

D issolve , , ,

it to as low a temperature above freezin g as may be c onveniently

, ,

attained .

Collect drain and dry the salt

, ,
.

S OD IUM TH I O S UL PH A T E .

S OD I I T H I O S U L PH A S .

N S O3 S 5H QO .
—
2 48 .

S odium H y posulph ite .

Thi s salt which is a m onot hi o s u l p h a t e may be prepared bv boil

, ,

ing sulphur with a solution o f sod ium hydroxide and then pa ssing
sulphu r dioxide into the l iquid until c olorless The solution i s .

then brought to crystallization .

It may al so be made by boiling sulphu r with a solution o f s o

d i u m sulphite .

Commercial Sodium thiosulphate m ay be purified by r e c ry s ta l

li za t i on
. For th is pu rpose it shoul d be dis solved in its own weight
60 8 S OD I U M THI O S UL P H A T E .

o f d i s t il le d w a t e r the solution filtered and evaporated slowly

, , .

L arge crystals are easil y obtained .

It should be kept in tightly closed bottles .

D e sc ri p t i on
Colorle ss od orl ess crystals soluble in
—
part, ,

°
o f water at 1 5 C and in about 0 5 p art at 2 0 C Insoluble in
. .
°
.

alcoho l .

[ S odium hyposulphite 1 8 an un fortunate mi sno mer for rea l

“

sodium hyposulphite is N a S O 2 ] z
.

S OD I UM V ALE R A T E .

S OD I I V ALER I A NA S .

N a CS H Q O z : 1 24 .

I amylic alcohol
S O-

Potassium dichromate
S ulphuric acid
Wa ter
S olution o f sodium h y droxi de su fficient , .

D ilute the sulphuric acid with on e hal f o f the water D i ssolve -

.

the potassium dichr omate in the remain der o f the wat er with the
a id o f heat When both liquids are col d m 1 x them with the amylic
.

alcohol in a retort or flask with oc c a s 1 0 n a l brisk a g itation until

, .

the temperature o f the m ixture has fallen to about 3 2 C Con °

.

n e c t with a condenser and distil u ntil about 4 parts of distillate

‘
,
'

has been obtained S aturate the distilled liqui d accurately with

.

the sol ution o f sodium h y droxide remove any oily fluid which ,

floats on the surface evaporate until watery vapor ceas es t o

,

escape and then raise the heat cautiousl y until the salt is l iquefied
, .

When the product has cooled and s olidified break it into pi eces , ,

and immediatel y put it into a stoppered bottl e .

R e a ct i on .

C H 1 00 2+
2 KQ S O4+ c rz 5 04 ) ) l " I I H 20
3 5 2 “

3
°

N ot e s The dichromate o f potas sium is decomposed by the sul

.

p h u r i c ac i d the products being

,
potassium sulphate and chromic
aci d The amyl ic alcohol is then oxidized by t h e chromic acid
. ,

and when the mixture is subj e ct ed to distillation the distillate ,

consists o f v a l e r i c acid and amyl valerate ( or apple oil )

'

.
610 S T RON TI U M C AR B ONA T E .

the filtrate heated at a temperature of 1 0 0 C a su fficient quan

,
°
.
,

tity o f sulphur ou s acid to caus e the disappearance of the char

a c t e r i s t i c color o f the chromic acid and the appearance o f a g r e e n i s h

color due to the formation o f chromic s alt meanwhil e main ,

taining the temperature at the boil ing point o f water B oil t h e .

liqu id until the excess of sulphurous acid is expelled Continue .

the boiling and add enough strontium carbonate to cause the com “

p l e t e precipitation o f the chronium by the strontium carbonate .

Filter Pour the filtrate into a filtered solution o f sodium car

.

bonate used in excess Wash the precipitate until the washings

.

are tasteless and leave no perceptible residue on evaporat ion D r y .

the product at a moderate heat .

D e scr i p t i on .
—
An amorphous wh ite odorless and tasteless
, , ,
in
soluble powder .

S TR ON TI U M CH LO R I D E .

S TR ON T I I C H L OR I D U M .

S trontianite in powder ,

H y drochloric acid ( 3 2 % o f H Cl )
S trontium hydroxide
Water

M ix the p owdered s t ron t i a n i t e i n a porcelain d ish with the water .

Heat the mixture to about S tir well A dd the acid in s ev .

eral portions waiting after each addition until the e ffervescence

,

has subsided before adding more When all o f the acid has been .

added heat to boiling for hal f an hour Then add the strontium .

h y droxide an d stir well The solution shoul d be alkal ine in r e a c

.

tion ; i f it is not a dd more o f the strontium h y droxide to produce

,

an alkal ine reaction Keep the li quid hot for an hou r longer
.
,

stirring frequently Then filter A dd enough hydrochloric acid

. .

to the filtrate to render it acid E vaporate to-

sp w S e t it
. . .

aside to c ool an d cr y stall ize D rain and d ry th e cr y stals . .

The mother l iquor yields more salt on evaporation in the usual

-

way .

R e a c t i on .
 S T RON TI U M C H LOR I DE . 61 I
N ot e s The strontium chloride thus obtained i s not pure The
. .

principal impurity is barium chloride for the strontianite contains ,

barium carbonate Calcium salt is also contained in the product

. .

It m ay be p a r t i a ll v purified as follows

D issolve it in water A dd enough ammonia water to impart

.

an alkal ine reaction on l itmu s paper S ti r well Filter A dd . . .

enough diluted sulphuric aci d to the filtrate to render the l iquid

decidedly acid in reaction L et stand for two days Filter A dd
. . .

enough pure strontium carbonate to neutralize the free acid and

leave an excess o f strontium carbonate undissolved S e t the mix .

ture in a warm place for a day Filter again E vaporate the . .

filtrate to dryness D issolve the res idue in three times its weight
.

o f water filter and evaporate to crystall ization

, ,
.

The barium chloride may also be partially precipitated from the

solution o f strontium chloride by the addition o f alcohol in which
strontium chloride is soluble whil e the barium chlori de is insoluble
in it O r the strontium chloride may be dissolved in al cohol the
.
,

solution filt e r ed an d evaporated to dryness the salt being then r e ,

crystallized from a water solution .

D e s cr i p t i on .
—
L ong colorless del iquescent crystals readily s ol
, , ,

uble in water and in alcohol .

S TR O N T I U M H Y D R OX I D E .

S T R ON T I I H Y D R OX I D U M .

A dd 8 parts o f water to 5 parts o f the oxi de A solid crystall ine .

mass is formed D issolve th is in 4 0 parts o f boiling water ; filter

.

hot ; let the filtrate cool sl owly Collect and d r y the cr y stals . .

D e scri pt i on .
—
Transparent colorless del iquescent crystal s
, ,
.

S TR O N TI U M IOD ID E .

S T R ON T I I I OD I D U M .

M ay be prepared from iron iodide and strontium hydroxide

Calcium Iodide p ,
.
612 S T RON TI U M I OD I DE .

D e s cr i p t i on i
Colorless transparent plates ; odorless ; taste
—
,

sal ine bitterish D el iquescent B ecomes yellow on exposure to

, . .

a ir and light S oluble in

. part o f water at and in
part o f boiling water A lso soluble in alcohol . .

M ust be kept in tightly closed bottles protected against light -

S TR O N TIUM LA CT A T E .

S T R ON T I I LA CT A S .

S trontium carbonate 1 pa rt
L actic acid su fficient , .

Place the strontium carbonate t ogether with 5 parts o f distilled

water in a porcelain di sh over a water bath A dd the lactic acid -
.

gradually stirring constantly until but l ittl e of the strontium car

, ,

bonate remains undissolved Continue heating the mixtu re at the .

maximum heat o f the bath until the lactic acid it saturated , ,

adding i f necessary a l ittle more strontium carbonate so as to

, ,

have a su fficient excess to insure c omp l ete n eutral ization L et .

the liquid cool filter it an d evaporate it at a temperatu re o f be

, ,

°
tween 6 0 and 8 0 C until a crystalline mass i s formed on cool
°
.

ing D ry the product in a current o f air without the aid o f heat

. .

Keep it in well stoppered bottles -

.

D e s cr i p t i on
white granular powder ; od o rless ; taste sal ine
.
—
A , ,

slightly bitter S olubl e in 4 parts o f water at

. in less than
one hal f its weight o f boiling water A lso solubl e in alcohol
—
. .

S TR O N TI U M N I TR AT E .

S TR ON T I I N IT RA S .

S r( N O3 ) 2

S trontian ite ,
in powder
N itric acid ( 68 % o f H NO
S trontium h y droxide
W ater
614 S UL PH UR .

ammonia water an d digest for three days agitating occasionally

, , .

Then add 1 0 0 ml o f water tr ans fer the mixture t o a muslin ,

stra iner and wash the sulphur with water until the washings
,

ceas e to give an alkaline reaction on test paper Then drain pres s -

.
,
‘

strongly dry it at not over 4 0 C ( 1 0 4

, and powde r by
°
.
°

running it through a N o 3 0 S ieve . .

N ot e s The obj ect o f this process is to neutral ize and wash

.

away the sulphuric acid which i s alwa y s present with sublimed

sulphu r an d the digestion for three days is intended to rem ove
,

al so a ny arsenic present To e ff ect the extraction o f the arsenic

.
,

conti nued digestion is required and three days is not too long as , ,

the ammonia i s very diluted Care should be taken however .

, ,

not t o us e higher heat than 4 0 C ( 1 0 4 F because above that °

.
°

temperatu re a go od deal o f ammon i um hydrosulphide m a y be

formed and at the boiling point the sulphur will dissolve as long
,

as su fficient ammonia remains to act upon it Boiling water is .

,

therefore not to be us ed It is under all circumstances necessary

, .

to wash out all the ammonia and ammonium salt from the sulp h ur
be fore drying it .

It i s important to dry the washed sulphur thoroughly before

putting it in its receptacle for the presence o f any moisture Would
,

result in the formation of sulphuri c acid a gain rendering a repeti ,

tion o f the washing necessar y .

R e ac t i on . A szS 3 H
+ 2 5 0 4 + 6 H 4
N O H

D i
e s crp t i on A fine yellow—
odorl ess and tastel
,
ess powder ,
. In
soluble in water and in ofli c i a l alcohol .

Pr e ci pi ta te d S u l phu r .

S UL PH UR PR A E C I PI T A T U M .

S ublimed sulphur parts 2

L ime 1 part

O ffic ia l h y drochloric acid water each su ffici ent , ,

.

S lake the l ime and make it into a uni form mixture with 1 0 parts
o f water A dd the sulphur previously well dried and s i fted mix
.
, ,

well add 25 parts o f w ater and heat the mixtu r e to boil in g for
, , .
 S UL PH UR . 61 5

one hour stirring constantly and replacin g the water lost by

, ,

evaporation Then cover the ves sel allow the contents to cool
.
, ,

pour o ff the clear solution filter the remainder and unite the , ,

liqui ds .

A dd gradually h y drochloric acid p re vI ou s l y diluted with an

equal volume of water until the liquid is nearl y ne utral ized being
, .
,

care ful to leave it still distinctly alkal ine in reaction and o f yellow
color .

Collect the precipitate on a stra iner and wash it with water ,

until the washings are tasteless and no longer give an acid re a c

tion on test paper Then dry it at a gentle heat
-
. .

R e ac t i on s
The lime is first slaked
.
,

Then when sulphu r is boiled with the calc ium hydroxide the fol
, ,

lowing reaction occurs : l —

3 H O
2 The
. solution containing calcium t e t r,a t h i o s u l p h a t e and
calcium thiosulphate is next treated with h y drochloric acid when
, ,

sulphur i s precipitated :

N ot e s The quantit y o f l ime used i s purposel y somewhat i n ex

.
,

cess o f the amount required by theory to make up for carbonate ,

contained in it A larger excess would however result in loss

.
, ,

because the compounds then formed would yield larger quantities

o f H S when the hydrochloric acid is added
2
.

By long boil ing the calcium mono thiosulphate is spl it up into -

sulphite and sulphur A portion o f the sulphite is oxidized to sul

.

phate which i s precipitated

,
.

I f the first portion o f hyd rochloric acid is added very slowly no

hydrogen sulphide is formed because the reaction then is ,

When more aci d is

added however the reaction j ust described is followed by
, ,
‘

—
2H 2
S .

The directions o f the Pharmacopoeia are to onl y nearly n eu ’

t r a l i z e the solution and to be care ful to l eave it slightl y a l k a l i ne

,
.

The obj ect o f this precaution is to prevent the precipitation o f

any arsenic present The calcium thiosulphate i s not decomposed
.

unless enough h y drochloric acid be added to impart an aci d r e ac

tion to the l iquid Hence the sulphu r which enters into the
.

structure o f the calcium th iosulphate i s lost But i f enough h y .

d r oc hl or i c acid be added t o decompose the thiosulphat e ( 2 Ca S S ,

the arsen ic will also

616 S UL PH UR .

be precipitated as follows :
3 Ca C12+
2 S .

When the liqu id is alkaline however all o f the arsenic remains , ,

in solution .

Care should be taken to arrange so that the h y drogen sulphide

gas i s led off t hrough a flue or t h e operation should be carried ,

out in the open air The gas i s evolved in large enough quantities
.

to be very anno y ing to the operator .

The aci d must be added to the solution of the sulphur salts and
not vi c e ve r s a ; moreover the acid must be diluted as directed ; ,

otherwise an oily product ( H S ? ) i s formed which a fterward s z z

is diffi cult to el iminate and which but slowly decompos es giving ,

o ff H QS .

The well washe d precipitated sulphur must be rapi dly but

—

thoroughly dried at a moderate heat and kept in tightly closed -

bottles .

D e s cr i p t i onodorl ess and tasteless pale yellowish fine

.
—
An ,
-
,

powder insoluble I n water ; readily soluble in carbon d isulphide

,
°

als o soluble in ether chloro form fixed oils an d volatile oil s ben
, , ,

z in and benzol M elts a t I 1 5 C and at a higher heat volatilizes

, .
°
.
,

without residue or burns in t h e air forming sulphu r dioxide

, .

S UL PH U R D I OX I D E .

S U L PH U R I S D I OX I D U M .

S O 2: 6 4 .

Copper turnings or scraps

Concentrated sulphuric acid
Water

Put the sulphuric acid in a p orcelain dish o f about one

l iter s capacit y ; set the acid into rapid whirl ing motion by cir
’

c u l a t or y stirring in one direction with a glas s rod Then s l ow ly .

pour the water into the acid continuing the stirring uninterrupt ,

e d l y until all the water has been added .

Put the copper into a roun d bottomed flask o f about one and -

one hal f liter s capacity Provide the flask with a twice perforated
—
’
.

rubber stopper carr y ing a thistl e tube and a del ivery tube Con .

’
neet the delivery with a wash bottle o f about one hal f liter s . - —
6 18 S UL PH UR I OD I DE .

S UL PH U R IOD ID E .

S U L PH U R I S I OD I D U M .

Consi sts chiefly of 8 21 2 2 3 1 7 .

Washed sulphur
Iodine

M ix them thoroughl y by trituration in a glazed porcelain mor

tar ( or in a glass mortar ) Put the mixture into a flask beaker .
,

or wi de mouthed bottle close the top loosely and apply gentle

-
, ,

heat ( not exceeding 6 0 C ) by means o f a water bath until the °

.
-

elements combine which is known by the fact that the mass as

,

sumes a u n i fo rm l v dark color Then rai se the temperature until

‘

the mas s becomes liquid Pour the fused sulphur i odi de upon .

a porcelain til e or plate or upon any other conven ient cold sur face
not a ffected by it B reak the cake wh en cool into small pieces
.
, ,

and trans fer the product to small glas s stoppered bottles -

.

M ust be kept in a c ool place .

N ot e s The s ulphur and iodine when previousl y int i mately

.
, ,

mixed combine eas ily The compoun d S I 2 is however not

,
.
2 , ,

stable I f during the process of h eating the iodine an d sulphu r

. .
,

together or in the fusion o f the iodide any portion o f the iodine

, ,

shoul d become volatil ized and condense upon the si des or in the
upper part o f the container in which the reaction is performed ,

this iodine must be returned to the l iquid portion by bringing i t

in contact with the fused mas s which is easily accompl ished by ,

inclining the container in the direction required Full water bath .

-

heat is su fficient to eff ect the liqu efaction o f the produc t The .

flask or other vessel in which the iodide o f s ulphur is made may

be covered with a watch cr y stal during the operation .

D e s cri p t i brittl e gra y ish black cr y stall ine sol id o f s ome

on .
—
A ,
-
,

what metallic lustre having a n odor o f iodine and an acrid taste

,
.

Insoluble in water ; soluble in 6 0 parts o f glycerin D ecomposed .

‘
by a l c oh ol a n d ether wh ich d i ssolve the iodine leaving the sul
, ,

phu r It loses iodine on exposure D ecomposes when heated

. .

l ong or to a high temperature ; but it shoul d l eave no residue on

volatilization .
 TI N C HL OR I D E . 619

TI N CH LO R I D E .

S TA N N I D I CH L OR I D U M .

S
( tannou s Chloride . Tin S alt ) .

T in granulated
,
1 00 parts
Hydrochloric acid ( 3 5 70 o f H Cl ) 1 75 parts

D issolve the tin in the hydrochloric acid by digestion Finally .

heat at about 6 0 until all action c e ases and the acid i s saturated
°
.

L et cool and settle D ecant the clear solution and evaporate it to

.

the s p w o f . . Then set it as ide in a covered dish to cr y stal

lize D rain the crystals well in a covered funnel an d dry the
.
,

product in a desiccator over sulphuric aci d B ottle the salt as .

soon as dry
‘

R e act i on . S n + 2 H Cl n C12 + H 2
.

D e scri p t i on Colorless crystals soluble in

.
—
, part o f water at
D ecomposed by more water .

ZI N C A C E T A T E .

ZI N GI A CE T A S .

Zn C2H 3 O z ) 2 . 2H z O —
2 19 .
3 .

A cetic acid
D istilled water

M ix 60 0 ml of the acid with the whole o f the water i n a flask ,

add the zinc oxide agitate gently and warm the m ixture to about
, ,

6 0 C ; add the remainder o f the acid gradually continu ing the

°
.
,

digestion until no more o f the oxide is dissolved Heat the solu .

tion to the boiling point ; filter whil e hot add a littl e acetic acid ,

( about 1 0 ml ) to in sure that the acid is present in slight excess .

S e t the solution in a cool place for t w o d a y s to cr y stallize De .

cant the mother l iquor evaporate it over a water bath to one hal f
-
,
- —
,

acidulate w ith acetic acid as be fore i f necessary and again set , ,

6 20 Z I N C A CE T AT E .

aside t o cr y stallize in a cool place Put the crystals in a funnel .

to drain ; then d r y them on filter paper or on a porous tile with ,

out the aid o f heat .

M ust be kept in a tightly corked bottle -

.

R e act i on .

N ot e s . The same result will be obtained i f 4 2 0 Gm of zinc

carbonate be used instead o f 3 0 0 Gm o f the oxide The carbonate .

shoul d be a dded gradually on account o f the e ff ervescence caused

by the liberation o f carbonic acid an d the solution formed is then ,

to be boiled a few minutes t o expel the carbonic acid per fectly .

When the preparation is made on a manu factu ring scal e from

comm ercial z inc oxide or carbonate it is necessary to digest the ,

solution o f acetate o f zinc for s everal days with some pure metalli c
z inc or with pure zinc oxide in order to remove a n y lead copper
, , , ,

cadm ium and i ron that may be present By this digestion how .
,

ever some bas ic z inc acetate i s formed which must be converted

, ,

into normal acetate by the addition o f more acetic acid before

crystallizing A solution o f basic salt w ill not cr y stallize but th e
.
,

presence o f a l ittl e free acet i c acid facil itates the crystallization .

When the first crop o f cr y stals h a s been coll ected the m other ,

°
l iquor must be evaporated at a temperature not above 8 0 C .

( 7 6 F ) until a pellicle forms a fter which it i s set aside in a

°
1 .
,

cool place I f the evaporation is carried too far a precipitate o f

.

zinc acetate containing but one molecule o f water o f c ry s t a l li za

tion will deposit .

Z inc acetate may al so be made by double decomposition from

'

3 p8 a r t s o f lead acetate an d 2 9 parts o f zinc sulphate each dis ,

solved i n 8 0 parts o f distilled water the solutions being filtered ,

and then mixed The reaction is then .

D e scri p t i on .
—
S o ft
white pearly crystals o f a faintly acetous
, , ,

odor and an astringent a fterwards metallic taste S oluble in

,
.

parts o f wat er and in 3 6 parts o f alcohol at in 1 5 parts of .

boiling water and in 3 parts o f boil ing alcohol R eaction acid

,
. .
6 22 z1 N C C ARB O NA T E .

D issolve the sodium carbonate in 4 0 parts o f the water in a

porcelain capsule D issolve the z m c sulphate in an equal quantity
.

o f boiling water Place the capsul e containin g th e s olution o f

.

sodium carbonate on a sand bath s o as to keep the solution hot ; -

then gradually add the solution o f zinc sulphate stirring briskly ,

.

B oil the mixture for fiftee n minutes a fter the e ff ervescence has
ceased ; th en let the precipitate subsi de D ecant the mother l iquor .
- -

and throw it away A dd 1 2 0 parts o f boiling water to the p r e c i p

.

i t a t e and stir well let settle once more an d repeat the washing
, , ,

by a ffusion and decantation o f hot di stilled water until the wash

ings cease to give any precipita te with test solution o f bariu m
,

chloride Collect the precipitate on a muslin stra i ner or on a

. .

paper filter let i t 'd ra i n thoroughly an d then dry it at a gentle

, ,

heat .

R e act i on .

5 N a 2 C O 3 + 5 Z n S O , +3
H z O

2 2n CO , .
3 Z n ( OH ) 2
—
5 N a Q S O ,
—

3 CO z .

N ot e s The solutions are used hot in order to expel all th e car

.

boni e acid which i s set free carbon dioxi de escaping with e ff e r ,

v e s c e n ce I f cold solutions are u sed a portion o f the precipitate

.

redissolves in the carbonic aci d held in t h e liquid The z inc sul .

phate i s to be added to the sodium carbonate in order t o keep the

latter in excess and by having the soda solution hot the further
, ,

advantage is gained that the precipitate is more readily washed

free from sodium salt .

D e scr i p t i on .
—
A fine white odorless and tastel es s insoluble
, , ,

p owder .

ZI N C CH LO R I D E .

Z I N GI C H L OR I D U M .

Z n C12 .

A solution o f zinc chloride i s pre p ared as described in the

article bel ow It is then evaporated to dr y ness and the residue
.

fused o r the product is granulated It must be bottled while

,
.
 ZI N C C H LOR I DE .
62 3

warm in warm dry bottles and should be kept in small tightly , ,

stoppered bottles .

D es cr i p t i on Zinc chloride shoul d be perfectly white It is

—
.

very deliquescent Its solution is strongly acrid corrosive and

.
, ,

o f acid reaction .

Z i n c Ch l or i d e S ol u ti on .

L I QUOR ZI N GI C H L OR I D I U . S .

The o fficial solution o f zinc chloride ( U S P 1 890 ) con ta ins . . .

,

about 5 0 per cent o f Z n Cl z It is prepared as follows .

Granulated zinc
Hydrochloric acid
N itric aci d
Precipitated zinc carbonate
D istilled water su fficient ,
.

Pu t the zinc in a glass or porcelain ves sel an d add 1 5 0 ml o f ,

distilled water Then add the h y drochloric acid gradually D i

. .

gest until the acid shal l have becom e saturated D ecant the solu .

tion from the undissolved excess o f z inc .

A dd the nitric acid to the solution evaporate the mixture to ,

drynes s and heat the dry mas s to fusion at a temperatu re not ex

c e e d i ng 1 1 5 C °
.

L et the fused zinc chloride c ool and then dissolve it in a s u ffi

cient quantity o f distilled water to make the weight o f the solution
one thousan d grams .

A dd the precipitated zinc carbonate agitate the mixture occa ,

s i on a ll y during twent y four hours and then set it as ide at rest

—
, , ,

until clarified by subsidence .

Finall y separate the cl ear solution by decantation or by means

o f a glass syphon and k e ep it in glass stoppered bottles
,
-
.

R e a ct i on . Zn -
Z n C12 —
H 2
.

N ot e s The metal dissolves in t h e hydrochloric acid with the

.

l iberation o f h eat and the evolution o f h y drogen Instead o f .

adding the acid to the zinc the metal may be added to the acid ,
.

The eff ervescence caused by the escape of the h y drogen mav

b e very active at first but subsides as the zinc chloride increases
,

a n d the acid diminishes When but little acid remains digestion.

6 24 Z IN C C H LOR I DE .

'

is necessary to cause complete s a t u r a t i on a n d further digestion ,

is des irable to cause the separation o f certain foreign metals which

may hav e been contained in the zinc .

Commercial zinc is usually contaminated with one or more o f

the metals copper lead arsenic cadmium ir on and manganese
, , , , ,
.

When an excess o f zinc is used so that a portion of it remains ,

undissolved at the end of the digestion s everal o f thes e other ,

metals dissolved together with the z inc are precipitated by th e

latter on prolonged digestion .

But one o f the most common impurities is iron which can not ,

be precipitated by digesti on w ith an excess o f zinc To remove .

the iron ( and manganes e ) nitric acid is added to convert the

ferrous chloride to ferric and the solution is evaporated to dry
,

ness and the residue fu sed to expel the excess o f nitric acid The .

fu sed zinc chlo ride ( containing any iron chloride derived from
the iron in the zinc used ) is then redissolved and the solution
shaken with precipitated zinc carbonate which removes the iron ,

which is precip itated in the form of hydroxi de .

S olution o f zinc chloride cannot be filtered through paper be ,

cause the latter swells until its pores are closed and is then cor
roded I t may be filtered through powdered and washed glass
.
,

or through purified asbestos D ecantation i s sometimes s u ffi .

cient A dilute solution may be filtered through paper but the

.
,

organic substances then taken up by it blacken the product as

soon as su ffi cientl y concentrated by evaporation .

D e scri p t i onclear colorless odorles s liquid o f astringent

.
—
A , , ,

sweetish metallic taste and aci d reaction Corros ive in its action
,
.

upon organic matter S p w about at 1 5

. . .
°

ZI N C C Y A N I D E .

ZI N GI CY A N I D U M .

Prepared by precipitating a solution o f zinc acetate w ith hydro

cyanic ac i d .

D e scri p t i on .
—
A
colorless salt insoluble in water and in alcohol , .

but soluble in solutions o f alkalies with wh ich it forms water

solubl e double salts .
6 26 ZI N C OLEA T E .

200 parts o f hot water A dd the col d soap s olution to the solu .

tion o f zinc acetate stirr i ng briskly D rain the precip itated zinc
, .

oleate on a muslin strainer and wash i t s everal times with Col d ,

water D r y it on paper or muslin without the ai d o f heat

.
, .

R e aCt i on . 2N 3 C1 8 H 33 0 2+
Z n C2
H 3 og 2
2 211 Cl g H gg
oz ) 2 +

2 N a C2 H 3 O2 .

N ot e s The sodium acetate i s eas ily washed away from the

.

precipitated oleate The yield is about parts . .

D e scr i p t i on —
A s oft white powder having a
, , s oa p y
'
fe e l .

A n o th e r M e th od .

Zinc sulphate 3 parts

Powdered Castile soap 5 parts

D is solve the zinc sulphate in 3 0 0 parts o f water and the soap in ,

2 0 0 parts o f hot water Keep the soap solution at the temperature .

o f about and a dd to it slowly and with brisk stirring the

s olution o f zinc sulphate Collect the precipitate on a musl in .

strainer wash it with water o f 4 0 temperature drain it well and

,
°
, ,

dry it at not over Pass the dried friable mas s th rough a

S i eve.

O ffi c i a l Z i n c O l e a te .

Put th e ol eic acid in a r oom y porcelain dish an d s i ft the z inc ,

oxide into the aci d stirring well so as to mix the two thoroughl y
,

and avoi d the formation o f lumps L et the m ixture stand s everal .

hours stirring occasionally Then heat the mixture over a water

,
.

bath u nt i l t h e oxide is completel y d issolved

‘
.

R e act i on . Z n O + 2 H C1 8 H 33 O -

2
: Zn ( O .

N ot e s ; I f the quantities operated upon are smal l the zinc oxid e ,

 Z I N C OLEA T E . 6 27

previously s i fted may well be mixed with the oleic acid by t r i t u

,

ration i n a mortar the aci d being gradually added to the oxide

, .

The mixture should be allowed to stand at l east two hours before

it is heated .

It will be observed that a very large excess o f oleic acid i s used ,

so that the preparation is a mixture o f zinc oleate and oleic acid .

The zinc oxide used must be quite free from iron ; otherwise
the pr oduct will be pinkish or reddish or yellowish according
, , ,

to the condition and amount o f iron in it .

D e s cr i pt i on soft white homogeneous ointment is formed

—
A , ,

out o f zinc oxide and oleic acid when the percentage of zinc oxide
is s u fli c i e n t ; with les s zinc oxide the product is fluid or semi fl u i d -
.

Tru e zinc oleate without an exces s of oleic acid is a powder

, ,

The o fficial zinc ol eate obtained by the formula here given is

, ,

soft ointment .

Pure z inc oleate i s prepared a s d escribed under Z i n c i O leas .

ZI N C OX I D E .

Z I N CI OXI DU M .

Z nO

Calcine the o fficial zinc carbona t e in a d ish at a low red heat

until a cooled sample mixed with a little water no longer e ff e r
, ,

vesces with d iluted hydrochloric acid .

R e act i on . 2 Z n CO , ) 3 Z n ( O H ) 2 :
.
a O

N ot e s T oo high heat renders the pr oduct yellow and thi s

. ,

yellowish tint m a y be retained for a l ong time [ A ll pure zinc .

oxide turns yellow whe n heated but becomes white aga in on cool
ing unl ess it was heated too strongl y A zinc oxide containin g .

much iron is alwa y s discolored even i f n ot overheated in the proc

ess o f calcinatio n ] O verheating also makes zinc oxide less so ft
to the feel .
6 28 ZI N C P H ENOL S UL PH ONAT E .

ZI N C PH E N O L S U L PH O N A T E .

ZI N GI PH E N OL S U L PH O N A S .

( S ulphocarbolate of Zinc ) .

Crystallized phenol
S ulphuric acid
Barium carbonate
Zinc sulphate
Water .

A dd the phenol the acid mix well and heat the m ixtu re at
to , ,
°

5 5 in a porcelain dish over a water bath for several days A dd -

.

4 0 0 parts o f water and mix well Then neutral ize by adding the .

barium carbonate stirring the whole thoroughly Filter R ej ect

, . .

the precipitate To filtrate add the zinc sulphate previously dis

.

solved i n 2 0 0 parts o f water N ow filter away the precipitated

.

barium sulphate slightl y acidulate the filtrate with sulphuric acid

, ,

and evaporate to crystallization .

Puri fy the product by repeated r e crystallizations -

.

R e acti on s . 2H C6 H 5 S O , + B a CO g

CO and then ,

B aS O4 .

N ot e s The solution o f zinc sulpha te shoul d be added to the

.

solution o f sulpho carbolate o f barium until exactly precipitated

-

that is the further ad dition of zinc sulphate must be discontinued

,

as soon as it no longer causes any further precipitation S ulpho .

carbolate o f zinc c rystall izes more readi l y and without reddish ,

color f r qm a solution acidulated with sulphuric acid

,
.

D e scri p ti on —
Col orl ess crystal s readily soluble in water an d
,
in
alcohol .
6 30 ZI N C S UL PH A T E .

moved by digestion with an excess o f z inc but lead copper and , ,

cadmium i f present are thus separated The gray fl oc c u l i which

, , .

are formed when the zinc is dissolved in the acid are mainly lead .

Pure zinc dissolves with di fficulty in the acid ; i f it contains

iron it dissolves more rapidly in proportion to the iron in it .

I ron is removed as described below in the recrystallization o f

zinc sulphate .

The solution shoul d not be too concentrated for crystall izing ,

for when the salt is cr y stall ized from a warm solution ( over
“

)
°

3 0 C the
. crystals formed contain les s water of crystallization
The cr y stals shoul d be dried without the aid o f
heat or at least at a temperature not exceeding 3 0 C
,
°
.

Impure zinc sul phate may be purified to a great extent by r e

crystall ization The salt crystallizes best from a slightly acid
.

solution .

Zinc sulphate may also be made by saturatin g sulphuric acid

with zinc oxide and crystall izing .

I f large cr y stals are des ired l et the saturated solution be evap

orated S l ow l v at the ordinary temperature and without d isturbing
it
.

Colorles s transparent cr y stals ; odorl ess ; taste

D e s cri pt i on .
—
,

metallic astringent S olubl e in

, part o f water at
. and in
part o f boiling water ; also in 3 parts of glycerin Insolubl e .

in alcohol R eaction acid . .

R e cr y s t a l l i z e d Z i nc S ul ph a t e .

White vitriol 5 parts

Water 3 parts

ake a solution A cidi fy it with 1 part o f dil uted sulphuric

M .

acid Boil it for a few minutes Filter Conduct a current o f

. . .

chlor i ne i nto the warm solution until it acquires the odor o f it .

A dd a small quantity o f iron free zinc oxide or zinc carbonate to -

produce a sl ightl y turbid mixture contain ing but little undissolved

zinc compound D igest for a d a y or two shaking oc c a 5 1 0 n a l l v
.
,
,
.

B ring it to the boiling point Filter A cidi fy again w ith diluted . .

sulphuric aci d Cr vs t al l i z e i n the usual w a y

. .

White vitriol contains iron and consists o f an opaque

N ot e s .
, ,

granular more or l ess dirt y salt mass When its solution i s

,
.
 Z INC S UL PH A T E . 63 1

strongly acidified and boiled it can be filtered quite clear Chlorine .

converts the iron present into ferric sulphate The iron is the n .

eas ily precipitated by digestion with zinc oxide or zinc carbonate

in slight excess The se paration o f the iron is facil itated by boil
.

in g A fter filtration the solution is again t o be acidified by the

.

a ddition o f about I part of diluted sulphuric acid because the salt

c r v s t a l l i z e s most satis f actorily from an acid solution .

I f copper l ead arsenic cadmium or manganese be present

, , , , ,

these metals are removed as well as iron by this method .

ZI N C S UL PH I T E .

ZI N GI S U L PH I S .

Z nS O3 . 2H O: 1 79 3 . .

Zinc sulphate
S odium sulphite
D istilled water su fficient ,
.

D issolve each salt separately in 2 0 0 parts o f cold distilled

water and filter the solutions A dd the zinc salt solution to the .

solution o f the sodium sulphite stirring wel l A precipitate o f ,

.

zinc sulphite will be formed in the course o f from twenty to

thirty m inutes .

D ecant the m other l iquor Wash the precipitate with a lim ited
-
.

amount o f cold water until the washings are nearly tasteless and
no longer contain sodium sulphate D ry the product without .

the ai d o f heat .

R e act i on . ZnS O,

N ot e s Col d solutions are used and the product washed and

.

dried at the ordinar y room temperature because zinc sulphite is

l iable to be decomposed at a higher temperatu re bas ic salt being ,

,
form ed .

s i
D e cri p t on —
A white crystalline powder
, , p rac t i c a l l v insoluble
in water .
632 Z I N C VALERA T E .

Z I N C VALE R A T E .

Z I N C VALER I AN A S .

3 .

S odium valerate
Zinc sulphate
D i stilled water su fficient , .

D issolve the salts separatel y each in 2 0 0 parts o f water ; heat

, ,

the solutions to boiling ; mix while hot ; let the m ixture cool Col .

lect the cr y stal s wash them hastil y with cold water and dry them
, ,

between fi l t e r paper -

A nother crop m ay be had by evaporating the mother l iquor to

2 0 parts cooling and separating the cr stal s formed
, , y .

R e act i on . 2 N a C5 H OO z+
Z n S O ,
: Z n C5
H g
O z) 2
—
N a2S O, .

N ot e s . A s the zinc valerate is lighter than the solution o f so

d ium sulphate the crystals rise to the sur face as they are formed
,
.

The salt may also be made by dis solving 3 parts o f zinc oxide
in a mixture o f 5 parts o f valeric acid 2 00 parts of alcohol and , ,

2 0 0 parts o f water ; but th e cr y stal lization is tedious on account

o f the necessity o f us ing but moderate heat in evaporating the

solution .

The crystals must be dried without the aid o f heat .

D e s cri pt i on —
S oft
glistening white crystal s solubl e in about
, ,

1 0 0 parts o f water and in 4 0 parts o f alcohol T aste sweetish .

astrin g ent finally metallic

, .
 TA B LE OF ATOM IC W E IGH TS .

L d
ea

o o o o o o o o o o o o o o o o o o o Li thi um

M ag ne si um 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0

0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 M a n ga n e s e 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0

M e r c u ry o o o o o o o o o o o o o o o o o o

0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 N i cke l 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0

0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 N i tr og e n 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0

0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 x
O y ge n 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0

0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 Ph os p h or u s 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0

Pl a ti n u m 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0

O O O O O O O O O O O O O O O O O O O O O O P ot a s si u m O O O O O O O O O O O O O O O O O

0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 S i l i c on 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0

0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 S i l ve r0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0

o o o o o o o o o o o o o o o o o o o o o o o o S od i u m o o o o o o o o o o o o o o o o o o o

0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 S tr on t i u m 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0

S u lp hu r 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0

0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 T in

o o o o o o o o o o o o o o o o o o o o T u n g ste n o o o o o o o o o o o o o o o o o

Z i nc
TA B LE OF T H E R M OM ETR IC EQ U IVA LE N TS .

A c c o rd i ng to th e Ce n t lg r a d e a n d F a h re n h it
e S c a l e s .
 A CE T I C A CI D .

A c c i
or d n g to O u d e m a ns .

S p ifi G vi ty
ec c ra S p ifi G vi ty
ec c ra S p ifi
ec c G ra vi t y
at 15° C . at 15 ° C . at 15° C .
 H YD R O B R O M I C A C I D .

A d i g t
c c or Bl l
n o e .

H YD R O C H LO R I C A CI D .

A c c or d i ng to G . Lu n g e a n d L . M arc h le w s k i .

G ra m s of S p i fi G vi ty
ec c ra

H 01 i n at 15°
1 L te ri .
( H 2O at
 N IT R IC A CID —
C o nt i n u e d .

at 15 °

(E QO at 4° 1

PH O S P H O R I C A C I D .

A c c or d i ng to A . B . Ly on s . *

S p cifi G vi t y
e c ra S p ifi G vi ty
ec c ra Spe c ifi G vi
c ra ty
at 15 0 P e r c e n ta g e Of
at 150 P e rc e n t a g e of
at 150 P e r ce n t a g
e of

H P0 , H PO c H 3 P0 4
(H O at 3
( H g () at s
( 11 2 0 at
. .

F r om the P h a r m a c op oe i a of t h e U n it e d S t ate s .
 S U L PH U RIC A CID .

l l
‘

A c c ord ln g t o G . L u n g e a n d M . s e r .

G ra m s
S p ifi G vi ty
ec c ra

of H S O, at 15 °
Q

i n 1 L te r i .
( 13 2 0 at
S U L PH U RIC A CI D .
—
C ont i n u e d .

at 15 °

(E QO at
 S O LU TION OF PO T A S S I U M H Y D R OX I D E .

A c c ord i ng t o G e r l ac h .

S p ifi
ec c Gr a v i ty P e rc e n t S p ifi G vi ty
ec c ra P e rc e n t S p ifi G vi t y
ec c ra P e rce n t

at 15° C . of K OH . at 15 ° C . of K OH . at 1 6° C . of KO H .

S O LU TION OF S ODIU M H Y D R O XI D E .

A c c or d i ng to Ge r l a c h .

S p ifi G vi ty
ec c ra P e rc e n t S p ifi G vi ty
ec c ra P e rce n t S p ifi G vi t
ec P c ra y e rc e n t

at 15° C . of N a OH . at 15° C . of N a OH . at 15 ° C . of N a OH .
 I N D EX
TO TH E S EC O N D VO LU M E .

A c t e t a t e , al u m i nu m 2 5 6 ,
. A cid s ,
ac ti o n on h y d ro xid s e .

am m on iu m s o l u ti o n 2 66 ,
. acti o n o n m e t al s 1 2 0 ,
.

b
,

a ri u m , 2 9 2 a c ti o n o n n itrit e s 121 ,
.

a c ti o n o n o x i d e s
.

c al c i u m 3 17 1 21 , .

a c ti o n o f su l p h i d e s
.
,

c h rom i u m 3 42 . 121 , .

a c ti o n o n s u l p h it e s
,

co pp
er 3 47 3 48
-
1 21 ,
.

fe rri c s o l u ti o n 3 6 8 c a r e i n h a n d li n g 1 9 7 200
—
.
, , ,

fe rri c ti n c t u r e 3 7 1 n ot e s o n 215
or g an i c
. .
, ,

s o l u b ility O f
,

l e a d 448 4 5 1 -
1 49 ,
.

s tr e n g t h o f 8 1 0
.

g
, ,

m a n e s i u m 4 68 .
,
—
.

s u l p h u ri c 2 9 3 0
,

p ota s s i u m 5 24 , .
,
-
.

s o d iu m 5 72 5 74
-
A e t h i o p s m i n e ra l i s 5 1 0 ,

A i r d a m a g i n g e ff e c t s O f 1 3 8 1 40
. .
,

z i n c 6 1 9 6 20 -
,
-
.

b A l b u m i n a t e ir o n 3 7 2 3 7 4
.
, ,

A c e t a t e s s o l u iliti e s 1 4 8 1 4 9
, ,
-
1 50 .
, ,
-
.

A l c o h o l a s a s o l v e n t 3 3 1 49 1 5 0
,

A c i d a c e ti c 2 1 6 2 1 8 -
.
, ,
.

ti c a s a s o l v e n t 3 2 3 3
, , ,

ace ,
. A l c o h o l l a m p s 1 49 1 5 0 1 8 7 1 88 — -
.

A l k a li s ol u ti o n s s tr e n g t h 8
, ,

ta bl e 63 9
,

a c e ti c , , .
, , .

a r s e n o u s , 2 90 . A l k ali e s d e s tr u c ti v e a c ti o n o f 200 ,
.

b e n z o i c 2 1 8 2 20
,

-
. A ll a n it e 3 3 7 .

b o ri c 2 20 222
, ,

-
. A lu m 2 5 3 25 6
,
-
.

c h l o r o p l a ti n i c
,

5 23 , . c h ro m i c 3 43 , .

c hro m ic 3 44 ,
. ir o n 44 5 4 46
,
-
.

c itri c 2 2 2 2 2 4,
—
A l u m i n a t e d c o pp e r 3 55
A l u m i n u m c o m p o u n d s 2 5 3 26 3
. .
,

h y d ri o d i c 2 2 4 .
-

A l u m i n u m c o m p o u n d s s ol u b iliti e s
,

h y d r o b r o m i c 2 2 5 22 6
.
,

-
~ .
, ,

h y d r o b r o m i c t a b l e 6 40
,

, ,
. 1 43 .

h y d r o c h l o ri c 2 2 6 2 28 -
. A m m o n i a w a t e r, 2 6 3 — 26 5 .

h y d r o c h l o ri c t a b l e 6 40
,

, ,
. t e r ta b l e 6 45
wa , ,
.

h y d r o c y a n i c 22 8 2 3 1 ,
-
.
A m m o n i a c al c o pp e r su l p h at e , 3 54 .

h y p O p h o s p h o ro u s ,
23 1 - 23 2 . A m m o n i a t e d c o pp e r , 3 53 .

l a c ti c 23 2 ,
m e r c u r y 49 2
m e t a p h o s p h o ri c 2 43
. .
,

A m m o n i u m c o m o u n d s 26 3 2 80 p -

n itr i c 2 3 3 2 3 5
,

b i
.

p
.

c om o u n d s s o l u il ti e s 1 42
i n o x i d a ti o n 1 2 4
.
, .

p b
, ,

n itri c A m o r h ou s s u s ta n c e s 7 8 1 0 1
n itri c t a b l e 6 4 1 6 42
.
, , , ,
.

, ,
-
. A n ti d o t e fo r a r s e n i c 4 1 3
p
.
,

n itr o h y d r o c h l o ri c 2 3 5 23 6 ,
-
. A n ti m o n a t e ot a s s i u m 5 25
p
, ,
.

ol e i c 23 6 A n ti m o n y c o m o u n d s 2 86 2 90 -

o x a li c 2 3 7
.
,

b
.
,

c om p o u nd s s o l u ility 1 45
p h o s p h o ri c 2 3 8 243 g
, ,

pp
.
,

,
-
. A ar a t u s fi tti n s , 7 4 .

p h o s p h ori c t a b l e 6 42 , ,
. o utfit 1 95 , .

s a li c y li c 2 43 245 ,
. s tan d s 7 6 7 7 , , .

s u l p h u ri c 2 4 5 2 48 ,
-
q
A u e o u s fu s i o n 1 8 1 9 87 1 3 3 , , , ,

s u l p h u ri c
.

a r o m at 1 e 2 48 A r c h i m e d e s l aw o f 1 5 3
g
. .
, , , ,

s u l p h u ri c t a b l e 6 43 6 44 , ,
—
. A r o l s 5 28, .

s u l p h u r o u s 2 48 2 5 0 A r s e n a t e ir o n 3 7 4
-
,
.
, ,
.

t a rt ari c 2 5 1 ,
. sodium 57 4 , .

v al e ri c 2 5 2 . s o di um s o l u ti o n 5 75 , .

b
, ,

A c i d s a c ti o n o n c ar b o n at e s 1 2 1
, ,
. A r s e n a t e s s o l u iliti e s 1 5 0
.
, .
6 48 I N DEX .

A rs e n i c c om p ou n d s, 2 90 - 2 9 2 , 3 74 , B r o m i d e s s ol u b iliti e s 1 46 1 49
, , ,
.

574, 57 5 5 26, . B ro m i n e 20 0 20 2 3 1 4 3 1 5
,
-

, ,
.

c om o u n d s , p
s o l u b1 11 t 1 e s , 1 45 , B u c h n e r fu n n e l 4 7 , .

1 50 . B u r n e r E rl e n m e y e r 1 8 5
, , .

A r s e n it e ot a s s i u m 5 26 p B u r n e r s 1 83 1 86 1 88 -

g
.
,

b
, , , .

A t om i c w e i hts , t a l e s 6 3 5 63 5 , , B u r n e r s u pp o rt s 1 89 ,
.

637 . B u oy a n c y 1 5 3 1 5 4 , ,
.

B al a n c e s , 1 8 1 1 8 2 -
. Ca d m i u m c o m p o u n d s 3 1 5 3 1 7 ,
-
.

h y d r o s t a ti c , 1 5 5 1 5 7 ,
. c om p o u n d s s o l u b iliti e s 1 43 .

p
, ,

B a ri u m c o m o u n d s 2 9 2 2 98 -
. Ca l c i n a ti o n 2 1
p b
, , .

c o m ou n d s s o l u iliti e s 1 42 , ,
. Ca l c i u m c o m p o u n d s 3 1 7 3 3 4 —

x
.
,

B a s h a m s m i tu r e 3 7 1 c o m p ou n d s s o l u b iliti e s
’
, . 1 42 , ,

B at h s 1 89 1 9 1 -
. 1 43
B e a k e rs 1 1 0
.
,

,
. Ca l o m e l , 5 1 0-5 1 4
p r i p it t d 5
.

B e ll o w s 1 84 ec a e 10-5 1 4
B e n z o a t e a m m o n i u m 268
. .
, ,

, , . Ca lx 3 7
,
2
b i s m u t h 2 99
.

,
. su lp h t 33 u ra a , 2 .

c al c i u m 3 1 8 , . Ca rbon, 334 .

fe rri c 3 7 5 , . di xid
o 5 335 e ,
12 , .

lit h i u m 4 64 , . di lph id
su 3 37 e,
rb m t
.

m e r c u ri c 4 88 . Ca a mm
a e, i a o n um , 27 2
p ota s s i u m 5 2 7
, .

, . Ca rb t
ona e , mm i a on u m , 27 2 .

s o d iu m 575 . b ri m 93
a u 2
B e n z o at e s s o l u b iliti e s 1 48
, ,
.

, , ca dm um , 315 i
B i c a r b o n a t e a m m o n i u m 2 69
, .

, ,
. l i
ca c um , 3 1 9
p ot a s s i u m 5 2 7
.

,
. bis m u hy 306 308 t l ,
-
.

s o d iu m 5 76 5 7 7 ,
-
. ir on, m as s 3 78 , .

B i s m u th 2 9 8 , . ir o n s a c c h arat e d 3 7 6
B i s m u t h c o m p o u n d s 2 99 3 1 4
, , .

,
-
. l e a d 45 1
c o m p o u n d s s o l u b iliti e s
.
,

1 45 , . lit h i u m 46 5
m a g n e s i u m 4 6 9 47 0
.

B i s ul p h i d e c arb o n 3 3 7
,

—
,

g
. .
,

B i s u l p h it e s o d i u m 5 7 8
,

,
. m an 4 82 an e s e , .

B it a rtra t e p o t a s s i u m 5 2 8 p t
,

, , . o as s um , 5 33 535 i -
.

s od iu m 5 78 i
s o d u m , 5 7 9 5 82 -

B l e a c h i n g p o w d e r 3 42
. .
,

. tr ti
s o n u m , 60 9 .

z i n c 6 2 1 622
,

B l o w e r 1 84 ,
.
,
—
.

B lu e st o n e 3 52
-
Car b o n a t e s a c ti o n o n a c i d s 1 21 .

B o ili n g p o i n t s 6 3 7 2
, .
, ,

. s o l u b iliti e s 1 47 1 50 .

B o ili n g v e s s e l s 6 6
, , , ,

,
. Car b o n i c a c i d g a s 3 3 5 , .

B o n e p h o s p h at e 3 28 , . a c i d w at e r 3 3 5 ,
.

B o rat e s o d i u m 60 6 , . Ca rl s b a d s a lt 6 0 4 6 0 5 , .

B orat e s s o l u b iliti e s 1 47
, ,

, , . Ca s s e r ol e s 5 0 , .

B o r a x 60 6 , . C e n t r i fu g a t o r , 96 .

B o r a x t a r t a r , 5 29
~
C e r it e 3 37
B o r o c itr at e m a g n e s i u m 469
. .

p
,

, ,
. Ce ri u m c o m o u n d s 3 3 7 3 3 8 ,
-

p ota s siu m 5 39
.

p
c o m o u n d s s o l u iliti e s 1 43 b
B or o gl y c e ri n 22 1
.
, .

k p p
, ,

. Ch a l r e ar e d 3 20
B o r o t a r t r a t e p ot a s s i u m 5 3 0
, , .
,

, ,
. Ch a r c o a l a n i m a l 3 3 4
p ota s s i u m s o d i u m 5 29
,
.
,

-
,
. Ch e m i c a l s o l u ti o n 3 7 , 1 1 7 1 1 8 1 2 1 -
,

B r o m at e p ot a s s i u m 5 3 0
, ,

, ,
. 1 23 , 1 24 .

B rom id e a m m on iu m 27 0 27 1 , ,
-
. Ch l o r a m i d e m e r c u ri c 493 .

b a ri u m 2 9 3
, ,

,
. Ch l o r a t e o ta s s i u m 5 3 5
,
p ”

,
.

c al c i u m 318 ,
. s odium 5 82 , .

fe rr o u s 3 7 5 , . Ch l o r a t e s s o l u ilit y 1 4 6 1 4 9
,
b , , ,
1 50 .

lit h i u m 4 6 5 ,
°
. Ch l o ri d e a l u m i n u m 2 5 7 2 5 8
, ,
-
.

m e r c u ri c 4 8 9 a m m on iu m 274 27 6 —

p ot a s s i u m 5 3 1 5 33
. .
, ,
-
. a n ti m o n y 2 80 2 8 1 -
.

b
, ,

s od ium 5 78 579 ,
-
. a ri u m 294
b
.
,

s t r o n ti u m i s m u th y l 3 1 2
z i n c 62 1
, , .

,
. cadm iu m 316 ,
.
648 I N DEX .

A rs e n i c c om p o u n d s, 2 90 - 2 9 2 , 3 74 ,
B r o m i d e s s o l u b iliti e s 1 4 6 1 49
, , ,
.

5 74, 5 7 5 5 26, . B r o m i n e 20 0 2 0 2 3 1 4 3 1 5
,
—
, ,
.

c om ou n d s , p
s o l u b1 11 t i e s , 1 45 , B u c h n e r fu n n e l 4 7 , .

1 50 . B u r n e r E rl e n m e y e r 1 8 5
, , .

A r s e n it e ot a s s i u m 5 26 p . B u rn e r s 1 83 1 86 1 88 -

g
,

b
.
, , ,

A t o m i c w e i ht s t a l e s 6 3 5 6 3 5 , , , B u rn e r s u pp o rt s 1 89 ,
.

63 7 . B u oy a n c y 1 5 3 1 5 4 , , .

B al a n c e s , 1 8 1 1 82 -
. Ca d m i u m c o m p o u n d s 3 1 5 3 1 7 ,
-
.

h y d r o s t a ti c , 1 5 5 1 5 7 ,
. c om p ou n d s s o l u b iliti e s 1 43 ,
.

p
,

B a ri u m c o m o u n d s 2 9 2 2 98 -
. Ca l c i n ati o n 2 1
p b
, .

Ca l c i u m c o m p o u n d s 3 1 7 3 3 4
,

c o m o u n d s , s o l u iliti e s 1 42 ,
.
,
-
.

B a s h a m s m i tur e 3 7 1
’
x , . c o m p ou n d s s o l u b iliti e s 1 42 , ,

B a t h s 1 89 1 9 1 —
. 1 43 .

B e a k e rs 1 1 0
,

,
. Ca l o m e l , 5 1 0- 5 1 4
p r i p it t d 5
.

B e ll o w s 1 84 ,
. ec a e ,
1 0- 5 1 4 .

B e n z o a t e a m m o n i u m 2 68
, ,
. Ca lx 3 7
,
2
b i s m u t h 2 99
.

,
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c alc ium 3 1 8 , . Ca rb on , 3 34 .

fe rri c 3 7 5 , . di xid
o 5 335 e, 12 , .

lith i u m 4 6 4 ,
. d i lph id
su 337 e .

rb m t
,

m e r c u ri c 4 88 . Ca a mm
a e, i a o n um , 27 °

p ot a s s i u m 5 27 rb t
,

,
. Ca ona e , mm i a on um, 27 2 .

s od iu m 575 . b ri m 9 3
a u 2
B e n z o at e s s o l u b iliti e s
, , .

1 50 ,
. cadm um , i 315
B i c ar b o n at e a m m o n i u m 2 69
, .

,
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ca c um , 319
p ot a s s i u m 5 2 7
,

bi
.

,
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-
30 8 .

s odium 5 7 6 57 7 ,
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B i s m u th 2 98 . ir o n s a c c h ar at e d 3 7 6
B i s m u t h c o m p o u n d s 2 99 3 1 4
, , , .

,
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c o m p o u n d s s o l u b iliti e s 1 45 , . lith i u m 4 6 5
m a g n e s i u m 4 6 9 47 0
.

B i sul p hi d e c a rb on 3 3 7
,

g
.
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,

B i s u l p h it e s o d i u m 5 7 8 ,
. m an ane s e , 4 82 .

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,

, , . o as s um , i 53 3 535
-
.

s od iu m 5 78 s od u m , i 5 7 9 5 82
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,

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z
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B l o w e r 1 84 i n c , 62 1 6 22 -
.

rb t
.
,

B lu e ston e 3 52
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Ca ona e s , ti id ac on o n a c s, 1 21 .

B o ili n g p o i n t s 6 3 7 2 l b iliti
.
,

. so u 47 5 e s, 1 1 0 .

B o ili n g v e s s e l s 6 6
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,
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.

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Ca r s a s a 0 0 , ,
.

B o rat e s s ol u b iliti e s 1 47
,

, , . Ca s s e r o l e s 5 0 ,
.

B o ra x 6 0 6 , . Ce n t r i fu g a t o r , 96 .

B o r a x t a rt a r 5 29
-
Ce r it e 3 37
B o r o c itra t e m a g n e s i u m 4 69
. .
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, , . Ce ri u m c o m o u n d s 3 3 7 3 3 8 p ,
-
.

p ot a s s i u m 5 39 p
c o m o u n d s s o l u iliti e s 1 43 b
B or o gl y c e ri n 2 2 1
. .
,

k p p
, ,

. Ch a l re a r e d 3 20
B o r o t a r t r a t e p ot a s s i u m 5 3 0
.
, , ,

, ,
. Ch a r c o a l a n i m a l 3 3 4
p ot a s s iu m s o d i u m 5 29
.
, ,

-
,
. Ch e m i c a l s o l u ti o n 3 7 1 1 7 1 1 8 1 2 1 -
, ,

B r o m at e p ot a s s i u m 5 3 0
, ,

, ,
. 1 23 , 1 24 .

B ro m i d e a m m o n i u m 2 7 0 27 1
, ,
-
. Ch l o r a m i d e m e r c u ri c 493 , , .

b ari u m 293 ,
. Ch l o r a t e , o t a s s i u m 5 3 5 p “

,
.

c al c i u m 318 ,
. s odium 5 82 ,
.

fe rr o u s 3 7 5 , . Ch l o r a t e s s o l u ilit y 1 4 6 1 4 9
,
b , , ,
1 50 .

lit h i u m 4 6 5 ,
0 . Ch l ori d e a l u m i n u m 2 5 7 2 5 8
, ,
-
.

m e r c u r i c 4 89 . am m onium 27 4 2 7 6 -

p ot a s s i u m 5 3 1 5 3 3
,
.
,

,
-
. a n ti m o n y 2 80 2 8 1 —
.

b
,

s odiu m 5 78 579 ,
-
. a ri u m 294 ,

b
.

s tr o n ti u m ,
i s m ut hy l 3 1 2 .

z i n c 62 1
,
'

,
. c ad m iu m , 3 1 6 .
 I N DE X . 6 49

Ch l ori d e ,
ca c um,l i 3 20 . b
Cru c i l e s 1 7 1 8 , , .

co pp r e , 3 49 . Cry s t a l m e a l 7 8 , .

fe rri c , 3 7 9 3 82
-
. w a t e r , 1 8 20 8 5 8 7 -
,
-
.

fe rri c , s ol u ti o n , 3 82 3 8 7 -
. Cry s t a lli a ti o n 7 8 9 7z ,
3
.

fe rri c , ti n c t u r e , 3 8 7 3 90 -
. Cry s t a lli e r s 9 2 9 6 z
g p
.
, ,

fe rr o u s , 3 90 Cry s t all o r a h y 8 1 8 4 ,
-
.

g
.

ol d , 3 5 6 Cry s t a ll o i d s 98 .

b
.
,

g ol d a n d s o d i u m , 3 5 7 3 5 8 -
. Cu e s 8 1 8 5 , , .

lit h i u m , 46 5 Cy a n a t e ot a s s i u m
, 5 40p , .

g
.

m a n e s i u m , 47 1 47 2 -
. Cy a n i d e m e r c u ry 4 9 3 496
, ,
-
.

g
m a n a n e s e , 4 84 . p
ot a s s i u m 54 1 ,
.

m e r c u ri c , 48 9 49 1 -
. sil v r 5 6 7
e .

zi 6 4
,

m e r c u ro u s , 5 1 0 5 1 4 -
. nc , 2 .

o f li m e , 3 42 . Cy a n i d e s ,
so u l b iliti e s ,
1 46 , 1 49 .

p ota s s iu m , 5 37 . D e can a t ti o n , 48 5 0
-
,
1 09 , 1 1 1 .

v
s il e r , 5 66 ja r ,
1 09 .

p
.

s o d i u m , 5 83 5 84 -
. D e c r e it a ti o n , 8 5 .

s tr o n ti u m , 6 10 . D e h y d r a ti o n , 1 8 1 9 .

q
,

ti n 6 1 9 . D e li u e s c e n c e 2 9 96 1 3 0 1 3 4 1 40 , , , , , .

z q
,

i n c , 6 22 D e n s iti e s o f s o li d s a n d li u i d s , 1 5 1
b
.

Ch l o ri d e s , s o l u ilit y , 1 4 5 , 1 46 , 1 49 , 1 66 .

1 50 . D e r m a t o l 3 08 ,
.

Ch l ori n e , 1 2 5 , 3 3 8 3 4 1 -
. D e s i c c a ti o n 1 8 1 9 96 , , ,
.

w a t e r , 3 39 3 40 —
. D e s i c c a t o r s , 96 .

Ch l ori n a t e d li m e 3 42 , . D i a c h y l o n l a s t e r, 4 5 9 p
p
.

C h l o r o l a ti n i c a c i d , 5 2 3 . D i a l y s e d ir o n 99 4 0 3
b
.
, ,

Ch r o m a t e , a ri u m , 2 96 . D i al y s e r, 98 .

l e ad , 452 . D i a l y s i s 98 99 ,
—

p p
.

ot a s s i u m , 5 44 . D i c h r o m ate o ta s s i u m 5 42
x b
.
,

Ch r o m e a l u m 3 43 D io id e a ri u m 2 9 6
g
. .
, , .

Ch r o m i c a c i d , 3 44, 3 46 h y d ro e n 3 5 9 3 6 3
“
—
.
, .

a n h y d ri d e , 3 4 4 . D i s s o c i a ti o n O f s a lt s i n s o l u ti o n s
p
,

Ch r o m i u m c o m o u n d s 3 42 3 46 ,
-
. 28 3 2 -

p b
.

c o m o u n d s , s o l u iliti e s , 1 44 . D i s till ati o n 7 0 7 7 -

.

p
,

Cir c u l a t o ry d i s l a c e m e n t , 3 7 . p
D i s u l h i d e c ar o n 3 3 7 b .

v
, ,

Citr a t e a m m o n i u m , 2 68 D o n o a n s s o l uti o n 2 9 1
’
.
,

b
.

v
,

i s m u t h , 3 00 . D ru m s i e e 1 4
x
.
,

fe rri c , 3 9 1 3 9 3 -
. D ry o i d a ti o n 2 1 .

p
,

fe rri c s o l u ti o n , 3 93 39 6 -
. D ry r o c e s s e s 4
q g
.
,

fe rri c , w it h uinin e 3 96 400 ,

-
. D ry i n c l o s e t s , 1 9 1 7 9 , .

fe rri c w it h s try c h n i n e , 400

, . E ffi o re s c e n c e 1 9 8 7 96 , 1 3 0
x
.
, , ,

lith i u m 4 66 E li ir s 1 2 9
g
.
, , .

m a n e s i u m , 4 7 2 47 5 -
. E l u tri a ti o n 1 3
p
.
,

ota s s iu m , 5 3 8 . p
E s o m s alt 4 80 ,

k
.

s o d i u m s o l u ti o n , 5 8 4 E rl e n m e y e r fl a s s 1 1 0
b
.
, ,
.

Citr a t e s , s o l u iliti e s 1 48 , 1 5 0 , E t h y l a t e s o d i u m 5 86
O
.
, ,
.

Citri n e i nt m e n t 499 , . E thy l s ul p h a t e s o d i u m 585

q
.

v p
, ,

Cl a ri fi c a ti o n o f li u i d s 4 7 6 2 -
. E a o ra ti o n 6 3 69 -

b p b
, , .

Co a lt c o m o u n d s s o l u ilit y , 1 4 3 , . d i s h e s 67
b
.
,

CO e fii c i e n t s o f s ol u ilit y 44
-
,
. x
E s i c c a ti o n 1 9 2 0 , , .

C o ll o i d s 98 F a c t or s o f r e a c ti o n s r o orti o n s p p
b
, , ,

C o m u s ti o n o f m e t al s 2 1 , . 1 0 2- 1 04
p rrat e d al b u m i n 3 7 2 3 7 4
.

Co m o u n d s , t r u e c h e m i c a l , 2 9 . F e ,
-
.

Co n d e n s e r s , 7 3 7 6 -
a m m o n i u m c h l o ri d e 3 82
g
.
, .

Co n d e n s i n w a t e r 7 1 7 2 -
,
-
. F e rri c a c e t at e s ol u ti o n 3 68 3 7 0 -

pp p
, .

Co e r c o m ou n d s 3 47 3 5 4 a c e tate ti n c t u r e 3 7 1
-
, .

p b
.
, ,

c o m ou nd s s o l u ilit y , 1 44 , . a m m o n i u m c itr a t e 392

kb
.
,

Co r ore r , 7 5 . a m m o n i u m t a rtr a t e 40 6
v b a m m o n i u m s u l p h at e
, .

C o rr o s i e s u li m a t e 489 49 1 ,
-
.
4 4 5 44 6
-

b e n z o at e 3 7 5
.
,

Cr e a m O f t a rt a r , 5 28 .
, .
6 50 I N DE X .

F e rri c c h l ori d e , 3 7 9 3 8 2 —
. F las sk g ra d u a t e d 1 5 9 , 1 6 1
, .

b
,

c h l o ri d e s o l u ti o n 3 8 2 3 87, ,
-
. F l e tc h e r u rn e r s 1 83 ,
.

c h l o r i d e , ti n c t u r e 3 8 7 390 ,
-
. F l o r e s m a rti s 3 82 , .

c h l o ri d e , ti n ct u r e e t h e r e a l F o w l e r s s o l u ti o n 5 2 6
’

3 90 .

z g
, .

x
,

c itrat e 39 1
-
393 . F re e i n m i t ure s 3 0 3 1 ,
-
.

b
,

c itr a t e l ti o n 3 9 3 396
so u -
. F u m e c h am e r, 1 80 .

w it h q u i n i n e 3 9 6 4 0 0
, ,

c itr at e ,
—
. F u n n e l , B u c h n e r 47 , .

w it h q u i n i n e s o l u ti o n pp
,

c itr a t e , cro e d 48

g
, , , .

400 . c o rr u a t e d , 5 8 .

c itr at e w ith s try c h n i n e 40 1

, ,
. fi lt e r 5 8 , .

fe rr o c y a n i d e 409 ,
. h o t w a t e r 60 ,
.

h y dro x i d e 4 1 0 4 1 3 -
p e r fo r a t e d 58
h y d r o x i d e w it h ma g n e s i a 4 1 3
. .
, ,

,
. F u r n a c e R o e s s l e r 1 87
h y p o p h o s p h it e 4 1 4 b
.
, , ,

, . F u r n it u r e , l a o r a t o ry , 1 7 9 1 80 -
.

m al a t e 4 0 8 ,
. F u s ion , 1 6 .

n itr a t e s o l u ti o n 4 0 1 40 2
-
. q
a ue ous 18 19 87 1 3 3 , , ,
.

pp
, ,

o l e a t e 4 22 . Ga s a a ra t u s 1 2 5 1 2 6 1 2 7 , , , .

oxi d e b
,

42 3 G a s u r n e r s 1 8 3 1 86 1 88 —

p
.
,
.
,

ox i d e
,

s a c c h ara t e d 43 3 G a s o e ra ti o n s 1 1 7 1 2 5 ,
.

v
.

o x y c h l o ri d e s o l u ti o n 4 0 2
, , ,

G a s s t o e s 1 83 1 84 -

b
. .
,

p h o s p h ate p r e c i pit a te d 4 28
,

. q
G l a s s li ui d o r s ol u l e 60 3
p h o s p h a t e s ol u b l e 429 43 0
.
, , ,

b
,

, ,
—
. Gl a u e r s s alt 60 3 ’

, .

p ota s s iu m ta rtra t e 40 7 , . Gl y c e ri n a s a s o l v e nt 3 3 ,
.

pe p h o s p h at e p r e c i p itat e d , Gl y c e ri n b at h 1 9 1
G ly c e rit e b o r o g l y c e ri n 2 22
, , .

43 1
s l bl
,

p r p p t
.
,

y o h os h a e , o u e, 43 1 fe rr o u s i o d i d e 4 1 9 .

l e a d S u b a c e t a t e 463
,

43 3 .

b lp
.
,

su su h a e , 44 1 t . l e a d t a n n at e 4 5 9
b lp
, .

su su h a e s o u o n , 442 t l ti . G ol d 3 5 5
, .

sulp t
ha e , a s c , 44 1 b i . G ol d c h l ori d e 3 5 6 .

lp t
,

su h a e s o u o n , 443 44 5 l ti -
. c h l o ri d e w it h s o d i u m c h l o ri d e , ,

t t
anna e , 447 .
3 5 7 3 58
-
.

v lrt
a e a e, 447 . G ol d c om p ou nds, s o l u b1 l i t y , 1 45 .

F e rri c y a n i d e ota s s iu m 5 44 p . G o u l a r d s e tr a c t 46 1
’
x
b
.
, , ,

F e rri c y a n i d e s s ol u iliti e s 1 46 , ,
. G r a d u a t e d c y li n d e r s 1 6 5
k
.
,

F e rr o c y a n i d e ir o n 40 9 . fl as s 1 5 9 1 6 1
p
, , , , .

o ta s s i u m 5 4 5 5 46 ,
-
. G ra d u a t e s 1 8 2 1 8 3 ,

b
.
,

F e rr o c y a n i d e s s o l u iliti e s 1 4 6 Gra d u a ti o n o f m e t al s 1 5
x
.
, , ,
.

F e rr o s o fe rri c o i d e 4 24 4 2 5
- -
G ra n u l ati o n o f s a lt s 9 0
p p
, .

H a ll e r s a c i d d r o p s 2 4 7
.
,

h o s h a t e , 4 2 5 42 6
’
-

p
.

H e a t i n e v a p o r a ti o n 6 8
.
,

F e rr o u s a m m o n i u m s u l h a t e , 4 4 1
H e a t d a m a g i n g e ff e c t s o f 1 3 7
. .
,

a rs e n a t e 374 ,
.
,
-
1 38
b
.
,

r om i d e 3 7 5 . H e a t i n s o l u ti o n 3 8 40 -

b
.
, ,

c ar o n at e m as s 3 78 , , . H e at s t e a m 1 9 1 1 92 -

H e a t m g a pp a ra t u s 1 8 2 1 9 4
.
,

c h l o ri d e 390 ,
.
-

H o m oe o m o r p h o u s s u b s t a n c e s
.
,

i od i de , 4 1 5 79
g
. .
,

i o d i d e l y c e rit e 4 1 9 ,
. H o o d 1 80 ,
.

i o d i d e s a c c h a r at e d 4 1 5 . H ot a i r c h a m br e s, 191
p
, .

i o d i d e s y ru 4 1 6 4 1 9 -
. H o t w a t e r c o il 19 1
g
, , .

l a c t at e , 4 9 422
1 -
. H y dro e n , 3 5 9
l p h at e pp t
.

m on o m e ta - —
su 440 . a 5 a ra u s , 12
x lt 4
,

di xi d
.

o a a e, 22 . o l ti 3 59 363 e so u on , -

ph ph t 4 5 p r x i d l ti 3 5 9 3 63
.

os a e 2 . e o e so u o n, -

p h ph t y r p 4
,

l ph id 363
.

os a e s u ,
27 . su e,
l p h i d pp r t
.

l p h t 43 7 4 3 9
su a e -
. su 5 e a a a us, 12
l p h t d ri d 44
,
.

su a e, e 0 . H ydr m t o 6 66 e e rs , 1 1 -
1
H y d xid
.
,

l p h i d 447
su e, ro l m i m 5 8 60 e a u nu 2 -
2
b ri m 9 8
. , , .

F ilt ti
ra on,5 6 2- 2 a u 2
gr b i m th 3
. , .

Fi re d an e s , 20 2 . s u ,
02 .

Fl m
a f b r
es o 86 u ne rs, 1 . ca c um , l i 321 .
6 52 I NDEX .

Liq r uo s od ae c h l o ra t a e , 5 89 . N itr a t e tro n ti u m 6 1 2

,
s , .

s od i i 57 5 a rs e nat i s , . N itr a t e s s o l u b ilit y

,
1 49 1 50 , , .

s o d i i c i t ra t i s , 5 84 . N itrit e s odium
, 592 ,
.

s o d i i s i l i c a t i s 60 3 , . N itrit e s a c ti o n o f o n a c i d s
, 1 21 .

s o l u b ilit y
,

z i n c i c h l o r i d i 6 2 3 6 24 1 47
—
.
,

g
,

L
.

ith a r e , 4 5 7 . N itr o p r u s s i d e s o d i u m 5 9 2
L
,

p
.
,

ith i u m c o m o u n d s 46 4 4 6 7 -
. O l e a t e a l u m i n u m 2 60 2 6 1 -

p b
, , .

b i s m uth 3 04
,

c om ou n d s s o l u iliti e s
4 , ,
1 2 .
.

L it m p p r
,

us a e 1 22 . c o pp e r 3 50 ,

Liv r f lph r 55 5 5
.
,

e o su u ,
0, 1 . fe rri c 42 2 , .

L i x i v i ti 5
a on , 2 . l e ad 4 5 6
L r
, .

una ti 5 69c au s c, . m e r c u ry 5 00
Ly i m t r D R i
, .

s e e 4 44 r . c e s,
’
2- . p o ta s s i u m 5 5 8
M gm
, , .

a as , 1 12 s il v e r 57 1
M g
.

i m mp z i n c 62 5 627
.
,

a ne s u d 4 6 8 48 co oun s, 2
- —
.

mp l b iliti
, .

co d 43
oun s, so u e s, 1 . O l e a t e s s o l u b iliti e s 1 48
, , .

M l t
a a e, ir 4 8 on , 0 O s t w a l d o n s o l u ti o n s 3 1
g mp
.

O v e n s c o pp e r 1 9 1 1 9 2
.
,

M an an e s e d 4 8 48 6 co ou n s, 2- .
,
—

mp l b ilit y 44
,

O x al at e a m m o n i u m 2 7 8
.

co d ou n s, so u ,
1 .
,

p pt t w it h ir 40 5
.
,

e on a e o n, . c e ri u m 337 , .

M as s 1 5 3,
. fe rr o u s 4 22 , .

M a s s i c ot 4 5 7 , . p o ta s s i u m 5 5 9 , .

M a t e ri a l s , 4 5 7 8 1 0 1 O x a l at e s s o l u b iliti e s
g
.
, , , , , ,

M e a s u re s ra d u a t e d 1 6 5 1 82 1 8 3
, , , ,
. O x i d a ti o n a n d re d u c ti o n 7 2 1 1 1 7 , , , ,

M e n d e l é e ff o n s ol u ti o n s 2 8 3 0 ,
—
. 1 24 .

M e r c u ri u s s ol u bi l i s H a h n e m a n n i , O xid ti m y
e, an on ,
2 8 2 - 28 4 .

515 . r 9
a s e n ou s , 2 2
b ri m 98
.

M e r c u ry 4 8 7 , . a u 2
p b i m th 3 4
, .

M e r c u ry c o m o u n d s 4 8 7 5 2 1 ,
-
. s u ,
0
p b
.

c o m ou n d s s o l u ilit y 1 44 , ,
. l i
ca c u m , 3 27 .

M e t al s a c ti o n o f o n a c i d s 1 1 9 , ,
. c e ri u m 338 .

c o pp e r
, ,

M e t at h e s i s 7 1 0 1 , , .
35 1 , .

M i c r o c o s m i c s a lt 600 . fe rri c 4 23
b
.
, ,

M i c r o c r y s t a lli n e s u s t a n c e s 7 8
-
,
. fe rri c s a c c h a rat e d , 43 3 .

M ill s 1 0, . fe rr o s o fe rri c 4 24 -
, .

M i ni u m , 4 5 7 l e a d 45 7
g m a g n e s i u m 4 7 7 47 9
.
,

x p
.

M i tu r e s e r c e nt a e 1 67 1 7 8 ,
-
.
-

b
,

g
, .

M o l e c u l a r c o m i n a ti o n s 29 3 0 , ,
. m a n a n e s e 4 83
p
.
,

M ons e l s owde r
’

44 1 ,
. m e r c u ry , l a c 5 20 b k , .

l ti o n 44 2
so u ,
. m e r c u ry , r e d 5 0 1 , .

M o rt a r s ir o n 1 0 1 1 ,
—
. m e r c u ry , y e ll o w 5 0 3 5 0 5 -

p or c e l ai n 1 2 1 3 3 7
, ,

v
.

, , , . s il e r 57 1 ,
.

M ot h e r li q u o r 9 3 1 1 0 1 1 1
-
, , , . s tr o n ti u m , 6 1 3 .

N e u tr a li z a ti o n 5 1 1 8 1 2 2 , . z i n c 6 28 ,

N i c k e l c o m p o u n d s s o l u b ility
.
, ,

,
1 43 . O x b
i d e s s ol u iliti e s 1 45
x z g g
, , , .

N itr a t e a m m o n i u m 2 77 . O i d i i n a e n t s 1 24 1 2 5 -

b ari u m 29 7
, , .

x
,

. O y c h l o ri d e , a n ti m o n y 28 4
b i s m u th 3 0 3 b
, ,
.

. i s m uth 3 1 2
b i s m uth yl 3 0 8 3 1 2
, , .

,
-
. fe rri c s o l u ti o n 4 0 2
O xy g
,

p r p r ti
.
,

c adm ium 317 , . e n, e a a on , 1 25 ,

c e ri u m 337 . O y i d id
x -
b i m th
o e s u 313
c o pp e r
, ,

P r ffi b t h 9
.
,

3 49 ,
. a a n a ,
1 1 .

l e a d 45 5 ,
. P e a rl a sh , 533 .

ir o n s ol u ti o n 40 1
, , . Pe p t o n a t e d ir o n 40 4 4 0 5 , , .

m e r c u ri c 49 8 ,
0
. m e r c u ry 5 0 5
g
.

x
,

m e rc u ro u s 5 1 9 P e r c e nt a e s o l u ti o n s a n d m i t u r e s
m e r c u ry O i n t m e n t 499
.
, .

, . 1 68 1 7 8 -

p o ta s s i u m 5 5 6 5 5 8 g
.

-
. P e r m a n a n at e ot a s s i u m 5 6 8 p
s il v e r 5 68 5 7 0 g
,

x
, , .

,
-
. P e r o i d e h y d r o e n, 3 5 9 3 63
,
-
.

s od iu m 5 9 1 5 92 ,
-
. le ad , 45 8 .
 I NDEX .
53

P h e n o l s ul p h o n at e s o d i u m 5 9 5 , ,
. R e t o rt s ,
g
la s s, 73 74 ,
.

z i n c 6 28 , . R h o d a n k a l i u m , 5 6 2 , 5 63 .

P h o s p h at e a m m o n i u m 2 7 9 ,
. R i c e s l y s i m e t e r 4 2 44
’

,
-
.

b
,
“
c al c i u m 3 28 3 3 0
-
R i d e rs o n al an c e s 1 5 6 , 1 5 7 .

g
.
,

p
,

fe rri c 42 8 4 3 0 ,
-
. R o a s ti n o f s u l h i d e s , 2 1 .

fe rr o s o fe rri c 4 2 5 42 6 -
,
-
. R o c h e ll e s a lt , 5 6 1 5 6 2 -
.

fe rr o u s s y r u p 42 7 ,
. R o e s s l e r fu r n a c e , 1 8 7 .

bb pp p
,

lit h i u m 46 7 Ru e r sto e rs , e r fo r a t e d 7 5
g g
.
.
,

g
,

m an an e se , 48 5 R u l e s fo r a d ju s ti n and fi ndin
g
.

p t
o ass um , i 56 1 . str e n t h o f s ol u ti o n s a n d
i
s od um , 5 9 5 5 99 . m i t u re s 1 6 7 1 7 8 x ,
-
.

s o d iu m a m m on i u m , S ac c h ara t e d ir o n , s o l u l e , 43 3 b .

P h o s p h a t e s s ol u b iliti e s 1 47 1 5 0, , ,
. S a fe ty t u e s , 7 5 b .

P h o s p h o r at e d o i l 5 22 , . S a l s o d a e 5 7 9 5 80 ,
-
.

P h o s p h or u s 20 2 5 22 , , . S a li c y l a t e i s m uth 3 0 5
, b , .

P h y s i c al p r e c i p it ati o n 3 6 9 7 1 00 , , ,
. lit h i u m 4 6 7 ,
.

P i p e tt e s 5 0 . m e r c u ry , 5 0 6 .

p
,

Pl as t e r l e a d 4 5 9
, , . ot a s s i u m 56 1 , .

P l ati n u m c h l o ri d e 5 23 . s o d iu m 60 1 ,

z
.
,

c o n e fo r fi lt e r s 5 8 , . i n c 6 29 ,
.

P o ta s h 5 3 3
, . S a li c y l a t e s , s o l u iliti e s 1 48 , 1 49 b ,
.

P o t a s s a 5 46
, . S alt c o m m o n 5 8 3 5 84
, ,
-

s u l p h u rat e d 5 5 0 5 5 1 b
.

-
. Ca rl s a d 60 4
g
.
, ,

w it h li m e 5 4 9 ,
. K i s s i n e n 5 84 ,
.

P o t a s s i u m c o m p o u n d s 5 24 5 6 4 ,
-
. m i c r o c o s m i c , 6 00
c o m p o u n d s s o l u b iliti e s
.

1 41 , ,
. V i c hy 5 7 7 ,

P oti o R i v e ri 5 8 5 S a lt s o l u ti o n s c h e m i c a l n a tu r e o f
P o w d e ri n g 1 0 1 4 1 1 5
.
, , ,

,
-
. 28 3 2 -

P r e c i p it a ti o n 1 00 1 1 6
.
,

-
. s ol u ti o n s c o l o r s o f, 3 1 - 3 2
p h y s i c al
, , .

1 00 , . S a lt s o f t art a r 5 3 3
P r e p a r e d c h al k
,

b
.

S a n d a t h s 1 89 1 9 0
-

P r e s e r v a ti o n o f c h e m i c a l p r od u c t s
, , ,
.

, S a n t o n i n a t e s o d i u m 60 2 , 60 3 ,

p
, .

33 1 -
1 40 . S a o d u r u s 5 9 3 5 94 ,
-
.

Pr e s se s, 54 56 -
. m o lli s 5 5 8 , .

P ri s m s , 8 2 , 8 3 , 85 . S at u ra ti o n 1 1 8 1 2 3 , , .

Pr o c e s s e s , d ry a n d w e t , 3 - 5 . S c a l e salt s 1 28 , 1 5 0 , .

Pr oduc s t 3 8
-
S c h li p p e s s a lt 2 8 6
’

g
.
, ,

v
.

d am a e d h ow e a e d , 1 28 , tr t . S ie e s, 1 4
p r rv ti
.

e se a o n o f, 1 3 3 - 1 40 . S ili c a t e s o d i u m s ol u ti o n 6 0 3 ,

v p
.
,

fi i h d
un n s e ,
u se s O f, 1 28 . S il e r c o m o u n d s 5 6 5 5 7 2 -

bl b
.
,

Pr iu s s an ue , 4 09 .
p
c o m o u n d s s o l u iliti e s 1 4 5
p t p
, ,
.

P r u s s i at e of o ash , ye ll ow , 5 45 S o a s 5 5 8 5 9 3 5 94
, ,
-
.

54 S o d a 5 86
p t
, .

of o ash , re d , 5 44 . S o d a wate r 3 3 6 ,

p
.

P u ri fi c ati o n of c h e m c a s , i l 1 1 6, 1 28 , S o d i u m c o m o u n d s 5 7 2 60 9 ,
-

p b
.

1 30 . c o m o u n d s , s o l u iliti e s 1 42
b p
.
,

Py c n o m e t e rs ,
1 5 8, S o l u iliti e s o f c h e m i c a l r o d u c t s ,

Pe p h o s p h a t e , fe rri c , 4 3 1 4 3 3 1 4 1 - 1 50
-
.
.

s od ium 600 . O f ch e m i cal r o d u c t s s u m m ary p

p h o s p li a t e s ,
,

b
, ,

Pe s o l u iliti e s , 1 47 , 14
I 50 - b
S ol u ilit y , 3 3 3 5 4 1 4 5 -
,
-
.

P y ra m i d a l c r y s t a l s 8 5 , . S ol u ti o n 2 4 4 -

R e a c ti o n o n t e s t p a p e r 1 2 2
,

, . ch e m ical 1 17 1 21
R e a c ti o n s c h e m i c al k i n d s 7
.
, ,

, , . c h e m i c a ll y c o n s i d e r e d 3 32
0 -

p ro g n o s i s o f 7
,

Lr
.
,
’

, . e as 43 3
R e c e i v e rs 7 3
, .

, . S o l uti o n a t h s 1 9 1
-
b , .

R e d l e a d 45 7 , . S o l u ti o n s M e n d e l é e ff
, on, 28 .

R e d u c e d ir o n 3 66 3 68 ,
-
. O s t w al d o n 3 1
g
.
,

R e t o rt ir o n 1 8 4
, ,
. s tr e n t h o f 4 5 4 6 ,
-
1 67 - 1 78
v
, .

stan d s 7 6 7 7 , , . S o l e nt s , 28 .
6 54 I N DE X .

S p t l
a u as, t l s ee 1 2, 13 p
S u l h it e m g i m 48 a ne s u 2
p i fi gr v ity
. .
, , ,

S ec c a 5 1 53 1 1 -
p t i m 5 63
o ass u
gr v ity i t
.
, ,
.

a ns r u m e nt s , 1 55
-
1 56 . di m 6 5
so u , 0 .

v l m 66 z i 63
,

o u e ,
1 . nc, 1 .

S p irit l m p 87
a s, 1 —
1 88 . S l p h it
u ti
e s, f a id
ac on o ,
on c s, 121 .

S p irit f m m ni
o a o a, 26 5 . l b iliti
so u 47 e s, 1 .

of a m m o n a , a o m a i r ti c , 26 6 . S lph
u b l t
oc ar d i m 5 95 o a e , so u , .

of i M n d e re r u s , 266 — 267 . zi 6 8 nc , 2
S lph y t p t i m 56
.

S p rit z b o ttl e s 1 1 3 . u oc an a e , o ass u 2

S lp h vi t
, ,

S t e a m h e a t 1 9 1 1 92 —
u o d i m 5 85
na e , so u .

S l p h r t d li m
, .
,

S tirr e r s 6 8 ,
u u a e 33 e, 2 .

S t o v e s g a st 1 8 3 1 84 li m l ti
‘

e, 334 so u on , .

p t
.
, ,

S t r ai n e r s 5 1 5 4 1 1 2 -
55
o a s s a,55 0, 1 .

S lph r 6 3 6 6
.

S tr o n ti u m c o m p o u n d s 6 0 9 6 1 3
, ,
-
. u u ,
1 -
1
di x id
.
,

c om p ou n d s s o l u b iliti e s 1 42 . o 6 6 6 7 e, 1 1 .

S u b a c e ta t e l e a d g l y c e r it e 4 6 3
, , ,

. i od i d e,
p r i p it t d 6 4 6 6
, , ,

l e a d s o l u ti o n 4 6 1 ,
. ec a e ,
1 -
1 .

S u b c a r b o n a t e b i s m u th 3 0 6 3 0 8
,

,
—
. w h d 6 3as e 1
S y ph
, ,

c o pp e r 35 1 . 0 on s,5 5 0- 2 .

S y r p f rr br m id 3 7 5
,

ir o n 43 5 u ,
e ou s o e, .

S u b g a ll a t e b i s m u t h 3 0 8
.
,

f rr e i di d 4 5 4 8
ous o e 1 —
1
p h ph t 4 7
.
, .

S u b li m a ti o n 2 1 2 3
, ,

,
-
f rr e ou s os a e ,
2 .

S u b n itr a t e b i s m u t h 3 0 8 3 1 2
.

-
. h y d ri d i a i d o 4 c c 22
h y p p h p h it
.
, , ,

S u b s u l p h a t e fe r r i c 44 1 , ,
. o 3 5 os es, 2 .

fe rri c s o l u ti o n 4 42 hy p p h p h it w it h ir
'

O 3 5
os e s, on, 2
ir n q i i
. .
, ,

m e r c u ry 5 0 8 o , d ty h i
u n ne an s r c n ne
p h p h t 43
.
,

S u g a r o f l e a d 4 48 4 5 1 -
. os a e s, 0 .

S u l p h at e a m m o n i u m 27 9
,

, , . ir o n , s ac c h a a e r t d 4 35 ,
.

al u m i n u m 2 6 1 262 -
li m e , 3 23 .

g
.
,

cad m ium 317 m a n a n e s e i o d i d e 48 4 , .

p p
.
,

c al ci u m 33 1 ,
. h o s h a t e s of i r o n q u 1 n 1 ne ,

c e ri u m 3 3 8 a n d s tr y c h n i n e , 43 0
t b
. .
,

c h r o m i u m 3 46 T u e s, 74
-

C o pp e r bl
.
,

3 5 1 3 53 ,
-
Ta e of a ce id 63 9 ti c ac ,
.

c o pp e r a m m o n i a c a l
.

354 a m m o n i a w a t e r 6 45
a t o m i c w e i gh t s 6 3 5
. .
, , ,

c o pp er a n d p o t a s s i u m 3 5 4
at o m i c w e i g h t s
.
, ,

m u lti p l e s
.

fe r ri c b a s i c 44 1, ,
.
, ,
6 36 ,

fe rri c n o r m a l 44 3 44 5
, ,
-
. 637
fe rr o u s 4 3 7 4 3 9 ,
-
. o f hy dro rom ic aci d 6 40 b , .

fe rr o u s d ri e d 440 , , . h y d r o c h l o ri c a c i d 6 40 , .

ir o n an d a m m o n i u m ( fe rri c ) ,
n it r i c a c i d 6 4 1 6 42
-
, .

44 5 4 46
-
. p p
h o s h o ri c a c i d , 6 42 .

i r on an d a m m on u m i ( fe rr o u s ) , p ot a s s i u m h y d r o i d e s o l u ti o n x ,

44 1 6 46 .

m a g n e s 1 u m 4 80 s o d i u m h y d r o i d e s o l u ti o n , 6 46 x
g
.
,

l b iliti e s 1 4 1 1 5 0
.

m a n a n e s e 486 ,
. so u ,
-

s u l p h u ri c a c i d
.

m e r c u ry 5 0 7 5 0 8 ,
-
. 6 43 6 44
p p
,

S ul h ate , ota s s i u m 563 , . th e r m o m e tri c e q u i v al e n t s 6 38 .

w e i ght s a n d m e as ure s 2 1 1
,

s odiu m 60 3 60 5 -
.

z
,

T an n at e b i s m u th 3 1 4
.
,

i n c 6 29 6 3 1
,
-
.

lp b
.
, ,

Su h at e s , s o l u iliti e s , 1 47 1 49 , , 1 50 . ir o n 447
lp
.
,

Su h e t h y l at e s o d i u m 5 85 , ,
.
l e ad 459
lp
.
,

Su h i d e a n ti m o n y , 28 5 2 9 0
,
-
. m e rc u ry 5 2 1 ,
.

c al c i u m , o 3 3 2 . T a rt a r 5 2 8 , .

fe rr o u s , 447 e m e ti c 2 84
g
, ,
.

h y d ro e n 3 6 3 ,
. T a rt a r u s b o r a x at u s 5 29
-
, .

T a rtr a t e a n t i m o n y l p o t a s s i u m
,

m e r c u r y 5 09 5 1 0 ,
-
.
—
2 84
p ir o n a n d am m o n i u m 406
, , .

S ul h i d e s a c ti o n o f, o n a c i d s , 121 .

b
,

ir o n a n d p ot a s s i u m 40 7
.
,

s o l u iliti e s 1 46
‘

g i
, , .

Su lph it e , c a l c u m , 3 33
i ma ne s u m , 482 .