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___.aceut1cal .......n�1neennb0-
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P,·inciples 'and fractice�

I

• I

•
C. V.S. Subrahma..qya -
M.Phann.• � ·.

· J. Thimma Setty
· ,. M.Pharm.

l\1rs Sarasija Suresh ·

•. M.Pharm., Ph.D.

l\1rs V. Kttsum Devi

. ..� -.
Mobile : 01712-090073
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DHAKA GRANTHA BITAN
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All Kinds of Medical, Pharmacy

Books are Available Here •

v· ALLP:..BI-I PRP..K.:'\StI1��
 '

•. .

•
1Conte11ts
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c:11:1ptrr 1. I:: D'l ! ST.Rl"\L P'JiOCF:SSl�,G & BASIC PRINCIPLES J-2�

lJnit ,Opl!rati,()ns LJnit Process��: 3
lJnit 10pcrations · - Scic11tif;c Fotjfldntions 5
I
Dirncnsio,ns, lJnits, S) Stems. ;ind· �ntcr-Con\1 crsions · 11
1

l),i,111�n.sions--I:tJrmulae, E(1uation.5 and Anal1,sis J,6 ·

Stoich'i,1r11ctric Equntio,ns 13.alancin'g 20
Question Bank · 23
•

(�hi1ptrr l. Fl"'O\V OF FIJUI DS .25-55

•
. ..
r:1 u id Statics 2 6 .'
., \.,/
,
' !

1:luid Dvnnm ics 31 •

. I

flcrnt)ufli's .I .. l1eo1·c1n J�S " ,

• .. l�11erg)·..
l_,OSSCS . 39 '
..
i\ 1L"' a:;,ur�111cnt of Rate of Flt)\\' 01· fliJids 43
-

1 ..

<..)L1cstic1n l3ank ..'i -/

1" t i ·��'

(.':t,::J)ter 3. TR:\NSl > ORTATION OF. FLl�lDS 56-88

\I a I ,. e 5, .5 7
I , u 111 r1 s 6 2 •

f�t;ci
. rr<)('�!t i rig 11- u n, .rs •

l{<1t,1r;.: l > um ps . 7../

rv1i:sccll�1ne0t1s J ) un1ps 86
Qtit.�sti0n l1;..ir1k ('\·7

Cl1a1lter .i. ('ON\' E \' I N'G ' - 89-102

"'
.· l�clt ( on\1 C)'ors 90 ..a;. ,.

. .,,
.
• [ �1 i..:u 111 :1t i c
) t: or,\' C\ l1 rs 1
96 . ••

(. 'h :i in ( o r1,·-.: \··ors 9(q •

J (J(J i,
•
- �

l\t1ck.cl ('l)nv·e)·l1rs •

St or �l ,.._t! e . l) f� Sol ids I n I

t

Qu�stit)ll l"J�nk I 02 ·
-...
( J aptrr S. � LO\\' OF IIEA T 103-1-13
•
f\. · 1 "-· L· 11 an i � n1 s c, f · I I � , l t l: 1 o , , ·
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('c,r1tlt1t ti,)Il /().,,::;
c (' t i c ) n I I .1
( " ( > 11
..
t,·li,1til)n /27
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••
.
. • '
· 1

Equipn1cnt 11cat l�xch·anger a11d I-teat l nterchangcrs · · I JI '

•
Q cstion nan� / ./2 ..
' . �
. .
• •

Chapter SIZE REDUCTION t'-:� t.i4-176

(\

�1cchanisn1s of' Size l{cduction / ./7,

'
' ••

i\1odet or Stress applied i11· Size Ilcduclio11 /./8

' Classification of Size Reduction Equiome11t /48
Size Reduction Equipn1cnl l ./9 •
Selection of a Mill /66 .. .
·r11co:.ics of Comt11 inuti<)n 169
•

. .
Energy for Comn1inution I 71 · . '

•
'

.,..
Question Bank . . 17../ ·,
••
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Chapter 7. SI.ZE SEPARATION · 177-198

. ·: Official Standards for Po,�!dcrs J 78 · . •
'

- .. .. �
'
.. .
-�: · SiC\'CS' I i9, · . . . ..

.. . . ,_.. Modes ot· Nf otion in Size .Separation IS./··

�
•

.··: . Sie,,c Anal')'Sis "fcsting_ of Po,\·dcr 18 i

•

- .

. Equipment tor Siz\! Scp:;·ration /9 / .

· Question Bank 198 '

•
Chapter .8. i\·tixing '
199-247
Section 1-l\1i�ing of Solids 199-224
lntcrparticle Intcracti_o_r:.s Segregation 201
Mccl1anisn1 of tvtixing in Solids 202 · ...
�1ixing Process-Steps· 203 ' · -
Degree of f\1ixing and Statistic,tl l�-,·a.luatto11.
· ,2
. {.):-l· . ;· ...
.. .
·
·;.
"'
..:; '

f- acl(l1·s I 11 ll ucncir.1g ML, i11g 212 •

Classitication of I·:quip�\11c11ts i· or S{1liJ �1ixing 21..3

- .-... .
·�
Equipmen·t. 21-1 .. . . , . .. . . .. . ;:
·Qucst1on. . 8 ank, ....,'-'4.1 - , • ,

.
Section ll-l\1i.xi�1g of Liquicts . .. ' .
225-240
'.'
• •
•
•
Mecl1anisn1s ot· �ixing 226
· · Mixi11g Vessels ?2 7 · . r -. '• •

- ..
. ., . .. . '... ..�. . .:... . .
'•

tvlixing De,, ices' Flo,,· '<,•at.tern

.... � M:,
.... I '.
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., · · Equipn1c11t c" 236 J f
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.. _ . · Question Bank 2./fJ - · ·
.. .
. -·
-
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Section lll-1\·1ixing of ln1n1i-sc:·t>le Liquids 241-245

•

Equip1nc11t 2-1 I
:

•
. ... '(

• Sect.ion 'IV-1\·lixing of Semisolids • . . .245-247

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. I
, Equipment 2,.J5 •
· ;·· Question l�ank 2-17
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Chap_tcr 9. J...ILTR...\1'ION 2.l8-275 •

t\1cchanisms <lt· i.:iltration 1.50 . •

•
.. •
•

' •
•
•
•
• •
•
 . •
'

•
•

·1 .corics of· 1 :- iltration 252 •

l:.!CtOrS l11·nL1cncing f.iltration -,5

- .- �

r:ilter Media and Piltcr ,\ids L)

•
')-­
.' t

('lnssification t)f Filtration f�quiptnent 2.59

: :· 1ui pn1 en t 2 6-0 •

()ucstio11 IJ�111k 2-:5

I ,• .
Ch:1J)tcr iO. CENTRII;UGA�ION '
•
276-'292, _,. .,

l'hcl)f)' of Cc11trifug<.1tion 2 ..,7 ,,

•

r
(� l �1ss i ti c ation C) !· Cc 11 t ri l'L Ig es ? 8 (J
•
E q Li i p ,n c 11 t. 282 '
Question 11<1nk • •
•

Ch;11Jtcr· I I. DISTILLATION 293-336·�

·rhcor\'., ·295 ••

·
Gencr,11 I:qL1ipn1cr1t for Distil.lation ]()()
Classification of Distillat1on. . Methods. . 3()4
.
s·in1ple Distillation· 30-1
J � I ash Disti11at i c_'In 3 ()8
•

rr actio 11 al Disti11 ation 3 In -

/\zc()tropic and Extractive Distillation 322 ..
•
•
f)istil!Jtion tinder Rcduccu PrcssL1re
•

•
•
•
S t c <.1 n1 l) isti 11 atio r1 3 2 7 •
'
:v1olecL1l3r Distillation ·330
• . · Dcstructi\·c Distillation 33-f
Compression Distillntion · 33:5 -
Qt1cstion Bank 335 , "
.
• "·
Chapter 12. EY�POR.�TIO� 337-360 •••
Factors Influencing· E\'aporation 3 38 I

Classi ti cation of Evaporators 3-11

Equipm�nt 34 I
., · 35·3
Thcorv
Multiple Effect. Evaporator 356
Question Bank 360
'

Ch�pter 13 .. CRYSTALLIZATION- 361-381 •

. (�t.aracteristics c)f CrystJ!s 362

Pl1armaceut ical Sol ids 1·erminology 366 ••
l�hcory of C:ry·stall'ization 368 '
[:quiprncrit 373 .
• 4

.,
c:aking of' Cr) St(.11� 379 1 •
.'
Qucstio,1 Bank 38 J
•.

'
• •
�----­ . ---- ·--,.
...�h a pt c r 1 4. DR '&' I NG v . -
382-406
·1·heor\', of' Dr)·innb 383 \
•
• •

l'lzissification of· Dr)·ing f:c1t1ipr11cnt 39() f

.;

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�. quipmcnl JYO
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·Question _Bank ./05

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Chaptci:- IS. IIU1\11Dlf.lCATI.ON A.ND DE1�1u·:VJIDIFICATION ;-t, 40_7-430

l lun1 idit. y Cl1urts and Its lJti.l i�y .J ,�, ..,
• - ..
l-lu1n iJ i Ii cat iont · -11-1· · · t
':
T

•
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J
•
•

l)cl1um idilication ./ 15 , " .

l{cl..rigcration ./ I 8
.t\ir Co11J1tioning ./2./
Question [lank -429
..
., ..
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•

. � c·haptcr 16. CO�ROSION - ·'

, .
• •
·;.-i · -; 431-449
1�11corics of Corrosion ./J2 " . ..

I Factors lnflucn�ing Corrosion - 415

\
•

.
. · � T)'pcs. ot· Corro.sion -!38
.
'-",,
•

Pre,·cntion and Control of· Corrosion 44./

Question l3ank ././8
I

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.
- I .: -,
- ,c • -
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.. •,-:
Cha11ter 17. :l\lATERIALS OF CONSTRUCtION.- 450-466
'; -.. , .

--
Factors Influencing the Selection ot Ma�-�ria!s . 45:1- . : :
,_. 1· ),

. Classification of Materials f·or l,lant Con-stru;cti'on-· � . -453 • I

� � F �rrous �1ctals 45-1

":_ ., }
' ' •,

..
.
.
Non 1:-errous
. '

..
�1eta1s .J5i .
. - -

Nohn1ctals . Inorganic. +�i 9 . ·

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N n�ctals-Or an.ic ./6.: ." l

Q·�. cstion. Bank, 466 · - -· ·

. -...
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•
f.

Chapter 18� PHARi\tA. INDUS"fRY - EST·A-8LISHl\1E-NT. · - r

'. 4 6 7 -485
...
Pharn1accutical
. lndu·str)' - .· ·167
Plant Location 468·
· ··. : ·e ,·. Plant �r ayout 473
.

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Utilities and Services ·· 476
J

.
c 8 ..
- Industrial Pollution and C .ln-trol: 4 ·7
\ Industrial.
Hazards and Safi.!ty 480
Question Bank 485
. .
APPENDIX-I�·· : Fractions. alnd: l\1uitiplications or Units · � ·
' •
487
,p

APPENDIX-II ·: ·Notations and Abbreviatio·ns .� ·�· . -.

• • ' • 0 "' 0 �.. ... L.'• ... J
, ,·, 483:
APflENDIX�lll :· Inter Conversion ·or Units··-: -�
!"> •• 1-- ·

· 490
APPENDIX .. ( v t
: Definitions and·, !\'leaning's �
.
�
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492
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501
l· - • •

AP[> ENDl�X.-iV : Bibliograph)'

SUBJECT l·N·DEX 503

 �
Industrial Processing and Basic .Principles

Unit Operations-Unit Processes

Unit Operations-Scientific Foundations
Dimen:;ions. Units, Systems and Inter-Conversions
Dimensions-Formulae. Equations and Analysis ':
Stoichiometric Equations-Balancing

Pharmaceutical engineering is conc\!rncd with the study of industrial

processes in which r.�w . materials arc changed' or separated into
pharmaceutically useful proi:lucts such. as drugs and excipients. A wide.
. .
variety of proccs��s arc.involved in th.ese conversions.
· Some of them
arc as follows. . . · ih
. :, tr! J
l. · Production of dosage forms : .Conversion of drugs (chemi.cals
.
as raw mate�ials) into
. medicines. (dosagefo,',ns),
' '. ·which
� are suitable'
>1 .•., ! for
. , •)
use by the patient. Example is conversion of diclofenac . sodium i[:l_t�
.
. . . . t. .·, ); > JI
dosage. forms su�h as tablets,. capsules. suspensions and injections.
,,

.
. • \' l. � ·, •.

2. · Production of bulk drugs : Chemicals ·

(raw
.
materials) are
i1�1i·1; ·r,:·'1·
converte� in�o dr�1gs. F�� .examp.lc, salic. ylic_ aciq J.s �cetyla�� d t�:,?}?.t,�.i.�
:
acetylsalicyl1c acid (asp1nn). This area IS known as.prodµs;t.i�nr.P.L{!u,!�
Drugs. Conversion of chemicals into intenn�diates, which· in turn)1rr 1
used for produdion of drugs in commercial scale, is a.lso incl. udcd i� in'i�
area. . : ;!··.n ·!.,··\·.,,.,,. ,: i.
. ' • ·I; . ,• ', ,' •�•:;�'.•#, 1!,h,f,·.111.t'.; • 1 ri1"
· 3. Production of antib_iotic� : Manufa�tt,1re of,��s.)�mi�jmi9f).
using_ JTiicrobes with the ajd of precursors . •.is1 anQther area ofjrite�e.st )o
.•. ·1}... ,1 1 "'1.1 .•t>Ji,,:.:1 ,(l

'f.�r
• . . . .,,, ., 1
the pharm�cist. Jhis area .is knO':"I� 'as fer'!1ent<;1t.�9.ri )7C.l!W?-!?gy.-i1 f
example, ,penicillin G is pr?'dµce.d ��ir)g Per1f�i/liJ1��i f/rY.f.0.lJ,fJ�W?}, �Y}.�
. ·
the aid of precursor. phcnylace�ic ac:id
". · . ,::'.:n;,,,n
4. Production of biologkals ; .Extract1on:PfA�1:1gt f�<;>I)}, 1�.9\1pals,
.
plants and minerals from native . raw .materia\�.inJo,�µJ:itJ(;� A(of ��·
purifie'd) producJs.,are of interest to the phar.m;ic;i��-: �Q111.<r:���!))pl��:at�
va.ccincs, insulin. strcptokinasc
.
and.recombinant'� DNA ..., technology
.
prod·\""
ucts.
 /
IPI.ES 3
Pl IARMACFI J llC,\l FNCilNEl'RIN<i ('h-1 INDllSTRl1\I. l'ROt'l:SS\N(j A�I) l\,\SlC l'RtNC
standing plrnr-
information and prcrequisill'S that arc necessar for uridcr
y
Each proct:ss is clevclopcd systcrnntically from a lahoratorv scale to· :
· pilot scale and tinally to an ind ustrial scale. In each case. process is maccuti1,:al engineering.
. undertaken by employing a number of equipment. The areas of interest
with reference to equipment arc: , : llNIT OPERATIONS AND UNIT ,PROCESSES·
· - design
, ' • . , , ; ,. ... '1 ( ,• •: • ! • I ' • :·,� I ' �I

Normally, every process involves a 'series of steps.. E�ch step is

•

- fabrication · economical
performed individually. Thjs approach is an way
assembly ' · ' o�· ?fganiz-
ing a given task. ··
-· operation
0 •
·
- maintenance Unit Opcrntiom
of
Similarly, each process has to be followed scrupulously in terms of: Each chemical process frequently consists of ·a fewer number
. ;. .
· · - effectiv ity di�tinct individu al slq�s. Each step is called unit opera(im1 ...
A
efficiency tach unit operation is based on one type o� scienti fjc. principle.
listed ·
validity few exvmples of unit operations and underlyil}S• principles are
·· ·- safety Q . ..

below. ,·. ·;· , . .: .. ,.! ·.·

economy 1re
' . Drying : It is a unit ,operation used to remoye .liqu!d ,or .11}oist�
drymg
fjfectin!ne.ss refers to the quality of .what is to he actually accom- from solids by ev;-iporation with the aid of ht;at. _For .�xan1pl�.·
. plished. Ejficie119 means accomplishing tasks with a minimum of
1
process is employed to remove' excess moistu re (above 'equilib rium '
wasted material. time and money. In the popular management clich�. moisture content) from the wet gran u. les :i n 't he produc tion oX,tahl ct,s .
. ,·''.( .... v �'{ ....·

efficiency is doing things · - right, while effectiveness is doing right or

Size reduction : This is a u nit operation in which dr u gs (vegetable
things. s or i
tine
;, chemical origin) are reduced to smaller pieces; coarse. partic)c
Validution is defined as a procedure that demonstrates the ability of powder. This process is extensively used in the manufacture of ·talcum
consistently producing a product with the established specifications un­ powders and tooth powders (cosmetic industry).
. • ' .·�
· i.

der ideal conditions. iiquid into vapo u r

. Safi.!/)' refers to the pr<>tl'Ction of produrts, pl'rsonncl, factory etc.
·Prevention, of accidents and p'rotection from fire constitute important
a.peels. Suffici,mt care sho uld he exercised so th;-it human factor is ·
removed from the hanrds by making _protection a permanent and auto­
matic.
Economy refers to th(' protection of laciory from financial problems,
The i��ustrial activity �sscnti:1lly involve� the con\'ersioq of raw materi­
als into value added pmducts. The sh.'ps arc initiated for the optimiz.1tion
of parameters for an operntion · and process. so that econoiny works out
for the factory as well as customer (or consumer). Standard Opcratinµ
Procedures (SOPs) are helpful to obtain a qua I ity pwduct coupled with
economy.
Therefore, a broad understanding of the basic prin�'iples involved in a
procc.ss. knowledge about the construction, workin� nnd skills in han­
. dli;,g thC'm arc o( vital importnn(;t'. This d1nptcr' provides the basic
Distillation : It is a unit operation of converting
r liquid by condensing the
by heating and reconverting vapour again int<
vapour. This unit operation is used. for obtaining essential oils from
various parts ofthe plants. ExamJ>lc is lemoi:t-grass oil (perf�mc indu�t,Y ).
. · [,· .. �oration : It is a U'}.it operation· �hich inv�ves fr�c, e�c.apc of,
·.-apour from the s urface c,f a liquid below its ooiling point: For
example. ('Yaporation techniqu� is ·e)_<tensively,.��cd for co11centratmg the
,
. syrup in th.c manufacture of sugar (sugar in.dustry).... , · . : . { , J,
.
l he �dvantage is that ea;�b., u.nit operation is a common.. technique
and cmployed··-iri diverse chemical and p�arm�ccutical industries. For
. example, the operation of mass' transfer is involved in humidification."'
evaporation, distillation, extraction and drying, The Jmit operation of
drJing is u sed in the· followin& industries.
ti) "Pharmaceutical ind�stry : In ·the, production of tablets. the
powdered, mass is converted into �ct mass, which is s ubse­
quently dried in order to o):>tain free flowing dry granules.
 ('h-1 INIWISTRtAI l'ROCFSSINCi ,\ND llt\SIC: l'RINC'IPLES 5
4 Plli\10,IACU ITICAI. FNCil\:l· 1· Rl\:C i • J •
/
In the above process, three unit process�s arc involved.· These arc
In the manufacture of herbal drug extracts. a lar!!e n(1mbcr or nitrntinn. n:cluction and acct�·lation. Ea:h unit process ·is in tum· made of
plants are used. The piant extracts an: dried in order io �xtend a.number of unit operations. For example. in .the nitrati<);l of bcnz<.·nc to
thl! shdf life. Otherwise,' the prt)Juct may ddcrioratc. l·\1r
11itrobciw:nc. the unitJ operations involved are:
example. in the preparation or belladonna Jry c:,:tract II'. liquid . . . .. .. Y.���, l,�->�-:·, j ·�

l'xtract of belladonna is dried compktcly. Othcrw1si.'--it gets ....---,----i··....

. deteriorated. Fluid flow Heat transfer ., Fluid flow

Charging of Cold brine is.passed Addit':in of �
(:?), Food industry Grapes. cashew. alml:11,l" and other typ.:-s of nitric acid into to reduce the sulphuric acid
the reactor temper�t�re to 15 ° C
ti·uits arl! dried to obtain dr\ fruits. li1csc products kt\C cx­
tcndcJ storage life.
(J) Sugar industrv :. The crvstals of sut!.ar arl! dried to rcmo\c l
rcsidual water..so that the �uga� will b; dry and free flowillg. Heat transfer
Fluid flow
Add1t1on of
Unit operations arc based on both science and experience. The Filtration Heating to 60 °C benzene in
for 1 hour small quantities
thc:ory and practice must be conibined judiciously for achieving profi­
c.icn�y in handling equipment. ·
'tJnit Process .Crystallis�tion
(.'n il /Jl'OCCSS is defined as the one in which Sl!Veral Ullit opcratib!JS
arc combipe�. in a seqL1ence to 'achieve the objectives of a c.:hcm.ic:11 or The:-c cxa'mples illustrate .that unit operations an\. l.lrgcly used tn
w
physic.:a I process.
,
,·Unit process-Physical process : Consider the example of ma·nufac­
conduct the physical steps such as:
1. · Prcpnratiory of the reactants,
. .
" Separation and puri tic ation of the product�. ...

-
ture of common salt. The u:iit opcratio,ns involv<:d arl!: i .

Transportation of
fluids and solids
-. Transfer
of heat
Evapora.tion.
3. Recycling of the uni.:on\'crtcd rc::ictams.
4. Controlling·of the i:ncrgy transfer into or out of the chemkal
reactor.

l Thus·. several steps· arc carried in a sequential order to .achieve a

Screening - I I-
Drying Filtration - Crystallisation
process efficiently and economically. ... ... . .. -·,, ,

UNl.T OPERATIONS-SCIENTIFIC FOUNDATIO�S 1· ,.'

Unit p�occss-Chcmical process : Consider the production of para- A large n�mbcr of unj� operations are simultaneouslY,i,hand_J cd i11 a.
\:hemical proc'e ss. Hence, the knowle�gc of the elementary. physical and .

l
cetamol from benzene.
nitration chemical laws (Figure l-1) is cssl!ntial for the application of scienti lie
Benzene ---------• Nitrobenzene principles and. techniques. Some of these la,�s are:. ·, ; ,,
Basic· laws:
' , Laws of conservation of matter. . .. .:·
red�clion
At I H2S04, 1 h Laws. of conservation of energy.. •• I I � '.;
� \.
:··:· ,:li {'r'
acetylation Special laws: U[!ivcrsal g_a!'> laws (Ideal gas_.equation).
Paracetamol p-Aminophenol
�celic anhydride I Dalton's law of partia_l· pressures.' , ··· \ . ;r'·,,
sulphur:c acid , � . ·;; ,·; ·J :.' I

Sequence of reactions for th..: pw<lt'1ction of naracctamol ( or ac�t:11ni11ophc11 ). ' �.} I

'<
j I
 Ch· I INDUSTRIAi. l'IU>C:ESSING AND 11,�SIC' l'RINCll'LES 7
6 1'11·\ It\ L\CFt: I ICAI. Fl':< ilNl:I: IU �( i
' . ment, or to the entire process or any part of'it. A simple acc?unt of
. Special laws arc d_iscusscd in detail in diffi:rent books m�,nti�ncd in
biblio�raphy. The basic laws are highli�ht1.'<I below.< material balatice
· 1.
INPUT = OUTPUT
UNIT OPERATIONS Amount of Amount of Amount of

l
Governed by physical raw maierials changed + unchanged
and chemical laws materials materials

Radioactiyc process is an exceptio11 because it docs not obey th_e

Govomod by
material balance calculations.
Ad\•a111ages : The mass balance calculations can provide inforn}ation ·
Basic Laws such as yield value (practical and theoretieal) and percent recovery.
Laws of conservation Currently, validation or processes and equipment has become important
Ma/ �9.Y in the certification of ln.ternational Organisation' for Standardisation
(ISO). Mass balance calculations have assumed ccntr.al place. in the·
current industrial dcvelop!ncnt.

l
Material balance
input = output
Energy balance
input = butput
· Estimutio11 of maierial balance : In a chemical .rca�tion,- ·material
for illl forms of balance can be accou111ed by mc;asuring the amount of all the compo­
energy nents (constituents). Normally, the amount is expressed in· concentration
E;tim,tea' units; moles/litre, molal units, mole fraction µnits, % w/v, % w/w etc.
Some of them arc reported for ready refcrcnct:.. . ,· ..
(a) molal cone. Mole : In a chemical rcactio_n, the molecular unit is.gran� mole or
(b) mole fraction, X2 ,r· .
f'Olllld mole. So111c important expressions
- • i

(a) heat · . a;e molal units and mole

'(b) mechanical fraction units. · ..,.;:.,
· (c) elect{ical · In th� mass balance calculations, mole 'is a better term and used
(d) chemical
frequently. For an individual �omponent, mo:c is dctjl�d as quantity qf
·�-
(e) radiation
that substance whose mass is •numerically eqµal to its molecular weight.
I

rigure 1-1.• Scientific foundations in unit ,:nass in grams

opc1ations. Basic laws arc incltHk<l. Gram-moles
· of a substance = -- · . , ( I)
'
nfolecular weight
.. l
Basic Laws (if\"'""
These valuef•.arc useful while ·selecting the amount of each ingredient
Th� general law of conseryation can be applied to any process. It is to be added to the reaction mixture based or the stoichiom�tric _equati9n
1
er12ploycd in engineering in the form of: " ' • '·' • ,
and coefficients. for e'xample, .,· grams of oxygen gas has been math-
(a) Material balance .... 'O
ematically expressed as:
(b) . Energy balhnce
x grams of c:;;ygen x grams
1\latcrial balance : ,ThJ lirn.' oj co11sermtio11 of mailer 'states that Numher uf moles = r---- = ----
molecular weight of oxygen. 32
material cannot be destroyed or' cr'eat�d. it can·· be'· c'himgcd from one.
form to another. Average molecular weight: When a mixture of substances is .involved
In other words, th� material entering a process must either accumu­ in a reaction, the avcra�e molecular wei,�ht of the mixture' may be
late or leave the process. The given input must be accou"t1ted for a:i wrill1:n as:
outp�t. The principle of material balance can be applied to an equip-
 0 !(•:
9
Ch-I IN! >IJSTR,?'il. PROCESSING ANl) OASIC PRINCIPLI-.S
8 l'l lt\RMACl'lJTll'A I. ENGINHIUN< i

IVa + IVb -t We+ ... ... ... . The �um or the mole fractions of all ccmponents .!11ust 'i,c c�ual to
.frcra.�e molecular - ---· ··----. ----- ... ··-·- unity. Mole fraction is used'frequently fn experiments involvin,g}hco­
11'1:ight of mixture. 111 \V" \V1, w,. retical t:0nsiderations. The advantage of. mole fraction notadon i�. that it
- + --- + _. - + .... . e:,,;pressc� the relationship betwee11 the reactants and other compone·n.ts in
Ma Mt, M,. a simple :md direct· way.
. .;l ••.

Enc:r�y balance : Energy is the capacity to. exert a force through a

I
where W0 • IVb. We etc. are the weights of individual components a, b, c.
etc. ' Ma, Mb, Mc etc. are the molecular weights of components a, b, L uistanl·c and manifests itself in various forms.
etc. The unit of energy in SI system is J (lloule)� The energy per unit
mass is known as ·specific energy. which has the unit ctf'J/kg. Engineer­
Molality : for individual components. molality is expressed as:
· number of 1'noles of substance
. ing processes involve: (a) conversion of energy from one form to another
. (b) tran\lcr of �nergy from plac"e to place (c) 'sfoi�ag� of.energy in :various
· · : . McJlality, m .· -- ··- ··--
(3) forms 11tilizi'ng a working substanc�. The . first law of th�npodypamics is
c:

. number of kg of medium-("s0lvent) , I., l .,� l , • . .

a state1m:nt of conservati�n 'of energy. It cxpr;�sscs the fact that energy
The' ur;it is. �ol kg·-1. · It is designated as m.. Molality (molal) l'.innot be neatc:d or ,destroyed. though energy qn he transported from
notation is frequently trsed in theoretical studies. Th<.:
.
advantages art'.� •

one kind to another. . 1• ' ·

• ,.. . I .

I . ' • 'i •., .• . \.'. J.•.

enumerated below. . �·-·· !,, .
Thi..' /,11r o(cn1m.-1Tutiu11 of <.'11(:rgy states that 'he energy output,must
,(a) It does not change :with temperature, i.e .. contraction or expan­ bl.' s;11111: ;i.; tl�e cnergy·'input in a chemic�! proces1;. , ,
sion of a liquid with temperature·does not afkct the ca]culatiogs.
Tht• l'nl·;·gy bal:mcc l'quation must includ� all .i)'·rc� �f energies.
(b) The weight of solvJnt (reaction medium) is rons:der�d. Vol�mt>
has no influence. since it is not precisely kno" n always."
• IH:at * mechanical· efi:ctrical *
, ., _.
* radiation
� ·1 , I t ,j

. "' chemical· 1

Mole fraction ·: Fdr, individual component, ntok fraction 1s c:-.-

• �· •
1
·, ; 1 • ' • � \ •

Wh1:n· one kind l,f ei1.:rgy is destroyed or co,nsum,fl. an equal amount

,-

pressed as: ' 1•

of anotl1t·r � ind must be formed. -
number of moles of one constituent . .;.{ ·., ..,<,,

Afole fraction of A, XA ----·-·· --· -.....------··--·-·-· . Acplil·u1i�J11S: The principl'e of _conservation �f energy- is applied in a·
total number of moles of all constituents
' ' .
1 •
numlwr lll' instam·l..'s. A l't>w or thl..'m arc mentioned h,:!(t:. • · ·· •
It is designated as .Y. One constituent may be solute. Total number (I) In the study orrnuid flow. Bcrnoulli'.s theorc1��' is applied, which
of moles of all the constituents refers to moles of solutes and solvents. is�, special case of the law of cons�,rvation of:cnergy. ,.: • · .'-'1
. .
lt is in· general notat.ions as: . {::?) J·:nergy is c011vcrtcd from onc.fo�ni' to anothek 1'his'principle'is
0

t uscJ in the, �vor,king of .a ,pump wherei1' 11 kine-tic energy is c·on. -

\at,sd into pressur.e head for pulflping:the liqtiids: ' 1 ".•.-
Mole fraction of A. X.1 � (3) Encr!.!y losses due to friction can be .accountr.d, while a fluid is
W11 Wt, \V,. flowing through p.ipcs. It is.·also 'h�lpful ff�." adopting" suitable
-+-·-· +-·­ .
MCI Mt, M, measures to reduce losses. ) . ·, .'. '"""" ·
i
(4) ·Sit_ll'�· l..'ffickncy"and economy arc� important parameters- for any
pm<.;l..'ss. (clicmical or, physical), , •?.nergy. cal i�lations" and 9aln�c� ··
,'
<-n i11g have assumed importance. When rene:gy is ob'!ained from
II {I + lib + 11c -l ... ·11l111;rcn1,:wable sources, bala11cir:.g of'enerf1Y will be a critical
. i·:.·.
l�1c1or. ·· "' 1'

wh<:re 11 11, 11b, lie etc .. are the number of moles of individi1al components
a. b, c, etc.
..
1;,,,,.,:
 JO · l'I IARMACEUTICI\I. ENCilNEFRIN(i Ch-I· 11':llllSTRl,\I. l'l{OC'l·.SSl:--(i '.,\1-il> IIASI(" l'IUNCll'l.l·'.S 11
Some Basic Concepts Dll\H:NSIO.NS, UNITS, S')'.STl·:l\.lS AND INTER-CONVERSIONS
Rate of a process or reaction : The rate cf a reaction can. be For 1h.: pmposc or measurement (dimensions), tluei:: systems have
understood by studying th,: time course cha�gcs in �c.conccntrati�n·. In
been used, nam.:lx:
general, rate is �xpressed mathematically as a differential equation:
Cgs system (Cl'lll i 11H:tn:-gr:1;11---ccond) ·--AI so known as r�ctri'c system
dQ dF driving force
Rate�of reaction "' -· "" -- = --------- Fps systein ( t"oot-pou11d-scw11d )·- -··A !so known as i!ritish. syst�1n
(5) •' ' _
.· .. , . dt. · R resistance ,\lks or S'l (rlli:trc-kilogram.-second)·-1\fodcrn systc1! 1
)

,. .· ,
1
where Q = quantity being transferrcd or reacted
The basic quantities idrntifid for this purpose .ire length. mass. time
':a time
etc. Tlrcs9 arc cxpn:sscJ in various ways in difforcnt sy�tcms. $011;,e of
F: driving force
the important principles in dimensi�ns are givqn in Fig'ur� 1-2. ,.
R "' resistance
The units 111cntionccl in any sy!:>tcm for cxprl!ssing t.hc physical qµan­
According· to equation (5), the rate at which a 'system approad,cs tilics arc known as .f1111clamc11tu( 1111its or pri111W)' 11i1its.
equilibrium may bt" exp1'�sscd as the 'con1birn:d effect of two factors.
·: · .� · ·. h,r c,a111plc. length is cxprc;;scd as ccntimetrt: fo cgs. system. foot in
These are: ;
• 1·p< ...yst::111 and 111ctrc in mks system. The' offici,il international system of
(;) Potential fa�tur : It indicates the driving force necessary to make unit, is .the SI system (Systemc Internationale d'Units) and commonly
(proceed) the reaction. employed in engineering �nd science. The basic units in SI system arc
·i· (b) Resistance JaJror: 1/i'ndicates ·h/capacity to i1;1pedc the speed given in Table 1-1. Primary units arc the basis f�� obtaining derived
for a given potential. units.
t •
In 'the ex�1�1plc of heat transfer from ,the hotter end of the iron rod to Scxondary units or' derfred ·ynits are those tha.t are · made· by the
I , 'fr
the colder end. the driving force is· the"diffcrence in temperature (.17). inclusion of primary units.
At the same time. iron also offers certain amount of resistanc.c to heal For example. acceleration is a secondary unit. It is expressed=>as
.
flow, on acc0tint of poor thermal co1iductivity. · k11l!thitime 2 . Other e,amplcs or derived units in SI units are given in
: ;· ......
Steady state and unsteady state : In a system, if the operating ral;k 1-2. For these units. a!,tcrnativc bas,; units any given in 13 part.of:,, .
conditions arc varying ,vith time, then suc. h a s'ystem is said to be in
unsteady state or transient state. . . Appendix 11.

For example, consider a ,tank of cold water. A:coil in which constant

Basic Units in SI System
pressure of steam is maintained is immersed in the ta�k. buring the heat
transfer through tre coil,. the operating conditions such as temperature Ah1os11rc1.ud11t/Q 11w 11 i1_1 Unit .s:rm ho/
diffe�cnc6 .. l�ctwce:0 the coil a. nd water do noi 'remain same ,_vith time.
l.cnglh (L) ivktrc. Ill
Similarly'; thermal res.isiancr I between the. coil and water changes with
· Mas� ( 111) Kilogram kg
ti�ne., nr
\ ''i\l
Time (I) Second ' s or s�·l·
A system is said to be at steady state, if the conditions do not vary
· A11wu111 of substance t\folc 111o I
with time.. ·,
TcmpL'raturc Kelvin K
For example, copsider water in a pipe is flowing unde'r' Hrn �ohdi­
tion5; (A) \Yater, etltering' the. tan�, at constant temperature 'add flow rate. I :t.:i.:1nc i:urrcnt Ampere ;\

(8) A jacket in which steam is maintained. .at constant temperature I .u111i11ous intensity Candda cd
surn?unds .th� pipe. Condition may vary. from .section to section along
the pipe; but at any one cross -;ection, it does not vary with time.
12 1'11/\RM/\l'J'.l 'I Jl'/\l. EM.1INLTRIN<i
th·I 11'\IWSTIU,\J PR<lCF\Sl!s:Ci A"-l> BASK' PRlNCll'U·:s 13
All physical quantities consist of two parts.
Applications : I.I is c,senti::d to be conversant :with all the systems
' I.. U11ii : It 'indicates a.bout •the quantity :llld gives the standard by . · and alsi, ri,eir inter-conversions·. In pharmaceutical engineering. it is
.which ii is measured (exarnpks arc ccntimctn:. foot. second. ,icl:..:s,,,r) [11 liandle :., large 11�1mber of ph:,;sicochcmical ·data. while
po�nd. grams)'. sclc..:ti 1 11.: th..: r.iLdll kind :)t' m�ill:rials for a process. Most of the literature
2. Number : It dcr,otcs the llUlllbcr of unit:-. llCCl,kJ (cxampks ar1.· dnla :ir; a�·ail;bk in thc old.er systems such as cgs and fps systems.
one, ) �VO, three CIC.).
I
·:·hercliir..:. it is necessary to bc e,1)(:rt in all the systems of units.
:J .· ' .·

lhese two 11at1s �ogcthcr they make a physi1.:al lJUa111i1y. It is

T,\BLI:: I ·2
essential to specify both· the parts. whcrn:n·r :i ph) sical quantit) · i�
s·omc Dcrin:d Units in S'I. System
expressed in the engineering.
. . .

; S11111Jl<!111.:111£1��1· 1;11it.y : T,wo suppkmcnt.iry 1111i'b arc at pr1.·��·nt de­ , .\-feus1•n·111e111/ Unit · Sym hnl
fined. the 'radian �nd the steradian. which arc the units or plane ;1nd solid ----
{!11011/i/\'
angles; rcspeclivelY: F0n:c· ncwtu11 N
l·:ncq;> jot11l:
'
1.MEAS��EME. NT OF QUANTITY I 1 1 11\\ c·r

.··-1
/, watt \V
l'rcs,urc· paq:;il l'a
1·rcqu.:11cy ht:rll Hz
1·.b:tric i:h,1r�..:· rnul0mb C·
Primary or fundamental units Derived or secondary units \I
l·.kc1 rical potl'll\ial ,oil
Choice is arbitrary Examples are:
Examples are: acceleration and.volume Fkctricd r..:,i,tani:c ohm n
lengtll; ' mass', time,

l 1
temp or any other
Inter Con,ersions

l J
. ') o'
Any quJntity c.111 b..: convert�J from one system to other by the use
A number AUNIT' of' com·ersion factors.
A number A UNIT One, two, minutes,
Co111·.:rs1u11 Ji1c1or is a purc 1111111bcr and simply the ratio of the
cm, m, f, three etc. · Cubic 'centimetre ..,:,
One. two,
g,Kg, lb, magnitude of th..: unit in one systcm to that of th..: corresponding unit in
three etc.
S, S, S,
Ce!ci_u�.
the other' system. .. ,

-
·C
Kelvin, Convt.:rsinn factors arc si,;1ply multiplication factors. For example,
Fahrenheit the k11gth e,prcssi.:d in fps systt.:m is. ·l O li:ct.. To convert it from fps to

l
SI system. the conversion factor is 0.3048. i.e.. 1 foot = 0.3048 metre.

,\ I knee. IO !'.!et 'd� .30.rn ,: Io "" 3.04S metre

.
SYSTEMS It is -�ll1ays '6'e;ter to 111�kc a ;·n.c11tal-pictL1re of a u·nit. wl1ich wi.11 give ., . I
CGS· older, widely familiar (cm. g, s) a hrge ligurc (i.e .. 11qmhi.:r). Thi.:n the com·ersion factor should be
.
FPS: older (f, lb, s)
SI (MKS) current. commonly used (m. Kg, s) applicd as direct proportionality (lr inverse proportionality. This can be
. illustrated her..:.
111 th..: ;i!,,.,ve c:1:;:i111plc. the convcrsio11 foctor is 0.304S. Metre (mks
Figur� 1-2 .. ll11i1 sysh:ms au: ,l 1..:lc,.1111 \\ay� ol c:1.prcs,111;; a q11antit). . s>·ste111) has higher magnitude co1n1)ared to feet (fps system)._ Therefore.
1n�·tre h�is a small nu111hcr compari.:d ·to the corresponding number in feet.
l·lt:11ce. t'ciot h:-1� lo be multiplicd by the conversion factor to get metre.
14 l'I IARl\1:\Cl:li I )(.'.\I .l'NCilNEl'Rll\C.i
<"h-1 l'.:lll 1 Sl IU.'\l. l'ROt.T.SSl;\;Ci /\Nil ll·\SIC PRINCIPI.FS 15
<>
IO li.:et � IO x 1,;onversion fa1;tor
0
IO x 0.3048 .,:· 3.048 metre "
g I I 'IIH\0) 1-.g: I ,·111' ·· I 1,JOO) 111·':
-'=

Convcrsdy, metre should be divided by conversion factor to oblain rl1, ,·1111\ nsi,111 fal·inr ma� be oblainc.J as follo11:;.
feet. For example.
,. ( I i I rn iO) k �'. I 01 IIJ<ll II) 1-. b' I OOU kg
.I l(l!)l) i._g,111 -'
3.048 metre"'--·---·- x 3.048" 1o'fcct. ,:111 \ I I .'IO(I)' Ill
I I llOll rn -' m -'
0.3048
1·1ie , •'11) (r�ion ra,·tm · I (ii}()
Inter-conversion between SI system and cgs system is silllplc. be­ '.\�II ..\!'ml., IOO() :· 2.7 k�i!n' ·' 27llti kt!!m·'.
....
cause both use same standards ti.)l" time and h�i11pcratun.:. M:iss ran be ,_ .

converted from one system to the other. Some ,�onvcrsion factors for . l'ral'lil·1• l'rnhh·m 1-J. In tlw litcralur,·. nwss 1ransl'i:r l'11cnil·icn1s in lhl:" l!as
primary and scc.ondary unib bct,,ccn different systems i1fl'. in tables I phas,· :ir,· pf; l'n l"l"p,u·t,·d in t,·rtns nr lb·nwl 1h·ft�-atl11. lklnrnine 1h1: conversion
and 2 of Appendix Ill. l:lrlor I•\ "hirh thl' alww 11:11�1 lw multiplil'J i11 11rJcr to n!,tain !Iii! l'OrresponJ.
ing \a·· l i ;i.. ,,1 ki;·nwlis·m�·l'a.
Te111pcratun..• is normally denoted in degrees by Celsius (''C). or
Solution: TIK0 gi\·cn un.ils uni!� into \\hich Clll\\·erted
Fahrenheit (°F) or Kelvin (K) scale. The thermodynamic temperature
lh·mol kg:11101
scale is called the Rankine scale, in which the temperature is denoted by ·--·· ---·- ..... 0
dcgrci.:s Rankine. Their relationship� arc given in Table 3 of Appendix' h·fl 2 ·atm . s·m 2·l'a
---------------------
111. ---·-------·------ ·
I r\1111 ,rn11ersinn Tahlc I of /\ppl.'ndi:,; Ill. the following ron,·.:rsion fa.tors
Practice Problem 1-1. The unit of vi�rn!,,ily in the· 1.:gs sy:,1em . is the poise� ran hc Ph,);1im;d.
,,hich is equal lo I d) .s·\:111�. II' the lluiJ h,1s a\ iscnsity or 0.20 poi�c. 1.:akulah; lh, ,,.1�:r, kg: ri2 "o.m� 1112 : h ,.- Ml• 110 s: atm.-.;" l.ill>2::i><IO' Pa,
the eorr�·spitnJing rnlu,· in SI units (.l'a·s). Suh,1i(l1ti11,! the \.ilu,·s in the i:qu.itim� i;i\es:
Solution: D,11a ·-Thc unils an::
lh·:n, ·I OA5J(, kg·mol
dy.s g
1'1,ise "' h·ft:'.,11111.

as:
Visco:;ity -- l>;1·s ., .,
s-·m·
.
·:,·m
1.337 • I !l s k :! /111:·h·l\1.
·1 h,· 1'1l_ll\l'I"Sinn fa,·tor J"nr lhtJt2 ·h·alll1. - 1,3]7
I X 1011 kg/m 2 ·i;·J'a.
The 'conversion fartor cun he cletl.'rmined as follo\\�. l'rnm 1hc l'llllV 'r�ion l
Prartirt· l'roblrm t-.i. Th�· 1wcrall rn,·nil·ii:11l of hl.'al transl°l'r is 100 Btu/
Table <.lf AppcnJi\ Ill. thc folh111 ing fact,irs arc ohtaitwd.
ldt�-1. ( 'omert the same into SI units l\\'/m 2.K].
I g =- (1111100) kg; I cltl = (I ii 00) m:
Solution:
By substituting the ahm e terms for units· Btu
(1/1000) kg 100 kg I kg n1,· �ii ,·11 units 111" into units or
- ·---- ·--·-- · -- ··---·-··-· --· � ·--·-··-- ·· 0.1 kg/m·s h.rt 2 · I- m2 ·K
cm.s S"-(l/lOO)m IOOOm><s IOm.s I Ii.· 11::1\ ,·qui\.ilcnt in SI units is .I/,. 11hilc .l.'s is equal w' \\'. Therl'l·orc, J/
0.10 poise ,.,. 0.2 " 0.1 Pa-:-. =· 0.02 P.i·s \ i, l'l>n,i,l,•1,·d in pbce of\\' for Phtait�ing l lll\Yl'ISiOn factN.0

Practice Pro1?,ltm 1-2. The density of tak is reporh:d as 2.7 glml. Expn:ss Btu .I
·10 .
the same in SI system (l..g/m 3 ). . . h'.ft�.°F s·m�·J..:
Solution: The given unit of lknsit) is g/ml is to he conn:rteJ lo 1..glm\ g/
ml is abo equal to g/cm 3 • From _the comcrsion Table I of Appendix I'.:. the · l rn:11 th-: l'Pl1Y<:rsin1l (;1!1ks I & � or :\pp,·ndix Ill. the r11lhm inr, rl'lntiOt1•
follow\ng factors urc obtained. ,hi 1 1s l'.111 b,· llhl;1i1kd.
l 11111 · I ll'i) I, IO' .1: I h .· (,O , <,Os: I r1 2 1>.:.? 1)(),; 10:� m�: 1 ··1· ,. ( l/1.�) I'\

'
 °
16 l'l l!\Rl\11\{'l:IJ'I ll '/\1. 1 ·N1 ,INl·.ERIN()
('h, I INl>lJSTl(l!\I. l'IWC.'1:SSIN<i ASI> ll!\SIC l'IUNCll'I.ES 17
Suhslitulin;; 1hc abm I.! Cllll\ .:.·�i,m laclors i11111 lhc ahn, I.! l.!llUati1111 �in:s: .
Btu 1.05:-1 • 101 .I The dimensionless equations arc derived from basic laws mathemati­
-······-- --·· ·----- cal�y. no matter hq,weyer co111plicated they may be. An equation .in
h.n2·''F 60 , 60 , 9.290 x w-· 2.1/1.8 s·m1·K which all terms have same dimensions is known as dimensionallv homu-
1.0551 .: I o3 .I " 1.8 18 1)9.18 J g,•11co11s eq uut irm. ·
-· ·----·· --------
- F
3(,op ·· •J.2•Jo " 1w·2 s· .m:·K :,.,4_.t,1 vm2·K ror example, consider -equation for Reynolds number._
,
S.6787 J.'s·m.2·K
Si1Kc .Ii� ·.. W. it c�n be induJcJ in lhi: .ihl>\..: ..:,pr.:s�1011 to g.:I 11.i1ls :'i.<1787 Dup
w:m = ·K. rhi:r..:l'or..:. th.: convcr�ion fo..:tor "' 5.67X7. Re = --- (9),
17 • t -;.
200 Btu h·lt:: 0 r .; 200 " 5.<1787 Wtm ::! ·K
.. {
1135.74 Wfin 2·t,.;, where D � <l.iai11eter of the pipe, m
--··---------
II = Ve)ocity of flow , 111/s
DIM.f.NSIONS-FORMULA E, EQUATIONS AND ANALYSIS p = d�nsit�· of the fluid, t�l.1113
;·
. °
,, ".' \'ISCOSl!y of the fluid, Pa·s
Dimc,,t'sional Formulae
Consider the units iq !l�e numei-ator in equa,tion (9)
. :1 di111cmw1w/ .fcm11ula is a .formula that explains the ,v�1y in whid1
fundamental units c11tcr into the opera�ion. ,. ,i, m .,.- .. kg· . kg ·
Dup "". 111 x -- x -- = __
· . Dimensional formula expresses the quantity in secondary units. For
example. the dimensional formula for acceleration is:
·s ·
.m3 · s·m
Consider the units fo th'c' dcnon�-i11a1ii-' in''-�qJ�tion (9). •' · ,,.
. r-· . .
[u] "' 1-t :. (6) I"\" I ·)

-� lt!i1gth •. tin1c··�- Jt
, J 17= • Pa·s-
' . .. ,
i' (.JO)
Since, Pa "" kg/m:s2 ; it can be stibstit'uted -in equation (JO
Equation l6) can be explained a:. follows. Accekration i� d,·linc.:d as . )
velocity per 1y1it kg x s · .. ·. kg
. . time.
-
\
. .-·- = ---
1/.fj,-
wlocity Ill x s2 . m·s
[uj "" ---------·-· (7)
lime Therefore, equation (9) m�y be, written as:
Velocity is· defined as a distan·ce per unit time. Therefore, accelera- . kg/in·s. Jo "(
tion can be written as: ;-�c = -·'� =.=; dimcns'ionlcss nuinber' ·'
kg,'.'m·s· ... 1 . ·
,:'\ . , ·, . ; . ,•;
bis tanee· {length) �;. . -\,1, . ,; � ':1'
Hcn� e cquatiqn,.(9.) i� <;�i1sidcrcd as dimensionless equation:
.

["J "" --�'-----·

. ··--- ·- - "'' I·r·, (8) .
timl! .. time
ti "

. C�nsi?er another. equation as'� var·iatio11. For exartiplc, fa!Ehg of

. '
a
The symbol [al means the dimensional formula ol' tht: quantity of ·a·. body Ill tune, t, can be expr sscd..as:
• ' ;. I. �• '. .
0
·' . � "
Applications : Dimensional formulae arc- used in order to convert the ·'. S =LI{+ (1/2)gtl (1 J )
secondary units nf one· system into another. In these cakulations.
conversion factors arc usc.:d <.:trntiously. Then. the.: physical quantity is where S"' vertical distance. length
obtained in another system. 11 == initial velocity; distance/time
t = time
g = acceleration due .to gravity, distance/tin1e2
,,
 .; -. ' 'I

C:h· I INl>.lJS'I KIAi. l'ROCESSINCi AND BASIC �'RI NCI Pl.ES 19

18 PIIARMACEllTIC. .\ I. FNGINEFRIN<, ' :rhe quantit.ics substituted for the terms m,ust be expressed in the
units mentioned above. For cxa1�.pl. c, D '0 may be substituted· only in
In eq,uation (11), first and second terms arc �xprcssed separ:llcly as
inches. not in feet. ..The reasons arc'that the numerical coefficients such
follo\vs:'• as 0.5, I .2S and 0.25 arc applicable for those units.
' , . • •.,, r'
Iii = velocity x time I , distance (length) . ,, The disadvanl'agc of 1l1is equation is that it h'as limited ..appJjcations.
--gt· = -----·--:--.,-- x hmc- 11 . is particularly used for calcul�tions of a system under specified
distance (length) 2 t1n1e-
- ----·------.. x time
= conditions. ·.
time
Dimensional Analysis
'.= distance (length) = distance (length)
In the pharmaceutical engineering; many physical problems have
'Each term has the units of hmgth. Equation ( 11) can be niadc bl:en solved compktcly by theoretical and mathematical methods. On
dimensionless by dividing by 'S' .. . the 9thcr hand. there arc still many situations whc.rcin e1npirical relation­
ut. I , gt2 ships have been established over a period of time;.. sinGe theoretical
I== --- + - • -� ( 12) rdationshi i:Js have failed to satisfy experimental results. Common exam­
S , 2 S ples rel.1ted to these problems �re. - 'tluid !lbw, heat flO\v and mass
I
.
• -

t1a11sfer. ' ·
I

ln cquatio11 ( 12), the dimensions get cancelled and each term is

di rw::ns; 0,1 lcss. Dimemioiwt ww/ysis is an important tool to convert the empirical
·0· ! he ad,·antagcs of dimensionless equations are: r..:!ntionships info tl11.:ordical principles on a ratio1fal basis..
l. Unit of any system (cgs ·or fps or SI) can be used �without Dimensional ;u1alysis assumes that there must exist a relationship
0

introducing conversion factors. For example, length in either ;11110ng all ti1c factn,:s· affecting a process. This technique involves the
ini:t;·cs or feel can be .substituted in equation (Ii)'. l\1l lowi11g steps. , . .
2. :,:);m,;ntionless equations arc based on the;1retic:1I principks. They (I) All the, fac.:lors arc to be identified, which arc important in the
Cl1nta;11 variables affecting the physical pr0ccss. problem. Initial stages. empirical _ relationship may be adequate.
(2) These Ja(;tors aic grouped t�g<;ther into fewer numbers and
Dir:�cnliionai Equations expressed a� dimensionless gr.oups.
,)1111rnsio11al equation is defined as an equation, which contains (3) Such gwups arc entered into final equation. ,
term:; of varying dimensions as it is obtained by empirical methods. (4) Such equations arc correlated to the possible physical laws.
Experimental results are correlated by empirical means. Therefore. (S) A possible mathematical solutio1� is obtained.
dimensional consistency is ignored. Such equations are also known as
In the above annlysis. the first step is to consider the units for the.
a'imrnsionally ,non-homogeneous, eq11.ations.
\'erilicalion of factors. For example, .in the experiments on the fluid
For example, the rate of heat loss tby conduction and convection) llow, the factors involved are listed belo\V....
a
from horizontal pipe to the atl,Tlosphcre may be written as: - pipe diameter (D), m viscosity (11), Pa·s
qc (,1iJl.25 - velocity (u). mis density (p), kg/m3
0.5---­ ( I 3) These factors arc vari,cd as Ol)C · at a time. Then the results arc
A (D'aJ°-25
combined. It is shown by dimensional analysis .(hat these factors must.
where qc = loss of heat, Btu/h appear in a dimensionless group as shown' below.
A = pipe surface, ft2 ...::,
Dup m kg I. 'kg m·s2 ·kg .
.dis= excess of temperature· of the pipe wall over that of atmos­ nr m-•--•--.=-·- =
---
phere, °F '·' s . m3 Pa·s s·m·Pa n::s2 ·kg 'I I
''
D'0 = diameter of the pipe, in

·,I'\;

20 Pl IARMACEUTICAL ENCilNEERING
This equation is expressed as Reynolds number. which has no
dimensions. This example illustrates. the :;ucccss of the .. dimensional·
analy�is.. But heat transfer experiments on fluids involve about 11 ·
factors. A total of five different expressions arc obtained. Still dimen­
sional analysis could provide ,a satisfactory equation to describe the heat
transfer process.
Ad\'antagcs : ( 1) Dimensional analysis reduces drastically the number
of independent variables that effect the problem.
°
(2) This analysis does not yield numerical values in the eqµation.
. .
(3) 1 This helps in' constructing dimensionless
. '
' . (dimensionally :·homo-
, ' geneous) equation. �-.
· ·(4) · Very useful for any system of units (cgs or fps or SI).
. Disadvantages : Dimensional analysis is a difficult process, if enough
kn�wlcdge is not available about the-physics of the situation.
STOICHIOMETRIC EQUATIONS-BALANCING
' Sioichiometr.1· means ·carrying out of calculations base.d on quantita­
tive relationships.
The numerical problems involving the use of stoichiometric equa­
tions are known as stoichiometric calc11/atio11s.
A chemical reaction is a symbolic representation of a chemical
change. Each chemical reaction is expressed in the fo�m of an equation.
This is obtained by balancing the atoms of each of the species involved
iA tl)e reaction. The initial constituents that take part in the rea�tion arc
called the reactants, and the final constituents that· are formed by the
reaction are called ·the p,;oducts. For exa!11ple, hydrogen and oxygen
react to form water. This reaction is expressed as:
( 14)
In -equation ( 14), two hydrogen atoms are present on each side. On
the left side, two oxygen atoms are present and . on right .side one oxygen
atom is present. Moles can be multiplied or divided by smallest possible
integer .to obtain a balanced equation. Hence, equation ( 14) may be
balanced as:
H2 + (112)02 � fi20 (1 S)
Balanced eqttation: 2H2 + 02 � 2H2 0 ( 16)
E4uation � 16) indicates that one mole of hydrogen and half mole of
'h·I INl>llSTRIAI. l'ROCTS�INU AND 11A:-;IC l'RINCIPL.ES 21
oxygen combine to form one mol.e of water. . The reaction· may a�so
, takes place in reverse direction. _The 9oefficients 2. J and 2 in equation
( 16) arc call·ed stoichiometric coefficients. ·
· . · . . ·· . · , . , '
Accor�ing to . the law of conservation of mass, total mass of r�actants
must be equal to the ·total mass of products in a reaction. In other-words,.
the number of atoms·of each kind in the reactants �nd products must be
the same.
A balanced chemical equ�lion indicates the exa�t number o� various
clements participating in the reaction. ·
Balancing is done by inspection. Balanced chemical equations arc
/quantitative exprcssi�ns of chemical changes. Hence, they enable us to
work out the inasses of substances reacting together. A few examples
arc given below.
Applications : (I) Stoichiometric equations (and balancing) helps in
understanding the quantitative relationship between different re­
actants .. For example, the ratios 2:1 (equation.1'6), I :I (equation
14) etc.
(2) The amount of reactants to be added for carrying out a reaction
can be .determined theorctica'II�.
Practice Prol>lcm 1-5. Nitrogen combines with hydrogen under 'suitable
rnnJitions to form ammonia. Writc the e4uation and balance it.
Solution: Nitrogen and hydrogen arc bi-atomic molecules. The formula of
ammonia is NI 13. The reactant� and prodt11.:ts can be written as:.
Skeleton equation: N2 + H2 � fHi (i)
Nitrogen atoms on both sides of equation (i) can be balanced by multiplying
N! t1 by 2. In the next step, hydrogen atoms can be made equal both sides by"
multiplying ,,H2 by 3. Now, the balanced equation becomes:
·"
-->' 2NH;
'
Balanced equation:: N2 t JH2 . (ii)'· • I
Practice Problem 1-6. Carbon combines with. oxyg1..'ll to give carbon
din,idc. Write chemical e4uation a:1d balance it. ..
Solution: Carbon normally' exist� if\ mono-atomic state (('). Oxygen exists
as diatomic {//2). Carbon dioxide is"reprcsented by C0 2. Then the skeleton
equation may be wriitcn as:
Skeleton equation: C + 02 --) C02 (i)
lhc number of clements prcscn.t •on the lcft�hand side of equation P> is
·qu.11 tu the tight-hand side of the equation. Therefore, balanced equation
· is
t1111c �,s the skeicton equation. ·
 l"h· I 11'l>llSTRlt\l l'RO<:I \SIMi t\1'!) llt\SIC l'RINCl!'LES .,_.,...
22 PHARMACEUTICAL ENGINEERING
5.U g of J.:(103 yidJ "! g of ,)xygcn
Practicr Problrm 1-7. Write the balanced equati{ln for the combustion of % x 5.0
ethane. -·----· ;= 1.958 g oro,yg,•n
245.2'
Solution: Combustion means complete oxidation of a substance in the
presence of air (oxygen). The products of combustion arc normally carbon lhc mass of o,)·gc1�
, ohwincJ. is 1.9;8 g.
dioxide and water. Therefore, the equation of the comhustion of ethane may be
·written as: c;1ou:1ry of �)·nillols
. I , l'i1�c suri"aci;:. fl:
(i) cgs ... ("cn1im,·1re:gr�1111-scc1111d.
I) •= l'ipc Jiu111c11:r. 111.
0

On. the left side of equation (i). the number of carbons is tm�. while on rigl�t
11 ,_. Viscosily. l'a·s.
hand-side the number of carbon is one. Therefore, multiply C02 by 2. Then.
equati6n (i) can be changed with respect to carbons as: F ,. l>rivin� force.
rps "' Fol',t·po11nd-sco.:onJ.
(ii) � •= ,\ccclcralion Ju,· 10 gra,·i1y. mis�.
' u ·� �· "' 1'fokn1l.ir \\ cighl or indi, id11al ,omponcnts.
On the h:ft hand-side of equation (ii), the number of hydrogen atoms is six. mks Mcln:-K ilogram-sccond.
00

11 ••• N11mlwr ,·,r 111oks.

while on the right hand-side, hydrogen atoms arc two. Therefore, multiply 1120
by 3. I!.wn equation (ii) changes with respect 10 hydrogen as:
I{ � l{csi�1ai1cc.
(iii) R = Rankinc.
p - D.:nsity. kg:'111 3.
On- h:1: hand-side of, equation (iii), the number of oxygen atoms is t\\ o. S � Vcrlical Ji�1ar11.:c-. m.
while cm the 'right hand:side, the oxygen atoms arc seven (3 + 4). Therefore. SI � S) sh:llll" !111·:rnatinnalc. ·, j
· multiply 02 by 7/2. Then, equation (iii) can. be changed with respect to 11 �, \' clncity. mis.
hydrog�n ..is: l � ·, inH�, S,

(iv) \\ · \\'.:i.ghl 111" inJi, iJ11al rnrnponcnts.

The 1:quation (iv) is balanced. But fractions can be removed by multiplying <� I'\
•

the entire equation by 2. Then, the balanced equation is: .. Qll[Sl"IOl'i BANK
Each question· carries 2 !!larks
(\ )
( I ) Dcs1:rihc thc principle of stoichiomc1ry with a suitable exrn11plc.
The above examples illustratcJ the methods of balancing chemical '-'qua­
· (2) I Jirhl ight .thc import.ince of unit opcralions in pharma1:cuticJI engineering
tions. _
(3) De:;crihc 1hc molecubr 1:onccpt of .s1oichiometr):.
Practkt Problem 1-8. Calcuiate the mass of oxygen obtained by the
( 4) ( ,i, c an e.\pression lo calcula!e the a\'crage molecular weight ,if a mi:,.turc.
complete decomposition of 5.0 g of potassium chlorate (K = 39.1; Cl= 33.5; 0.
= 16). ( 5) I low is the r.iil' of .i reaction. expressed'!
( C, J Distingubh b,·t"·een �lcady �_wtc anJ non-sleady stale.
S�lutlon: The equation for the given reaction ma)· he writtel1 as:
� . ( 7) Distinguish b1.·1wi.:en cquilihri11m ,.md s\cady stale.
KC/03 � KC/+ 02 (li) lklinc thc 11.:rm :dinll'nsionlcss cquution· with the help of an e:,.amplc.
13:ilandng of equation can be. with respect to the number of .moles of ( ')) lkf1ne Jimcnsionul equation. What arc its limitations'!
oxygen. l 10) Dl'line thc lcrm 'Jim.::nsionlcss equation'. \\'h.it arc its ad\'alltages'!
2KCI03 � 2KCI + 30 1
Earh 1111cslion carries S marks.
.
In ,pther words. 2 moles of.KC/0; >·ield 3 .mole$ of oxygen. (I) l>cscrihc ·11nil op.:raiion·· and ·unit process·. Give 1wo C.\amplcs c,ich.
. "
2(39.1 + 35.5 + 30 6)) g of KC/0/yields 3(2 x 16) g or ox men
> •

245.2 g of KC/03 yield 96 g of oxygen

l'
 1::
24 PHARMACEUTICAL f:NGIN'4f:PJNG
(2) Explain the term 'unit operation·. Dcscribc the
basic principles of various
unit operations used in pharmaceutical and other assoc
iated industries.
(3) E,i:plain the term 'mass balance' and 'energy balan
c�;. What arc its
. applications?
(4) Give an account of unit systems and their inter-conv
ersions.

; !.))
 .,,,,·

2
'. .. '
• , ,I : i'.1:,.',•

Flow of Fluids·

Fluid Statics
Fluid o'ynamics
Bernoulli's Theorem
Energy Losses
Measurement of ·Rate of Flow of Fluids··,

Fluid flow may be· defined as the· flow of su�stances that do not
. permanently resist distortion.
This definition cove'rs 'the no,v of liquids and ·i;iascs. Fluid is
consider�d to be a mass ·of a substance·: formed by a series of l�yers.
\Vhcr1 a� attempt ·is.made ·to change its shape, the layers of fluid slide
over one another, uriiil a new shape is attained: At the �nd. the fluid is .
· reJieved. off-the stresses that it encountered during the .flow. -
Flow of fluids is observed while handling inateri'als.
(a) Handling of liquids : Transportation of materials sucih as sol­
. . vents, solutions and suspensions is simpler, cheaper and less
·, troublesome than handling of solids in 'industrial operations.
(b) Handling of solids : Solids are handled in a finely divided state
in the form of suspensiol') of fluids, so that transportation
becomes �a'sy. This t\�o:.phase mixturr, is known as 'fluidised'
_ .
soltdr . · 1 - • . .

During ihc handling process, the behaviour of liqurds·. changl?s

transient)){,. Such changes have profound influence on heat transfer
irocess. energy losses during pumping, energy chang"'i in pumping etc.
Therefore, 'fluid flow is treated' i'n<lependently.
Flow �of fluids ls in�olved :in.�- ·�u�ber �f areas 'of pharmaceutiql .
inciustri.es. Som� of.thci11·are:
'

Passing ,,f rcac,!..\nis (li4uicJs m &!L'>�S) into the reaction system.

. ' • :, l;\�.J ' .

Transferring of air, nutrient hroth into the fcrmentcr.

IJottling of liquiJ (dosage forms) medicaments into suitable containers.
• I

25
 26 l'l l,\RM,\tTl1TI( ,\I. l:NtilNITKl'.,1 i
Ch·2 !'LOW OF FLUIDS 27
Transporling of st.:rik air and �h:rilc \\ah:r in 1hc prmlu..:tion or p;1rcntcr;d�.
M·i:>.ing or �olids ;ind liquid� in ca�c of susp�n�ions. Let the cross-s�ction of the column be S metre squar.e and is µnifonn
l'ackin:;. of s.:misolids in containers. · from top to 1 bottom. The force lfurther pressure) acting on thi: liquid at
differellt levels of' he liquid column ca'rl"be· determined. •The forces
The :1atun.: of !low inflw.:1wcs the type of equipment" used for lw1-.
dling. Fluw d1aract�·ristics through pipes and d1anm:!s an.: rdcvant. 1\t (newton) acting on each side (horizontal components) of the point 1 are
the same lime. the 111casurcmcnt of rate of flow is ncces�arv• for the mutually nullifi�d. The forces in· newtons acting below and above the
quantilic.ition of a'dt..!itivcs (r�actants) into a prnn:ss. point 1 ·arc evaluated. . i ,1
The subject or lluid flow ran b.: di,·idecl into lluid statks and fluid Force acting on the _. force on the surface + force exerted by
dynamics. liquid at point I ,.... · the liquid above the poinf l ( 1)
Fluid statics di.:als with fluids at rest in equilibrium.
- Fluid ,�rnamics dcills with lluids in motion. Substituting the force with pressure x area of cross section (S) in
If
, equation (I) gives:
I
FLUID STATICS Pressure at p_oint 1 (Pressure on the surface x surface area)
x_ surface area - + (mass x acceleration) ' · (2)
·' Fluid statics dcab with the fluids at rest in t.'quilibrium. Th,'. bd1av­
iour of a liquid al rest, the nature of pressure it exerts and the .variation
P 1S = P� + volume x,'density x acceleration due to gravity
. of pressure at di(forent la)'crs in the liquid arc some of the relevant
=p � + height x area x density
aspects in the pharmaceutical cngin1:cring.
x acceleration due to gravity
P�essure Difference Between La)"crs of Liquids (3)
, . Consider a column of liquid as shown in ·Figure :!-l(a) .. Two
openings arc provided to the wall of the vessel at different heiuhts. · The Sine<; cross sectional surface area is °'same, equation· (3) ma;' be
rate of flow from these openings is different (figure 2-1 a). T.l1is is due written as: J'
to the diff/rences in the prc�surcs exerted at different heic.hts.
� This '(4)
behaviour can be quantitati,cly expressed as follo\\s.
Similarly, the pre�sure acting on 'the liquid at point 2 may be written
Consider a stationary column of lluid as shown in Figure 2-1 (b ). The as:
pressure Ps pascals is acting 01_1 the surface of the fluid. The st:-itionar,· (S)
. column is maintained at constant pressure by ar.pl>·ing prc:.surc, i,
t: pascals at point A. , The difference in the pressure may be obtained by subtracting equa-··.

-----t
tion ( 4) from equation' (5) as:
Ps

=- =-=--:1�·
t
- - -- --
--
----- .Pi - Pi= g <Ps + h2p) - (I's+ h 1 p)g.

----- -- t1P "." (P� + hjp - Ps ..:..1,1p)g

-------
nP = (hi- h 1 )pg

-==-=-=-=-= ·1·�
--=------ '.�..
\.-\ = &,pg (6)

- --{ 1:�-_----
.�---=-=-=-- .J...rt;;.:.
_�
--=. =
- Therefore, the pressure difference (4P pascals) between any two
t,:;-:!�

-=--=�--=-
------�
- -- --�=
points can be measured by the distance,between those points in a fluid.
If the density of fluid (p kilogram per metre cube) varies with variation
of pressure, an av�rage density could be. used. The variation in densities
(a). (b)
is quite negligible for liqui<:ls and ·gases. Since the difference in the
Figure 2-.1. 1 lydrostalic pressure ohscrvcd heights (Ah metre) is necessary for the measurement, height can be
al diffcn:nl byers of a stJlionary. co::11nn.
measured from the bottom of the stationary column.
28 l'I IARMACEUTICAL ENGltJE�RING
( 'h·2 Fl .1 )\V OF FLIJI DS 29
Applications : The principle of fluid stati�; '"is· employed in the
working of manometers. In such cases, the pressure difference (&') is Pressure at point 2 = P J + (m+R)P11g (7)
measured in terms of difterence in the height:;,of the liquid column. It is
also applied for quantificatio, n or fluid now as in Bernoulli's theorem. where (m·I R) = distance from points 3 to 4 + distance f om points 4 to 5. r

Since. points 2 and -:; an: al the same level, the pressure at point 3
'Mano,mctct's may be \\'rittcn as:
Mano'n1etcts are the devices used for measuring .tii'e' pressure differ-
ence. · Three different manometers are available. These are: Pressure at poi11t 3 "° P 1 + ,(111+ R)P8g (8)
I . Simple . ,, 'if
The pressure al point 4 can be wrillcn
· from' the right hand-side of the
2. Differential
limb (f om P2) as:
r ...,
3. inclined ,, ·�
.
The principles and applications of these manom�t�rs arc discussed in Pressure at point ./ = P2 + gmPH ( 9)
,
the following sections.
J

In another manner, the pressure at point 4 can be written from point 3

Simple m'anomcter : This :inanomc'ter is the most commonly used'. (i.e.. from left h:rnd-side) as:·
The construc.tion of a simple manometer is shown in Figurd 2-2. It
Pressure at point 4. =; P 1 + p8 (m + R)g - P,1Rg · · ' ( I 0)
consists of a glass U tube ,filled with, 1 a liquid (A) of density, PA. '
' f. f' t "'. .

kilogram p..:r metre cube. Above liquid A, the arms arc filled with liquid Equations (9}and (I 0) represent the pressure at point 4 only. Hence,
B of density Pn kilogram per metre cube. The liquids, A and 13 arc these eqi1ations should be equal. This relationship may be ·,vrittcn as:
. '
immiscible and the interface can be seen clcirly. ' .(• ' '

I' J + gPu (m + R) - P,1R g = P2 + gmPo ·,

If two different pressures' arc applied on the two arms, the meniscus
of liquid. A will be ·higher in one arm ·than the other (Figure 2-2). · Let I' I - P2 = gmPo '- Pe (m + l})g + P ,.1Rg
the pressure at point I is PI pascals in left hand-side of the limb.. Let , '.1P = mPn:s - mp0g - Rp8g + NpAg
the pressure at point 5 is P2 pascals in ,the right hand-side of the limb. LlP = R(P,1 - p8)g (11)
From the prjnciplcs of fluid .statics, the pressure at point 2 can be written
as: ll The important conclusions drawn from equation .(11) are:
/ ( 1) It is easy to measure R value (metres), i.e., the difference in the
5
1 levels of liquid A in the two limbs.
(2) The value .1P pascals is independent of the valu� of 1i1 and also
liquid the dimensions of the U.tube.
B
When wide ranges of pressure are applied, the sensitivi,ty of liquids
·' employed in the measure1ri_en·t is important. If the pressure differences
are large. mercury ·(high density, liquid A) can be used as manometric
liquid. If the pressure differences are small, liquids such as alcohol,
water (for gases) and carbon tetrachloride are used.
Applirntir!n.c (I) Simple manom'eter helps. in measuring the con­
sum pl ion of gases .in the chemical reactions. (2) Manonieters are used in
' I
conjunction with flow meters for the measurement of flow of fluids. For
exampk. \'enturi meter and ori tice meter are used for the measurement
ltquic:t' A or pressure head using a manometer: Pitot tube measures the velocity
I . ',
Figure 2-2 .. The �ons,truction of simph: ma.nomi:tcr. he:id using a ma;1ometer.
 '•1 I
'
30 l'IIARMACEUTICAL EMil:-.IEERIN(j,
I
Ch-:' Fl. OW OF Fl.lJIDS .:; I
l>iITcrcntial nrnnomctcrs : Differential manometer� find occasional
applications. This mano111c:cr is suitable for measurement of small lnclinl'd manoml'tcrs They have limited applications· and. thcre­
pressure \;liftcrem::es. It is a sensitive dcvic'e and useful for measuring t f-\'.;
.'ron:. not discussed
·. ... here.
evt:n small gas pressures (heads).
The con'.>truction ofa' differential manometer is given in Figure 2-3. 'fLlJl'o DYNAMICS
The differential manometer is also. known as 1wo-jluid U-tuhcJ 111a11cJ111-
elcr. It rnntains two immiscible liquids A and 8 having. nearly samt: ·. Fluid c(nwmic:s deal'S with thl! study of fluids in motion.
,,1 , I , , , •

densities.. The U tube consbts of enlarged chambers on both limbs. Study of llow propcrtiC's of liquids is important for pharmacists
I lem:c. the 11h.:ni:.rn:. of the liquid in these enlarged chambers docs not �rnrk ing in the manufacture! of dc>sage forms, such as simple liquids.
change appreciably with changes in the reading R. gels. oiniments. creams_ and pastes. · These sy�tcms d1angc their flow
Using the principle:of simple 1na·nometcrs. the pressure difference h;.:haYiour. \\lien exposed to difforcnt stress conditions in the following
. situatioi1s.
(.:1/' p.tscals) can be \Hillen as:
I

(I) i\la nu facture of dosage forms : fvtaterial:;; un�crgo processes

. ( 12)
· such as mixing� llowing through pipes and getting filled in the
. Equation ( 12) ir1. �icates that the. smaller the di !Terence (Pc -- P,1). the
larger will bl! reading on the manometeri(R metres) for a given value· of 111i.,inti equipment.
.
co11t:1in�·rs. flow rel,\ted · changes influence
'
the selection of

,1? ..
I , '
(2) Handling of drugs fqr adnJinislralion : The syr,ingcability of
Mi.crnn1a11orneters based on ·the liquid column principle! :.m: available the m�dicim·<,pouring .of the liquids. extrusion of l1intmcnt from
commercially. They measure \he reading with cxu:cme precision and tubes· etc;, depend on the changes in flow behaviour or dosage
sens1t1 \· 1ty. Th<.:sc are free from errors due to capillarity and rcquire no forms.
calibration. apaJ't from checking t�e micrometer scale. Titus. !low .behaviour of liquids is of relevance in .pharmacy. Per­
fonnancc ,,r
.a product depends on the net <:fti:ct of all the! above
Pz mentioned processes. Therefore. flow properties arc! used as· important
• 7
quality .contnil tools to maintain the superiority of the product and to
reduce the batch to bat�h variations .
. 'In general. ehgincering of fluid tlo\v considers the macroscopic prop­
-·-; erties. The molccullr level interactions ·arc beyond' the scope of this
book (Refer the book Physical Phartuac:eutics by C.V.S. Subrahmanyam.
Va.1 labh Prakashan).

Nature of fluid flow-Reynolds Experiment

The flow of fluid through a c.:losed ch:rnncl (pipeline) c�n be either
viscous or turbulent. These can be observed in the classic�I Rt:ynolds
3
experiment.
Tlw assembly oT the apparatu� · for th•: Ri;ynolds �xpcrimen! is sh own

Figure 2-3. Construction of a differential 111a11,11nc1cr.
-
111 Figure 2-4. l.
-
i\ l!lass tube is ccm11ccted to a ·reservoir of wati:r as shown 'in fi 1.: urc
2-4. The rate of !low of _water through the tube can be inc.reased�or
decreased at will through a valve. A i'eseryoir of coloured solution is
connectl'<l to 011e end of thc glass· tube with the .::help of .noz.zle(s). •,, ,
Therefort'. coloured solution can be introduced' into the glass,tube as n
 / ,'\ ·. ;:-:;:t,;fii�,...
32 1'11/\RMACEUTIC/\L. EN<ilNEl:RING
·' / Ch-2 FLOW OF FLU.IDS
tine. stream. From this experimental setup, the following observations
When the flow attains a certain velocity, .it. no longer remains
may b e made a·nd conclusions can be drawn. .
. . . steady, a_9d edd� -currents. �ppear. Al I the O�id p\lrti�lcs· aw d isf�rl?ed
(a) When lhc velocity of water is low, the thread of coloured water and get mixc� up wi91 each oJhcr. !hus, th.ere is a �ontiAuo�s tr�nsfer
maintains its identity throughout the tube... _By i.ntroducing similar jets of of momentum to adj_acent ,layers. Such a diffused floY<'. is c�\lcd wrbµ-
•
colour.cd water at c!ifferent points in the cross section _of the glass lube. it lent flow. · .. : . . ' ".:l ·,.· · · · 1.
can be noted that no part of the tube exhibits the signs of mixing� 'In . ... . . 1, .
' t
•(c) The change over of ·the flow' froin vistous .·to. turbulent is a
p ' � '

other words,. the colour streams are seen as parallel lines. The flow of · ·
. critical factor.
' ' '?•
• ' ,f· " ...,,. -- i· ' ,_.' •
waler is considsr,cd to be viscous or streamline or laminar.
1'.l
• · · · ' •. ·
• ' • • t I • ' { I' t{

Critical velociJy
,,
is defined as average ,velocity of any fluid at which
' '1 I ·•••' . .
viscous flow changes into turbulent How.
Reynolds. number : In Reynolds experiment, the flow conditions arc
affected by four factors.
t ' • ' ''

Diameter of pipe, m (D)

; '
, Average velocity, m/s (1 11) .,
· Density of liquid, kg/m3 {p)
Coloured Viscosity of the fluid, Pa·s (I/) . ','',
water
These .factors are ,.'grduped into·: a particular .expres'siotf as given
below. .. ·rt
i-r J · '·411P
Reynolds ndmber, . Re = --· (13)
Coloured · Glass
1J
liquid jet. tube Reynolds .number is obtained by tne follo�ving,equation. · ··
(a) Laminar or viscous flow.
•.c I, • •:. mass X acceleration.
. ir1ef1i�I forces 10, of Eci�id flqwing
Reynolds number, Re = . . .
v1s.cous forces
1 -.=: ----·-----
shear stress x' a'rea
' lie" .
1 1
Inertial fotces arc. due to mass
t
and. 'tne'veiocity of the fluid partkles
trying to diffuse the fluid plriclcs. The visco'us .force is the_ frictic1nal
force dlfc to the viscosity of fluid, which makes the motion of fluid in
(b) Turbulent flow. parallel layers. .· · • .;, ·- .. · � · ...:: · · .J · " . '
'

Figure 2-4. The assembly of the appatatus of the .Reynold's experiment. Therefore, at low velocities, the· inertial forces· are less when com-
pared to the frittiotial forces caused by the viscosity::. The resulting flow
A iami,iarjlow is one in _which the 11uid particles move jn layers or
·\Vi11 be viscous in hature, Le.; the partic.les move in parallel layers. F9r
laminar with one la>•er sliding over the other. Therefore, there is no
this reason laminar flow is Scil�"!times known ·as viscous: On the other
exchange of fluid particles fr om one layer lo the other. Hence, tran_sfer
hand, whc� inertial forces ;;�e pr�doinina�t, the fluid laye�s break �p due,,
of lateral momentum to the adjacent .layers is not observed.
lo the increase in velocity, hence, turbulent flow takes place..
(b) When the velocity of waler is increased (by increasing the flow It is a dimensionle�s group, be. cause ·,he.units of fa'cto·�s mutual.ly get
rate), the threads ·or
coloured water disappear and the entire mass of cancelled. If Re< 2000, the·flov,; is said to be laminar and if Re> 4000,
water gets u'ni formly coloured.
\• .. It· indicates complete mixing of solution. the flow. is said to be turbulent. If Re fies between 2000 to 4000, the
Then, the flow of water is considereµ t.o be turbulent.·
. !low changes from l�minar -to turbulent.
/
I
34 PHARMACEUTICAL ENGINEERING
1
Ch-2. FLOW •OF FLUIDS 35.

:. .Ap;licat-ions : (I) Reyno,lds nulnber is used. 'to prcdi�t tH� natJ're of Since the velocity of the fluid is zero at the �/11 surface, t!'\ere
flow (viscdus or turbuien\) in a particular .s<;t of experimental tdnditions. should be some layers in viscou�Jlow near the ,pipe-wall, .which
(2) The physical stability of suspensions (or emulsions) depends. on ·:the acts as. a stagnant layer.. l
rat�'of settHng ?(particles (or globules). For the study of sedimentation Even if the flow is turbulent at the 'centre (of the ' pipe) . . . .and
� •\i•'
viscous at,Jh'c surface ,of the!' wall, a bum·r layer exists.·
of particles, Stokes' law is used. In this study, rate of sedimentation of
partJc!es
, i,"'
m.ust .not, be tQor ,
rapid-
,( ,,
,to.,,,create.
,l -.,
turbulence_I . Therefoie,
,;
type of A gradual transition from one region to another. , ihere exists a ..
flow (wh�ther laminar or turbµlent) i� important. Accordingly Stokes' boundary layer which is known as buffer lay�'r. This' buffer
equation is. modified to include Reynolds number. (3) Tbe rate of heat layer oscillates bct,veen v�scous llow and turbulent ll 0W •.
0

.
transfer_ i'n liquids also depenas �on the, flow, whether' viscous or turbu­
lent. It must be emphasized that boundary lay°er can never be eliminated.
, ,. ' ,� Increasing the velocity of the fluid over the surface will reduce the·
Variation in the Velocity of Flow Across the Cross-�cction ;r thickness of the layer, but it will be never eliminated entirely.
When the local velocity of the fluid •is plotted against distance from Applications : (I) Though the general principles; arc mentioned
the wait (Fi �ure 2-5), the,follO\�ing .conclusions can be drawn: ' ab6ve,,. considera_ble variation in velocity distribution· 'may be possible
.
-. The flow of fluid in the �Jddle of the pip· e is faster than the with changes in roughness, direction, temperature or'.cross section of the
'. fluid nearer to the wall.(·· · •. ! • • ,,J· '' · pipe. .Due to these reasons, the sl'\ape of curves may, be changed.
\ � '

-· Th¢:. yelocity\oL f]ui,d appro·ache·s· z��o as the pipe-wall is (2) The nat_ure of flow of liquid� in pipes' det!!rmines the rate. of heat
approacped. transfer. The buffer layer in turbulent flo,v and stagnant layer in -viscous
flow offer resistance to heat tr�nsfer. · Flltther discussion on rate of heat
- At the actual surface - - of the t pipe-y,alt,
�, the velocity of the fluid is
· transfer .is dealt in Chapter 5- 'Flow of Heat'.
l
, t
zero.
Since variation:; ·are observed· in velocity, of flow across the cross
BERNOULLI'S THEOREM
· section, there shoul� be some means of estimating aver�ge velocity.
When the principle of conservation of energy is applied to the flow
In viscous•condi,t.ions, the average velocity
' over. the whole cross
" .,., of fluids. the 'resulting equation is called Bernoulli's theorem.
section it0.5 times the m�imum.
Pumps generally 'supply energy for conveying liquids from o�e point
In turbulent flow,. the . ,:lverag� . v�locity over the whole cross
to anoth.er. Consider such a pump working under isothermal conditions
. syct1on ts 0.8 times. the maxnnum.
i • .1 ., , J ,. ( ' "" • .,,i. ,, �:4 \/, •
1'
·,. between points A and B, as shoYin in Figure 2-6 '. . •

' .r Pipe wall

. •

Bernoulli's th<!orem states that in a steady state. ideal flow' of an

n,,11 '

incompressible fluid? the tota,l energy per unit mass, which 'consists of
pressure e1icrgy, kinetic energy and datum energy,'at any point of the,
.. ...... .fluid is constant. ·•' ·,
� .,. . ·•. ··,1. 1·

,·· , .�
:3 ·�: +- Centr.l! At point A, one kilogram (unit mass) of. liqu_i_d is as�urried to be
0 enlcring. At this point, liquid experiences pressu�e. en�rgy, kinetic
!> 'o' t ·�
.. .. energy and potential energy, which are obtained as follows.
�..;.)/i

.•�-Viscous
.,,,,...�

� �'
- c.
_ IX .,u,
· flow Sinrc liquid is flowing through the pipe at certain pressure, pressure
Pipe wall energy in joules may be written as:
J'
,u'/umu
Pressure energy. :.:. __
PA.
.
Fi�ure _2-5. Distribution of flu'ia \ici'ocities . gpA
,. . (14)
across the cross section of a pipe r

J .. .,,
• I
 Ch-2 Fl.<>W OF FLUIDS 37
' ; l
'
.11, •
35 l'I IAl{MACl-'.UTIC AL ENGINEERING P1 1
Total energy at point A = _,.._ + X,1 + (17)
where P.4 = Pressure at point A, Pa . gP,1. .. 2g
.. � = acceleration' due to gravity. mis According to Bernoulli's theorem the total energy at point A is
PA = density of the liquid , kg/ml eonslant. Therefore, equation (17) is:.
Pot�ntial c11crlJY (datum energy) of a body. is defined as the energy , P -1 u/ ,, ·. , . · .
1

possessed by .the 6.ody bY, virtue of i,ts position or configuration. · The Total energy at point A = -·- + X,4 + -- = constant ( 18)
point A is considered at a height of X,1 metres above the horizontal gpA 2g
I

datum plane'. The· �?tential energy for one kilogra1n of liquid 'may be After the system reaches the steady state, whenever:onc kilogram of
written as: liquid eniers-at p,oint /)., another. kilogram of liquid lea\·cs at point B.
Pqtential energy = X,1 (15)' _ Therefore. energy content of one kilogram ·liquid that is· being displaced
at point 8 may be written (13ernoulli's tlieorem) as: · . ·., ·
Initial state, ... Final state . pI',,
' '
. 11,'
Kinetic• ue2 1.otaI energ y at po111t B � -- + Xs + ·-·--- = constant
,· · :
., Pressure (19)
.
Kinetic energy• u,A.
2g
2 energy 2g
__.,
energy
,n
!-:Ps .
. where XB ,.., height from the datum .'lo lhe pipe, ITl
2g J

· - rt· ;.1f° IIJJ = velocity' at point B, mis . . . ...

p
:.. 1·

Pressure
' energy
· '· • -. A .P11 = ·pressure al point 8, Pa
.P 9 ·
,.,
p11 ,: densit� at point 13'i ,�:g/m3
.:J Pump he11d, W. If thci'e is no gain or loss of energ)', the principle of conservation oi ·•
energy may be applied 'to the two points A and B.
Frictional ene'rgy • F
Xe 'INPUT � OUT PUT . I

Total energy at point A_ "" Tota� c1wrgy at point B

.. 'IA'
r'
• I

., + ---'

· . �·�yi
I',.,.
-:-·--:- u,(' ' '"": ---.+
+ X:1 + --·-
pll ;,·
):. uo··
o (20)
gP,.J 2� gPn 2g
. ,, ,.,
t� Horizon. tat datum Theoretically all. kinds �f energies involved in fluid flow should be
Potential energyI • X ' potential eri�rgy• Xs accdtJntcd. In the. transportatioi1 of fluid, the. pump has addfd c.crtain
. r !.":'.-�. .
.,
A
mnouiH of energy. which can be written a�:
·, Figure 2-6. Development of Berno'u;lli's theorem.
' J Energy addiJi1 by the pump';.: + wJ. (21)
. Kinetic energy of a body is defined as the er.ergy possessed by the ' . '
body by virtue. of its motion. Since liquid is under motion, the velocity During the transportation ,of I iquid, some energy is converted to heat
of liquid !11ay" b�. designat�d as u,1 metre per second at point A. The. due to frictional forces arid it· is .inevitable. ·Th� energy loss· may be
kinetic energy' ' m�y-be expressed ·a�: ': r written .JS:
. . U,1.2
. J•. '

loss of ene�XJ'. clue IQ friction in the line = 'FJ (::.2)

·1;,,,' Kinetic; energy = -.-·:. (16)
2g The ('ner.gy balance between points A and B can be accountJd by
. . The total energy at,, point A may be summarised by combining including equations (21) arid (22) in· equation (20). · This complete
:.·iquations (14), (15) and (16) as; equation rcprcsi.:nting such energy ma:, be written as:
. •. . ,· ....
Total energy = pressure energy+ potential energy + kinetic energy
38 Pl lAR�IACEUTICAL ENGINEFRINCi
Ch-2 Fl.OW OF Fl.Ul[)S ..§> 39
.
Bu't N (newton) "' kg·m/s2 • Substituting this term in equation (24)
P,( 11.-, 2 · Pll 11n2 gives: ' . . J . '· ·, ,,,
-;- + X,1 -� -- � F + W =. --- + X3 + - (23) . kg x m x s2
_gP.1 I
2g1, I .} 1
gP/J ,;1
J.
2g Pressure energy =. ----
· -· = m.
Equation (23) is called. Bemo11lli 1s · eq11alio11. Bernoulli's theorem. . . s 2
x kg ·,, ·
a{though derived here .over two· ends of a· system, 'it is · applicable . Thus, press1:1re energy ISi 1�') metre, i.e., as a height. Therefore, the
bet�veen. any_ two points in a system. � . "" " ',;
height is tenncd as head in the discussion ofhydraulics;j Hence, pressu�f '
tqLJ:1tion (23) is numerically correct. B�1t it is not corre�t theo�eti­ energy is called· pressure head. 1.,,
cally, since caclr,of the terms in-•eqtiation (23) is actually ei1ergy term In an anal_og(Yus manner, there arc different heajS''in the Bernoulli's
and should be measured in the 'tmits'of joules per unit mass. ln'p'ra�ticc, equation
these terms. arc always referred a� the heights and 'often measui- · ( 18), namely: .
. ' cd in potential hca'ds (.\)
terms of height of a column of liqliid.: velocity· heads (zi2!2g) ·
Applications: (I) Cernoulli's theorem is applied in _the measurement pressure heads (Plgp)
of the' rate of fluid flow using ori.fice mctc·r, venturi meter etc.· Similarly, Fis known as friction head and JV is the head that is added
I,,\. ,\

(2) RcrnoulfFs theorem . is applied in. the working of centrifugal b� the pump.
.
pumps. In these pumps·, tht td�·et,[c energy is ,co11vert�d into pressure
head, which helps in pumping the liquids . ENERGY LOSSES.. ;
Bernoulli's equation in�ludes 'the term 'loss of energy' in the pipe.
.' � I

(3) It is easy to measure heiglns and apply tbem as energy terms,

which is a contribution of B,ernoulli's theorem. According to ,law .of �onservation of energy, energy· ba\an. ccs have to be
f' 'I properly accounted. Therefore, ·it i,5 necessary, to c�.lculatc the energy
Concept of Head (Pressure Hc;i d) .
1
losses. Fluids expericn�e �energy� losses in ·sevcraJ·ways. •while flowing
'T'he terms in Bernoulli's �qu,ation represent energy and supposed to through � pipe. Somf of th�m arc: , .I':
'
have: the units of energy. But l}Umerically these terms gjve the units of I. Friction losses '.
j .....,
l·
metre.· Therefore, energy terihs can be measured in the u1�its of metre, 2. Losses in fittings
which is a unit of height. Hence the.se terms arc known as heciJs. 3. Enlargement losses
The prc:.uure head is defined ·-as the height of a column of liquid of 4. Contraction Losses
known density, which is numericatly equal to pressure energy t�nn.
,.:, .', ''

. These arc discussed in the following sections.. ;

'• I,
fhe units of height can be, �btained ·b y considering trye, _• pressure < ·;,

eneigy term. i.e. equation (14). ...

1 •
Friction Losses
, ; - j'f,
During the flow o( fluids, fricti9nal forces:.�a�se ;a: 1.��s ii} pressure'
P,1 pressure
['rps,ure e11ergv c= -· ::, ·--- (/JP/ pas1c'als). The: lluid flow can �,e eitJ1er yi. �cpu,� Qr _turbu,lent, whic�
. ' ·.. gp,l acceleration due gravit�·J x density .
to also influ9nces the losses.. In gener�I,. th� pr��s�rc, drop _(M,j) due to
. .r ' ' : friction in a fluid is:. ' ' . .. . : ' ; .
.· Consider the units for equat-ion ( 14). ·, , - directly proportional .to the velocity of the fluid (11), mis
l
) ' . . N I -· dircctly•proportional to the density of thc';f uid (p), kg/m3
Pressu·re energy =. --.., • ---.., · • ----',- - directly proportional to the length of the pipe{l), n'I
' · m- (mis-) (kg/m )
-· inversely proportional to the �iameter of the,pjpe (D), m
N x· s2 x 1�-'· · N·s2 These relati6nships are proposed ln Fan11ing cquatio11 for calcµlating
-- = --·
of the na:tµre of tlow ·(visco. us 'o� tu'rbu-
1
(24)
m2 x m x kg kg tht: friction losses, irrespective
'·
lent). · ·.•
' 4� ' • •. • .

· ·, " · · ,, · · · ...
r

J ·�.
40 Pl IA RM/\C:E\JTIC AL ENGINEERING C:h-2 FLOW OF FLUIDS. 41
2J,i2Lp equation is applicable for the losses. When fittings ar� intr,o d.uced into a·
· Fanni,ig equation:· Llf>J = -- -- (25) .
(viscous or turbulent) D straight pipe, they cause disturbances in tl,1e _fl ow, ,,:J\jcJi'.;; result�- in
additionnl loss of energy. It is difficult t'o specify the loss,.dtt'e' to ead.1
when: f =:=/ friction factor
type,. bcc:rnse of varying typcs of fittings.
Jpl ;. pressure drop, Pa-
' Losses 111 fittings may be due to
Equation (25) considers the .friction losses when the fluid is passing change in direction, for example elbow fittings,
' through a straight pipe. The value offdepends on: -- �hangc in the types of fittings. fdr'example, 5.oupling, union,
- Nature of flow of the fluid (turbulent or viscous). valve or meter.
- Roughness of the inner surface o[ thc.,pipe.. The roughl)css Losses in jiuing}, by convention, is exp:-es$Cd i,1 ·terms
factors for some conditions of pipes are givt:n below. _ of an cquiva­
lent length of straight p.ipc, which is given as.� certain.number of pipe
. · . t·
.Cvndition ofpipe Ro11gl111ess factor -d1ameters. .·
. · , .. . •
r .
.
Smooth bfass, copper or lead pipe 0.6
New st�el or �nst-iron pipe 1.0
Old steel pipe I.(, "' 1� ·:

l3adlv.. rusted cast-iroo

. '
pipe
, ,. 2.5

Tse numerical values· reported in the above table give ai·,rough . Elbow 90 fitting Tee fitting ,.
e:;timate �flhe. magnitude of the ·effect, which contributesto the frict'.on Equivalent length: 32 Equivalent length,: 90
factors. Frictional loss can be reduced by the addition of soluble, high
molecular weight polymers in lo�)concentrati'ol\S.
_
In pn1ctice, fluids arc nm:ly ·handled in viscous flow.. r�t· �iscous

I
flow.· Ha.rien-Pniseuille equatinn could be employed for calculating the ·.

[[]]
pressure drop due to friction.
·'

32/.1117
!

Hagen-l'oistuille equation: LlP = �------ (26) L 1'/

·., .. ,.
,.• ;,
( viscous flow) IY' ._____.J .,.__..,.. : ! !
Coupling fitting Globe valve coupling I
where q= vi�cosity of _the liquid, Pa·s Equivalent length: !)egligible Equ!vale,nt ;le_ngth:, 300
. ,1.p = pressure drop, Pa
f · Figure 2-7. Friction losses in !ittings of a new sm:wcd ·,p-ipe.
If the .vjscosit)' (17). is known, H�gen-Poiscuille.'s equation permitsthe ·.
calcula,tiori of pre�s't,�e drop due to''f!\tici11_. HO\\'C�er. cq�ation (26� is Equivalc;nt lengths for a few. snewed fittings. are shown _in Figure
. 2-7. For example, a globe valve is fitted in .a pipeline, having, an internal
norma'ly used to. �'akulate the viscosity, by experimentally estimating
,1[>, diameter of 50 millimetres. Globe valve has an c,quivaler�t length of
' ,I '
300. Then, ,·,.i ; ,
i='rictipn losses are permanent,· since potential ond kinetic energies arc
converted intq, heat. · Equivalent length of �his fitti�g = 300 x 50 = 1500? ri1n:i.or 15.0 m.
. .
,, . That means the contribution of a globe valve is equivaleni td I 5
Losses in Fittings . ._ metres ·of a straight pipe towards the losses. This length is adde� to the
Normally. a larse nun1ber of fittings are. include� in a pipcpn� · st�aight section of the pipe and substituted in the Fanni,ng �q��tion (25)
_ ·
(Figure 2-7). · · For a liquid· passing. through a straight pipe, Fanning to obtain energy lossesdue to fittings. ·. , · , . "
 l .

42 l'I IAltMACUJTIC/\1. EN(ilNEERlNG Ch,:2 FLOW OF FLUIDS 43

'(\,' I

Enlargement Losses The constant K depends on the relative areas of two sections. For
If the cross section' of the pipe enlarges gradually, the flui_d adapts example.· when the ratio �f the· areas is 0.5, K is. equal to 0.3. For
itsit f to the changed section without any disturbance. Therefore, there is rounded entrance. K value for turbulent now is· about 0.04. For laminar
�
·u
no loss· of encr�y at this point.
•.

nbw. the loss is 'negligible.

• . ! • u

MEASUREMENT OF RATE OF FLOW OF FLUIDS

•
Whenever tluids are used in a process, it is necessary to measure the
(bl Sudden enlargement
rate at which th9 tlqid is flowing through the pipe. This is r�quired for
.· (a) Gradual enlargement
No loss or energy Loss or energy optimizati.on of process parameters in a chemical. industry. Measure�
. . . ments are required for the calculation of .auditing (for example, town
If the cross section of thi.: pipe changes suddenly, loss of energy is planning of water supply) and .cost of usage ( for �xample, cost of.water
observed due to eddies.· These arc, great�r· at this point than straight used in the houses). Methods of n,easurement may be dassified as:.
pipe. Due to. these disturbances. the loss of head will be ob�erv�d. In
I. Direct weighing or measurin$
sudden enlaroement, the velocity. of flow at la�ger _c_ross-sect10n 1s less
th�n the vcl;city at smaller cross-section, i.e., u2 < 111. For sudden 2. Hytjrodynamic, methods
enlargement, the . loss is represent ed by: .(a) Orifice meter
' (b) Venturi meter
(111 ..:_ u2)2 .. ....!

Sudden e11/arge111e111 lasses: L1He=---- (27) (c) Pitot tube

2g (d) Rotameter
where t.1f-le ·-= toss of head due to sudden crilargcmcnt, m. 3. Direct displacement meter
Some of the above mentioned meters are discussed 1n the following
Contraction Losses
sections.
If the, cross scctiO}LOf th\! pipe is reduced suddenly, the fluid flow is
disturbed. Noi·mally,''the diameta ·or the fluid strcam would b� kss than Direct Weighing or Measuring Meters :,, 1
. the initial value ofthc'diamcter. This point of minimun1 cross section is
. •.
The liquid !lowing through' a pi·pc is c�Hect�d 'tor a· particula� pe�iod
known �s .vena cv.11 /racta. · The velocity of fluid at smaller cr6ss-section l
at any point and weigl1e< or 'measured... Tl;i us, rate �f_ ryow4:�n be
will be far grcatcr·than that at larger cross-section, i.e., 1�� > 11,. Th� n. detcrli1incd. Gases cannot be weighed. On commercial' scale, it is' not
U / may be considered negHgible."fhe .losses due to add1ttona
l- eddying convenient.to. \Veigh"thc liquids. Therefo�e� tliesi! methods are impr_a'ct_i·
as: ' · ' ' ·. . ·
are observed.. Such contracti. on losses .can be expressed cable. .
.

• . Kur) !.
'

. u· .
, 1 , �:i,'..i' ''-./ /
q'

S11Clde11, co111ruction losses: tJH. = -- (28) Orifice Meter ' :;! · , ·.'i \..,,,, ·1. . ·:,q
.,.·% ·• .

I J- , � 2g . Principle :. The orificetitiWi,�ter, is. a thin plate ·containing a narrow and

where &-le ·= loss in h�ad due to sudde'n contraction, m sharp aperture. When a fluid. stream is suddenly allowed to, pass thro11gh
K = ·constant the narrow constri�tion, the velocity· of. the fluid at the. orifice meter
112 = velocity_, m/s increases compared to the veloc ity of'thc fluid in ,the upstream. This
ct· a r.ontracta
results. in c orresponding decrease in. the pressure,, -head. , Bernoulli's
� theorem provides the basis for correlating· the increase in the velocity
�-uz
head with the decrease in the pressure head between two'·points. The
.
. . difference in the pressure head (_M{) may be read ·from, a manometer. . \ . If
the diameter ofthe orifice is small compared to the diameter of the pipe,
0 . .
' · (a) Gradual r.ontract1on. (b) Sudden contraction
No· loss or energy Loss or energy
velocity of the fluid at the point before enteri_ng the orifice may be
 /
44 l'i 1/\RM/\CEUTICAl. ENGINEERING
Ch-'2 Fl.OW OF r:1.ums J
consi<.lcrc<.I negligible. In such cases the manomclcr reading directly
gives, the vcJocity of the Ouid. . � Orifice plate
The velocity of the fluid at the·thin constriction may be written as:·'
1
'

110 == C',/.J 2g. t1ll (29)

· Downstream
where 'lfo ' = velocity of fluid at the point of orifice mctci·, mis
( '0 � a ·constant
i
,1H = difference in head from manometer, m
The tJ.H can be measured using a manometer. '\\'hich is connected to
the pipe section between the initial stage and the orifice section. It can
be substituted in. equation (29) in order 'r? get the velocity or the liquid '>.
I
flowing through the orifice. When crtiss,scction or the pipe is known,
the volume of the liquid flowing per hour can be determined.
Copstruction : The ori ficc meter is considered to be a thin plat:..: ,, .
containing a sharp aperture through which 'a fluid flows. Normally, . ,,
Figur:c 2-8. Const�uc�ion · and a�sembly of orifice
orifice plate is placed be'twcen long straight pipes, so that other fittings me.ta.
do not alter the flow rate that is being measured, Although it is possible
to place ori !ice meter in the side. or bottom. for the present discussion,
. �
,..
If th'e diarncter f the �;rfi·c·� !S I/5th the pipe
is. sn�all compared to 110 •• Then: 11,;1 .• term' may
·�fdiameter or less, ll..t
� · be; nei:!lected. Then
the plate is introduced into ihe pipe (Figure 2·,8). , A mnnometcr is equation (..,Q) becomes: .. -' � · · · ·
. connected at points A and [3 as shown in Figure 2-8. Ji: .•
J

. ·,• ,(#ro,rking : Ori lice meter is referred to as variable i1ead 111('/er, i.e., it (29)
· S�-f ca11 be _measured using a mano111,e�er.
measures the varjation in the prcssures across a fixed constriction placed It can be substituted in
equa 1on (29) 1n order to get the velocity ·
in the path or ll�w· consisting of a coil�t�nt area. _ � . : of liquid flowing through
�rdi_cc. pip�..,When Fross. .sect1on of the ,pipe' is known, the. volume of
When fluid stream is allowed to pass through the cro_ss·scction or the liqu1c.l)lowmg per hm1r can.be direct!Y determinc
o'rifice, lhe'· velocity of fluid at point, .B. increases at the expense of. cf:." . " n ,

pressure hiad. As a result, the pressure at point A i,s higher than. at point .' 1\-�a�h�m a, ti a� treritmefit' : <;�nsider' a fluid
�. flO\Ving through' a ;pipe
B. Bernoulli'.s equation provides the basis for correlating the increase in .• at a eertam _veloc ity (11,1). If the edge of orifice i� shar
,, , • p·, flui'd do'"es not
velocity head with the decrease in pressure head. The difference in I�se• t'Ile ve 1 oc1• ty· at nee·, \\•hile p ssing through' die orifice. T,vo points,
_ � �
pressure (6.H metres) may be read from a manometer, connected to the A an� 8 on e1tl er side of. the orifice meter are
equation 1s _ � ·chosen -and Bern · oulli
· 's
points A'.a1ld B as shown in FigLire 2-8. · applied. The Bernoulli's equation is:·• ,.
,; p , .I• .• ·. ? . • ' ' .. • '. '
BernoulW·s equation n' iay be applied for two points (A and�) for the ... ,, · 1i;1· · · · PIJ . u,/
---· t-X;1 + -- - F + W = - + X +·�
given experimental conditions, as given below: �P,1 2g gp8 ,,
n (23)
. ,..'.- .. .2g....•,· ....· 'i
· In eq�ation (2?), th� fol,lowing assumpti
: �11> - 11�/ =,· C0 �2g.M1 . .1 (30) the work mg of on fice meter" (Figure 2-8). . ·
ons may--b�- 1��de based ��
where 11 0 = velocity of- fluid at the point of orifice meter, m/s .
"A = velocity or·fluid at the point A, i_.e.; before orifice meter, mis (I) Let the s1�ctions of pipe be horizontal, so .
th;t the he·.tghts (me•
' ) o·r t11e
.•
· C,r = a .constant , tres 1.: pom • ts A and . B are· same · (Figure 2-8). 'cT·he.
. . , n'• two X
!':t.H'"' difference in head. ni terms are 1den t1cal and get cancelled. r , 1 ' •
/ (2) Let the friction losses will not · be apprecia
ble �nd con:cie/ed
negli�ible. Then. \ term becomes zero.·
J ·,,
 46 1'111\RMt\Cl:l;TICt\l, EN(il�EERIN(j · Ch-2 FLOW Of FLUIDS 47
.forc, P.. 1 If the diameter of the orifice. is I/5th of the pipe diameter or less, u,4
(3) The fluid llowi 1 ig through the .orific� is the same. Thcn:
is small c.ompared to 110• Then,_ 11;1 term may be neglected. Then
is equal to p11, and can be termed s_in�ply p. . . .
liquid. since no equation (30) becomes:
(4) No \\'0;1· ,5·. being· d{�1ic O!� the 1quid or.by the
pump is used. Therefore, �I' t_er�n, !? e�ual to zero.• l/0 = C:o.../2g.&�. ,,(29)
Substituting ·th�se -�t1,i·n1s in. . eH_u<:tion .. t23) giv"cs an e4uation. which
can be rearran1.?,cd as follows.
·
:
· ·
. I :; · -· where,_· llo = velocily of nuid at.ithe point of orifice meter, m/s
C,, = a constant
·.-1 ,,,

. - . .;�· . 11} P1) :··;,;/

.i L11{ = difference in head, m:
-·-· ,- . ' -·· - . �-t --·
gp . 2g gp � 2g !JI/ can be'r11easurcd in metre us'ing a manotncter. It ca'n be substi­
: tuted in equation (29) · to get the velocity of liquid flowing through
I. I ;
,_· (11n1 -1i}) = �tP�1_:. I'JJ) '0 orili�e pipe. When cross'·section of the pipe i's known, the volume . of
2g .<.;P �· liqu!d flowing p.er hour tan be directly determined. '.. , :.,.
"'S
1 � - '£
-
l/lJ• - II 1 • - .,..-_ ··. tl' ·I '.7'-·. J>�H)·• .(31) . Applications : Equation (30) is useful to determine:
(I} vcl9city at either of the poinif A or.. B. Ratio of 110 and 1111 can
.•· ' " ··1 • '

gp
. SH. ") 0 . ,, . be related to ratio of the area ot· the orifice to the area of the ·
,11.r ""', -- "-�.
l!B.. -
"). ') (32) -� A I) pipe. which is normally known.
·'JI. . .� l!.
' ·, 1
P (2) rnlume of the liquid flowing per hour :when 11,j. and ·cross-section
.
� I �-

ucing
'. lf�o·111 tfic ptinciplcs of statics, (.JP;,gp) = Llil jn �)�\r�s. Introd
_ \.

of the pinG arc k:,mvn.

• this terin in equation (32) givt>s:,
�·' \ � .,. ,.,
113· - uA· =-= 2g.,1}{
' ' Venturi Meter
1
,/ ,f
A T . 1 1 . Principle : Venturi meter consists of ilvo tapered �ections in the
113./�·.�f]
:�(; . ,1.,.,,L.11
- .,;;�I A / ') (33)
0

I : .,: . .
.id 'streahi wool(! be l �ss Jhan tA\.e
. pipeline with a gradual constriction (throat) .at its <;entre. · When fluid
Norm aWv. the Jiame te' r '{if the• nu stream is allowed to pass through the narro,v throat, the' ve'tocity of the'
of the orifice· (Figure· •;2�'8).. This point of ·n,inimuin �ro�s
I

diameter fluid increases at the venturi compared to the velocity of the upstream.
f.l ll ' f.l\qt11d
�ection is known as \he-�-'ella co11tr�1sf(J.· J"l)oug.hJ,he. pip<? is '. ; � _ This results in corresponding decrease in the pressure head. Bernoulli's
C�IStS ,!nd ;,_JS
on both., sides of the. orinc�,,� s,ti'll }he Vella C0/1/raC(Cf, theorem provides the basis for correlating the ,in�'rease in the. velocity
co11(re;,rtc1.
. surroundtd by 's\,·i,rling .ljquid.. ,Po\nt B i� 1:r9csen at the wna head with the decrease in the· pressure head between two points. The
l.n -�s;�cii,ce. the diam\!ter of the strea1�l 'at the, l'i!I/(/ 1ccimlra cta n �t
_ _
! !:' difference in the pressure head (&{) ma·y bc{ read·fr�m a manometer. If
known, ·Qut that. or the :orifice diamc\er ,s known. A o , nsta1�1._ ( r1• is.
I

the diameter of tl,e venturi is' small co�-ipared to the diameter of thSJ)ipe,
t the d, flcrcn�cs
therefore. included in equation (:;3) in order to- correi: velocity of the fluid at t\1e point . before entering the venturi may be
crefor�. equation
between velocities at orilin· and at 1\•11a co1111·lll'f11. 'J!'-h considered negligible,. In such cases, the �anon1eter. re�di�g directly
!
rifice (110)-
(33) may be mndilicJ in terms of the wloci�y throll):!.h the o
· •

gives the velocity of the nu.id.

v

��
''.
1
;) • r,.,-
\llo-
2 ·-- c·,,11\;_g.�;, •:;.,
- IIA
(30) The velocity of the Ouid at the. narrow constri-ctibn:(throat) may be
.. written as:
n.. 11 depends
The constant ('0 also includes. s.ome .losses du,;: to (rictio . .
011 the,: co�strn,ctj�n (r,ati9.,of' the orif.'ice diam ct�r to the pi pe i,;unctcr and . .. 1/tw;-:- ·cvV2g.L1H (34)
_ � (Reynolds ,,
,liquid
..:. )
ure of flow of
, position of tl,e orifi�c taps) a\:� the nat_ where 111• == velocity at the throat of the venturi, m/s
number). ,1
C" = coefficie-nt of the venturi meter
(-; • .I .... {II
!JH = difference in head from manometer, m
48 1'11,\IU.,ft\�TUTICAL 1:NGINEl:IUNG C:h·2 Fl.OW OF FLUIDS 49
� .. · .

t1H can be measured using a manometer. It can be substituted in ../11/ - u/ = Cv..f2g.&I (35)
equation (34) in order to get. the 'velocity or' the liquid flowing. through ·, . ··"
the venturi. When the 'cross-section of the pipe' is knQwn, the volume of where 11,. :: velocity at the tl1rpat of the venturi, mis
"'' velocity at point J\ (venturi throat). m/�
liqu'id flowing per l!olir can be detcr'ITlincd.
11,. 1

. . (\, = coefficient(=' 0.98)

.
Construction : _A venturi meter consists of two tapered sections '

lr'the diameter of the smalllif�section is one-fifth of the pipe di�m�ter

inserted in a pipeline (Figure 2-9). Normally, venturi meter is placed ,
or less,. 11/ is .r..oi,sidercd to be 'small compared to u}.! The.re fore. u;t
between long straight pipes, so that other fittings will not alter the f1ow
term may be disregarded. A simplified form of cquat_ion p's) is: · · ."
rate that is being measured. The upstream cone is normally shorter than '
..( .·
,, :
.

the down stream. The tapers arc smooth and gradual. .Therefore, eddies
' . . I ,. '
(34)
in ,the down stream are absent and no power loss is observed. ., In
· addition. 1 thc cross- section of th�. high velocity p�rt of the stream is weH The difference in prcss�re (L1!-/) can be_read ln �ct�ctch�cctly fro;
_
defined. A manomctc;r is· connected at points A and B as shown in the manometer. Thus velocity of. the fl,ow may be measured .. The v;ilue
Figure 2-9. · given by the venturi meter is average \·elocity of,the flow. The velocity
then decreases and the original pressure is recovered in'thc down' stream
Velocity head. increased
r' ., cone.
Pressure head decreased
'Outlet Applications =. Ve1ituri meter is commonly used for liquids, esp,:­
Inlet Short cially water. It can also be used for the. measurement of gases ..
_,.'_, t-----·�
section section 'I

?
tapered •• 1• .t. r , :b. . .
n ·{./V�T-�;_��- Di�advantagcs : (I) Ventu.ri meter is expensive. (2) •Venturi met,:r
J
f�
� _r
�...:_ _
occupies more space. (3) The ratio of throat diameter tl'i pipe diameter
' ' . ., . ' '
cannot be changed.
A -> • �+--- B Oow::J . . '')';

,-., TABLE 2-1

Long t'apNed Diffcre,ices Between Orifice Meter and Venturi Meter
' L section
f 1. Orifice meter Ve1it11ri meter
';
·( l) Cheap Expensive
(2) Eu�y to install rubrication is highly''fcdinica
I,

( 3). Construction can he ma Jc ll should ht! puid,.i�cu from the"'

at home instrument denier
I•

. .
F igure 2-9. Construction of a venturi meter. ( 4) l lca<l losses arc mon: 1-lcad·'lo�sp arc in!,i�nilicant: . :,
.

.
(5) l'owcr losses arc 111on: p:irticularly Power los�cs arc lc�s
Wo�king : Venturi meter is referred to as variable head meter, i.e.; it
on nuid that is carried for Icing
' m�asure$ the. variable differential pressure acr�ss 'a fixed constriction
periods of time
placed in the path of flow consisting of a constant area: .In a venturi
meter, th\! veloci�y .of,. the fluid is increased at, the throat, due �to the
t; (o) Normally used for testing purposes, llsed in on-line instal1;1tion;
· l'or c:>.:11nplc. stcam lines etc.,
constriction. This results in decreased pressure in the up-stream cone.
'. .• • J � ...

The pressure drop in the upstream cone is utilised to measure the rate of · ( 7) ( iii:atcr lkxibility Not llcxiblc; pchi'ianc' nt ..·
flow using a manometer. Venturi meter nearly confirms the theoretical Reading or the orifice meln
. The reading of vcnturi· mete� is
(li)
equations obtained for an orifice meter. On similar lines of equation is largcr under identical COlllparntivcly smal Jcr ;ll ndN
(30), an equat.ion for venturi meter may· be written as: cnndilion� identical con<litions1,.
50 ('h·'.? Ft.OW OF FLUIDS .·f ,\
51 r
j
Pl IARMACEtJTICAL ENGINEERING

Differences between orifice and venturi meters: The differences This is the theoretical veloc'ity. Actual ·velocity is given· by:
bet�/een ori !ice and venturi meters are explained in Table, 2-1. ..:
Lf! "" Cv'Y2g.Alip (36) . ,
,j

Pitot Tube where C1• = coefficient of pitot tube. 'l .1,.• '

Principle . : Pitot tube consists of a sensing clement with a small I ,'

constriction compared to the size of the flow channel. When the sensing
element is inserted at th� centre of the stream, the velocity of flow is D_ownstr�am
increased. This results in decreased pressure head. Tube at right angles
to the flow measures pressure head only. The tube that pointed upstream Limb measures pressure
measures pressure head and velocity head. The difference in the above and velocity heads -Z.,,,,, � limb m�asur�s
readings in1dicates the velocity head. pressure head
Ac�ordingly to' Be.rnoulli's equation, velocity head of the fluid may ·•�·,· . . .r
be obtained using equation (33).
. ul
LJ.llp = - (36)
2g Figure 2-10. Constru,i:tion and asscm9ly of pitof tube.
where u = velocity of the flow ·at the point of insertion, mis
. , Normally, _Pitot _t�bc �easures th.e::�elo�.lty at o.ne particular point,
jjfII ' = di !Terence in head from manometer, m L� ... at th po11 t ot 1nscrt1on. · !he avera
. � '. gJ ,velocity (across the cross ·
Therefore. the reading (R) of the n1anometer measures tl1e velocity section ot the p1pc). may be obtq}JJ;d by eitl.1er ways.
J
head in metres.· (a) Pitot tubi:; may be irm11�d at the centre of the·
. · p.1pe
· and 1t·
measun.:s t�1e m:ixu. num, \ycl9city.' Average veloc
Constructio:1 : The construction. of a pitot tube is shown in Figure 2- ity mav be
calculated lrom this maxirhii'in by me,1ns of calibcatcd
10. Pitot_ tube is· also known as. insertion meter. The size of the sensing . . ch.arts.
· (b) AJ� st 1ble pitot tube 111ay be used to
element is small compared to the size of the flow channel. . The point of u � . take readings from differ­
measurement may be at the centre of the channel. ·one tube is perpcn­ ent p�m!s 111 th: cross scdi'on. Mean velocity may be
found by
diculi1r to the flow direction and the other tube is connected parallel to graphic mtcgrat1on. It is a uif0eult process.
the direction 'of flow. The two tubes arc connected to the legs of a Advantage : Pitot tube measures 'the velocity at one point
only.
manometer or a suitable, devic.e.
. . .· -' . Disadva�tage s : (I) The pi tot t9,bes t�emscl vcs c.ausc
_ more distur­
bance:· Eddies w1th1. 11 the pressure tube disturb the �eadi'ng
'

Working : Two tubes are inserted into t.he pipe in the manner shown
. s.
in · Fiiure 2-10. Pilot tube isi used to measure the l'elocity head (?f the (1) They do not'�i:ve"ave.ra�: vclociiy directly. .- .. ! ,,,
flow. Jn this tube, the .velocity of fl,uid is increased at the narrow . _,,,\ •
(3) For gases, th� r�adh1(1i xtr�mcly sn1a 1'. · F r g�s�s
constriction. This results in decreased pressure. Tube at'.right angles to , � ; ! \�orking 011
low pn.:ssure, �omc. t.orm of rnulti.i�lymg gauges must9 be u SCd
the flow measures pressure head only. The tube that points upstream · n , ,, .�· ' ;_, • ,,, .. · .
meast.res pressure head and velocity htJd. The difference in the above Rota meter . '
readings indicates vel.ocity head. Therefore, the .reading (R) 'of the
0

· Rotameter. is a variable �rea meter, i.e., it measures

'the area o'f flo�v,
1
manometer measures the velocity head. so as to produce �-constant head' differential. · Therefore
_ /rotamcters 'a'rc-"
, • , r

As seen in the .Bernoulli's equation. velocity head of the fluid (IJHp) known as area meters. · '· ;, ·, , ·
may be obtained' fr.om an equation similar to equation (29), which can be 1

Principle,: Rotamctc.r consists of a vertical ta.pered

/l '

represen�ed as,
1 I ) • , "

. . . . - ,. and t'ransparcnt
tube 111 which a plummet 1s .. ... .flow , through th.e,
placed. During :the fluid
. .. ,,
 52 Pl IARMACEIJTICAL ENGINEER-ING,
.
Ch·2 Fl.OW UF H.UIDS '.
tube, the plummet rises and ,falls be�au�c;;eC·variat i. on jlJ ;flow, As .a Normally. manufacturers supply the. necessary df!ta and charts along
·- with the meter while purchasing the instruments.·
result. the area oftl1e a_nnular space.between the plummet and the tube
varic�. The head loss across the annulus is ct1ual to the weight of the Uses : Rotamctcrs arc extensively used in chemical industries, such
plummet. The upper edge,of the plumm�Hs;used' as ,an index to note the as bulk drugs. 111 the fcrmenters. 'the.; supply of �ir is controlled throqgh
_ . 'I
reading on the tapered tube. This value indi.c��!cs th_: flow of the fluid.
. .,, ·,
I
rntamctcrs. Rotametcrs arc satistactory b.oth for gases and for liquids. at
.•

high and low pressures.

f ' ' •

Construction : Rotametcr consists of a vertical thpered tube, which r

is mounted with ti ·n;rrow end down (Figure 2-11). The, tube is usually Advantages : (I) Operator has a direct vi�ual index of flow reading,.
made of glass on which a linear scale is e�ched. A solid plummet is It is satisf'a�tory for manual contrq,J. of processes for cxpcrimcn_tal work.
placed in-the tub�. The .d_iamet�! of the plum1�et is.,s 1�aller .tl,1?11 the
O
1
(2) It docs not rcquire _ the .�ondition, that straight :,ipes. should run
narrowest part of the tube .. Rota neters are available with electric and be fore and atkr the meter.
electronic t;ansmitters for rec_ordq,ng. Floats of different densities arc
available
.... ' so that a 200-fold rang.�e. of flow .can be measured accurately. Di.rcct Displacement Meter ·
Floats may be made of lead, aluminium, gfa�s and plastic. ., . ,., Displacement 111\!tcr is used t.'or meas4ring' domestic water supplies.
·, r 11"'°"" , 1
',. � . • • , .
l l11S has the adva!:tagc that the total volume of liquid that has passed
.,

1:an bc re.id directly. .� l:

,.., ,, .... �
�-

J>ri�ciplc : Displa�em�nt meters i}re .used for measu,r,ing th� fl.9;,y rate
ot· fluids in small lines. In these meters, a stream of water enters the
' ' ' •1 '
. .'· i;. '

)1 ' meter and strikes' l he lllO\'.i ng mC;l;ber (disc as 'in Ji'sc 1netcrs'bt bu,ck(:ts
;1s in current meters). The rate of rotation of the movin'g member ;is
1iroportional to the .velocity of water passing through· the mctc't. The
displacement of moving member is transmitted through. a train of gears
to the counting dial. which is .prcsc1,lt in the ·top of the memb,er.
Advantages : The displacement' meters have '.'111 advantage over
.venturi or orifice meters in the sense that the reading' repr�sents the total
.,.1·.
volume of fluid that has passed. This volume divi'ded by a definite
period gives the flow rate. .J,
.
' .
' :,r, ,· 1'1° • '; t Glossary of Symbols'
Figure 2-11. The -Construction of a rot�mctcr. C 0 � Constant for the orifice meter,
�l ' J• ' '
'. • • ', • ' p; ' �I , •
';

Wo;king: As the flow is.Hrward through a t�P.C.fFd,tube: the flow of C,. :.· Constant for the pitot tuhc.
.
fluid varies. The plummet. which is �urmu�de� ...h>' the fluid,. rises a1)d Cv = Constant for th�. venturi nietcr,
D = Diameter of the pipe, m
falls dep<rnding on th'; rate ?'r no,v.. }�� g�eatc/,thc ll<n� r�te. the h,igh�r 11 = Visc osity or lhe liquiJ, J>a·s.
, . .
the plummet rises in' the .tube� 'In ro�ameters, the pressure drop .1s r = Friclio'i1 la1.:lor.
constant or nearly const.int. g =- t\ccclcratioll Jue to gravity, m/s2 ,
.-Q,�rin,g the .fluid. 09��� the ?rea of the. �,mu),)fr space be.tween t\1e h 1 == !-kightor 1he liquid column at a.point. 111.'
plumn1ct and the ,ube ,\laries,, Therefor<;, lj1e head loss acros� the t.11 = LossofhcaJ,'m.
annulus is equal to the weight of tpe plu1.nmet. The flow m�y be read t'.\11, � Loss ofhe�d due to sudJcn cnlargemenl, m.
usin!' the upper edge of the plummet as an index .. The area 1s prorrrly
_ t.l lc =- Loss of head due to sudlh:n contraction, m.
calibrated'. to the flow rate-.: The reading' may be'1trn11sm11ttcd for record- ' :I
ing: integrating ·and controllir1g:. j •
!.'ii Ip = Diffaence in- head from manometer in pilot tube, m;·
 54 PHARMACEUTICAL ENGINEERING Ch·:? Fl.OW Of' f'LUIOS 55
�h = Height difference between t,vo points,' m. 4. Describe Reynolds cla�sic experiment elucidating different l)'pcs of no,v.
r ... '""" "
path:ms, when a liquid nows lhrough u ·closed channel.'
L = Length of pipe, m.
s". Expl:iin 1hc choroctcristics of different types of now. Add a note on,
P = Pressure, Pu. ReynolJs number: r, �,:; •
P5' = Pressure on the column of a liquid, Pa: \1mp11N 1111d 11lrust lhe .idv,mtagcs and disadvantages of pitot tube and
�.-
(1,
�Pr= Pressure differcn�e-· due to friction,' Pa. rot 1111ct1:r.
Re � Reyl)olds number. 7, Wh t urc the mcrits and d�mcrils of vcritur"i ni'cter over orifice me,tcr? '
p = Density of•the liquid, kgtm3.,., ) 8. Wh.1t Is 1hc ·ondition of hydr�static equilibrium? Obtain the barometric
s_.=,Surface area 'of.the liquid column, m2. equt11lo11·.
u = Velocity of the fluid in pipes, mis.
�nch <JU tlon curries 10 marks
w = Enet_"gy 'head added by the pipe, J. ' 'j

X = Height of the liquid pipe from horizontal d.:tu� •. m. I. I ·duce rck\'ant equ:i:ions for calculation of flow rates using .orifice meter.
:?. cri\'C Bernoulli's equation stating the assumptions. •
' ) ,, ii 1·c a n,;al skclch or two nuid manometers and, explain its working
:; t � • .; l

. QUESTION BANK
principle.
Each question carrits 2 marks
4. E:,..plain 1he working. prim:iplc and con-s!ruction•o'fvcniuri meter. Writc"the
I. Draw a labeled diagram of pilot tube and explain the working of the same. c.,prcs::ipn ·fonhe v,olu1111::1ric llo.w talc or lluid,throJgli it· . � ', ,.
2 .. \Vh'a� is thej �s� �fa pi�ot tube? �rite ,its advantages and disadvantages.
i
5. E:--pl,1in .thc;cncrgy 'iosscs that' m:cur · �"iicn a fluid llows• throug�"a pipc1 {vith
3.�',V�ite the Fannings equation �nd explain the-trrms. What is its importance? rc.h.:,·ant 74u.itions. ;1 f �,
4. Express the Hagen-Pois�uille's relationship. What is its importance?
5. Explain the term ,\head'. List the different heads in the Bernoulli's theorem.
. What is meant' by-'equivalent pipe length? What arc its applications?
What is Reynolds number? Describe its importance.
, ,8. List the advantages and disadvantages of rotametcr.
. ,9: How arc losses of energy due .to enlargement in cross section measured?
' · .',.Give relevant equation -and explai11 the terms.
'
'

I 0. Giye Reynolds number and explain the symbols -used therein.

11. ,What is a 'differential head meter'? Name some devices under this
· · category;
12. What is a pressure head? How is it calculated?
�·' 1'3. What are vertical head meters? Describe one :o:uch meter. '
14. Differentiate between constant pressure and constant area meters. Give
exai:nptcs of devices under each category.
'1

Ellch question carries 5 marks

I. Describe the types of flow patfpms exhibited by liquids in motion.
2. DifTcn:ntiate between fluid statfcs and fluid dynamics. Name the fluid flow
meter, which gives point velocity.
3. Write ncrnoulli's equation- and expla, in• the symbols usc9 therein with a
labeled diagram. i fl

J
 57
• Ch-3 TRANSPORTAT.ION OF fLUl[)S
. of semisolid preparations
5. Scmi-;olid pha rmuccuticals : In case
ined by passing the'.n
(ointments. pastes etc.), fluid flow is obta
,.. it is' easy to handle them in
3 through a hot jacketl!d pipes. because
jl 11 iclisecl state i.mJcr molten conditions.
n of injcct!OrJS, ste�ilc
6. Injection dosngc forms': In the productio
the place ot production
Transportation of Fluids air nnd s\crilc wuter are transported from
to the site or manufacturing operatipns.
is the order of tne day,
' �. � I

111 this m dcrn age. wherein m tomation

number of innovative handling
Valves pham,:iccutical. industry has evolved a
Pumps ., techniques.
�eciprocating pumps · I,,'

, Rotary pumps ,· ' VALVES

· Miscellaneous pumps
• . . I '
., .· ,
Val�·es arc used to cont rol the rate of flow of fluids in a pipeline.
ng maintcnance.''bf pipes.·
,I

., The.,transp,orta\ion is involved in handling of the raw materials, materials Va l ves arc placed between pipes. Duri
disturbing the. other con- .
in m'anufacture . and finished· products. , Transportation is also important valves can be removed and repaired without
a manner that they should'
in . mixing, conveying them for, filtration; ,,.filli,ng .. ,into the containers. nected units. Val:vcs are designed in such
sealing ·et,;. Transportation of fluids ·is more convenient and economical \Vithstand the following cffrcts:
than· transportation of sol ids. The ip1portance of transportation of fluids Pressure· of !low.
is highlighted in the following areas. - Tc1nperature changes.
I. Bulk drftgs : Specified qu�ntities of reactants arc transported to Strain from connected pipes.
the reactor. For example, gases such as chlorine and hydrogen Distortion from the sealing surfaces.
as brass, iron, bronz�,
are passed (in chlori nation and hydrogenation) into the react ion . Normally. valves are made of 1n aterials such
mat,crials that may come 111
system. Similarly, large quantities of water are transported to and cast iron, depending on the nature of
igncd. Some of them are: ·
heat or cool the reaction vessels; contact. A number of valves have been. 'des· -"""
,:: 2. Fermentation products : Medium constituents are transported to (I) Plug cock va lve
the !ermenter. For example, sterile air, nutrient broth etc.,'"llrc (2) Globe valve J
pass.ed into the fermenter. (3) Gate Yalvc . (

(4) Diaphragm valve

3. Liquid oral pharmaceuticals : Production of dosage forms, (5). QO (quick opening) valve
such as solutions and elixirs, employ fluid flow. In the produc-.
. (6) Check valve
tion of liquid orals, production operations are conducted in the ons.
first floor. The bottling and packing arc carried out in the These arc discussed in the f6'h.owing- secti
..i-�
··
1
ground floor. Therefore, fluid flow in this case involves gravity. Plug Cocks .
3-1.
4. Suspension dosage forms : In the producti;n of suspensions, The ·c onstruction of a plug cock valve is shown. in. Figure
ing in whic h a coni c� ! plug
fluid flow is obtained with the help of a pump. Normally. it is a Essentially plug cock consists o( a body cast
cal bore) through which the
mixing process. When suspended solids settle at the bottom of is (ittcd. The plug has an opening (cylindri
included aro�nd the st�':1. to
the tank, these are pumped to the t�p of the vessel continuously. liquid passes. Some packin_g materials arc
be parallel or tapered- too
· close it. The sides of the plug· should not
lete opening or complete
much . These valves are used when either comp
56
cl o ing is desirable.
 58
59
�,�.
PHARMACEUTICAL ENGINFERING Ch-3 TRANSPORTATION or, r-LUIDS
I '

,,,
I
The passage of fluid is through a circular opening, which can _be opene·d
Stem CI:', ' Packing or closed by inserting a disc in the opening. ·
· � ' , material

' ·· Conical
plug Horizontal
I· .
. . partition
� Figure 3-1. Construction .of plug vafvi.:.
.
Cocks of wi er esigns are available with
. � � specially shaped openings, High
\\he r: the opening is nearly proporti_onal to
the angle through which the pressure
pl�g .1s turned,.
side Seat
·c
lubmc�: ci�l.dcsign �·,alves include ,tubricants at the stem of'the cock. This Figure 3-2: Construction of gfobc.v.alvc.
.:ant is transrrptted t�. the working faces
through· small holes drilled
I '
' •

through the body of the 'plug.
Uses : (I) Plug cock valves are used for
(2) ':hc�c arc u c d for the purpose
�_
closing cond1t1ons. .
.. . ,
,°.isadvantagcs : Though it is simple, it has
.·
" Tl:c disc is positioned on.the ring, \\;hich is kno{vn as seat ring. The
disc can be rotated freely on the stem. Globe valve is install�d in the
handling compressed air.
1 high-pressure side connecting•\::i,e narrow portion of the disc. Globe
of. wide opening or complete valves can be 'connected in horizontal lines as well as in vertical lines. ,,
The main difference in the variety of globe valves 1s the construction
of the valve, namely disc and , alve seat. Nonnall);, ch'eaper valves, have
· st:veral disadvantages ·
1

These are:
no separate scat ri�g., Good valves have _the seat ring, which pe.rmits,.the
( i) Plug cock v.ilvs:s a�e not suitable. for ease of renewal. Angular valve is· a modification in which an etbo·w
stc�m or water. because of
the cock material. · fitting and a globe valve are combined in one compartment. ·, ,
(2) !t is difficult �o turn the valves when
the plug gets easily wcdoed Uses : Globe valves are main!/ used in pipes with sizes 1101 larger
111.the body tirmly. This problem is observed than 50 millimetres. In horizontal lines, these· valves prevent complete
when the side; of
the·.plug are too nearly parallel.
·· drainage.
(3) Sometimes the plug comes out of its scat,
if the plug sides arc Disa,Jvantagc:S Rust·, scales or sludge prevent the opening of the
Japered too much.
valve.
(4) It is �ifficult to regulate the flow. Ji, norm
al designs, the area of
o�e1�tng changes rapidly even with slight Gate Valves
rotation of the .stem.
�lmtlarly, flow does not change appreciably The construction of a gate valve is shown in f-"igurc 3�3. A wedge­
when the valve is
op�ned fully. shapcd. inclined_.�eat type of gate is most commonly used. The pressure
on the gates is .control )ing factor in large valves.
Glo�� VaJ,,cs , :·, Two types of gate valves are available. In. non-rising stem valve, the
'fhe co�st;uction of a gl�be _valve is. shown
in Figure 3-2. A globe thread of the valve stern ·engages the gate. The gate can -be raised and
valve consists of .a globular body with a horiz
ontal internal partition. lowered without the movement of stem through the stumng box. The
ndvantage is that the overall length of the stem required is fess. In the

/
60
rising stem val Ye. the length of the stem is more, since the stem and gate
l'IIARMACElJTICAL EN(ilNFl:RING
Ch-3 TRANSI•bRT'I\TION OF VLUIDS
- 61

are ,(single piece. ., · 1

,
Uses •: Dilppragm valves are more suitable for fluids . containing
suspended so.Ii! stSpccjal types of diaphragms can. befe�as[ly, sf�riHs�Q so
'·t
\.- J •.

that they
'
can used in the produc�i.on ofsfcrile produc'ts.
l, . . • . ' '.,.' .·
· · Adnrnta.gds : ,(I) Diaphragm val;es, can- be installed i� any posi!ion;
· (2J Pressure drop is ncglig,(1,l?l.C·
t. t"

(3) ��omplc-� draining in ho(izontal lines is possible.

1� '
(4) Simple. • ' ,.

(5) Excellent operation (perfqrmancc). · , ' . '

,, i,J. \.
I''
(6) �<:placement of'diqphra'gm is easy, t�7re is nq need, to.,reJl)�ove
th.c valve from the li;ne. , ,, i; :

Disadvantages :' (l) Diaphragm'\'alves ar� applicable' to pressures• of

approximately 340 kilopascals.
Figur.c 3-3. Conslr�ction of gate , .Ive. ' 'J . . ' ,,,. ·. ··¥' ,. .. .
(2) Maintenance cosf (·increases' b.'ecause 'o f . 'replacemerlt of' faulty
Ari vantage� : (I). Ciate valves are avaifablc in large sizes. diaph�agms. · · · ,,, · ' · w·,,1, ' ,:
' (2) These are available in a variety of,dcsigris to suit the conditions. . (3) Th�se valves are expensive. .• ' I

-1'r ; . · . � '!.: JI,..

(3) Gate valves minimise the differential pt·ess'ure during opening ''"\ i

:i .. ·' · and stop�ing· the flow.

Quick Opening Valves (QO Valves) .n , . : , ,
• � ·'� 1 �·
, . ' , • / , , ,it�}· .": 11 In the gate t:ilve. stem is thre'aded:'· Therefore, a m1mber of'turns are
Di apqr�iw Valves necessary to clpse the v'alv.e co�pl;ete,ly,.1 QO valves have smooth _stems
Th�.� cor.1struct;on of ,.a <l,iaphrag� v�!vc is sho�n in Figure 3-4. and are opened or c!osec;! by lever handle in a simple operation. These
Diaphragri; is· a flexible physical. ba�ricr. These valves arc made of are convenient( ·�It involve tht danger ·of W�te{harnme'i". ' '· ·
• . . ' .: .f•. : ). .:r
fabric reinforced, natural rubber, and/or synthetic rubber faced with
I ,l ' '• • •
I ' �· !�'·' ' • ,, . • ·' _i ; ,; ; •'
t: :
Water. haip1n.�r : When a liqui,d .is. f)owirig in <} ,pi,pe, i� is <}Ssqcia,teq
' ! ' ":"'

Tefl on, a tlu'rocarbon resin. · . •. with consid�rhble kin�tic energy due to its ma�:; aod ·velocit)'. Wfel n
<·Spechll .grades o.f .,rubber diaphragms c .o atcd with PTFE such a ·flo\v :is suddenly stopped,. the velocitx is -.�\1dd�n!y destrqyed.
(poly(etrafluoroethylenc O{ teflon) are resistant to repeated steam stcrili� Since liquids re incompressible, the energy appea'rs as an intense shock,
sation. Som'etimc's;· t is':shd'ck1 ·caf r be about·60 times the ,veloc'ity of the fluid.
p
i· '/ St�m.,., Hence, QO v Ives are i.;scd only in _short lioes ..on large',Hnis, the valve
ShoqJ. d be cl scd-slowly, ..; ! .,,./.
Check Vah s ·
The:.;.: v. ves,arc used, when unidirectional flo�v. rs des.ir.1ble. Pr.otcc-
. ,. '. �- ..�.i.;
. " . .

· tivc mecha ism is included to prevent the reversal of now.· These are
aut()mati(al y opc1iccl,, wlh·n the .. ilow of fluid builds up the pressure.
•
u 'e ;\, 1

(a) s, ·ing che.ck:.:.

Diaphragm (b) I� fl check
·, (c) Li t check. vertical.
F.igurc 3-4. Cons�ruction ,or .a diaphragm valve. Thl' con�tr iction of check \'alves is given in figure 3-5.

·,
62. / PHAllMACEl)TICAJ,.. ENGINEERIN(j
C:h·J TRANSPORTATION OF FLUIDS 63
reciprocating pump, .the pu�ping clement moves forward (down .stroke
or delivery stroke) to push the liquid out as a discharge (output), later it
recedes (suction strike) to draw the liquid in as an i1)put. Normallv. the
pumping element is either a piston or a plunger. ·
"
The reciprocating pump is a positive acting type. i.e., � displacement
pump. The pump creates pressure and Ii fts the liquid by the displace-
.
{,f Swing check {b) Ball check (c) Lift check
'

ment of a moving member. · ·

vertical
Figure 3-5. Construction of check vah..:s.

_Valves arc classi tied depending· on their functions'. These arc: Uses : These are used .for injection of small quantities of inhibitors in
·,

polymerisation units and corrosion inhibitors to high pressure systems.

Rec.h.icing' vah·'es : 'These val�es arc · used i11 order to 111aint�1in
These arc also. used for boiler feed water applications.
uniform pressure in one ·pait of a system lo\�cr than the pressure in
anot� , er part of the. syste111. These valves arc n1crelY. a �pccial e�se of Any form of power may be utilised to drive the piston rod. The
regulating valves. . .. · .1 · 1�ovements may be applied through' a piston rod or a crankshaft using
. ·
'' .

,:: T�_cse v""lves.. are i�st�lle,d in .;l. high pressure st�am line to give a either steam (steampwnps) or power (power pumps).
.
cons\ant, but_ lower pressure ofsteam in a steam coil. Steam reciprocating pumps : In these pumps. the steam cvlinder
Regulating Ya Ives : These valves arc used to control ;the flow so as contains a piston, which is directly connected t� a piston,: rod· of the
to maintain some other variables such as temperature and concentration water cylinder. This is the most common in reciprocating_'purnps. Steam
at cor:stant ·values. pumps can have one steam cylinder with piston (simpl�X: pt11n1,'at steam-.
., end) or two cylinders· eai;h having separate piston (dupfox pump· at
, I

steam-end). Normally, these two cylinders are mo:.rnted side by side in

PUMPS the same casing. . . · · · ·
.
I

Pump is a m:echµ.nical device. to ,increase the" pressur\c enei·gv of a

, , �.Ii'. i •J , , , , • t .,_,. -�
. .
Power reciprocating pumps :.The power pump<; includ� all fonns of
liquid. In most ofthc �ases, pump is used for raising tiuids from ; lower
reciprocating pumps, in which the piston is actuated by some. form of
.leve"i -'f-0-·a higher' kvel. . A nur11bdrtof pumps have been\, developed to
energy other than steam. An exainple . is an electric motor. The
mc:et a variety of opcrafing conditio ' ns. Their pri14ciples of working and
movement of the crankshaft is usually through gears by ;i .belt from a
construction are \viclely different. The classification of pumps arc:
line shaft using an electric motor. The c9mmon' fonn ofsuch �·pump is
Reciprocating pump�, cxampJes are pi�ton pu,m. p, lunger · pump· the vertical, single-acting triplex power pump. .. ·
•

, :·. , -
·\ , .. j1 . '· I .

· :and'ldiaphragm pump. In gen<.ral, the reciprocating p_umps are classified based on the con-
Rotary pumps, examples are centrifugal pumps and gear pumps. struction of wa�er cylinders.· Ttiese are ,two types. J
(a) Piston Pumps
Miscellaneous pumps, example is peristaltic pump..
. .
(b) Plunger Pumps
Some of them are'·di'scussed in the following sec.tions. · These are discussed in the following sections.
..
,,., '
. r· Piston Pumps
' '/.
,{
•··

RECIPROCATING PUMPS "

In piston pumps, the piston reciprQcates in the enclosed space of the
In reciprocating pump�. thc·pumping clement moves in forward and
water cylinder. The piston carries the packi'ng material, along. :with it.
backward ?irect_io�s in cylinder. This c�linder 1is kno1 n as �1•aier
'.a
_ As the piston moves,\the packing material also moves alon g with it. The
cylinder, since 1t 1s tisually used for pumpmg of watei:. v_In a simple
eneral classification of piston pumps is given in Figure 3-6.
0

•
• I
,·.( , "•\...) ,' •
'
•

I
\
64 l'l lARt-.1'\tTUTIC'Al. FNCilNl·.l'lliN(j

Piston Pumps
l'h-J ·1 R,\NSl'OIU"ATION OF FLUIDS 65
liquid out of the cylinder. Single-acting pumps have limited capacity in
l Number. of water cylinders
handling iiqui<l Jnd the discharge is pulsated.
l
Simplex
l
Duplex
l
Triplex 2. Double-acting piston pumps : These displ.ace wale� on both
piston pumps piston pumps piston pumps" . halves oftht: cycle. Such a plimp requires a niinimum o_f four valves. Two
.,
Drive ·mechanism valves arc used for suction (to receive fluid) and two valves 'are mea11t
for pu1nping the liquid out. Several valves arc used in order. to pump the
l l d1scliargc :it high vclo!,:i_ty and more volume of water, during one-h.alf of
Simplex, single-acting Simplex double-acting
piston pumps piston pumps the stroke. The mechanisms of action of these valves are illusfrated in
th-: sirnpkx, doubk:-:iction, steam-driven, deck-v:J.lve, piston pump, which
,---Gased on type of valve "'_•d · is given in the later section.

Simplex; single-acting.
l
Simplex, single-acting,
Since valves .ire employed in the pumping. the construction of valves
is important for its effective functioning. These
. are classilied -as follows.
deck-valve. piston pumps p�t-valve, piston pumps
- Deck valve .
•'
·
Figure 3-6. Classification of piston pumps. Further dassili· - Pot valve
cation for duplex and triplex piston pumps follows the same
• · ;sequence as that of simpl.:x pu1np brunching. DL'ck 1•e/re : In this valve. springs arc attached to the stem, which
f
hold the valve disc against the valve scat. The valve is :.i non-returnable-,
Piston pumps are classi ied based on the number of water cylinders. one way. s� that the tlo\'.... is unidirectional. For high prcssur�s deck
iYymber of Name Connecling system from vaive is not :suitable. Some times: bigge; sizes of'deck valves are
cyli1,ulers · steam end to water end 11ct:1:ssary to give a high-pressure discharge.
Pol 1Yilv.: : Pot .valves usua;irf have m�tal discs. which are often
·one Simplex piston rod is joined
provided with gui'<l·c vanes to keep the.m in right alignment. The valve is
. Two Dup_lcx pi�ton rods an: joined scparntcl)
a non-returnable-one. way, so that the flow is unidirectional: These arc
Three Tri'plcx piston rods arc joinc.d separately requin.:J,. when 111.!ids arc handkd at high pressures. In dst: or viscous
liquids and liquids with very, hig.h· pressures, loose metal .balls arc used
In a dupl_ex pump, .'t�vo water cylinders are arranged separately side in place of the v._:ilve disc, since these �re not· strong enough �o withstand.
by side in the sa111<! frame. Their piston rods are connected separately to
two steam cylinders, which are also arranged side by side in the same . The general principles described above arc combined and illustrated· ·
frame in the· steam end. Connecting several cylinders has an advantage using a model piston pump given below.
of making the di�charge more uniform and free from pulsation. Simpl�x, Do�ble-Acting, Stcam-DriY.en, Deck-Valve, Piston Pump
. Ea�I{ wat1:r cylinde� .may have diffe,rent drive 1�e1.:hanisms and further i
Constru�tion : l he construction qf a simplex. do,ublc-acting,. steam-.
cla�silied as: µriven deck- valY.c, piston pump is shown in Figure 3-7. In the water
I. Single-acting piston pumps: cylinder, a piston cons,sts of two discs with rings. of packing bdween
2. Doublc�acting piston pumps them. Thcs.: arc arranged such· th�t outer packing can be drawn up to
. 1. Single-acting piston.pumps :. These displace water on one half compress it> -The piston m�y operate· in a cylinder bored directly in the -·
of the cycle of the piston movement. norm�ll.y during the down,strokc. pump casting. In s_omc pu.mps, the piston operates in a removable
bronze liner.
During the other half of the cycle (backward-stroke), the cylinder 'J

receives the fluid. S4ch ·a pump requires a minimum of two valves: one
for receiving ·the liquid into the cyli11der and the other for pumping the
. .
This pump has' four valves, i.e., double-acting. · The lower· row
valves, EI a'tld E2, arc suction valves and the. upper row valves, F 1 and
F2 arc dischar;:c valves. For this purpose deck valves are used. The
I
66 I
PIIARMACEUTICAI..ENGINEERING
.• ,t •
(h.3 l lUNSl'OIUATION 01 l'lll!DS 67

valv,e pisc is mad� . of hard rubber or metal. The valve is a non­ the cycle. Large volumes of fluids and at high velocity" can oc trans-
returnable-one way so that the flow is unidirectional. ported. since four valves arc used..
I
'/ Q •, . Discharge Uses : Piston pumps are used for l1.cads
. up to 60 metres. These
Delivery ·
pipe Piston pipe pumps can be used, if the liquids are not too. viscous, corrosive or abra-1
� Discharge valve, F 2 sivc. Pistqn mechanisms arc employed in peristaltic . and HPLC pumps.
.p
Discharge Applications : Piston pumr.s arc extensively used for spray system in'
valve, Ft ----..i....&---..r-1------.,,.,,J!'�,-r--, Piston rod
(closed) sugar coating and film coating operatiOf!S.
·?:: l?aal-----=-----"-a, � Connective. shaft
to piston end Oisadva n .tag cs : (I) Pi::.ton pumps arc relatively
•
ex1;cnsi(c.
l • . ·. .

Suction i' (2) 'These arc not easy to dr.<111.

Suction valve, E 2 • <.ti:\ . ., '
valve, f1 (closed) (3) P_iston pt,rnps induce coagulation of lat1:x co:-iting systems under
(open)
Packing Water conditions of sig,nilicant line pressure._
material cylinder
Plungrr Pumps
Figure 3-7. Construction of simplex. double-acting. steam-driven.
In p/1111�cr p11111ps, a plunger 'reci1,rocatcs in cnclo;�d space of the
deck-valve piston pump. Working principle· is illustrated.
water cylinder. The term plunger refers to an clement. ,,·hich moves
Working : Steam is used at full pressure for' the 'entire stroke in past tl1e stationary packing. The general classification ts given in
order to maintain a constant oressurc on tHe water end. This enables the figure 3-8.
pump to produce uniform discharge (output). The steam pressure set� Plunger Pumps
the piston in 'motion at sJe�m end. This makes pis:t�n to reci. procate i11
-- Number of water :cylinders
the water cylinder.
The valves are unidirectional. The movement of the piston creates Simplex · Duplex Triplex·
vacuum and atmospheric pressure forces the water tip through the sue ... plunger pumps plunger pumps plunger pumps
tion- pipe into the cylinder. The liquid pressure in the water cylinder ·
Based on_ the placement of packing material
allows the discharge valves (or delivery valves) to op'cn.
1
Wh�n the piston is moving' fro� left to right, the events..occu� in .the
Simplex, inside-packed Simplex, outside-packed
following sequence. plunger pumps P.lunger. pu. mps
left side cycle Right side cycle Method of packing material
fixed to the cylinder
E1 (suction) valve opens : Water l:2 (suction) valve closes : Water do�s·
7
enters the cylind�drom left side. not enter the' cylinder due to pressure...
Simplex, outside­ Simplex, outside­
Fi (discharge) valve closes : Water F2 (discharg�) valv� opens : Water (that e;entre-packed, plunger pumps end-packed, plung�r pumps.
will not be 'discharged from this . is already present iri the water cylinder) , ,
· I Based on t�e of valve:used
left side. · · · _goes out through the discharge end:
0
.--������-'-��---.;.,,
The/efore; when .th�-piston mov�s from left to right, w�ter discharges Simplex, outside-end-packed Simplex, ·outside-end·pa\:ked
throu·gh ·the valve, F2. When the piston moves in the reverse direction, . deck-valve, plunger pumps pot-valve, �lunge.r_ !)umps
i.e., from r.ight to lcfi, i_t provides disc �arge from valve, FI· Thus, the Figure 3-8. Classilic�tion of plunger pumps. Furthc/�Jas- ·
pump is a do�ble-acfron pump, since it displaces.water on both halve� of silication for duplex and triplex plunger pumps follows
the same sequence as that of simplex pump branching.
r
 >'
69 .•
68 1'1 IARM,\CHITICAI. ENGINEF.RING Ch-3 TRANSPORTATION OF FLUIDS

The general principles described above arc combined ·and illustrated

Number. of qiindt::r.� Name Connecting system from steam ·
end to the wa/t:r end
One· Sim�lex plungc:r rod vi;1 shall
Two Duplex via crankshaft
Three Triplex · via··wmkshaft
When the number of,. cylinders is more, these arc connected in
parallel to .t crankshaft. For example, in a triplex pump, t.hree plungers.
arc connected to a crankshaft ut points 120 ° apart.
Connecting several cylinders has an advirntage of m:1kin12 the dic;­
charge more uniform and free from pulsation. It is better to t�c sl:!veral
cylinders each of small size, tl:ercby it is easier to huild up high pressure
and maintain packing. . .
. Since packing m�t�rial i� permanently fix�d in the, water cylinder, it
cnn be placed in any position. Based on its placement, plunger pumps
are classified :1s:
(a) lnside-p:icked
· (b) Outside-packed
In �(��-p.ickrd plunger pumps : Packing m.aterial is pennancntly
_
t1xed J11s1Je thl! ,,ater cylinder, ,vhicl, is enclosed in .the casing of the
pu1��· Replacement of packing is difficult, because the entire casing has
to be di.srnantkd.
· 0utside-packed plunger pumps : In many situations, frequent re­
placement of packing material. is desirable. If pumps arc larger in size.
replacement can be made easy, provided packing is made· outside the
pum� : Normally, replacement of packing is more frequent, if the liquid
, :
� onta1�s suspended solids. Therefore, outside packing fa more con�e11-
1ent to handle such replacement because of its rtcccssibilitv. Further.
outside packin� can· be done in two ways.
Outiide-cehtre-packed ptung�r. p uinps: In this type, the· stationary
packin& material is placed at the centre of the water cvlinder. Though
the water cylinder is accessible, still packing is not e;sy to replace �r
repair..
· ·
;; 011tside-end�packed plun�er p ump� : In this· type. the liq�tid can be
pump�d at high pressllies, because packing can be more easif'y fuain­
tained. Repairs and detection of leaks are easy, if the packing is outside
and end-packed in a water cylinder: · · ·
using � m(?del piston pump given· belo�v. ,
er
Uupkx Outside-End-Packed, Power-Driven, Pot-Valw, Plung
i>ump
Construction The construction of the water end of a duple:-:
outside-end-packed plunger pump is sho,•.;r1 iri figure 3-9. In the pltinge:
pump: a plunger moves past the stationary packin2,: Sin :e the pump i;
. duplex, the water c·ylinder is divided into two ·pm1s (A and B) by a
partition. Two plungers arc used. Both halves of the p'.ungcrs A and n
a1c connected. to the same driv:'ng mechanism and power supply.
Di�charge
. valves
Plunger
�·r---------
.....
/¥ Cc,nnecte:l
Plu(lgr,r to crankshaft
rod
S.iction
Su(tion
val'lc valve
Figurr 3-9. Construction ()f duplex outside-end-packed.
plui1gapump. Working principle is illustrated.
h becomes necessary to replace the packing more frequently, particu-
1:irly while pumping liquids containing solids. It involves the dismantlin�
of the plunger. Many a times•. packing should be checked for. \�ak:..
Hence. it is placed at the outskk-end due to itG case in rcplaccment and
maintenance. The pot valves with meta'\ discs arc used. If it is desirable
to handle liquids :1t very high pressure� and · for viscous liquid. valve crr�c
is replaced by metal ball in the valve construction. Each plunger ,· s
. and one discharg- e va-fve.
rnnnl.'ctcd to one suction valve
Workin� : Through an elcclric rn.otor the line shaft is rot:itcd. which
Jurther rotates lhc gears through a belt. The gears set the two plungers
in motion in :he two waler cyl;ndcrs (A. and B). Eai..:h plunger is
nlllllCl:l\:d to 01,!7 ·S\ICtion' va\V� ';:ind one disc:hargc· valve.
 70
1'1 IARMACEUTICAL ENGINEERING
The. v_ ,alvt!s a re onc-way so tI1at Ch-3 TRANSPORTATION OF Fl,Utbs 71
· i s unidirectional. The
t I1e fl ow.
moveme. nt. of the · plunger creat
es vacuum and atmospheric pressure bottom. Diaphragm is fabric ated with the materials such as metal,
�orc�s the wate� up through the. suction pipe rubber and plastic.
liq� 1d �r,tssure m the water cylin into the cylinder. The
der allows the dis�harge valves (or
deli�erx, valv es) to open. Working : Through an air chamber, suction is a,pplied so .that �he
, r
. }he two plungers arc a)!owed to ncxiblc diaphragm is pulled up (expanded). As a result, the _suction
reciprocate. in su�h a manner that at valve is lifted up and the liquid enters the water chamber.· When
any morn,ent , water enter s into left-
side cylinder, while waf
_
throu�h t!1c nght�s1de . . er discharges sufficicn� pressure i. s built up, the liquid lifts up the discharge valve.
. cylinder or vice versa. This ensures
pump mg ()f water (non�pulsating) continuous Then the liquid !lows out'. At this stage, both valves arc opened so that
. , .. Large volumes__ of fluids at. high
veloc1ty ·can be transported, since fou suction and discharge operate simultaneously. There t"<? re, n on�pul sating
_ r valves a r e use d. in this
case. . . discharge is achicvl.!d. Thi!' stroke can be varied arid 'di�charge. can be
Uses : Pl�nger pumps are suitabl · · · ·
e for handling liquids
at high controlled within ac curate 1imits.
pressures. Viscous liquids can be
transported. These arc used for'
transporting liquids C()ntaining susp lJscs : Diaphragm pumps are used_ in tr�nsporting liquids containing
ended solids'.
solids. Hazardous, toxic and corrosive liquids can also be haii�led.
Diaphragm Pumps
Adrnntages : (I) Diaphragm pumps are simple' and r�ggcd.
The diaphragm pump is classified und
· er the category of r� ciprocatino (2) They can be casi ly rr.:paired.
pumps. 0
. . . (3) The rate o f discharge can be regulated.
. c__onstruction : Tbe constructioi1 of ·a diaphragm p�mp is t4) Packing and seals o f the- diaphragm pump arc not expose� to .the
F1g. ->-I 0 It con 1sts of two secti show n in
_ : � ons scparatrd by a flex fluids. 'f
with a ffap of discha rge valve at ible diaphragm
.
the centre and su ction valve at the j·,

Recip roca t ing Pump Theory

'
.
.
�
Air chamber As. mentioned in the constru ction of pumps, all spe cifications o f the
pump should be mentioned, while procuring a rcciproditing pump. Spe,�
I cial attention is paid for the followii:g spe cifications in the or�er.
I. The size ,(diamet�r)' of the steam cylinde r, because it regulates.
. the pressure to be generated pn the piston in t he water cylinder.
2. The size (diameter) oi/•(.1e water cylinder, as' :it controls the
· desired di scharge.
,,· ·

''-liquid 3. The length of tmv el of the piston.

. . ;·. �. Since piston displacement is essential (or the discharge of fluid, it is
.. outlet
necessary ·to evaluate the water' cylinder in quantitative tcnns of effi­
_
Liquid ciency. The displacement in_ the. waler cylinder may be theorettcal_ly
. ':··,.� · chamber · expre�sed as:
11zeoret ic.:ai dispiacenient
piston speed (m/min) x

r
, f do11bie-acti11g
o
area of the piston (m2) (I)
pump (m3/min)
· Tlzeoretica{ disp/aceinent (1/2) piston speed.�.
·t-: Liquid.inlet
of single-acting - area of the pi�ton ' (2)
F.igur� 3-10. ·co�st��tion of a diaph ragm pump. p1imp (m3/min) .

I
72 /
PI-IARMACf:UTICAI. ENGINEERINC. Ch·3 TRANSPORTATION OF FLUIDS 73
When the discharge is . equal to the theoretical displacement, then Several measures may be followed' in order to obtai_n desired naltire
displacement is ,considered as l 00%. It is not possible to ac_hieve I 00% , of discharge as given below. ... . ., ,: .
theoretical displacement,.as there are losses during the functioning of a
·- i>ulsating discharge can be removed by using a duplex pump,
pump. These l!)Sses are due to:
with a piston set half a �troke apart (Figu�e 5-11 b). ..,, . ', 1·,.
• slippage past the piston ·• imperfect packing
··· For high pressures, a triplex pump is more suitable, since · it
• leaking o� �alves . • failur� of a valve· to close instantly
avoids shocks and pulsations. The theoretical discharge from a
In practice,' the actual .discharge could be 50 to 90 .% of 'theoretical triplex pump is shown in Figure 3-'t t c. ' .
displace,ncnt. The actual discharge is known as vo{u�netric or water-':nd · - For VCI:}' ·high pressures, pump with five cylinders on a single
� l''(\11" • • t.

efficiency� Normally, low-speed pumps are more efficient, provided _ pack­ · crankshaft is employed to make the·dischargc still more uniform:
ing o� the materi�I and valves arc in good condition. The lower figures
_ -- A large air dome connected to the discharge sicJe further reduces
of water-end efficiency represent poor packing of pumps and working at
the fluctuations. The air in the 'cylinder will be' compressed,
high speeds. _Such conditions produ�e excessive wear and tear on:
when water piston is accelerating and will be expanded when it
• val'ves • valve springs •· packi11g 'is decelerating. .I · :
Steam -�yl.indcr end..: Since steam c.ylinder is responsible fo� driving
•1;., :· ;.: •

the pist�n in the water cylinder, the force applied is evaluated as:
Force acting un
�I

:steam pressure (Pa) x

. • �

fhe piston rod in area of steam piston (m2) _(3)

steam cylinder (N) Time
Water cylinder end : In the absence· cf friction, the entire forct'. . (a) Discharge curve .of a sin_gle actirig simplex pu"".P·
would ·be transferred to the piston of the water cylinder. Under ideal
conditions, 'it is expressed as:
force acting on the piston rod (N) .' • \I'

Theoretical maximum (4)

water-end pre;sure (Pa) . area of water piston (m2)
Time-
Normally; it is expected that the piston remains stationary, if the tot:,!_ . (b) Discharge curve of a single cylinder, double acting pump.
force on .the steam piston is equal to the total force on the water piston. ' , • I •

In order to do work on the liquid and to overcome pump friction, total

for.ce on the steam piston should be greater than the theoretical force
theoretical pressure on. ' ,
Steq1n-end dr · the steam p_i...:.. ston (Pa) _ x ,,'<-_
,= _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _
.
100 (5)
p,:essure efficiency actual pressure needed (Pa) ·Time--•
1
(c) Discharge curve of singhf acting tri;l�x pump.
. Thi� .efficiency varies from 60 to 80%.
Figure 3-11. Discharge curves of differcnt pumps.
Natu.r:� of discharge : TheJiquid discharge in a single cylinder :
1:•.:''
pump is shown in Figqr� 3-11. ln a single cylinder pump, the discharge
is zero at the beginning of the stroke. As the piston reaches full speed at .ROTA�Y P:UMPS
'1
\
'
the centre of the stroke, the discharge rises to a maximum. From this
I �� '\

Rotar pump is the one by. which the liquid can be ttat,1sporIted based
. . . .
y
point, it -decreases to·ze.ro at the end of the stroke. Thus the discharge is
on the mechanism of rotation of one or more 'elements within a station-
not uniform, 'but pulsatihg (Figure· 3-11a). '' ,·>'· ·'' 1'� . ;
ary casing.
,, {1 .·:1! 'l_,, I'

·,
 Ch-3 TRANSPORTATIQN OF
Fl.Urns
74 Pl li\RMACEIJTICi\l. EN(ilNEERIN(j 75
Uses : A gear pump 'Can han . . '
Tlic pump consists of two ci1·cular discs with lobes. which ;ire geared. vegetable oil animal oil . dle viscous or.· �ea
.. : ... ,
vy liqu ids such as
gre es
. .
•�-:>each other or single circubr impeller with vanes. In these pumps, thi.: o I asses brine, semis9lids ari w x
· lt is extensiv�ly used i i/ aqu=� , � : d a es.
rotary mechanism thro\�S the liquid away from it and pumping is . w e ra ing. It ca.9 1 tr �nsfer liquids· 'of
id nge of viscosities., It is �:e; �:it
;ichicved. In general. rotary pumps arc cbssilii.:d based on tile naturl! or u n the spee . ds arc not ve!)' high.
�otary positive-displacem
ent (gear ti . ) p ump
force c;1pplicd in pumping. Thcsl! ;.m.:: . Uids that do not contai . P 1:1P is used to 'handle liq-
·c·· . . n ,abras1ve mater
ial. , . ·,, . ·,·, ...
l. Positive displacement pumps
11.' Centrifugal pumps
. .
� .,,
. Advantages : Gear pumps . . ·., .
develop h',gh pressure., .
It gi_ves,a djscharge
., "i
nearly free from fluctuati .
ons anJ ,_ndepe� dent of
, These are discussed ·in the following sections. . pressure. ·. .
, , . . · · · .· ,):, .d, , · ·
.
Disad
• vanta,i;e;s . G r
1ea pumps are not em �O . . ·,.. :., . .
I. Ro_tary Positive Displacement Pumps solids �n suspensions. It
. requires more· �: ) �� for.A�i��S,�,. 9rtat,1on of
It is likely that latex coa . comp Jcate c,le�:n;-up pro.
In rotary positive displar.:e111e11t pi1111ps, the liquid is mi.:chanically ting s ste m coagulate cedures.
dcvelopc;d as liquid pas �'}./�S�lt o( �iiear
displaced by. the.rotation (by prc�stire) of one or more clements within a s es th ro: h �mp. head. .
c�ccss_ivc wear of cle111 cnt 1�,:1s' �-�sq lik ely that
stationary housing. occurs :,hi�c pumpin . .
v1scos1ty coating liquids. g hi,gh,l� 1p1gmented, !ow
A va(i ety of rotary positive pressure pumps arc available with signi Ii­ .: ··, ..
cant variations in design. One example, iear pump is explained below.
• ·, ':- ':.�1-'

_It Centrifugal Pumps

,
Gear pumps :- The construction or a gear pump is given in Figure 3- ... The gcn�raJ constructio
n oJ centrifuga I �. umps . . . . . .
12. It consists essentially of two circular gears, which mesh with each lJ. In· · centrifqg is shown in Figure 3-
· al ·pumps ' tlfJ,e!'(f!'blad es of 11npeller ro .
other. Thes<:: run in close contact with the casing. The gears arc rotated red u ct1on in pressure . ta.te by· which a
. is I)roc I uc e d at its cen.tre (F'tgure ....
by some external :ig ency. As spaces between the teeth of the impl!ller suction draws the liquid . :,-J 3a) . Thi s·
0

in1, 0 the. pump (Figure

pass the suction opening,· the liquid is caught between them. carried • 3-1,3bf : the basic
around the casing t<.1 the discharge opening. The teeth come into mesh, /' Discharge pipe_
which forces the liquid out. The pump can work without valves also.

·Gears or
impeller

Suc.tion
pipe
.-- Stationary
<:a�ing ,,._,. Impeller

Impel!er � Volatile
I Liquid inle�
Figurc3--13,Th�gi,;·nc· . . . . ·., ·,. ', ·. ·
· Figure 3-12. Construction of a gt:ar pump. r,lI construct.Jon. and parts ·
.
. of a ccn tn·1·ugal ·pump. .
.
function of a: centrif
The number of teeth on each inipellcr varies from 2, 3 or more. The ugal p ump is to rod. uce ',·i � '·. .,', .
of ce1�trifuga,I force and k netic .��ergy b y tbe\ac,
two or three lobed pumps arc generally known as r.:yc/oidal pumps . .If then conve: ti s e:1er?y tio n
effectively reducing th�. u ?art1:aHy. t� ,pr . essure by
the discharge valve of these pumps is closed while it is running, the vclOCI·1).. ·r h US l1qu1d
pressure is built up inside the pump, which leads to either stopping the ·
pressure and then trans
ported. .
·
.
IS. p1.f
· � .�-� ,..out •at l11gh
. . . .-.�..,.,1.
a·· . ·
pump or b reakage. In these 'pumps, the discharge rate is directly , :·· ';.:·'II

p roportional. to the speed.

·.
-�... . ..
·, '�
'
7(> Pl lARM,\(T.llTICI\I l'l'J(jl:--ll· l' RING
Ch-J TRA"-SPORTA'.flON OF n.ums 77.
In short. the centrifugal punlp' hdps to rise liquids frolll a lower level
. Turbin e pump.� : A. pump in which a diff�si.on casing_ �qµipped wi�p
to a higher level by creating a ·required ptcssure with the help of vanes is known as turbine pump. In this type of centrifugal
centrifugal action. pump, a
stationary diffusion ring is interposed between the r peller
Centrifugal pumps have several advantages �uch as si!nplicity, low i:n and casing·
chamber. As a r�sult.' the change in the· direction is' smooth.
mainh;nat1CC requircmeril. (o\V initial fOSlS, (jlllCt •Operation and non­ 'without'
� . shocks ·during pumpmg. 'J heretore, It does not involve
pulsating flow. · These plm,ps occupy less floor space. Centrifugal e'nergy losses
_ due to eddies as observed ·in volute pumps. · Therefore.
pumps. can be built with corrosion resislanl materials. !hcsc have no
. arc more efficient. However, these are expensive. . tu'rbine · pump
. .s
limitation on the- capacity of the pump. Therefore, ccntn fugal pumps arc
found practically in every service. Single-stage p111nps : In thi� type, .01�c i1ripeller. is emplo
yed: Singlc­
stagc volute pumps are common and t,he cheapest. Howc
Classification' of centrifugal pumps : Centrifugal purnp5 arc classi­ ve��hei�
fied ba�ed on the type of casin.g of the pump, voiumc dif usion.. Such
f
�r efficicn,cy is the least. The single-stage, turbine. pu1np
maximum head of about 90 metres.
.,
c�n generate
a classifkation or centrifugal pump� is givt'n Figu1c 3� 14. j
.Multi-stage pumps : In this tyP,e, two or more i;1ipellcrs'a
re placed ·in
�entrifug.al Pumps series. The liquid from the tip ol' 01ie impeller is delivered
to the inlet. of
· the next impeller with minimum loss. Multi-stage
.' \ Depends on the t_vpe ot casmg volute pumps.are not
cominon, sinc'c �he losses in�t;i�h stage would add. up·
tea.ding to a 10\�
r _____i_::=____ 1 overall efficie+1cy. In turbine pump, multi-stage can
be employed· to
Volute pumps Turbine pump:; increase the ('fticiency of a pump. 1-.le?ds up to
300, met,res may b�
�ve mechanism generated. l·lowe,1 cr, · multi-stage turbin . e p'umps are more expensive ..
'.
These pumps (volute and turbine) are furthc.r·classified
� as follo,vs.· ·

· l·
· Single-stage vulu\c.pumps Muth-stage. volute pump�,; Ope1i-i11ipdler p11111jJs : In. this type, the impeller.is open'
to the vol�1te
(Figure 3-1 Sa). The fit bdwce,i the impeller and the'
Bilse� o� tl;e tri'.!e of impeller used casing is USltally
poor, Therefore. some part of the discharge 'leaks
r . --·--·-i (i.e.. back leakage). As a result, these purrips are' less
'to the suction-side
efficient' and also
Single-stage, ope11- Single-stage, closed- less expensive. Many small pumps of general purpo
se c9ntain open-
---,
1mpeller, volute pumps impeller, volute pumps
imp'ellcr.

Single-stage, open-impeiler, Single-stage open-impeller. . ,':'1'

single-suction. volute pumps double-suction. volute pumps ·,,

Fiourc 3.14, C!a:-sific,,1tio11 l,r ri:n1rifu�,1l pump,. Further cl.Jss1lil:ali11n n11 ' .

iuri,uii: pum·p� foUo,b 1h.: s.inh' proi:.:s:-- ;1� thal of, olut,: pump bra11d1111g.
I

l'o l uti: 1,wnp.� : A pump that is equipped with ,·olute ca�ing. i!> known . ·�.. \

as v;,lute 1 1111 ,,p. In this type of centrifugal pump, wate_ r entc1 1ng al the
_ ,
suction point is thrown outwards into the volute by the � otal1on _ �)f tl�e (a) Open impeller
curved vanes. As a result, .the liquid suddenly changes its d1r� ct1on 111.
(b) Closed impeller· ..
· Fig1:1r'e 3-15, P·ut�p· im_pcllers. . .· ,. 1'1 ,J • .,.,.,.

the volute, which decreases the velocity head and consequently inc�eases . ' ·\
.
the pressure head. Thcs.: chang�s facilitate, the_ pumr.ing of the liqu1�. Closed-i111peller pumps : In this type, the impeller
vanes are enclo·sed
the step to change the dircctio·n of liqu_id flow 1s not smoot�.. Thcrefo1e. between twb metal sheets (Fig'ure 3-1 Sb): A
close· ti� is maintained
these pump:. are least.efficient. These arc also less expensive. between the circumference of the impel)er and the
er;itran'ce of the volute
(or between the hub of the impeller and the corre
sponding point on 'ffie '
78 r
l'IIARMMTUTICJ\L l'N<ilNITIUNCi Ch-J TRANSPORTATION OF r-u;ios . �.
79
casing).. Thcn.:fore, back leakage of fluid is not observed. These pumps �ressure' at .the �ye o: the irnpelle:r. He1;i
arc more efticielll and inorc cxpensiv�. nnpeller through ·the mlct suction 'pipe. This
e, the (iqu , id ·nows into the
liqu;a· is force'd .out .ard
Si,igle-s11�1io11 p11111ps : In this type, the liquid enters the impdh:r along t_he bl�des at increas11ig tai1gehtiaI 'vel�
· .'i ·
blade trps and pa;;ses into · , . . city'
. .. ·The
. 1 liqui d .•lea,esv. the. f
t 1e volute chamb er '. In this'°p
.
from one side only. When such an impeller is allowed to rotate at high . roces s 'its veloc-
speeds. suction is crdtcd at its eye (centre), which pulls the impeller , ity head decreases and consequently pressur�
head 'is 'incr�5s;d . \he I' 'd
away from the shaft. The disadvantage c)f this pump is the unbalanced moves along the �asine, finally.. tl)e liqui
d leaves the discha rge pi���·
hydraulic pressure. As a re!iult, end thrust is produ<.:cd on the bearings. '. • . • 1 ,·.
Discharge
,,,1

Do11h,le s11clio11 p11111ps : In this pump, the liquid ·enters the. impellers ,! :_··, ,·,
• l

from both sides. The pu mp consists of two impellers placed back to l,

back and united in one casing. ' Therefore, hydraulic pressure is well
balanced.
The general principles described above arc combined and illustrated
using a volute pump given below. ,·: .. �

Volute pumps : The space between the edges of impeller and the
casing of the chamber is known as volute. J\ pump that is equipped ,vith
volute casing is known a� volute: pump.·
In this type o(ccntri fugal pump, water entering at the suction connec­
tion is'thiown ot1twards by the rotution of the curved vanes into the volut e
(f'ig
_ urc 3-13). As a result. the liquid s u ddenly changes it's .direction i11 the
volute , whi�h decreases ihc velocity head '.ind com.equcntly increases the
prcssurc· llcad. These changes facili.tate the pumping of the liq u id. Th'e
�igure 3-�6. Constructi�n of sidgJ��stagc,
step to change the direction of liquid flow is not smooth. Therefore, these . s�ngJt��iction, _opef1-�npeller 'volute pum
pumps a:e least efficient. These are also less expensive. , p. _'1 :
Uses : Vol u •te pumps arc used . . • :
· . ,: • \ (; •
9r vi, s�o.us 11qu1ds ""d liquids cont2in- .,
Single-Siage, Single-Suction. Ope11-!111peller Volute Pump rnf s�I.'.'d matc�� afl�. gren _!�'pelle��-,��9�,u��.d,,,for \his purpos
r

Cons/ruction : The construction of a single-stage. single- suction, �.: ....• , :i�-1;,,,

·Acf.vantpges :, Volute. pumps are 1.cheapes . '. :r(:1±
open-impeller vofute p ump is sho�vn in Figur e 3-16. The impeller . t'iof
, 'all c�n trifug"a l··''·pump s.
.,_ . . . , a( ''· ' .. ,_ ., :1d :;,
• consists of c u rved vanes c�tending from the hub. In the casing, impellers Di. sad!•a11tage�· : ('I) Volute. um s are ' •ri ,: .
...... pow ,.... er 1osse
i· - · .,.•. ,. . ,,R, v . P t qe l east efficient b ecaus•" of
arc placed, in suci1 a way that the surfaces of the vanes are in close s du.�:,1° ·t" th, e ''fioI_p I w'Iuw. ., . . . .. ' '
. ..re ·"" oe ' ·l·'•
...asons ·', .. ;., ,· ,,
contact ,vith th e �wo hah·cs of the cas(ng. Since impeller is an open
. (a)... , . Wdhen wa!ter
. . .._. r1···
i � thr;w�
.
o�r b
;'·
;
· ":· ..
, , , . . ... ·, .,,. ),., �.d1 �Jly mov. in g.vanes
. ,. . .. • :
. •-!:•' •• '·'."' :/= '...
runner, 'the edges of vanes arc free witho�t any attafhl]lent of rings SU den I y c'hange,.,'the direction: .as, i(�nt�is" the ·V�I�.te .
1tmust
(Fig'dre 3-16). Since the impe li e r is a single-stage, only one impeller is sudde. n change resuIts m, · tur " ·, : ,,,, "'. ,. .
· bu 1 ence . ',.· Such / . a1
u sed for pµmping. �1 --.. . " . •. , which con sumes some pow er
_ m·the form of friction.. , , , .. , . ··· ,, ...., . , . , , . , ., . .,, .
· l \,� f •

The impeller is attached to a shaft, which is rotated by the u s e of

� \ · 1, •, • ·v '·.•II f �# \ _ -�.- , , ·� 'f, y

· (b) Thesqire cheap pumps. henc. e

'

n �t . �:curately,.. fi n ishe d;" '

· · . .
power from outside. Nearer to the centr e ( e ye)·of the impeller, provision ;' ..��-n .·. and ''· The .fit
. betw
' . '; th' ..
e .
11np e II er the casmg .IS' usually ·poor. A. art
is made. in the casing to· receive the fl�id by suction. At the top of hq d dr�,charge l�aks to the .suction of'
side.'. To. prevent thi�

-
casing. an exit for discharge is provided to which volute is exposed. �'.
lqakµge, a closed, rmpell er is used. · · bac k:
.. . " ... ,. , ·'
Working .' : Pow e r is appli e d on shaft to rotate. Along with it, (2) In these pumps; the suctio11 sid/
ofimpeH d .,.,,:,. ::r·,.
the blades of the irnpeller are also, reyolved. This results in reduced .• ' . wh.ich is, ,less than the 'atmosp·herf '. ;>.. • . ,,e· r. . -�IS un. �r .I?�:�su�e.;
o pressure A s a result, a ir may
:
80 l'llt\RMI\CEl)TICAL !;N(jlNl:l'IUNCi
c;.·· bl! drawn into the pump through the stuffing box. Thi$ _air
great Iv dec1'ehses the rate of discharge or, even, ,e ntirely stops· th!.! '
• i ) . J� ..
pump. · $('alii1g the gland_s ���1 p_rcvent thi�". A stnall. amount of
liquid under 'the prcs�urc of the di�chargc· is· dir�c.ted . through
seal r,ipes to lantern rings il\Jhe packing..
Tt1rbinc1. pumps. : , lhe diffusion ca�ing 1:qtiippcJ ,vith vanes is
kno\\ n as tu1 binc pump. In this type ot ccntri fugal pump. a station.l1')
diffusion rim! is interposed bctwcen tht/ impeller and casing chamber
(Figure 3� 17 ). As a result. the change in the direction is. smooth. withoul
shocks during pumping. Thc1cfore, it docs not involve; energy losscs
d11c to eddies a:,; 0bscrved in volute pumps. Thus turbine pumps arc
more efficient.
...--,�......__ Parts in
��---,.,c, -.diffusion rin!J
i�pellcr ·' J •
.. \! ,
Figure J-17. Design of impdlcr in h simpl.c Rirl1i11c pump.
i;, •
The design of the impeller Md the gcll'era\' e,ohstructio1,1 of t.hc turb_ine
' L ' '•
('
pump is similar to tl,1e volute pump'. :· b,nnecting' more . r1�1;1ber of
impellers in ,.s�rics can gc.ne1;at, e, , the maximum head: The overall 'effi­
ciency of,s·uch a.puinp is hi�_\1., b�cause•the.l!q4Jd:fr�m w e tip of.q9nc
_ . _ '.' : ! �: i.
impeller'i� :dcl.iyered to the 1�1let 'oC, ���; n�xt 1n�peqet, w1�h a ipu11m�1m.
.
loss (multt·stage). Therefore, heads up to ..,QQ metre� may be generated.
f
· The general principles des��ibcd earlie�· ;r; dombin�c and Jllustr:�;d
, using a model turbitie pump given below.
:.
>J;•'
Si11gle-Stqge, Singlt!-Suction, Turbin<: Pump f : ' :,
. Constructio11,: The construction,rof. a single-stage,· single-suction;
turbine pµmp is shown in. Figure. 3-18. The· impeller is a· puinping
mechanism, whicl\, consists of curved vanes ,eXitending frcHn the hub. In
the casing, impellc_r is arranged in such a way that the·two halves of the
• casing are.c.losely in contact w\ih l�e surface of the. vanes. A diffusion
ring cont.iins passages, wh(ch change gragually in cross.': section and
I to be handled are non-corrosive to iron or bronze.
Ch-:l TRA1'Sl'OR'FATION OF H.UIDS
dircc1ion. Since the impeller is singlc-st;lge, only one impeller is used in
the pumping.
ring
To
drive l
Im pelter
Volute
suction
..,: .. : ...
· ,,
Figure J-18. Si11gk-stagc. singlc�sucti9n,, turb.inc ptimp:·.
The impeller is attached to a sh�ft. wh,ich is rotated hy the ,use-of
power from outsi_de. Nearer tci the centre (c);c) qf the i'mp�llcr,' provision
is made' ii1 the rnsing to receive the fluid by suction .. At tljp top pf.
casing, an exit for,dischargc:is provided to which.v11utc is exposed.".'. ' .. . ,,
Worki11;.: : Power is applied on ·Shaft to rotate: Along with it; fle·
1
. b!adcs of the .impeller arc also revolved. ; This results in ) reduction in;
press·ure at. the eye of the i1t1J?fllcr. Hence, the liquid' flows into' t�b'
f' '> impeller throu�h' thc inlet suction pipe. This liq'uid is 'forced· outwa�d
along ihc blades at increasing tangential velocity) The' liquid· rclcas>!d0
from the tip of the 1mp!,!llcr is caught in these pas�agcs .· and turn.:d
gradually and smoothly into a discharge valve witho' ut shocks. and
eddies. .
.f .' •• ,.r ..
In a si�gle suction turbine pump, the impell�r pro�u�es, �h.�' cnq thrust
on the sha'ft, which is partly overc_ome by holes in the. impeller. This
partly equalizes the hydraulic pressure behi�� and front of t}ie impeller.
The rest of end thrust is taken up in a thrust bearing. , ', . ...: . . · ·
Uses : Turbine pumps arc used in handling of :clear, non-viscous. and
non-corrosive liquids. Vertical turbirie P,ump.s, which are particularly
suited for pumping water from deep well. are often cal.led .de�pall'C:11
p11111ps. ·
Double s'uction, single-stage puinps are used for genera� ��it�� s�pbly
and circulating services. Chemical pumps can' he used when . the liqttids
 Ch-3 "TRANSrORTATION OF FLUIDS 83
/ � 1'(�
82 i'I IARMACEUTICAL ENGINEERING
pressure head. ·such a conversion depends on:
1
Turbine. purnps arc widely used for handling organic solveilts, Angle of tAe vanes
organic heat transfer. liquids, light oils, toxic or hazardous liquids or - Velocity of the liquid at the outer tip of vanes
, , where leakage poses an economic problem. friction and leakage losses
- Changes in viscosity
Ac/vantages : (I ) Turbine pumps do not involvf energy losses du_e to
Performance of a centrifugal _pump : The p�rformancc of any
eddies, because of the presence of a stationary diffusion ring.
.The change in the direction is smooth without shocks. ..
particular centrili1gal pump is expressed by means of curves. called
charcu.:teristic: curves. These arc usually supplied for pumping water by
.

(2� S;ngic-stage turbine p�mps are available for a variety of services. manufacturers. The performance of a pump is measured in terms of four
(3) Turbine pdmps can be connected in series to improve the effi­ characteristics. . . : .
ciency (multi-stage pump).
Capacity : It is expressed in metre cube per hour for liquid pumps
(4) Chemical pumps ·a re available in a variety of materials. and in metre cube per minute' for gas pumps; for a given inlet tempera­
(5) Turbine pumps are available with the capacities up to and over ture. ' and pressure conditions.
400 metre cube per second and heads up to 480 metres. .
If speed of impeller (revolutions per hour) is increased, the rate of
discharge abo increases co'rrespondingly. This relationship is expressed
�isadwmtages : Turbine pumps cannot be built with special materi;;i.1.
So corrosive liquids cannot be handled. as: ., r- -
. ..
Rate of discharge oc. speed of the impeller
Air Binding And Scl(Priming Pumps
Q ccN (6)
When ; centrifugal pump is switched on, the fluid does not instanta­
neously �evelop pressure. During initi�I period, air enters the impeller The volume of discharge depends on the cross section of the pas­
and thcri lluiJ follows. The head ·generated (in metres) by air may be sages. Therefore, the size -of a centrifugal pump is usually specified by
comparable to the head degenerated (in metres) by the liquid. However, the dia'meter of the discharge connection.
the pressure propuced by ,the same air is. very small in terms of liquid ·- For high heads and small volumes' of di�chargc, centrifugal
head. In such situations. the pump practically stops delivering the pumps having impellers of large diameter"s; but with.narrow slots
liquid. This process · is known as air binding: This is one of the are used.
disadvantages of the. centrifugal pumps.
- for low heads and large volumes of discharge, centrifugal pumps
Air binding can be _prevented by• employing some of the following having impellers of small diameters, but with - wide slots are
measures. . used.
(1) A check valve is provided in the suction line, so that the suction Pressure head: It is the energy supplied to the flu,d.;er ·u n_it mass
line and casing will not drain off the liquid, when pump is sh�t (increase in pressure/fluid specific weight), i.e., head development (me­
. -
<;I.own.. · · ·.. . . . . . , ·_ . . , tres). The quantity of fluid discharge is increased as a result of
. ·, the
(2) A self-priming pump is provided, so that air can be· removed enhanced head developed by the pump.. Thi - relationship i� · expres
from casing. � sed
as:
(3) Centrifugal -pumps ··are located at a place, so. that the pump Head developed oc. (r�te of dischar&e>2 -"13
suction is under a positive he�d and thus necessity of priming -is

. ·�
H ex: Q2 _
eliminated. : \ (7) .,
It is generally expressed ·as column of fluid eq:ivalent to the to"ial
Centrifugal Pump-The(?ry pressure differential measured imrriedfately before and after the
device,
··. -As mentioned in th_e "'orking principle of centrifugal. pumps, the _tor a given adiabatic condition. Head devel9ped by centrifugal pump
· velocity head of the liquid at the top of the impelle� is converted into a s is
 l'h·J Tllt\1'Sl'ORTAT!ON OF H.lJlDS 85
84 PHARMACEllTICJ\I. ENGl:-IEERINU This can be minimized by:
(a) dc1.:reasing the distance between adjacent vanes
determined iargely by: (b) putting more vanes on the impeller
Angle of the vanes.
Speed of the liquid at the tip of the impeller. ·· pump and
Such mod.itications increase the· cost of the · enhance the
friction losses.
Power : It is the energy consumed by the m.ichine per. unit ti!nc
Work done or efficiency : The centrifugal '·pumps arc usually rated
(kilowatts). High speed, of impeller, large .. head gcn�ration and. _hig l on the basis of head and capacity at the' point
_ _
discharge rate obviously. consumes more power. 1 his relat1onsh1p, is
_� · of maximum efficien�.
Th1: work done is expressed as: . . '.
expressed as:
Work done rate of fl.µid flow x
=-=
J ·:. ·
Power consumed � Rate of discharge x head developed differential height of the column of fluid
WocQ x ll (8) Work dune (kW ·h) � capacity (m3/h) x head (m) · ( 12) .
Or IV cc Q2 x Q cc Q3 (9)
:Vork must �e dor 1� on the �i !11p system.in order to lift any liquid
W cc N3·· against the grav1�.· _I he pumpfnctual.,
ly raises the liquid and forces it
Or po) into a pressure vessel or it may provide enough head to' overco
me the .•
Equal-ions (6 to 10) arc used for th�_. �ompari�on of two pumps. pipe friction. In such cases. the /;)'drau!ic ejficiency is e pressed
� as:
· Efficiency : Energy supplied to the flui_d divided by the enct£Y power of the runner (kW)
f{ydru
· ulic: ejficicmcy = · · . .
. to the machine is referred to as efficiency.
supplied
actual input power (kW)
(I 3)
energy supplied to the liquid It is possible. to estimate the thc.oretical work required of a pump
. (i.e., power consumed) (kW) �s
E:ffrciency of a /HllllJJ · = ---------­ ( I I) shown below.
energy supplied to H Qp
. ' . machine (kW)
the Power output (kW) = ----- (14)
0
This theoret1ca• I . reIa1·1ons111p
v .1·s a rou.gh guide to understand the 3.670 x 10-5
-performance of centrifugal pumps. where fl"' total dynamic !;iead of liquid, m.
p = density of the liquid, kg/m3
Power losses : A certain amount of power is lost on . account of Q =. capacity, m3/h
various reasons, which are listed below:
The dy11:1mic head (fl) of a pump can be c·alculated usmg
t f Mechanical losses : These are ·d ue to friction in bearings, stuff- equation ( 15).
the.
ing-box packing etc'° . .,.,
H � total discharge head - total suction, head . (
2.· Leakage losses : These are due 10 leakage of the liquid from the - . 15)
· tip of the impeller back to impeller suction. The power input of a pump should be greater than the po,ver outpu
t,·
J: Hydraulic losses·: These include: because the internal losses rcsqlting from friction, leakage
· etc. Th1.:
(i) the friction ·between liquid and casing efliciency of a pump is therefore defined in simple terms as:
(ii) the friction between liquid and faces of the vanes . · power output (kW)
· (iii) losses due to sudden change i�· the direction_ in the vol�te . Efficiency of a pump = . (16)
, (iv) losses due to sudden change m cross-section. where liquid power input (kW)
· leaves the impeller Reciprocating Pumps Vs. Centrifugal Pumps
4. Recirculation./nsses: The velocity.of the liquid is not uniform in A comparison of features of reciprocating and �.entrifugal
_ pump
the space· between two adjacent vanes of the im�ell�r. !h1s given in Table 3-1.
· · · . · -- l · · ·,,s is,
. .
difference in velocity produc·es circulation of the liquid w1thm
the space between the vanes. Such circulation consumes power.
86 PIJARMACEUTICAL ENGINEERJNG Ch-3 TRANSPORTATION
OF Fi.lJIDS
TABLE 3-1 sio n resistance arc valu 81
able. In 51 hospital .
Comparison of Characteristics of pumping parenteral nutrit setup, these are used for
Reciprocating and Centrifugal Pumps . . ion i n tius1ons to tho;;
mg In case of surgical patien ts and blood pump
operations. �
Reciprocating pumps Centrifugal pumps Advantages : (I) Simple . . .. . .
and inexpensive (to purchase and operate·
I. These arc designed for higher heads. These are designed for lower heads (")
- [-'· . to c 1·can.
•.isy )
2. The cost of these pumps is lower The simplest pumps arc cheaper than Disad.,·antagcs : (I) Lin
than centrifugal pumps for the the simplest reciprocating pumps. cacity an d o titen, accuracy
p_ump speed i 11 creases. decreases .is the
same capacity. For the same capacity, centrifugal .
pumps arc costly. (2) Accuracy varies as
. , .the tub·mg \\,ears and .
(3) Effectiv . fatigues.
3. The efficiency of these pumps is
constant over a wider range of
In moderate sizes, the efficiency of
these pumps is higher. ·
eness is limited by 1qu ' .
.
.
1 d v1scos1ty. r
Glossary of Symbols
discharge rates.
. 1-1 "" Dynamic hcaJ. m.
4. There is no possibility of air Air binding is possible. So special ' I I :a Ikad. m.
binding provisions arc made for priming. N = Spc".:J ()r the impe
ller,
5. These pumps are more flexible Less flexjblc. in their operations. Q = Ruic or discharge . m3 r/�.
/h .
in their operations. �' Density ()f the liquid,
\\· "' Power consumeJ. ).; kg/m3
�
6. Discharge of liquid may be Ddivcr liquid at uniforn) pressure) Wh.
pulsating in low�r versions. without shocks and i:,ulsation.
7. Common types arc steam driven. these arc commonly power driven 'QUESTION BANK
8. Distribution of steam and Distribution of electric power is Each question carries
collection of exhaust are not simple. simpler. 2 marks
I. \Vh.it t)•pe of pun,p
would yo:, rcconimen,,f
9. Used for liquids that arc not too These can handle suspensions with . o'
:,O� solids? Give reasons. . r pump 1.11g, slurries with
,or
viscous. corrosive and ahrasivc. large solids and corrosive liquids. 40-
2. lkscrihc the worki r.g . .
of.u sc . ·If p1 am· rng pump.
3. ,,\: hat
• is.,
meant by 'air binJing'.
l)r()11> cm·>. in pum',,s?. I-lo,,· d(> ·
MISCELLANEOUS PUMPS you i>,·cr�·ornc t:ic
4. What arc the des·, .,. rcs and mer
. agn 1·1.:atu
Peristaltic Pumps its. of a tur b"rnc pump'J.
"i. . W n'te notes on check .
Principle : In peristaltic pumps,' silicon rubber or other suitable valves. r
elastic (resilient) tubing is clamped in a U-shaped fashion against a . Each question carri�s 5 marks , , -·
�ptating mechanical device (such as 'finger' or 'rollers'). The tubing is I. Wril,I! lhc comtr�c1io:1 :.
compressed in stages by means of rotor. As the rollers rotate, they and working of.a tur . .
-· D.esen·h.c the con�truc1
"J b·
me pump .
flatten the tube against the tract at the points of contact. These flats ion '<Jnd princi ple of.
pump for liquid lrnnspori. ··� . .11vc
rota�. pos1 . displa
c. enl'cnt ., .,.
move the fluid by positive displacement and the flow can be precisely .
3, Dcscribc lhl· constru
'I

controlled by" the speed of the rotor. The tube quickly recovers its ction anJ a PP i'·icc1l1 .
., · ons. ot. any one. pos
pumn, · · . itive ,•l 1'.,"pla cement
original shape after squeezing.
:t, C:omparc lhe charac1e • n,u ·�
·uses : Peristaltic pumps are particularly useful for biological fluids ristics ,fH'c. cnt gal pumps .and n:�1 .
.. · proeutm
_ .
. ::,. Classify rcc·,iiroc •
atin"°o pumps ,,,·111I ucscr . . .
., g pu
where all fonns of contact must be avoided. These arc increasingly used \ mps.
.
6. Draw the di agraar• of . . ipt1 ons . of vari
. .
ous , ,
ter ms.
for pumping emulsions, creams and similar fluids in laboratories and ::i piston type
of reciprocating pu�p
operatio n. . .
jndustry,
� where freedom from glands, avoidance of aeration. and corro- . • and.'\ exp· Iarn Its
 88 Pl IAR�IACEUTICAL ENGINEERINU

_.. Each question carries 10 marks

1. Describe the· principle and construction of a centrifugal pump of your
choke. How do you compare a centrifugal pump with rcciprocaiing
pump?
2. Dcsdibc the construction, working, merits and demerits of a double-action
rcciprpcating pump .
 J

4
'·1 . •

Belt Conveyors
Screw 'conveyors
Pneumatic Conveyors
· Chain Conveyors
Bucket Conveyo,rs
Storage of Soliqs

The t�'rm ·conveying IS applied to the transportation of sol· ids.. The

· transportation of liquids is ·much sim.pler. chea�\!r' and !es.s"tr9uhlesome
than handling solids. In many.operations. s'oliqs· are handled'in a. fi nely
divided state •. sp th;it they remain suspended in a stream of fluid.
However. such a syskm is not suitable .for handling all types of solids.
Therefore, it may b� necessary to trarsport solids as. s1,1ch: This unit
0

operation is important. in the storage . and handling of raw . ' materials,

finished products rind packed goods. The advantages and°obj�ctives are
given belovv.'

Efficient and Effective Conveying-Objectives and Advantages

I. Decreased product costs and increased manufactudng capacity.
2. Decreased cost of ra; .material. For example; 'peii'atty charges
arc levied when cars are not loaded or unloaded '�ccording to
schedules. Losses que to spillage or tor� ·co11tainers. is reduced.
3. Decreased pr.ocessing time and'conse�vatio;·�r·��ergy.
' ' '. ·i ' J

4. Rigid in-process controls leaping to decreased qu1,1lity control

and quality assurance costs. · · · ·
.. 5. High degree of uniformity; reproducibjlity of the':ptpcess and
compliance with the cGMP regulations (current'.good manufac-
turing practices). ,,'., .}
6. Minimum contamination and dust formation.·::_ ·
7. Increased empl�yee safety and redµced )abour c�s�.' ; ,·. ·
/

89

.J
 ·,
90 l'IIARMAt'l:IJ'l l('AI. Er-.:(il1"U:RIN(j
If raw materials are no\ moved as required by production schedules.
the manufacturing process will be slowed down. · In addition. machine
time and operation time will be wasted. }\s a result in-process invento­
ries will be increased.
Improper handling and storage can lead to damage, outdated and loss
of materials. Improper handling of granules, strips, bottles and chemicals
can place en1ployecs in physical danger. This can often lead to employee
frustration and reduced morale due to constant production delays..
In today's world of automation, solid co1wc)�ing has gained a greater
importance:· It is often necessary to prevent the wntact of material with
the persons. in order to avoid contamjnation (as in case or antihiotics).
Similarly working personnel should not be, exposed to poisonlH1s and
obnoxious substances. Therefore, a closed conveying system is ·css1:n­
tial. Such a dosed circuit manufacturing operation calls for automatic
handling systems. The feeding o_f materials into a reactor is always done
mechanically. Similarly, discharge should also be made automatic.
Conveyors are 1.1seJ in �l;ic production of all dosage forms such as .tablets.
capsules, liquid orals, injections.
� . . .
Conveyors ate classified into five major groups. These are:
I. Belt conveyors 2. Screw conveyors
3. Pneumatic conveyors· 4. Chain conveyors
" Burket conveyors
Some important co1we) 01 systems. constructio11, working. anJ appli�
cations are discussed i11 this chapter.
BELT CONVEYORS
. The basic t:lcments of the belt conveyor arc:
I. Belt and belt tightening systems·
., Belt drive and power supply
3. Roller supports for belt
4. Feeding arrangements
5. Discharge :irrangemt'nts
Principle , simples� belt drive is a bare steel pulley actuated with ·some 'source of
Horizontally or inclined placed motor driven rotating belt on pulleys
convey the n1at.eri�I from feeding point to the discharge point.
Construction
The construction of a belt conveyor is shown in Figure 4-1. Belt
comeyor consists of a core or carcass (meaning skeleton or backbone for•
Ch-4 CONVEYING 91
. '
the belt) of several piles of cotton duck, each layer is impregnat�d and
bonded with rubber. The carcass is then covered with· a thin layer of
rubber that binds the piles together. Both the ends of the b�lt are joined
together, ·so that the belt can revolve 'continuously. The. belt may run.
horizontally or slightly inclined from the feed point..._
- If the beh is too thin for its' width, it will sag\.etween idlers.
- If the belt is too thick, it does not tr ough properly. ·
.
. Sometimes, the length of belt is increased .due to a v;:1riety of factors
such as temperature nnd humidity.of the atmosphere. In such cases, it is
nccrssary to keep the belt taut. Hence, tighteners (or take�up) a�e
installed to mairitain an even-_tension on •'the belt under all conditions.
The _simplest !akc-up consists of a ca.st 'iron'bed with a 'travelling block
movmg along a screw. · ·
.
.,;;,,
l
Non-troughing
idlers
. . Dischar!je bin
power
. ..
Figure 4-1. Construct!on of belt conveyor system.
The belt is allowed to· move with 'the. help of � belt 'drive·. The
power. The drive of the belt conveyor is fixed at the discharge end (It is
rarely arranged at the feed end). There"should be appropriate contact
between the b_elt and pulley. Introducing snubber idlers just below the
pulley can increase the contact. '·.., ....
The belt is s�pported by rollers, which are arran&ed on a·, shaft.
These a�e called idlers. The .idlers arc carried. on bush bearings lubri­
cated ,v1th grease-cups. The idlers arc generally troughed to depress the
I
J
 92 Pl IARM,\CEUTICAI. EN(i11'EERl:,,:c;
I
Ch-.\ CO:S.:VEYf}.;(j 93
belt at the centre and rise al the edges (Figure 4-2c). This permits the
belt of a. given width to carry more material per linear metre without Pharmaceutical 'Applications'
spiUage. Thi! b_clt returns on ordinary, non-troughing rolls. Belt conveyors arc used in_ transporting containers for filling, cap­
ping, senling, lnbclling, pasting; visual inspection etc., in the production
of injectables, liquid orals, ointmcr1ts and jellies.
In the strip and blister packi11gs of tablets and capsules, strips arc·
conveyed on a moving belt. During this process, the strips arc packed in
the c<.1rtons. :
Belt c0nveyors arc used in the manufacture of lozenges. It is a·
continuous process of candy ·base cookies. When a mass of sugar base is
(a) Flat belt on continuovs (b) Flat belt on flat belt idlers on the con\:eyor. the water is removed. At the end of the belt. the candy
plate (non-troughing) (or non-troughing) base i� mixed. tempered, fcnned. roped. melted, acidulcnts and flavours
arc addl·d. cooled and sized.

Advant;1gcs
��Belt
(I) Belts can be madl! of asbestos fibres, neoprene. :cflon and vinyl
'yi----i-�� Idlers polymer. Cord belts arc also used.
(2) Belt conveyors are for general purpose installation and available
(c) Troughed be!t on 20• idlers. in relatively large sizes. These can travel several kilometres as
Figu�.c .t-2. Construction of support idlers in wi<lLIH\ i:;c descriptio'n. in case of coal mines.
A hopper is. placed at one end in such a manner to load the feed :..t (:;) Routine maintenance of belt conveyor is �asy.
. .
the centre of the belt. Cleaning dcviccs such as revolving brush· and (4) Bcit conveyor is economical in terms o'f cos\ per' unit tonne that -
· ·
rubber scrapper blades arc placed in tlic path of the belt in order· to "it can handle.
clean, if the material sticks to the bclt. 1 Provision is mack at the otht.:r
Disadvantage
end for discharging.
B_clt conveyor is expensive.
Working
. . Selection of Belt Conveyor
When power is applied to a conveyor, the belt starts rotating.
The capacity of a belt conveyor depends on the cross section of the
As the. pulley moves, the belt begins to travel in forward direction,
load and the speed of the belt. The cross section of the load depends on
because of its close contact with the pulley. Snubber idlers also help in
the width and slope of the belt and size. of the material. · The selection of
• maintain_ing the close contact between the pulley and belt. . �
a belt conveyor depends on: .· . ·, : . ·· , .. · . .
The material (to be transported) is lo.!ded on its centre of the belt Power required. """"
with the help of a hopper. The _material lrav.els above the belt. The bdt
- Mechanical and tensile strength of the belt system to handle
moves forward- on troughing idlers. This permits the belt tt) carry more the wider yarieties of materials. J.
mafi::rial per linear metre with.out spillage. The amount of feed delivered Lump size. . '"
depends on the width and speed nf t. hc belt. .At the discharg1.: end. lhc - Troughability of the belt.·
material· may be unloaded manually or mechanically. Ability of the belt to support the load between idlers.
Once the material is unloaded, the belt· returns on lighter non­ - Chemical resis1anc� of the belt to the materia·I to be handled.
I JI.\ > • • ·• •

troughing rolls to the point offceding. Manufacturers of belt conveyors publish charts .or formulae for the
construction of con�eyors, size and power requirements. ,
 94 Pl IARMACEUTICAI. ENGINITRIN< i
SCREW CONVEYORS Ch-4 CONVEYING 95
/
The _b'asic ekmcnts of the screw conveyor. are: transmitted through the shaft to the flight. The shaft is rotated around an
I. Trough system . 2.. flights and power supply axis and remained . nearer to the bottom of the trough. The feed is
3. ·feeding arrangements 4. Discharge arrangements. normally introduqed, by plain spouts, which gives uniform flow of
.. '' Prin�iplc material. At the discharge end, arrangements are made to receive the
.
Horizontally or inclined or vertically placed motor driven screw like moterial using open-end trough or open-bottom trough. '.·
flight copvey-.; the material in the trough fro1n the 'feed point to discharge Working
point.
When power is applied, the drive rotates the shaft through the bevel
gears. = h.: screw element starts rotating. The tlight is rotated round
r
Construct. ion . . .... .
•.':' . ) :., .. , ; .
. The tr.ough i� 0a U-shaped , cssel in which .th<: material is enclosed an axis a11d remained nearer to the bot.tom of the trough. · Feed is
durfng cop:vcying (Figure '4-3 }. The' trough is USLially made of a sheet of normally introduced by plain spuuts. The mat�rial will. be trapped
steel mid ·,iyailablc in st:uidar<l kngtlis. : If .i trough of mon: length· is between the gaps of the spiral blades. As the flight moves, the material
required, tl�1:11 more number of such units· arc joined together. also moves forward along the path of the sections. The materiai is
.received using opc,�-end trough or open-bottom trough ....
Helicoid screw
arrangement c. ·e-
Applications
(l) Screw conveyor is used for transporting finely.divided solids or
. · ·
pasty solids'.
Maicriols having properties such as light-weight, medium-weight,
abrasive� n,on-�brasive and different densities can b\! easily·han­

/
Source of
(3 )
dlcJ using sci-cw conveyor.' it \s it vcfsatik conveyoi: system.
Spcc,ial flights and casings arc available: for operfltion.,. sue!'�as
111i.xing, ck-watering, heating and c�oling .. '
power
(4) It has the capacity tq handle the materials- '.]f about 280 metre • :,; '
cube per hour. .,
!

Bin
_Advantages
Figure 4-3. Construction of a typical screw conveyor.
. '· r
f, , ,-

(I) Materials .can be co1M!�;-d horizontally, vertically or. inclined .

. Scre�v elcmc;1t. usually .consi�ts of a spiral blad�. (conveying mecha­
(2) :screw conveyors are easy to operate and occupy 'iess space:
nism is ii'�e a screw). y.•hich is called Jliglit. The simplest form of the ·• ' :· l . -

flight is·thc sectional conveyor. Hclicoid flight is shown in figure 4-3.
It is made of a single long ribbon that is twisted . and \vrappcd into a
spiral shape. .These standard flights are welded to· the central shalt.
· Alternativelv the conveyer element' (helicoid flight elemen�) is sus­
pended \�1th the help of hangl!rs along the length of the_ trough. Usually
one hangei is used fcmeach flight section. Hangers contain bushings_ of
white cast iron, so that lul:lricants need not-be· used:
The dr-i�e end �nd discharge ends .are known as box-ends.
drive enff,: sha.ft is connected to· the drive by bevel ··gears. Po,.;·er is
.'j'
I
\'.
. (3) Differe�t c�nstructions are available and can be adapted for a
_variety of .·materials. Screw conveyors ca11 · be fabricated in a
v;1riety' of material� ranging from .cast iron to st�inless 'steel. '
(4) Screw con�eyor can be operated at positive and negativ� pressure�.
(5) High and low .temperatures can be maintained by insulating· the
casing.
(6) It can be made dust free.
Disadvantages
(I) Screw conveyors operate at. relatively low rotation.�! speeds.'
,
 l'h-·I CONVEYING 97
96 I Pl 11\RM,\CElfl ICAL ENG INHRIN(i
c·
Working
(2) �xtrcmcly cumbersome hanuling when conveyor.becomes larger.
The cycloidal blowers (or fans) produce air at prcss.urc 'about 7.0
(3) ,:\t.high spcedi., abrasive problems a-rise.
kilopascals. This air is passed. through the air slide at the rate or 1.5
(4)· Power_ consumption per unit wcibht tr,rnsfcrrcd. is high. IIH.:trc per minute. During ihis prncess, the rotary feeder ,,alve rotates
Selection of Screw Conveyor
anJ allo\\·S the feed to enter the pipeline. These solids a�c suspended
into a stream of air in a fluidised state until it reaches the receiving end'.
·c-The size and speed of a screw' conveyor are determined to 1�1a�e a The 111.1tcri:il is then admitted �o cyclone separator to remove large
choice ·of the design. The type of construction depends 011 the require­ particles and tine particles, if any. The large p_c1rticles arc c·ollcctcd into
ments Sllch as: i
tlw bin:· The fine particles are removeq· in a bag f lter. The gas can bc
Scale of opcration
recycled to the blower inlet in a closed system to save the valuable g-:ft
- Severity of service
Thcsc systems arc used for free flowing materials.
Value of the material_
Air oµt
PNEllJ\tATlC CONVEYQRS
The._l.:>.asic clements of the pnc·umatic conveyor arc:
I. Air s_upply ( or vacuum) �y�tcm Air pump
2. Air slide nnd pipeline �
Dust coll.?ctor
't.--· --
O::. ...l

· 3. · Feed arrantremcnts
4. Discharge ;rrangcmcnts (airand feed separation)
Principle
, , To bin
When a hir!h vclocity air is passed through a bed of solid p:1rticlcs, -cYClOne
,.
the individual particles. ·a rc dragge_d by the air. Finally they arc
__
suspended in the air. Such a system 1s known a�fl111d1z.<.:J h e,�, \\hl "\.!l is Pipe li11e separator
described as a condition of fully suspended part11.:lcs. In this _
_ cond1t1on,
the' suspension behaves '•l ike a de1ise fluid and can be transported frnn
i
. �
one point to another in processing plants. At the d,s�harge end, the gas '
To bin
.
Figure 4-4. Pneumatic conveying system, pressure type.
is separated and the sol ids arc recovered.
For-the design, and, .satisfae�ory operation, of pneumatic conveying, it
Construction . _ . _, - . is necessary to know ab,oy,t properties of :powders such · as - density, -
- The construction of a pneumatic conveyor is shown in Figure 4-�. particle size d.istribu-tion, cotJesiveness, angle of friction, angle of repqse
�r
Fans �y�loidal blowers arc connected to the conveying �ystc1:n. An arr and tluidization characteristics. . ' '
slide consists of a chute with a porous base through which air passes.
, • ! ' , . �I � · ,. , , • . 0 • �' • . • • ,
_'; 1 !' " \

The path of material 'travel may va.� from a few metres ·t o :everal Applications
hundred metres. Conveyor mechanism can be operated for honzont�I (I) Pneumatic conveyor is the· most important ha�glirig technique i1{
and :�ertic�I i:listances. The material' supply (feed) is connected to·t�1e a'.r chemic.ii 'industry. · ' · " · · __ · ' · ·
.
slide tprough a rotary_ feeder valve. The other end of the p1pelme is (2) It is uscq in: the, form,ulation c;>f p�wder-�k insufflati9ns. _
connected -to a cyclone separator. .CJ> aencraJly, light ·and bulky ·ma.tcrials such as - �ai�s can be -
8
_ ,transported ,easily. , __ ·.,.. .1;:
''
(4) Pneumatic c9�veyor i_s used for handling of unpleasant and:j
injurious (toxic) materials, since it is a closed. system. -·- ··
r

,·
 98 Pl IARMACElJTICAL ENGINEERIN(i
'h,4 CONVl:YIN(i 99

(5) Powders containing poisonous constituents can be transportc.d..
(6) Fine powders and pellets having th� size up to 6.0 millimctrJ!S
and bulk densities from 16 .to-.<�000 kg µer m_etre. cube can be
·,· . . handled by pneumatic conveyor., _ ·
supported by two chains of roller pintlc type (Figure 4-5) .. Scraper
conveyors with speeds of 30 rnc;trc per mimite arc common,. qpt the
speed may ranges .from 8 to 60 n�'ctres per minute;
.,,
flight

"£1
. ' I . :

Advantage� " · . . ,,
,
(I) �.hit�, conveying the material, the path involves many turns and
Hfts.. In such cases, other types of conveying become costly..
(2) Pn�umatic conveyor is econom.ical compared to other types of ) Chain�
conveyors.
(3) Friction losses are small.
Disadvantages
(I) 'fihe. pneumatic conveyor needs more power than other types of
conveyor s'ystems. Figure 4-5. Scrapcr/11jgh1 conveyor with• two chains.
,"'

(2) Erosioi:i of. internal surface of the vessel anq attrition of solids Uses: Widely used for loose material that is no.n-abrasive such as '
may take place. . · • . •
gram, food-waste, garbage, sawdust, chips and coal. It is 1101 suitab!c for
4

(3) Uneven contact of gas and sQlids is observ�tf. friable abrasive material such as 1clinkers,' gravel and crushed ore.
.
. q' . - . ·'• .; ,,
Ad,•antagcs : Simplest and cheapest type of conveyor. The. cost of
CHAIN CONVEYORS installation is also low. Scraper or flight conveyors have greater adapt­
' '
C.hain conveyor consists of two elements, viz.• chain elements an.d ability to a wide variety of conditions. It is suitable for steeper situations
.. that arc not possible by belt conveyor (inclination 45°). . .
' chain attachments.
Chain elements are made of malleable cast ,iron or stainless steel. Disad':antagcs : Semper or flight conveyor needs heayy power
'1 These links are so cast that they can ·be assembled and .detached without requirements. Repairing charge� ,are high.
use o'f tools. . · ·' • ' ' · ' ' '
Apron Conycyors
·Chains are endless and move continuously. The material is l9aded
into a suitable. container and place� on the chains� These are usually
1 Apron conveyors are usually used for heavy loads and short runs.
The simplest apron conveyor consists of t:wo endless.roller chains, which
constructed on the job� · ·' ·;
;uc connected by double beaded steel pa1;1s. ,:The beading 'prevents the
Advantag�s : Chain conveyor is a cheap and simple piece or'equip· material from slipping backward when conveyor is inclined. Wooden or
rnent. It can be adapted to a wide variety of problems. metal boxes arc fixed between the chains and the whole conveyor drags
.on the support. Apron conveyors arc used··for ·· ·
Scr�per/Flight Conveyors . ,, , ·:r· transporting heavy loads.
Flight conveyor �onsist.s of one or. two �ndless. c...h�ins passin� through short runs at low specqs.·
a trough or a 'set of guides. The chains have pl,�tes of wood or steel 'I
conveying 'material such as lumpy, :-�brasive and hot,. pro.�
( ' - J

called flights attached ·at regular''intervals. The flishts are shaped ,to fit ' vided that these ar:c not injurious to flexible. belts.
the troughs. The chains pull the flights and the material along the .�, '
- 'I
I':'
• \

trough and passes over sprockets at"the end of the run. One of the
sprockets acts·as the drive. In an elaborate form, flight conveyor is
 I Ch-·I CON\'l.:YING JOI
100. Pl IARMACEUTICAL ENGINEERING
The weight of the· con\:cyor results in the stretching of the chain
BUCKET CONVEYORS under load.. Therefore. tightening .'dcvic'e s arc generally provided for
Const'ruction . . . . . r . . . . . . ", altcri ng the position of the sprock�t �t t.he foot of the elevator.
Buckets are used for loading the materials. The .buckets are made of - In. hori:o_,pal nms. buckets ·overlap each,othcr and the feed, is
cast iron or stamped steel and available in many forms. Flatter buckets introdm·e<I as,a coniinuous str,eam of material.
arc used for materials that are stickv. Heavily stamped steel buckets arc
employed for large lumps,. for exa�ple. coal and crushed stone. In vei·tiral lint:�. the buckets arc •pivoted in such a way that they.
. · hang frc.::ly''betwccn the ch�i1�s. Tllereforc, convcyo; acts as ar:
The buck�ts are attached. �o belts or chains. The chains arc endl�ss elcva'.or. " ·. · ' · ·
and buckets are tix�d between two ci1ains (Figure. :4-6).� The chains 'are
.. At ,:fl1e foot of ·the elevator, a structure known as 'boot' is used for
O:" .! .

focdin�._ thc· buckets· and also· for tightening

._ the chains. : Buckets �arr· '

,somelirncs comrlctcly cnclosc·d in a casing. The casing is made of wooJ

1 •
or steel sheet. • ' , ·

\\'or.king , , . .,
Discharge The! ch;vators arc· generally driven from the head sprocket. At the
fool of an clc,ator, there is a structure known as 'boot', which helps in
·feeding. The buckets arc normally fed by digging into the materials
particiilarly in case of loose materi,11 and granular solids. The buckets
maintain their carry ing capacity hy gravity, but they can convey the
material horizontally or vertically or any desired path. Loading can be
Jone by the fiow of material through a chute into the buckets. Buckets
,• may be readily discharged at any. point by a t:-ipping device,. causing
each .bucket to turn through 90 ·degrees.. Th�..t·ypes of discharges arc
contir{uous:
'
positive
� and 'centrifugal.
'.�

.
Feed
Applications
l3ucket conveyors ·arc t1sed. in transporting coal, cr,;1sh\!d stone. grai�s
etc.
Advantage
" ·,
Boot : . .. ..,
f F\, <•

13ucket'convcyors . arc very nexible.

'I '' ;1 t l!t'.��

Figure 4-6. Construction cif a bucket conveyor.
• . .1 ·�
generally long pitch, straight and side. type. Th� buckets are spaced to
prevent 'interference in loading and unloading.. For heavier l�ads, two
chains may be &sed. ihe ,attachments are riveted to the ends of the
chains . .The attachments are slightly above the level of the chain so that
the ends of thd sprocketed booth do not strike the b:!r.k of the buckets.
.STORAGE OF SOLIDS
Attention must be paid to the storage of solids. Hie storage is an
•
. important operation, it' the ma1c_rial is too valuable or too soluble when
expo:;ed to c11111osphere as in outdoor piles. The following arc used for
storing sol ids.
Bun kcrs : These arc used l�r storage of pulverised solid �1atcrial.
During pbnt shut down. the solid material 'is stored in bunkers. Coarse
sol ids such as gravel and coal arc stored .outside in· large piles, unpro-
 102 ; PHAR!l,IACEUTIC:AL ENGINEERING

tected from the weather... Out :�oor. storage, can lead to. environmental
.· problems such:� dusting ar1d:.,jeaching. ..: • •
, ijoopers, bins arid silos : A bin is fairly wide and not so tall. It is a
cylindrical or rcctangular,v�ssel of concrete or'-t'netat A siio is tall. and
relatively small
D
in diameter. ,A hopper is a small vessel 'with. a sloping
bottom. It is used·, for t<.mpor.ary storage.· bcfor,; · feeding solids to a
process. These c:ontainer�, ;:ire l.oad,cd from the t�p by some kind of an
elevator and discharged ordinarily from the bottom.
Now-a-days,. there have been .extensive imprqvements in the use of
solid 'conveying equipment: For examP,le, granulation and tabletting
. 6perations are completely automated and computer controlled. . The
above system utilizes pumps and buck�t· conveyors to move t'nalerials
upward whe·ncver required. Examples are transporting granules and
transporting compressed tablets· for batching and film coating. These use
belt conveyors and pneumatic conveyors to· ·move the material· horizon­
tally.

QUESTION BANK

Each question carries 5 marks

L Illustr.itc the. concept of..solid trarispoi:t by fluidisation.
2. Dcscrib.:. th1: pri11dplc of pncumath.: conveyer with a labelled diagram.
3. Describe the diffcrc'ntt ypcs of conveyors used in phartnaeeutical industry.
4. List advantagl'S of screw conve):or and screw elev'ator. · Ho·\.;' do you
compare these with ·pneumatic transport of solids?
5. Describe the construction and working of a screw .conveyor.
• I ' r -' • • ,,_ .•

Each question carries 10 marks

I. Describe the construction and working of belt conveyor S):stcm for solid
transport.
2. Nan:ic thc <lcviccs used for transportation of solids.. Describe pneumatic
conveyor. . .
•
,,

/
 Flow ofHeat

Mechanisms of Heat Flow

Conduction i� •
Convect.ion
Radiation
�uiprrient-Heat Exchangers an 'd 'Heat lnterchangers

Heat is :i'form or energy. According!() the principle� of thermodynam-

ics. whenever a physical or clwmical "transformation occurs, heat flows .
ii1to or. k;wcs the system.
,\ number of s0urces of heht•ls used for ir;idustrial scale operations.
Stca1i1 a�d ckdric power arc the chief sources to transfer h�at. If is
essential to.convey st.c:ui1 w:thout any#losscs to tl{c appar�tus in·�vhich it
is used. The study of heat transl'er processes. helps in cksi"gning the -plant·
l'lfo:icntly and ccono111ically.

Ar.plications , . , , ..
I\ few areas of relevance to phannaccutical engineering are cnumer- '
.;tcd here.
Evaporation :,Heat is 'supplied in order to convert a liqtiid (vehicle)
into a··vapour.·which is subsequently removed. Thi� process is used for
preparing vegetable· extracts. A constructio11 si'n1ilar to :shell�and-tube
lu:at exchanger is c.:mployed in evaporators. The' heat f1ow· can be­
qu:mti ficd 50 'a:; to estimate tl1e efficiency of the process.
Distillation .: I lc�t is s,uP�.licd to. a liquid mixture fo; conv�11i11g the
liquid iilto vjpour so ,that' ,the individ�al vapour components arc con­
densed at 'ai1othcr place. In case of steam' distillatior;i, steam will be'"in
direct contact with the,material. · · ,,. � · : •
1

Drying : ·111 thc pro<lucti,01{ of tablets, hcal is pasied through a carrier

gas over �1-bcd �f w�l solid mass for achieving drying. In case of spray
dr:, ing. l1ea1' is supplied to tl�c solutions and
... 'suspe;1sions
. . ... · (as
. ...in case
. 'of.
production of milk products).
103
 104 ; PHARMACEUTICA!,- ENGINEERlt-:G Ch-S fLOW or I IEAT 105
Cry stallisation : Saturated solution is heated tb bring about �up,7r­ Radiation
saturation,' which' promotes the crystallisation of drugs. On the other When heat flows through space b>: meanS of electromagnetic· waves.
hand, removal of heat (cooling) from a saturated solution also facilitates such energy transfer is known as radiation. _,,..
crystallisatio�, as in case of purification 9f bulk drugs. For example, a black surface absorbs ·most of the radiation received
Sterilization : For the sterilization of pharmaceuticals. autoclaves arc by it. Simultaneously the �bsorbed energy is qua�titatively transfe,rred. ,
used with steam as a hea�ing med_iym. . ,Dry heat is used for the into heat. Fused quartz transmits all the radiation that strikes it, while a·· .!

sterilization of glass apparatus.and other containers. polished opaque surface or mirror will reflect most of the radiation that
In ad.dition, a number of other processes; . such .as boiling. exsiccation, strikes it. Solar water heaters, solar cook�rs, microwave ovens, micro­
sublimation and fusicin, also use"'heat. wave cookers, sonicator baths etc., arc few examples in which radiation
is utilized for ....producing
. ... heat'.'':,;;
In a laboratory setup, number of equipment involving heat arc used.
;.

In 'general·. these mec11an1sms may operate simultaneously. For

A few examples ar� air-ovens, incubators, dryers; re!ngerators etc. On
industrial scale. equipment are \1sed fot: ap.plying heat, removing heat
and preventing heat loss'. Th� ba�ic principles involved in heat transfer
arc understood properly for. the maintenance and efficient working of the: .
· 'y, . ''
equipment.
example. in ovens hot air is circulated by fan, so as to transfer heat by
forced convection; Simultaneously, heat is transfcr;ed by conduction
from th� shelf to the material' in contac.t. Heat also radiates from hot
walls of the oven ..
'

CONDUCTION
MECHANISMS OF BEAT FLOW
Heat can flow only when there is a temperature gradient, i.e., heat
Heat fl�\vs from a ��gio1,1, of high terriperatur� to a region of low flows from a hot surface to a .cold stirface. The rate of conduction
temperature .' Heat
� .
mav-� .flow
., • '
by one
r. or more of the three basic mecha- through solids can be studied easily, since it is" the sole phenomenon.
. ,
nisms . •, The basic law of heat transfer by conduction can be written in the form
··
.,,, of a rat�� ,equation as follows: •
Conduction
When heat flo,v in a body is achieved by the transf�r of the momen- · driving force
Rule = -·------ (1)
tum of indlvidual atoms or mo.lec1:1lcs, without mixing.· such a process is resistance
kno�n as co�1duction. . . .. The driving force is the temperature drop across the solid surfaces.
.. For �Xjlmplc, f16w of heat through the metal shell ofra,boiler takes The greater the' temperature drop, tlk greater will be the ,rate of heat
place by conduction as far as sol.i9 wall or �hell is considered. No flow.
mixing ii invol�ed. C::onduction is limited to solids and Ouids whose The now of heat will also depend on the conductivity of the inateri­
movement is restricted. 1·;
·
als through which it is flowing. For example, conduction· 'of heat is
, � i, r
faster through an iron rod than through a wooden log. This factor is
Convection ·. ,. : . repres·ented by the term resistance, which can be quantitative!)'
·. �xpressed
. When heatflo,v is achieved by actu<}l ,mixing .o�warmer P,�)lti.�n� with
.
, · ··-,
! ,. . J 1 •
by Fourier's law.
cooterp9riipns of the same' foateri�l, the· pr,occss is known.�s �·onvcct1011.
. • . . •••

..•• ,1,. , • 1 ... 1 . .-· .r . , _J J " .. . thickness of the surface (m) '.
F'or · �xample, heating of water by a hot surface (coil· type water· Resistance = ---· . · · ---
heater) is mainly by convection. Convection is restricted to. the flow of mean proportionality constant �W/m·K).
>< area of the surface (m.)
heat in fluids. (i.��· liquids1,and gases)..· Convection cu'rrents of air arc set
L
up.,'almo�t daily in the atmosphcrl' .These arc responsible for winds, land .
. . '. (2)
• and sea breezes, ocean' 'ctirrcnt{etc'. . ·'
kmA
Equation (2) for resistance can be obtained from the Fourier's law.
 106 l'I IARM,ACEUTICAL ENGINEERING
Ch·S Fl.OW Of I IEAT ,, o.,:; 107
Fourier's Law-Conduction of Heat through a Metal Wall
Fourh:r 's /air stati:s that the rate of heat llClw through a unif'orm gradient. For a steady state heat transfer, equation (4) chang�s �o:
.
material is proportional to thi: area and · the temperature drop and • dO . -k.A.dt
inversely propl)l1ionll to the kngth· of the path of flow; :__::_ = Constant = q = --- (5)
de . . dl
The Fourier's law may be mathematically expressed as:
· where q = r,\tc of heat transfer. J(s (or W)
area (111 2 ) i< tcn;pcraturc difference (Clt)
. flow oc.
Rate. of h.:at ·
thickness (m)
· 1
A.61 Higher temperature
q oc. -­ side (t 1)
l
k111.A.t!.t Lower
or (3)
l temperature
side (t2)
where k,,�=-· mean proportionality ·const nt, W/m·K,
�
DcJ"ivation : Fourier's law can be appqcd to a metal wall through
which the conduction of heat is taking place (Figure 5-1 ). The charac­
teristics arc as follows.
Area of the \Vall = A, m2 Fig�rc 5-1. l!eat transfer through :i nictal wall by conduction.
Thickness .of the wall = l. m
The temperature difference 'in the intermediate section is not known.
Face
· of the wall (I IH) is maintained at a uniform,. But temperatures a� the two faces of the wall are known.' The area, A,
d.:tinite and higher temperature = t /, K
may v'ary with L, but is independent of temperature. By separating the
Face of th<..: wall (CC) is maintained at a lower, variab.lcs. equation. (5) can be written as:
o but uniform temperature "" l!, K
q.dL .
The heat flow will be at right a�.gles to the plane A and is assumed to --=-kdt
A · ,(6),
be in a steady state. Consider a thin section of thickness dl at an .
intermediate point in the wall. Thi� section is parallel to the plane. A. .Int(,!grating equation (6) between the limits
For this section, Fourier's law 1nay be applied as given l,)clow. l =::: 0 when·t = ti and'
dQ -k.A.dt l � L (total thickness) when t = t2, ·
------- gives:
.
I
de dL'
I ldL f '1 ,,
where Q .� heat transferred, J q - ;:: - kd, = kdt
8= time. s () A IJ •. ,
1
k= proportionality constant, W/m·K •
. ',
ql . .
·t =-= temperature, K. -- = k111 (t J - 12) = k111:.1t ( 7)
. A
The 'c·onstant, k, is a function of temperature, . but independent of·
:} '·
leng\h.. The 'minus' sign indicates the decrease in temperature in the' Rearranging equation (7) gives:
direction of flow. In equation (4), (dtldl) represents the temperature
kh;.A . .dt
.q =---- ( 3)
L
·;,,\.,.'

.,
 1Q8 PHARMACEUTICAL ENGINEERING
Ch-S FLOW OF HEAT 109
when: km = mean proportionality constant, W/rn·K
In steady state heat transfer, · q' rcmain!i com,tant. In equation (3), From Table 5-1. the following conclusions can b� drawn.
the term 'L1t' i_ndicatcs the driving force. Equation (3) may be rear- - Thermal conductiv,i�ies of liquids and gases are very.small com­
ranged to obtain: pared to most of the solids.· I� other. words, the resistance
L1t offered by liquids and gases is high as 'far as the conduction is
'(1 -- ··-·-----· conccrricd.
L - In case of steam jacketed vessels, the kettle (in�er surface) must
k111.A have good conductivity so that maximum. tlmount of heat passes
from the steary1 to the contents. The hi,gh' thermal conductivity
Comparing the above equation with rate c:,;prcssion [equation ( 1 )]
of copper suggests that it is a suitable. _material for the construc­
i 11d icatt:s thai:
L tion of the kettle. At the same time, the metal used for jacket
N.esista11ce = -­ (2) (outer surface) must have minil'T)um conductiv.hy to prevent loss.
k,,,A of hent by conduction and radiation. The low thermal concluc­
Fourier's law is thus u,scd to define the resistance Ill quantitative!' ti,vity of iron sugge�ts that it would be suitable material for the
terms. cor'lstruction of the jacket. Such 1na.terials siloti'ld be resistant to
solvent or chclnical action -of liquid.
Applications Thermal conductivity is the rt:ciprocal of thermal
resistance. Thermal conductivity of a solid is expressed in terms or k as For the constr�1ction of evaporators and tubular heat 'exchangers
per equation (3 ). thermal1 _coni:luctivit); values are helpful. Thermal conductivity is very.
sensitive to changes · ip chemical cornpo�ition and temperature and,
· The cvejficiem of tliermal _co11d11ctivity is the quantily of heat that'
therefore, the above values canncl't �e applied to all situations. The
flows, across a unit sorfacc area in unit tiine, when the temperature clrop
materials and their usefulnes5 with respect to thermal conducti�ities are
is unity.
discussed in Chapter 17.
1 The coefficient of therrn.11 conductivity depend:: upon the material
with which the' body is made .and upon its temperature. · Thermal Compound Rcsist,rncc in Series
conductiviti�s or so_mc substances are given in Table 5-1. Consider a flat wall constructed of a series of layers as in · Figure .5-2.
I The cha�actcristics arc: r- ·
TAOLE.5-1
Thermal Conductivities of Some Metals Thicknesses of the three layers ,.,. L i; 'L 2 and L3, m
' Copductivitics of materials of which layers are made = k J ; k; and""k3,
11 '·
Muteriuls Thermµ/ conductivity, W Im· K W!in·K
Area of the entire wall = ,1: m2 J' . ·
. ...
Temperature drops across ·three lay�rs ·= L1t ,.· .1ti. and ,lt3, X
·I Copper 379.0 'I

Silver 57.0
' Resistances of the three layers � R t, R1 and R3
Steel 43.0 t � ' ,1 (�

Aluminium 24.:! For· the

• 'above descriptions, /h\! total temperature dn1p ma:y be written .
. '
lJ H ': ", I

t�) • • '. • •• .•
as: ' './

.
0

Stainl.:ss Med 17.0 ' l.

,
.
Drivi!1g farer, Llt = J.t t + L1t2 + L1t3 (8) · :"°
Glas§ (horosilicah:) 1.0 ,•·· .
. 4 '

Building hrid,s 0.69 . The rate , of flow o:fi. heat, through several resistances i� · series is
exactly analogous to the current flowing through several electrical
Water 0.62
resistances in seri�s·. ,. Ther_efore, the overall resistance (R) is equal to the
Air 0.03 · 1
sum of individual resistances.
(9)
110 l'I IARMAt'ElJTICi\l. ENCilNl:ERING
Ch-5 Fl.OW OF IIEAT 111
Direction of heat flow
cylinder at; the centre of the pipe.· The following characteristics rn�y be
enumerated.
Higher
Lower temperature
temperature side
�ide

, ' Low temperature

(t 2)

;:.,

c
Yigure 5-2. Flow of heat through.
H
..
I several resistances arrangcd in series.
. .' Figure 5-3_. Flow 'of h_cat ·
A�cbrding to Fourier's law, individual resistances, are described· by through thick-walled cylinder.
. '
equation (2). These arc incorporated in equation (9) to get:
Mean thermal conducti"vity 0£ material of cylinder =1k111, W/m·K
L1 L2 L3 Temperature of the inside surface (higher) = t1• K ·
R=--+--+-- ( 10)
k1A k2A . kyl , Temperature of the outside surface (lower) = t2, K
Radius of the thin cylinder = r, m
Since· entire heat must pass througµ the resistai:iccs in series, heat q Thickness ,of the thin section "'ii(''l, m
can be' written as: Radius 9f the ir.iler wall = r r, m
q��q1+q2+q3 · (11) Radius of the outer wall·= r2, m
Using the principles of conduction, the rate of heat transfer, <J-.. may Length of the hollo_w cylinder = N, m ·
•be expressed as:, , The heat row (in watts) is considered as P.araTiefand the rate of heat
4t transfe� (q) can be written as:
CJ = - (12)
R1 + R2 + R3 dt
q = -k-(2m·N) (14)
Tl;e contributions of temperature drops· to the total temperature in� dr
individual resistances to the total resistance can be expressed mathemati­
where 2 m-N is the area of the heating surface, i.e., the interior of the
cally as:
cylinder: The mean surface area (A 111) may be writtc� as c-ircumference
( 13)
multiplied by length of cylinder.
Heat Flow through A Cylinder-Conduction Consideriqg the variables such-as radius and temperature, equation
In a heat exchanger, hot fluid or steam is p�ssed thrriugh the circular ( 14) is rearranged to obtain:
pipe. The hot fluid transfers the heat to the inner surface of the pipe
dr -2JCNk
wall. Further heat transfer takes place by conduc1ion through the pipe - ----dr (15)
wall. The, rate of heat transfer by. cond_uction through a cylinder may be ,.
. r.
q
obtained as follows ..
Integrating equation (15) within the limits of
Con�idcr a hollow cylinder as shown in Fig11re 5-3. The heat is ·
r = r1, when t = t I and
flowing from in.side to outside the cyll_nder. Cons1acr a very thin·
"r = r2, when t = t2,

·,
 112 PHARMACEUTICAL FNGINEERING
C.:h-5 FLOW OF IIEAT
give�/ relationship is explair:ed below.
21tN , :·�
- The value r ,,-,."', < 3.'.!0 reflects ·, that the wall1 is thick. If, arithme")
kdt .
i I , . . ' .
·. tic mean radius
� 1

is used, the result will be )'lithin 10 %. of.t�at

CJ IIJ
I:
_obtained by equation 16 c1,.e.,1o�arith'mic rnea� r�d_i1:1s.Is us���:
2mVk,,, r
/11 r2 - In r J = · The value r,lr2 < 1.5, rct1ects 1 tha{the' walJ'is . ttiin: . Jf arithmetic.
(tJ ·'.; t2)
mea:n diameter is .usecl; the results· ·v.�hf'bc. within l o/o .·o( th�t'
obtained by cqu�tion 16 (i.e., logarithmic' meari r�dius i/�se'cii'.\
2mV km (ti - ti)
(]
=
------- ( 16) For rriost cases in pract.ic�, ·arithmetic mean )a�!\�� is'' �ufticiently
In (r2!r 1) .iccuratc. if the cy'1indcr is thrrt-wallcd'. !' For" thick· wa01'd tube; logarith-.
Equation ( 16) can be used to calculate the rate of heat flow through a mic mean radius !fas to -b� used. The use··of either an inner radi'us or an
• thick walled cylinder. outer rac.lius. dues not give sufficiently accu.��t<; results. : _.
... . • ;:· :. -,. 1
Conduction t·hrou.gh Fluids
.
It is desirable to express the rate of heat flow in a mo;c convenient . .. . . ,.,.,
form (similar to flat wall) as shown below. Coru.luction in liquids i� usually small and this p�cscnt� 1 a :consider­
�oe llicicnt x area x temperature difference able obstacle for heat trnnsfer. , Conductance in: fluid�)s because of
CJ = ··--- ------ 1
eddies setup b/ the'1ch:-inges in ctcrs.ityf·w'i'th'\e!flperaturc,· \\;hjch is.
I ength of the metal layer. observed in the boiling of liquids· (as in case of evaporation and distilla-
km.A11iJt1 - ti). tion of liquids): ·' .·, •. '-· · · , ',:. ·. · ··,·
. (17) Conduction through fluids rarely.occ1/rs in practice,' except ·�·hen heat,
'1 •
• •

q -------·
L ·
flows through thin films. In these cases. the thickness ·of the film is not
By equating the right hand-side terms in equations ( 16) and (17), the 'Cxactly known. Therefore. equations described earlier:'�ari;1ot be applied�
area (of surface) term may be obtained as: This difficulty can be overcome by the usc·'of surfaie� coefficient, which·
' • ' \ . ·'\l

. .

2m\' will be discussed later. If a body of fluid is lar�e; both convection' and
------
A,,, conduction may preyail. This complicates the d7ita analysis and faiis to
L /11 (r;lr 1) provide accurate predictions. · · :' ;o
'
r:1
, .. . , . ::i
" l -· . t . ••

Since l is the thickness, it is related to thick:less .of the tube, i.e., (r2
CONVE.CTION :,. ·
- r1) of the cylinder. This value is substituted for L ·and rearranged to
obtain A,,, (mean area pf a cylinder).. When heat flow is achieved by°' a�t�al mixirig.p(�artlle;' p�rtiori's
with cooler portions of the same material,. the. process . is known "'as
convection. · ·
. , , 2roV(r2 - rJ)
A = . .. (18) · '
·. : •· · : · , .·.· -:_,1 .p::.I ,. '.. ''. •· ·. :' ;',· .1
• I11 1Ir 21Ir 1.,
·,
.. . ' •.•.. Ill
· - ' · .• The heat transfer in fluid pccurs on account
1
.· . . of. . actual. mixing � of. its
·

layers. · , .., , · i!
A.111,.area may be considered as 2 ra-mN. From equation .( 18), mean '
. : . , .·.'. ··. ' . �. ; ':· .'.,:
radius , r111 , may. be written .as: . Forced convection : Mixing of fluid may. be obtaine_d by ' the use of a,
.

(i·2 - r1) �tirrer·or agitator _ or pu �nping, t��\lf uid for recircul_ation. Such a 'proce��
,..m =, ( 19) m h�at. transfe�,.;s: designated .as forced conve(!llOn. For e�ampl�,-�!P
/11 (r2/r1) 2. 303 log (r2lr 1) ·•
some types of tube evaporators, the evaporating li�uid is forced thr�ugh
In equation (19), the te.rm, rm, is called logarithmic mean radius. the tubes under pressure. .,Therefore
· .... �·'
fori:;ed convection is obscr,·ed ii' · · ·
I ··: · �- 1.:,.,,· L--··> ·· .. . . ". ···.· �······;:/,
Logarithmic mean is lcss-conyenient than the arithmetic ·mean. · The Natural convc�tion : Mixing of fluid 1nay .b,e''ac�ompli�h�1c!·
. by the
. is sufficiently accurate, if the:� �ube
arithmetic mean is thin walled. This currents set up. when.body of fluip isheated.\ s' i i' c h'a process•is km?�\11,
. ·,, , ., .,
Ii• ,- . . ,, .. ,:t: .· . ')·r · : . .. : .1"- • • �:•• .,_�

.\
 Ch-5 FLOW OF l lEA T 115
I 14 Pl li\RMi\CEUTICAL ENGll'JEERING temperature distributi�n across a column of flu_id that is being heated (or.
' .
cooled) is related to _thc velocity distribution across the sal!le. column of
as natural COi11'eption. For example. in pan evaporator. convection fluid.
.
v.; '

currents a�e set up in the evaporating liquid.

. . i '� .
Consider a case of heat flowing• from a h9t fluid through,a met�! wall
'. ·i� g��era" L lluid flow may. be _d;scribed as either laminar or turbulent. .
into a cold 'nuid.' At a speci fie point;' the·. ,variatipn of teinperature on
Th�se c�efte _probl�ms iR,)h i1 �stir:n,ation�. Some of them arc as follows. each "side of the metal wall is dep!ctcd in Figure 5--4. Several important
. .

When heat is, pass�d through the. tub.e, stagnant film� ,are important in
I. ' f .,
facts are evident from figure 5-4, aSi l&}ted below. ·
determining the rate of heat transfei.
r
' . , ,1 • , ': • • ·
-..;
1 .

When fluid exhibits viscous flow, the . veloc.i�y is zero at the

·• I ,• •
actual su_rfacc of the, \�all.,. It. means that t_he lqyer of. fluid
· a9jacent to the :wall ac' .ts . as a stagnant film. )

. A conwai-atively stagnant ftlm can be observed even in turbulent

COLD FLUID HOT FLUID
flow. At the centre, the fluid is in turbulent flow. while at t.he (Turbulent) (Turbulent)
surface the fluid exhibits viscous !low. A tit,;, of buffa layer
oscillates between these types oflluw. · ·.··1 r
•. ' • < · 1 r
i
. Some't' imes. scales a're cl'�p'osited on the .s.µrf�ce of the metal wall
. '
a nJ heat must be conducted through the scales.
r '. , I .,.· I ' •

When steam gives up latent heat, water will condense on the.

surface of the vessel (or tube). Again the he_at must be con-
., :ducted ·t!1rough thi3 ·\•later film. .
.·' . . :1 . . . Heat transfer·
.' For,hea� trans for in a . tub�� l��at m11�t pass through the stagnaa;: fiim
b'y co�duc:ipn. He,r)C.C. condu,ctivity of these films is important. Nor­ Figure 5-4. Tcmpcri11un: gradients in forced �onYcction, while heat
is !lowing from ;1 hol' 11uid to n 1:ulcl 11uid through a metal \\ all.
ena( Iv: thl!rtnal conduct: vi ties cf fluids are.., low. The conductivity of .the ·'
st�g�a�t film will be still less. .
Fqr example. the thermal conductivity-of Metal wall : The.: �haracteristics arc as follov,:s.
{), " . ' .
water is less. A tilrn of water has a rcsist:rnce of;abour500 times and that (I) Dotted I incs HH and CC represent the. boundaries of t�e films; in
of air film is about 13.000 times greater �an a copper sheet of the same viscous flow on the hot\nd cold 'sides,, respectiv�ly,' · on each
thickne'ss. Thus, 'tnc resistance offered by tQese films (though it is thin) side of the metal \Vall. !' · .. · · · · ·
is large for the heat flow. Be�c:ind tijese films. the turbulence brings ,.
· (2) The temperature gradient through. the line -lctd i� cc1u,�.c9 _by. t_hc .
aboltt'bipid equalization of temp·ciature. . . .
· · L flo�v of heat j)u1:ely by conduction through the )TICJal. whose .
Therefore, u,';
�esistance offered by the boundary film is of i1�por­ thermal conductivity is known.
.
tance in the flow of heat, particularly in' the evaporation process.
'1·,

(3) Metal wall thickness is l.

Forced Convcction"""'.Tcmperaturc Variation-Individual Heat Hot fluid side : The characteristics are as follows.
Transfe_r1 �oetlic)�nts.., · ,� , ·. · , . · · :· · . · .
"(I} To the right of HH, the fluid is in turbulent flow on the hot side'.'
·., fy'ti�ing·o'r a tlui�. m'ay be obtained by tli11use of a sti'rrer or agitator
(2) · t a is the maximum temperature in the hot fluid.
·or pumping the fluid for recirculation .. S.uc� a process in heat transfer is .
desJg�ateµ as forced convectiom
· (3) ·tb· �s the teniperature' at the boundary on the hot side (tu�b�lent\
1
· ':;, ·
· ·
Q . • . • and viscous flow junction).
forced convection ··is obtain.cd: in some' types of tube evaporators. . I

whereJn)he c:vaporating liquid is forcecl ·thro'ugh the tubes under pressure . ,.

.
: ·. J. n. a ch
, eat transfer! process, the ·overall· d,effieient depends upon' m'any
variab'lcs. It is necessary to break them into ind.ividual parts. The

._
 Ch-5 FLOW OF l 11:/\T 117
116 Plt..\l{\1/\(Tli lKtd. ENGINEERIN(,
Let q w.1tt (jouks per second) of heat is flowing from hot fluid. to
(4 )· le is the temperature at the actual interface· ( bet\veen fluid and
cold one. Same heat. must· pass through stagn' ant flt1id film on the hot
..solid surface). · ·· side. through the metal wall �nd through the stagnant, film on the cold
I 5) Curve ta ti:, le represents the temperature gra9icnt from the. bulk side. Let the following be the characteristics.
of the hot fluid to.t_l1e metal wall. This is caused _by the flow of Arca or the metal \�au· 01{ ti{J l�ot sid� =.·r1 1 . 1112
·
heat in forced com\�cticin. Arca of the m.:t:-il wall on the- cold ·side '""A,. ni2'
. ( 6.) t I is the average temperature on the hot lluid 'side represented by '\"crag� ar�a of' the metal ,vall ,=, A 1,,, !,i/ -

<' .
the line MM. In general .' for heat transfer calculation. average
Surface or J,/111 coefficient on the hot side : On. the hot side, the
tc:npertlturc is important.� This can be obtained by taking its
·surface coc�Qcicnt, 1 '11,-,is d�fined a�: •. . . . n ·,cs·',,.'. ., ,
temperature after mixing, ,.. · .
amount of heat flowing (W)I\.,, r.
Film coefficient on2 , .•_ --------··
Cold fluid side : The characteristics arc .
' as follows. the hot Hdc: (Wftn ·K) ..
. area (rn2) ·< diffi;renc in temperature (K)
'.·
_ f
(l) To the kft of CC, the fluid is in turbulent flow on the cold side.
q \ .'
c2) tr is the minimum temrerature on the cold nu;;i. I,,, = --- ·-- (20).,,;::,
· t (3) ,t� is the temperature at .the bo'i:mdary on the cold side (yi::,cous A 1 (th t,j
·
. and turbulent flow junction).I . from equations (20) and (7),,,it can_ r-c '�ecn that sur�cc coefficient
(4) t<l is the temperature at the actual interface (between fluid and (h 1 ) is analogous to the 'term, k!L for ;i nctal wall. Since UkA is,the
. '
resist;incc term for metal wall. the tern( · ·
solid):
.t .
(5) C�1rve tJ tc tr represents the temperature gradi.cnt' f om �he met:11
r
· I .
---- is known as thcr,mgl res.istancc on l1ot side .'
wall to the bulk I of the cold fluid. This
. is c;uiscd bv
•
the flow or 11,.-1, ".. ·
1Ji1�1.
·• ·
!1cat in forced convectioi-1.
(6) t� is the average temperature or. the cold !h:id .side, represented The thermal rcsis.tancc ,is due t o the com\1in\!d effect of tlJe vis�ous
, .
film HI-I arici the turbulent co1'e. This resistance caused the difference in\·
by the line NN. In general. for heat transfor calculation average '
te1_nperature, /11 •• 'b·
t�mperaturc is important. Tr.is can be obtained. by taking its
·,. ' '
temperature after mixing. . . Swfuce r;;. film coefficient 011 '·the cold sid� · Film coefficient on the
, r
� '
cold side can be written on similar'lirics as:
Surface or film coefficients ·: ln forced convection, the stagnant
films' (HH and CC) are of great importance in determining the n1te of . amoun of heat !lowing
Film coejflcie11t on the cold side = �---- --------­
heat transfer. Though these films are thin, the resistance offered by the111 area x difft ·ence .in.ternperaturc·
is large..Beyond these· film's, the turbulence brings about rapid equaliza­ .J·, ;" .: : •• .. � " •

a;:---­
({
tion of t�mperature. (21)
h2
Film coefficie111 is the quantity of heat flowing through _unit area of A2 (Id .-12}
./ f "
the fi Im for unit drop in temperature. And.
.I . . :· ·'·
I · ' • "
• I

It is 'the conductive··capacity of the stagnant film for the· tdnsfe; of

··-- is known as thermal resist.;l,nce 011 cold side.
heat. , �' . h2A2
It is difficult to determine the thermal resistances of fluid films. since
thicknesses of the films cann.9t be known precisely._ The thickn�ss of the Oyerall cocflicicnt :_ In the over· all heat tfan.;l'er, 'three· resistance.
film depe.nds ncit only on viscosity of the fluid. but also on the fluid terms ar<!..iq�olved in series..
circulation level (forced convection). Hence, the resistance offered by
these films-cannot be individually calculated. Therefore, indirect method
··1 '....
of computation of surfac� coefficients is employeq.
/
 Ch-5 FLOW OF BEAT
l'l li\RMACEll'rlCAL ENGINEERING diameter. The overall heat trans(e� coefficient for a tubular metal
118 , 'I- · ' "'· '· w�II
may be written as: : ,.,·
J Q �>..,: :} I
side.
.� is the, resistance on the hot fluid , (27)
h1A I ., · : 1 ! , · l l. • I · I LD1. D1
J .

. L. ., ·� ,, .' -.-+--· -i--·- ,,

--· is the resistance qf the .metal v.·all. h1 kDn-�, h2D2·
kA111 . . .
I . . : ;,.'
'I : ' ' . ., . . . ';
-- is the· resistance on the cold fluid side.
In some cases, one particular area is more: corlvenient than the bthir •.
S-�p�o�e '12 >� 11 1 , the (D/D2h2) becomes small in comparison to (J!h 1 ).
· h2.-!12 , . , · ,: ·, ,. Spmlarly, rcststanc� of the tubC.:�yall is also small, in-.com-oarison: with
. overall (1/h I) ., 1.lcnce, rJtios, (D/D111) and (D JID2) have :very, little '.significince
. Applying the. principle of compou'f!d rc'sista�cc· ''in s�'ri��:·'tlfo. and can be disrcgard�d. ,Then, equation (27) .becomes:· · ', , ,, '.. : . •.. '·
heat tran�fer may,bc wri.t:te,i-1 asr ,,,.. ,1·.·''
. • ,
,,I
I
J

,·.t
.... '

(22) U1 = ---,,.------ •, (�8)

q =---- ·• I . I ,L · I
1 L · -+-+-
-- + --· + ----- hJ. k . hi
lii vf, , · k.4 111 '11112
on <,22) · Equation (28) can' be used in case's of:
If .both nume.rator and denominator of th,� right side of equati (a) thin wallcif tubes with larger diameter
l· "

arc mul1ip!icd' by:A 1 , equation (23) is 'obtained. r· . .. (b) thin walle d plates
°
q=----- In these cas'cs, area A can be used for A 1, A m and A.,"'' sin�e errors will
I 1 LA 1 . . , Aj .
b c neg I 1g1blc.
. In such cases,
-+---+ . l,'·'
hJ kA III hy4 2 (29)
t I . . ,· ·' ' ,J'
cd by
lht�l},' the overall heat , trai1sf'"r. co�ff1cic.r,� U J ( W /m�·K) isid_tfi.!J
•'

When li,-is very small compared to h1 and (Uk), (Jlh i ) will be larger.
ec;uatio1"'(24) :''' . . . . . ' Therefore thc�c two terms iri the denominator arc disregarded. Then

I' u -
I
. , ·-...
' -·/ .
------
.,_' . (30)
I'.
], ·IA 1 · A1 1, ·
-+--+-- .
Thus, rate of heat flow fro1v one fluid tci another through the retain­
. _
.• ., ' . .I ,,·:
,, tng wall can be s11nplttied. Hence, numerical value of surface coefficients
1. ,f-
can be predicted easily.
nt that:
'l If equation (24)' is' compared with equati�n (23), it is appare
(25) Factors influcndng film coefficients : Se�eral factors influence the
·· q-= U1t1.tA1
surfa�c film coefficients. However, the factors that arc widely applied in
Equation (25) · states that practice arc a few \Vith reference to the processing conditions. These
Rate of heat transfer= overall heat transfer coc:flicient x arc: " . ........ ' l

· Thermal conductivity of the liquid

,· :.
.' 'I·
f ' ,•'1,nrea-1of'fhe'·hcut'ing surface v
Specific heat of the film
temperature drop I
• Density of the liquid
· ation (equa tion (24)) is based
, for, a t�bular·.w.aR: T.he above deri\· - Turbulence of the fluid ,
lfo,extendcd,''to
'on 'th� metal wall of thjcl,;ncss, L. This r�lationship may Thickness of th'e film . , ,·· ... 1
be writte n in terms of
a tubular metal �all. The heat coefficients may
' .·. f'•
..

the corres pon d ing tube

diameter (metre), since area is proportional to
 )
120·
; •
I

1'11,\RMAC'LUTICAI. t::--(il1'1TRIN(i '

Ch-5 Fl.OW OF IIEAT 121
If the tiltm;:m: thin. their resistance,; will he reduced. This ·can be
achieved by increasing the speed of tht steam on one side and the speed , surroundings both by ·radiation and by convection. At lower temperature
ranges: convection !s more predominant, while radiation is imp9rtant at
of liquid on other side.
hi�hcr tcmpcraturc ranges� In practice, liquid film coefiicients may vary
Flu ids. in Natural Convection foom IO to 200', dependi :it 01, the arrangement ,of apparatus and the
viscosity of thdiq.!'ids.. · '-
When a lluid is hca' tcd. the currents set up may cause mixing of nt1id. ·
Such � heat �ranstcr pr�1 t;fSS is knqwn as 11at11ra/ c.:011wctio11. . 'Application : Nat u��1' �onvecffon is obs'crvecL,when c�tracts. are
1
_
The 111ed1.111ism of natural convection is. depicted in Figure 5-5. . evaporated in open j)ans. � I I .; ',)' , \ '' ; ,

) ' '
Consider a case of single horizontal cylinder. J\. large vo·lumc of flu1d is_
! !�·:'.

Changes in Fluids during Hc,1t Transfer

present surrounding the cylinder. When a fluid is in con.tact with a hot
surface, the fluid that- is . immediately adj�cent to the tube absorbs heat. In heat lransfcr·by conviction, two liquids arc involved:,: The hot 1

The temp.:rature of this part or the tluid increases, which in turn de- r liquid gives heat, while the cold liquid'.rece°h·es it.' Eac�··Iiquid under­
creases thc 1knsity. As a result. the fluid rises from the surface and i.11. goes changes during heat trans(er. Steam condenses to �dve he.1t,'.while
·,: ':r' � ·
replaced b� the cold tlt:. id. This proccss continues thereby cffi:cting the· the cold liquid hoils. . :,r ·
mixing or hot ;md cold puil)s.
. Hot' lict uid-St��m boiler . : Steam' 'is igencrat�d i� .•� · c'cntr�I boiler
Fluid tin:ulation causcd b): changcs in. the dcnsitJ,es <l,uc to tempcr;1-..i' hc'luse 'at high pre�sure: The following are· the ad.vanta:ge�. . . ._..,. I

ture dilkrerll'cs in the fluid is termed as natural c:011vct'lio11.

''!
( 1) � ligh pre�sur� S�car� can, bt: ,t;SC� t?}riyc. aJur �i�C for, general-•.,
' 1 t
II ! • i. ,··.)' I < ' ' .. • •.; ·�

I .
. . l

' .. · ·.
mg electrrc power. • ·
�

F(uid circulation also changes with: ., ! . � • _

. i " •
0 ,

t • • ,a,

(2) Low pressure_ exhaust steain.ts used for pro(;css heati,ng.

r' ,l ,. • ' •' M :' I
< '

g1:omctry or the system, i.e., size. shape and arrangement

heating surface. (3) �e,�tral �en,cr�tio�1 is ·n,ore ecof10J!1it�I. . , .. ,1 .
- shape· of :he \·cssd in which the tluid is enclosed. . (·l) More .stc�m i� .stored OR;,,.O- boiler if higli pressure is. applied.
(5).· liigh p'r�ssurc steam mcaiis high temperature.
• . .' .. _.. . . . · . . ...
•d
Clrn_radl.'ristic.n> rl,e steam : ( 1) Steanj.'sh<;>l!.ld be ard!}; ;s. possible.
f

- ' thereby heat losses can be ·minimized."'· · · · .. ·' ·

{
! .
(2) Sin' ce thC'latent · heat i_f tl;e tiscti'1T hJat; st�am should be used at
Q the l�wcst pressi.',rc thh't will give a suitabl� teinper�t�'�e-·gradh��t.
CH. St�arn should be purnp.�d ;tt its saturated temperature.'. Sup��-
. '

hcated steam should not be used.' ':' ., -; ·: ·t,.\•:... ,/"'. •,; : , ·'.:
.:,��;,• .,•".

· (4). St�am should bc'rcplaccd continuously so that ..the process pro-·

,
,:;
.. I �· • �. 4 ' •• ._.� '.,', ,t'
' '

cccds indc!initely.
····� ': ·.,t.,.•·:,
I

',}lot . liqu ill-�oi1dcnsing of vapour : Stl:am gives ,it� heat' of va11odsa-

i. • ,�· • ;, ...
'I. 1 • : • i·· · ' ., . e \:•,, •'
,.
•

.. .
, t1o n during f�!1:d�_11sation. T�is. heat_ i�:. . �f�·?,�:::rrcd • to)J�!!_.,f?l{ liq�tid .
_
tluough, a nwtal wall. . "'
�.. '/ . (·l,;:·. .. ·
.. •:·, �, .. .,, ·. ./i
.. .
,'f\.
L\t, Deg K ., • ._.�f. ,... --

- ln a hea�er. steau1 i: s passed thrdugh fhe tubes or outside the tubes'. . In

Figure 5-5. Mechanism or hc;�t.: tran�fcr in natural comc1:tion
The physical properties of the 5ystc'n1 arc' individu:tlly c, aluatt:<l al
the mean· film teinpcratun:.. Generally. hot bodies lose heat to their
each case. the metal surface of the tube gets h�atcd up.· 'While trapsmit·
_
t111g heat to . a me.tr.!. s9r_f,w,e� th�. satu�atc_d •,apour .coti.Qenses into t,•,o
distinct forms b,ised 'on .the,.oature of wcuing of the m�hil su.rface: These
arc a-. follows. · .·. ;_, :'- .. ; ',.,_,._.:,�'"'' ,. ··· · ' ! ' V·

f
 122" l'IIARMACl:UTICAI. ENGINEERING
Ch·5. FLOW OF IIEAT 123
Fi/l,1 type co11densatio11 : In this type, the condensed liquid wets .the
: 1 ·····
surface on which it is condensing and forms a continuous film of fl,id Hotuid __
condei1sate. _ Uq,i
--
� �- � -

-- - --
;.
lf condensation is occurri.ng on the outside surface of a horizontal - ·�-
--- ---+' =-·. �
-- -:- �
metal tube (a very common case), this film bf condensate drops off
beneath the tube. If the tube is vertical. then it runs down the whole w&Y2?2' -� · �:=
4: ����
(a) (b) . (c)
length and drops off from the edge. Generally, smooth and clean ""' • �-
Heating
surfaces· tend to form film txpe. For film type condensation the film surface
coefficients are low. Equations have been proposed for heat transfer · Cold fluid
calculations.
Drop-wise condensation : In this type, the condensed liquid col.lects
as .drops that may· range from microscopic size up to drops that a�e seen
with the naked eye.
If the condensed liquid does not wet the surface, the drops grow and ; . ·. (f) '·( o, I

then fall off the surface, leaving an apparent bare area on which new
drops form. Nonnally, oily or greasy -surfaces tend to induce drop-wise
condensation. The coemcients for drop-wise ,condensation. may be
double or more than double that of film type under identical conditions.
It is difficult to estimate the coefficients of heat transfer for 'drop-wise
condensation.
In general, the film coefficient bet,veen condensing vapour and metal
wall .increases ,vith increasing" temperature of 'vapour. Film coefficients
decrease with increasing temperature drop. Whc;n steam is emplo) cd as 1
a source of heat,' it is necessary to remove non-condensable gases. Other­
' .
wise, they reduce the film coefficients, because of their accumulation.
Col� liquid-boiling of liquids : .W�en1 heat is s�pplied to a liquid, it
boils a�d the vapour ·pressure increases. This ·procesi co1�tinues u11til the
vapour pressure is equal to the a_tmospheric pressure. At this stage·, the
·, . temperature of the liquid remains constant, which is known as boiling
point. Qenerally, heat is supplied to a liq�id by passi11g
· through
· a ·h�ater
·
steam.
Consider a horizontal tube, which is imm�'rseJ iri a pool or' pure
liqui:d. · Stearn is passed through the tube'. The he�t transfc'r depends on
the differences in temperatures on ·each side of· the tube wall. The
relationship .bet\b'een temperature differences a�d heat transfer coeffi­
cients in liquids (boiling outsid� the hotizonta:I tube). is shown,in Figure
�-6. !'J.t. may he. defined as:·
Figure 5-6. EiTcct of temperature difference on the bcha�<
iour of a liquid boiling oulslde the horizontal tube. . , ·
The following conclusions inay, be drawn. from figµre 5-6.
(I) If L1t is very small, the rate of heat transfer (q/A) is not much.
Hence. liquid doesn't boil.
(2) l f L1t is increased, the rate of heat transfer (q!A) . w'HI be in-
. creased, because heat transfer coefficient increases rapidly. The
mechanism is as follows. The heated liquid at the: wall fonns
bubbles of vapour ancl gets de,tach�d · from the· surface.· These
vapour bubbles rise through .the liq'uid. , This type of boiling is
called nucleate boiling. The col.d fluid nO\V wets the tub�wall.
Thus bubbles produce a series of currents, \\.11ich have a stirring
effect. . :; . J ,
(3) If L1t is increased rurther, the surface temperature increases°con­
tinuously up to a poi�t,- 'where the heat' transfer coefficient
reaches a maximum. this tempera�urc is -.known as critical L1t.
At this .stage, the \J@bles begin to coalesce into a continuous
lihn-'\?f vapour, which'insulates the tube.
(4) Beyond crit,ical Lit, further incre�;e in ,Llt leads tq lowering 'of
heat transfer coefficients rapidly. The continuous film of vapour
i.nsulates the tube. $hereby the, effective L1t fails. to increase.
Thus rate of heat transfer is decreased.
. . . \

!'J.t = tub.e wall tcmperature-satorated .temperature of Fur some organic liquids. the heat transfer coefficient may decrease
liquid (= vapour pressure in spaces) rather slowly after critical· L1t. Therefore, maximum heat flux may occur
• :1 .. '
at higher L1t than the maximum t
coeffic. ent.
 124 l'l l.f\ltMi\CUlTIC/\1. EN(i!1'EERING .
J
'
Ch-5 FLU\\' OF l!lc/\ T 125
The factors influencing heat transfer in boiling of liquids arc: j' ' • 1 ' ' ' ' '• .; '

:n.ie tcmpGraiurc-drop a� tl1i. left-end is· p111ch ·greater t,hao at·the ·rfg,nt­
I•

- roughness of the tube

cnd. h means that heat transfer is faster at lcft-si9e,'"11;��;that" of the
type of roughness .
tendency of liquid to. wet. the tube rig.l�t-side. These chnngcs. ·-;1s occurring in a smalif scrtion. of the pipe:'··
diffe.rcnce in densities between bubble and liquid .· can be c:onsidered for the ,vhole 1$!ngth of the pipe.· ... , •. qii,''..> f,
1.'!
I .
� ,

Tb:re is no. equation. ,vhich can establish a rcl_ationship bct·.vcen · iVlatlwmatically, heat trnnsfrr · in parallel flo,v of liquids can he
cocfiicicnt and 00thcr factors. This is due to the diverse nature of written as:·
t i(>t'
apparatus (shape and size) and varying speeds of circulation. tlf.J "' l./.A. Lit (31)
Modes of Feed-Heat Transfer Equati,)n t31) is �;;sed on two assumpt,ions. (a)· The overall coefli­
lfrat't1'ansfor by convection is involved between t\','O liquids. The cicnt ( V) is considered constant:.throughout tbe. cqui pmcnt. (b) The
differences in the· modes of feeding large(); determine t�e cfiidency of a spL·cific heat 0f end, fluid is considered cons\ant.. . Integrating equation
· · :
hcHt proc_ess. (31) gi\'1:S:
.. ',;..
·.
Parallel heat now-Variation "in· temperature :· Heat transfer across , · .1t i -- ,_11,
a metal· surface from a hot fluid lo .a cold fluid depends on the tempera­ q = UaL--··--.::. (32)
ture gradient (Jr). Generally, it is assumed to be const..;nt for all parts of LJr I
/n - -
heating surfa<.:c. .1:2
When the hot fluid and the cold fluid enter the apparatlls from the when! L '"'· length of pipe. m
same· e_11d, the flow is parallel to each other. This arrangement is known a '." area of the pipe. m2
as parallel flow..
. f the hot fluid inside Comparing cqtiaJ.ion .(32) ,vith
·· th� general ,equation of heat tnnsfer
Consider a heat interchanger. The temperature o
(eq�atipn 25) gives;
a pipe d�creases. from Ti - to T_, by trnnsli:rring heat to a cold 11uid
outside the pipe. As· a result. the cold fluid temperature is im:r�·ascd '111 - £Jtz
from t1,to r1. This condition is repn;sentcd in Figurc·.s-7. ,1/111 = ---- (33 )
. At/'·· ..
I,
. ln-
tl tz
. . I
,,.-, J ••.•
··,

Thus !o-gar'ithrni� mean temperature difference' (-4tm) is used. The

tofal heating'' surfa\:e (A) is 'equal to' pLJ.He�t tra�sfer equation in
parallel flow heat exchanger is: .... , · ·
_q = VA'1tm (34)
1
lI:
The logarithmic me�n temperature difference · is us�d to account
varying t_emperature drop in parallel flow. \ If the.temp�rature. drop is.
nearly equal (Lit 1 = Litz), then arithmetic average temperatu�e, (,1/;,;) can
be, t,ised. which is a general expression for heat transfer.
J .,
f •

·)n ,parallel . heat. now, ·�h� heating obtained per unit surface area is.
Distance .mucJ1 icss effecti'vc. at u��.Jluid exit point compared to H at)he point of
1 •· _,. · '.
Fi�ure 5-7. Tcrnpcra!urc diffcn:ncc in parnllcl-curr�nl heat lllo\\. entrance of the. lapparatus: ,, . • .. • � :di . .',, ··
.
;;,.Ti.::
I • ��·
/'

Counter-current heat now-temperature gradient' : · . Whe' n the

. ..
• . �' • • - .• I.,, •.''

hot fluid is passed through one· end of the apparatus while cold fbid
 l'l lARMAC'lUTICAI. EN(ilNH.RING
126 127
Ch-5 Fl.OW OF HEAT
each other in the
is passed thro'l,\gh the other end, fluids pass ·and by pass
d-c111:re11t or
.' ,• :• 1 . ,t 1 \ I ff
l

n as c<i1111t Initially steam cools doYm t? the co�densing temperature as indi. c�ted by
opposite' dir.cctions. This arrangement is know
AB in .. Figure 5-9. Then condensation o�curs at c�nstant: l�mP,�·ratu,r�
c:ollliter-jlo II'. '. . .
. cr-cur r7nt Oo�v ·arc shown in. (section BC) ., �nd may further be··allowed· to cool (section · CD). Here·
The temperature gradients for the count
large errors '.would b'e. introduced; if AF.and ·;DE artt��k'cn.'.for Lti�·. and
Figure 5-8.,
/Jt2, respectively.· Separate heat transfer calculations must ·be do11e for
.- ·
the three sectii0ns ,iJ1 Figure 5-9 and then· are addecj. . w;, ·.. ,,, .

''1 .,

A
,,,: .· ; :� : ' ..
.: (

' i p

E . . '., ..,·. 1·,,

Distance
� . 'I
0
heat now.
Figure 5-8. T.::111pcr,1turc Jil'kn;m;c in ,ountcr-cum:nt '

the temperature di·op Distanct:·,

I

. From · the figure 5-8. it can be concluded that .

't·, ;·::
ant. In other ,'\'ords. .,
j

alonn the h:noth of the app:.uatus is. nearly const rn

figure 5-9. Tcmp�r:itur.: diffm:ncc i� countc::r-c.urrc::ni l;cbt ,, .
same at hoth ends.
J.

amo�::t of he:t transfer p::r unit area is. substa ntially

flow in which steam is usi:d ;J� the hcatinu
... ,;i��!ium.
ant tliro�g hout the apN ratus . .
The heating 'surface is nearly cpnst
. .

e of the hot ·fl uid is

. c' In counter-current heat flow, the exit temperatur
, f1! ,.· I :·

the cold fluid. Hettce' a

RA.DIATION
considerably less than the exit temperature of
. ' ,\

, ntent of 1
tl. e hot tl uid c�n be extracted for Radiation is a process in which heat flows.. Heat is transferred
forge proportion of the h�at co
If L1t 1 = tJ./2, temperatur_ � through space by means of electromagnetic �vaves.
a given entrance temperature of the' cold tluid: •
q ',!·.; ··��·i·i·,·:,

(Lit) can be taken as arithmetic average:.

t . • ( ., .' . ·· , .� ' • •

Th,:rm�l Radiation
• •

· 11 .
Lit 1 + Jt2 Heat transfer by radiation is known as·thermai radiation.·· · ·,·
dlav '-= ·-- -- (3 5)
Radiation is effective across perfect· vacuum and also t,hrough la\'ers
2 .·
' . of �ir.,
. .. . , -,;, , .;, , ,!; (··, .. •
t heat flow can be
Th� hea; transfe1; equa!ion for countcr-c1urren
. All soUd,bodies radiate energy when their temperatures.are above the
. written as: absolute zero: A solid surface emits radiant• energv11cohtinuouslv and
(36) distributes over all wavelengths (i.e.. from zero to -i�finity), altho.ugh a
�,it; heat to a colder body. major po11i?n is concentrated witlfin a relatively narrow'range · of-wave�
C6�sider a case, where steam is _fransfer;in ··
cons tant. The te'.11peraturc ,lengths. ..,. .
,, . ·,:,,,:;:,; . , .,., .. ,,., ..,·
Let th�, :pressure difference in steam be
1 •: •J, �

r is 'shown m Figure 5-9.

• •

Heat transfer (thermal energy) is predominant as:tlie .teinp�rat�re of.

difference when steam is in a heat exchange
�he body increases. The a·mount and kin'� of thermat' energy' radiated
.
111creases ··rapidly with teniperature. Thermal radiatio'n u suallv occurs
simultaneously w\th heat transfer by convection and conductioh.
 Ch-5 FLOW OF ,HEAT 129
128 j l'J li\R\L\i ·1 l I llt\l. l:N(il'-ll'IUN< i

Various Forms of Emitters Further the 'term, 'black' is nothing to do wH1';.the colour: 9( the. body.
\fariOllS forms of emitters U5e(! for the si1pply or radiant energy arc Similarly it has nothing to do with.the_ amo,unt of energyAr.ieiat�s.. '·:
given _belo\v: In theory, a black body is· conside,red to be � enclosed·space\vith a
Radii11 io11 so11rce AJJ{J/ic;a�?_,_s, ____ small (negligible) opening, Thectempei;ature. in . the ,_eij�lo�.ed )pace
should be constant.and uniform, because the amount of;eriergy escaping'
IR lamp (IOOO�CJ high i1:tcnsi1y rndi.ition.
through a small opening is negligible. ln practice, a convenient bla�k
.1 ;pill

Ceramic rods· a1id panels · '.!to -t pm Pha1m;1n:utic,1-l- purpMes. body is made from a tube of carbon. Both the ends are plugged, with t" ' �"
·a
•
•' . {'f t

he::it�d hy g.:is or dcctricity thcrn1<1l:ibilc substances.

small hole at the centre of one end. When viewed through ihis small
( 500° to 300 C C).
hole, the inside en.closed .space (furnace) is co�sideied as:a biack body.,
AdYantagcs : The radiation source corresponding to wavelengths provided the. temperature is uniform. Similarly· all objects within the
from O.�· to 400 pm is used for the thermal 1-.1di.1tion. For most (ascs of furnace (enclosed space) can be considered as black'·bodies. iii:<·', .·.
'
indw,tri�I interest. the range is narrowed fron.1/L,8 to 2) 11111. lb,liant . A good absorber of heat is a good emitter too: Conversely, a poor
energy ,penctrat.:s a sho11 distance ( I to 2 pm) into 1:1ateri;ils. The absorber is·a poor emitter. . .i·.1«' , .
.
'
!.
heati1H:"cffect occurs belo,\ the surface. For example, a lilm or solution
can b;, dri('d hy radiant h('al. whereas surf'.) CC s'kin retards the dry in,; Rate of Radiation
process.in case of convection 1rn::.thods.. Normally, hot bodies emit radiation. Stefan-Boltzmann law gives the
Fundamental Concepts total amount of radiation emitt�.d -qy a bl��k body. .
· .·
Thermal radiation obeys s:ime la,.vs of light, narncly­
(a) it travels in a straight line
q -� ''.
bA,TI' f (37)
(b) it may be reflc;;tcd. from t· he. surface where q = energy radiated per second, W (or J/s) """'
Suppose ; cold substance is plac('d in th(.' sight of a hot body insid.: .A = area �f radiating surface, m2 :, ,) .
I .
an cndos,cd space. Thc,col·d body intercept the raqiation emincd by the T= absolute temper<}.ture of the radiating sufface, K
hot bod,·. · The fraction cf radiation·,; falling on the body ma) b<.: b= constant, W/m21K4
reflected·. ,vhich is' kno\\n as rcflc·cfinty. p. l�he fraction that is absorbed According to equation (37), the·· rate of he�;ing dep�nds upon the
is kn0\\'11 as ub.,·or111ii·i1y. a. The fraction that is transmitted is kno,,·n as · temperature and surface area of the emitter. At, the same time, it also
rransmi�:sil·ity, r. The sum of these fractions must be unity or:
depends upon th� absorption ca.;.�acity of the material to be heated.
a+p+r=J For a blact body, the value of b is 5.67xI0-8 W/m2-k.4. Actual .•
In practice, reflected a11d \ransmit't�
, d radiat i0ns usually fall 011. otl�cr bodies do not radiate ,as much_ as the ,black body. Therefore; equation
absorptive bodies. The absorbed radiation is. transformed into heat. This (37) is modified for the actual bodies
fraction is not available fo.r the emission of radiation.
q ��'Ar<,' (38)
Black Bod\· where & is.equal to the emissivity·oft_he ac�al body..1,Emi�sivity may- be
All solid bodies radiate en_crgy at a temperature above _the absolute expressed at the same tempe_rature as:
zero, bq,vcver, not at the same rak. For the purpose of he'at transfer, a · .• · '"
ti '"i:. -�/�:\·:,/;,.·· ',
theoretic Substance is proposed and, desjgnated as black body. energy emitted by actuaJ:pody,:-r � ; · . . .· -
J
, • •• , ; ,I /'

Emis,$i1iity, c = . · · ·· · .. · · '.' ··:' 1l, (39)

'•I

iB/aak body is defined as a body that radiates maximum possible . energy .emitt�d byi black.body •
·.
'amount ,of energy at a given temper;:iture.
As per equatio.n (39), emissivity -is �-�e,for a b;lack �/' For ,actual
i; No physical. substance is a perfect black body. The black 111at11:
'bodies, & is less than 'one, because a fraction bf the radiation'is·..absorbed,
surfaq! approaches ,a black body, when visible light (rays) alont?, is
which appears as:-�eat. '.The ·.fraction· of energy abso�ed i� denbttd· by
· considered. Li!!ht coloured substances deviate widely from it. · Black
absorptivity; a (other fracti()ns are .either reflected or transmitted).
surfaces are better emiuers of heat r11di�tion than polished. surfaces.
I'
 Ch-5 Fl.()'.\'s_OF IIEAT 13 I
130 .1 Pl IARMACEUTIC AL ENGINEERINCi
t:q11:11inn (40) a�sum1..·s that all the heat r.lliiated b) a �o,)kr bod:· also '
A good absorber of heat is also a good emitter at·� given tempera­ ralb on t!?,' hll,!tcr body. ' ·,.
ture. If 'emissivity is equal to absorptivity. (c = a), then a substance is .� . ··r ··:,·;"' ,·�··..-�,..:P
.

con�idered as a �lack body. Since emissivi-ty of a black body is I. the EQlllPMENT "·.. , · ·... · · --'
absorptivity must be one. Therefore. the . black bodv• absorbs all the
', , )� ' •• • . ,I ·1 •

HE-\ T EXCHANGERS Al'iD HEAT INTElfCIIA�GERS · .. , ,·;.·f' '.

. �

radiati�n falling on it. . . . . ':,- ,. . . . . .· .. . ·, ., . • '' \ . .. . ,'!

Mo:-.t of the 1.:h�n�,-�al and pharmac��tical indust.rics ·�1.nplo) .ax1riety 1 r
G�cy Body of heat tr.insti:r equipment. ·1 h1: H1atcrials to be •h1..·at.:d niay h�. liquids .or ..
Absorption of energy by a substance depends on . its properties. gases and oc�.bion.ill) ::;�lids,\ \\hich .is a s�paf�lc c,a:./'t��·. it:..d,1} .Jne .; , .
. heating media may _be a hot ·lluiJ or condcn:.t.!J steam. S(,me of.the.
Faiily high aq1ount of energy will be absorbed by dark coloured,' opaque
and rough surface bodies. Least energy is absorbed by light coloured. pniceSSCS. which inYOl\'C the heat ·transfer encountered in ph;il'lll;lC)' are:
transpar�nt and smooth surfaced substances. .
. .
.
.. .. '
Prcparat10n of stan:h paste (steam Jacketed kettks) .lor.granu-
':.
� . . .. :.

At .i .given temperature. the value of a varies somewhat with the · 1ation , · · ··

·· ·,
wavelength of the radiation falling 011 it. This complicates the solving of Cry stallization·
problems in practice. Therefore .. the concept of gre) body has bl.'l.'n Evaporation
introduced. Distillation . ....:' : . ...:,_�-. ,·'.:.: ; . ' . '' I
·.

Cold body (�lack) .

In inµustrial processes, heat energy is transferred biva'.do\'1s methods.·
surface area, A
Temperature, T 2 The principles. construction and working of ·equipnic:nt iisc:d for the· '
' · '· ·
transfer of heat energy are as follows:
Heat exchangers : Heat exchu11gers are the devic.es usc:i.l for transfer­
ring heat from one fluid (hot gas or' steam) to another flliid (i'iquid)'
.thr9ugh a metal wall.
'·
Heat interchangers Hc!al interchanger� are· the devices'. used for
transferring heat from one liquid to an.o�her or ·fr.om
· one. gas to another
gas through a metal wall.
The classification given above is vague ind m,any times used inter­
.at transfer
changeably. Therefore, it is appropri:1te to ·�all the�' as he
. .
· · · r· · · '
equipment.
t ; ,t

Hot black body

Temperature. T 1 .
Some of them are discussed in' the followi'ng sections.
'
Heaters or Heat Exchangers:· j
·, ·"'
r.- .... ,Fi�ure 5-10. lk.it lrJnsfrr 1hro11gh raJia1i,•n.
"-.;.

Heat exchangers are the devices, used for transferring heat .from one
A �re:_,, ho,fr is dc!tineJ as that body \\hose absorptivity is con,t;tnt fluid (hot gas or steam) to ano_thcr fluid (liquid) through <J. metal wall.
. . I � . . ' ') I . , ' ., ,

al all.'> ;I\ ,·k11gths ot" �adiation:�il 3 gT;.�n-tcmpcratur<!.

Some heat tra.nsfer (or heaters) equipmerlt'are: .. ,: ,; .,,:.,,,, ",.
' ... •
-:

Con;iJcr a small co'ld body with a &urfacc area of .·I _and tc111re1atu1l'
·:1· . •

. (I) tub�].at. h�ater (shch�lna-tube· 'heater) ·, . '... , .

of T, '.i;:�wmpktely 1 surrounded bv a hot black body at temper.itu1e r, , ' • . , ,., . • ,i ' I
•Ii I 1' . � �';)·I
(2) mult1pass heater
�
. ·,
\

. ti-1gure ,:,_, u J. I he amol1,nt ot heat .transterred. in such a process is . ,

ex!)resJe,d by the Stefan law, which may' be written as: (3) two .pass tloating · head heater ,,·, .... .
•'
I
• "' i '

' .. )

.,1 ;· q = bA(T/ -- T/) (40) , .. �. .i r , ,. ,

'• , ./ ,, ; I ,
132 · /
l'I IARMACl:UTICAI. EN<i(:,..:Ernl!'\G
Ch-5 FLOW OF HEAT 133

· In he.it exchangers, the film coefficients on the steam side arc usually
much larger than the film coefficients on the cold liquid side. Therefore,
the overa!J heat transfer coefficients will be nearer t.o the cold liquid side
(becaus�' it· i5: smaller of the two coefficients). Hence, heat transfer
becom'es less: The efficiency can be improved by passing the liquid at a
high velocity. As a result, the thickness and resistance of the liquilfilm
decrease.. Normally, the space outside' the tubes is large, but steam
velocity is low. Still heat exchangers arc useful, because of the high
valUl!S Of the steam film coefficients.
Tubular .heater (Shell-and-tube heater) : Shell-and-tube heater is
the sirr1plest form ofa tubular heater. It is a single-pass tubular heater.
CoN�trnction : The construction �fa simple tubular heater is shown
in Figure 5-11. Tubular heater csrnsists of a bundle of parailcl tubes,
0
Working : Steam or other vapc>Ur is introdu_ced through a connection
F into the space surrounding the'tubes. The st�.am flow� down the tubes.
In this process, the tubes get heated. Tbe.concfensed vapour is draincd'at
G. Non-condensable gases, if any, escape_ through the vent K provi.d,ed
at the top of the casing.
The fluid t� be heated is pumped ,through the i::onnection H rnto
distributing chamber D2. Th'e fluid flows through the tubes. Tpe stear.1
and fluid arc physically separated, bufare in thennal'contact through the
-thin tube walls. The fluid in the tµbes get h.eated due to heat transfer by
conduction· through the met.i),,y;all, followed by stagnant layer aud
finally by conv:e.dion. The totar heat transfer is effected by single pass
0
of fluict'. Thus, the heated fluid reaches th?. distributing chamber 01 and ·
leaves through the \!Xif point, I

In the sheet-and-tube heater., the cross sectional area of the tubes is

which arc relatively thin walled. The ends ofthese tubes arc ex randed
larger. Hence, the velocity of the fluid inside the tubes is low.
into. :.wo tube sheets, 81 and 82. The bundle oftubes is enclosed in a
cylindrical shell or casing, C, to which the tube-sheets are fitted. Many Advantage : In single-pass tubular heater, large heating surface can
heaters h:.1\'e a cast iron shell. be packed into a small volume.
cOi;tri. butior. Tube Steam Disadvantages : (I) The velocity of fluid flowing in these tubes is

I(\ n
cra�.ber, 02 sheet inlet Outlet hot <e'.
·;;
low, because of large cross-sectional area or ·larger surface.
Vent, K (r

�� j1·
fluid
+F
j '
(2) Tht.: expansion of the tubes and shell takes. place due to differ-
�
ences in temperatures. This may lead to the loosening of the
r:o/Lh> s;,, ""'
.81 s .,
1� tube sheets or buckle·tbe tubes.
� Multipas·s heater : Jn a multi-pass heater, the velocity of fluid can
Side
cover be increased. As a result, !1eat transfer coefficient also increases. As the
r+1
t"' name indicates, the liquid to be heated is passed· through the tubes
.. Distribution several times be ore leaving the equipment. This facilitates the heat
f
. ;,, �

'
E2
t
ii
chamber, D1 transfer. Therefore, multipass tubular heaters are superior to_ the single­
c
I

l
�
t I
� �G pass shell-and-tube heaters.
Inlet cold Condensate Construction : The construction of a multipass heater is· same as
Casing outlet
fluid Tubes· tubular heater mentioned above, ho,vever, with some mod.ifications (Fig­
ure 5-t 2).
· Figure 5-11. Cpnstrnction of singk-p,;ss tubular heater.
Tubular multipass heater consists of a bundle of parallel tubes. The
Tw;/·�i��ribution cha�be;s'; D1 and 02 arc provid�d a� each end of ends of these tubes are expanded into two tube sheets. The .tubes bundle ' •
the c::i?ii)g C. Fluid inle.t is proviq1=d .to the distributiory chamber D2. is wrapped in. a cylindrical casing. Two distribution chambers are
The h�atccl nuid outlet is 'provided to the distribution chamber D1• Two provided at each end of the casing. Since the heater is multipass, the
covers: E1 and E2 are provided to c;lose the distribution chan:ibers from same liquid has to flow through several tubes back and forth. · In Order to
the sides. · Steam or· other vapour is introduced by a connection, f. facilitate this process, distribution chambers are partitioned by. means of
Provisions an� made for the escape of non-condensablc vapour K und baffles and their arrangements are different in the two chambers (Figure
condensed vapour to drain at G.
r
 , .'
Ch-5 FLOW OF IIE('\T 135
134 ,' Pll.\R\l:\CFl:nc.\l r '\(,::,.;EERING
. '
. :
; �{. Q·�:i Ii.:; ' . . enter only a fraction of the tub t;s by means of baffles placed in the
. 5�1.:!). The entrance and exit points of the fluid an: arranged in the same
. .disti ibutior\ chamber (right side). distribution ·chamber.
.
The liquid enters compartment A and flows to the left into·compart-'
Ol1tlet
1i1cnt B. back to the right to compartment, and so on in the same
sequence of alphabetical order. During this process, fluid in the tubes
get heated, due to heat ·transfer by conduction through the metal wall,
H
followed by a stagnant layer and finally by convectio,n. The net result 1s
enhanced rate of heat transfer. Thus, the fluid passes back 'and forth
'through ihe several tubes and then leaves the equipment at I.
Ir the fluid is to be introduced·at high veloci'ties, pumpl�g should be
effective, which increases the cost of the power, though the cost of
heater is low. Too low a vel?c'ity saves power for pumping, but needs a
(al When viewed from the side
\-cry large heater. Therefore, a balanced approach should be worked out
· Outlet hot fluid based on economy.-
Ad\'Ontages : M ultipass construction decreases the cross section. of
the fluid rath, thereby increases the fluid velocity. Thus, multipass
tuhubr heaters are sLipe.-ior to the single-pass shell-and-tube heaters.
Disucl\'(/11ru:,!.<-'S : (I) The fabrication of a multipass heater is more
complicated.· ('.?.)' The pressure-drop through the apparatus is increased,
because of enhanced velocity of fluid flow. (3) More number of e:--;it and
cntrance points increase th� friction losses. This increases the cost of
pumping of fluid.
Floating-head. h\'o-pass heater : In floating-head two-pass heater,
tfic �nds of the tubes arc structurally independent of the shell.
Inlet cold Construct ion : The construction of a two-pass floating head heater is
fluid
. shown in Figure 5-13. !Js construction is the same as tubular heater with
Left-side d1:a.tribut:on chambP.r R1ght-s1de distribution chamber some modifications.
(partitions· F and D are below the page) tP:irtitio.i E is below the page)
Two-pass floating head heater consists of a bundle of parallel tubes.
(b) When viewed fro!TI the front These are enclosed in a shell (casi�g). The.right-side of the ·distributi�n
· lll'l' ::;:12. Corhtrur.:tion t•fa multip;i,:, hl·ata. In thi� figtm·. th.:
j:·i� chamber is pa11itioned and fluid inlet a.nd qutlet are. connected to the
.
motiitirati,,11, ,,r di\trihution chamb.:r� .md p;irtiti11ns ar.: !-lwwn. same chamber .. The partition is such that both have ·equal nuJnber of'
tubes. On left-side. the distribution chamber is not connected to the
1ro/Jci11g : 'Skam is intrn:iui::e� thr.ough the 'co11nc1:tion into the �pace
casing.. 1t is structurally independent. which is knowh}ds floa/li1g head:,
surr;iunding thJ tubes. As the 'steam llows down. the tuhes get heated.
The other end of the tubes is embedded into t.he floating head. Steam of
The condensed vapour is drained. · "N',,1i-ct111dcnsablc gases. if any.
other vapour is introduced through i'nlet provided to the .shel,L Provi-1
1,,

esc;pc through . the , cnt provided at the top of the casing.

. .. . ' . ' sions arc made for the. escape of non-condens.ed vapour and ' an exit for
The tluid to be heated is pumped at high yelocities into the rigl�t\, the condensate.
·· distribution chamber through the compa11ment. A. High velocity fadli­ . ,,
tatcs the effective heat transfer. In this construction. fluid is directed to
.,
136 /
l'I IARMACEUTICAL ENGINEERING Ch-5 n.ow 01' HEAT 137
. � . . .
Working : Steam 'is introduced· through the inlet (Figure 5-13). As In heat int�rchangers, the heating medium is a hot liquid. !he. liquid
the steam flows down the tubes, they get he.ated. The condensed vapour to be heated is the cold liquid. In this case, the film 'coefficierits both
escape through the bottom of the shell. Non-condensable gases. if any. outside and inside the tubes are nearly of same magnitude. The value of
escape through the vent at the top of the shell. the overall heat transfer coefficient, U, will be near that of the smaller of
the two film coefficients. Hence, heat transfer is not efficient.-
Floatin;v Steam
head, inlet Vent · Outlet The Dim coefficients can be enhanced by increasing the velocity of
+ t hot fluid flow. from the point of construction, it is difficult to incre�se the
velocity of the hot fluid outside the tubes. However, surface area of
contact can be increased, by introducing baffles in the.construction. The
:.,.11
increased surface· area of contact enhances the coefficient. Thus the rate
,.,,,, of hcnt transfer is enhanced. These principles arc illustrated using
,·

..
clifferent heat interchangers.
� Partition
� Baffles : Baffles consist of circular discs of sheet metal, with one side
cut away. These arc perforated ·to receive tubes. To minitnize leakage,

Tubes·
j. Inlet
the clearance between the baffles, shell and tubes should be small. The
baff1es arc supported by one or more gui'de rods, which' are· fastened
Casing
Condensate cold fluid between the tube sheets by set-screws.
outlet
Working : Baffles arc placed outsid.e ihc tubes. These increase the
Figure 5-13� Construction of a two-pass floating head hcata. vclocitv., of liquid outside
. the tubes.
. B'affles. make the liquid flow more
�...,
ctThe fluid to ·be heated is intr�duced·into the distribution char.1ber on or less right angles to the tubes. which creates more turbulence. This
right-side of, the -heater. The fluid flows through few 'tubes prc�ertJ in helps in reducing . the rcsist.ancc to heat transfer putside the tubes. :..
that part of the partition. The fluid _reaches the floating head and Therefore. baffles cbnstitute an important part in the '"'heat· transfer. ' · ' • f

changes direction. Now it passes back to th� next part of the partition
chamber on right-side. · Therefore, the fluid flows twice through the
tubes, i.e., two pass. During this process. fluid in the tubes get heated.
due to heat transfer by conduction through the metal wall, followed by a
stagnant layer and finally by convection. Then the fluid leaves the
outlet ·provided in the shell.
Adv."antages ! In a shell-and-tube heat exchanger, tubes and shell may
get ex-panded due to differences in temperature. Similarly contractions '
are also: possible when heater is switched off.. It leads to loosening of
. tube' sheets or buckles the' tubes. .Theref ore, constructing
. � the tubes 'I
independent of the sheH can p.revent these effects. Such an arrangement
is poat!ng .head.
Heat Intcrchangcrs
Heat intcrdzangers are the devices used for transferring bent from
one liquid to another or from one gas to another gas through a metal
wall.
, The construction of a liquid-to-fiq.trid heat interchanger illustrates the
principle of.introducing the baffles into the �quipment.
Liquid-to-liquid intcrch.fo,;;cr : The basic construction and work­
ing of any hcat"l'ransfer equipment more or less remai"ns 'the same. Only,,
a few modi!ications arc included.
Constructio11 : The construction of a liquid-to�liquid heat ,interch?nger
is shown._in figure 5-14. Nornfally, tube.sheets, spacer rods a,nd baffles
are· assembled first. and then tubes are installed. The 1i10st i,nportant
parts in the con;;truction of the heat interchanger are the baffles..
Appropriate size .of tube sheets is chosen for the fabr.ication. One or
more guide rods are fixed to the tube sheets by means of set-screws.
BaflJes consist of circular discs of a metal sheet, with oqe si�e cut away.
13artks arc placed. at appropriate places using gLcide rods. The baffles
·arc ar;.ar.ged with appropriate spacing using short sections.. of. the same
tubing as shown in figure . 5-14. · Baffles have pcrfo.ratioi1s tl1rough
which t·ubes. arc insertcd. The.ends, of tubes' are expandcd)rito ·the tube
sheets. ·rhe above assemblY, is enclosed in a shell.
 l :18 ·PHARMACEUTICAL ENGINEERING 139
Ch-5 Fi.dW OF IIEAT
. .The $hell has a provision for introducing the heating medium, hot . " ·d-to-Jiquid interchan· ger, heat trans fer· is· rap
id
fluid .. The _outlet 'for the flui.d is at right-sid� top. Advantages . l n a 1·tqm
· as the liquid
' On each side of the tubes,. two di s tribution chambers are provided. s.
Left:side chamber contains an inlet for fluid to be heated. The outlet for ( 1) passes at ·high velocity outs!de the tu�e
.the �b�s.
the hot fluid (that is heated) is provided at the centre of the right-side , or less at right angles to
(2) .: flows more
" . .
distribution :cha�ber. Do�blc-pipc, heat intcrc,hangcr :· If1 ; a
ri qu1. d- to-riq uid heat.· .
�me,� throu�h ,th� tub �s'
Outlet hot ·,nterchanger the fluid to be .heated is passed only l
Inlet cold Inlet hot trans ti er in t its
liquid'
liquid Baffles liquid befo- r,·-·e it gets . arged, 1.e. s.t. ng 1 e pas�. The
.' disch ,:',, heat
.. bl d QUb\e 'p ipe
+ i i . case i� .not efficient. When fyw, tubes per
hea� interchanger is employed.
p ass is d}s_ir� ' e,. ,

Inlet hot
..
·i::
�
liquid
,-...
'e·

Pipe for
i, ..
\� ti(;

Outlet hot liquid

;

heated
liquid
/ ........ Outlet hot
.-- liquid

Guide
rods
Spacer
tubes
Drain •t;
-4--
�

�r::=:._-__-- -
l!.!,I
Figure 5-14. Co.nstruction of liquid-to-liquid heat interchanger .
Working : The hot fluid (heating medium) is pumped from the left­
side top of the shell. The fluid flows outside the tubes and moves down . Inlet cold
"7,...=�===-=--=--=--=-:f
directly to the bottom. Then, it changes the direction and rises again. • liquid· 1 .::.·Jr-- tt!p
.
:..

This pro�ess is continued till it leaves the heater. Baffles increase the Pipes
velocity of the liquid outside the tubes. Baffles also allow the fluid to \I

Outlet hot
' I

flow more. or less right angles to the tube, which creates more turbu- · liquid
Jenee. These help in reducing the resistam.e to heat transfer outside the
tubes. Ba'(fles lengthen the' path and decrease the cross. sectio'n of path , .. t;u�'tion of double-pipe heat interchanger.
F.1gure- 5- .I· 5..'Cons
of the. cold' fluid. The path of travel is as shown in Figure 5-14. The e hc�t i�tcrchan?fr is
baffles get heated and provide greater surface area for heat transfer. CunstrucliDn : Tl�·� constru�tion of a double-pip
. r· r1,;, 5 - 1 •.. <; \11 this . two pipes are used: one is inserted in the
shown tn ·1gu
�ng of_cold rtqu1'd to
Simultaneously, during the flow, the tubes also get heated. As a result, .
the film coefficient inside the tube also increases. other. The inside pipe (or tube) is used.for the pump
circ1:1lat1on of �he hot
be heated. The outer pipe acts as ,a jacket for the
' The iiquid .to be heated is pumped through the inlet provided on left­ .
liquid. All jacketed sections are inter-connected . .
. side distribution chamber. The liquid passes through the tubes and gets T�e lengt h of t_hc p i pe
Normally, the numb er qf pipe sectio ns ,is few.
heated. Ttie flow of liquid is single-pass. The heated liquid is collected constructions are
from the right�hand side� distribution cha'm?er. is :ilso less. Glass tube. standard iron pipe and grapht:e
ret urn
1. . • ,I • · • •
a vailable. Standard metal pipes are assembled with s.tandard .
. ·s are connecte· d · m para IIe I and
·bends. A proper ,.number of such pipe .
 140 PHARMACEUTICAL ENGIN�ERING 141
Ch-5 FLO\V OF IIEAT .
stacked, vertically. The pipes may h;avc longit.udin�l fins on its outer heat transfer in a heat exchanger. In double-pipe heat interchan�er, fins
surface. arc employed.

I: : : : : : : :+1 : : :: :: ::I"'
Working The hot liquid ,(heating medium) is pumped i.nto the ·
•Air F'
jacketed section. The hot flyid is circulated through the annular sp11ces
between them and carried from one section to. the next section. Filially
it leaves 'the jacket. In this process the pipes, get heated, while the hot Steam--..
fluid looses'its temperature.
f'"r
I
' •
· •
• .
\
. The liquid to be heated is pumped through the inlet provided at right
side. The liquid gets heated up' and flows' tht6ugh the bent tubes into the (a) Rectangular fins ' .·,,;

next section of the pipe. The liquid further g�ts'heated. The same liquid

____:_.....*
continues to flow and finally ·· · leaves
· the interchanger through the exit
point on the right side. f;o, fob,""""'"'"
Uses : Double pipe heat interchanger is yseful when not more than
0.9 to 1.4 metre square of surface is required. (b) Longitudinal fins
Finned tubes : The, general heat )ransfe( �ate (q) equation in a heat

IT v\
exchanger is:
""' /"\.
where U = overall heat transfer coefficient, W /m 2 .K
q""' UAL11
v· Q4.J.·t\ v�
Tube \\

A= area'o.f.the heating surface, m2 '• (c) 'Spiral fins

. .,
�
Figure 5-16'. Variations in the arrangeinents
•).,.
Lit = difference in:tefnperature on both-sides of the tube, K
' . .. ,, .� '(
of Cins on tubes in a heat interchanger.
Consider·the case of a heat ex.changer in which air is present outside
the tubes. and steam i� inside the 'tubes. Air gets heated due to heat Heat insulation : The distribution of steam throug� the pipe can be
transfe: -through the t\Jb� wall._ The hea,t transfer coefficient on the steam reduced using heat insulators. The pipes should .be. lagged, i.e., covered
side surface is very high, while it is extremeIi lovv on air-side. As a with � layer· of porous, poor conducting material s·uch as· kieselguhr.,
result, the overall coefficient, U, approximates that of the lower side, i.e., asbestos and gbss wool.
air-side. Since, U is decreased, the only way to increase q is to increase 1\ltcmatively, several layers of aluminium foil can be qpplied for
�·' the surface area term, A, on the air-side. cf(ect.ive insulation. The surface of the foil prevents the ,radiation lo�ses
' . .
As metals generally have high thermal conductivity, the temperature and air trapped between the layers minimizes convection losses'.
of the · metal surface · approximates to that ot steam. : Surface area of
coota!?t is enhanced by fixing fins on outside of' the tubes, without
putt.ing',mo,re numb,�r. of tubes in the heater .' 11 Glossary of Symbols . ,
I
• ·:, �·
I ! '/ I: j
• ' :") • ,I , F j ' ' •

' •• ' ,\ = /\rca of the hc:iting surface, m-.

· . ,C<;mstructir.»1.,;:A variety of fins are used as shown in. Figure 5-16. /\� = Mean arc:i of a cylinder, m 2 .
Fins may. be placed on the inner ,val! as well as on the outside of th� b = Stefan Boltzmann's constant, W/m2 ·K4.
tubes. Rectangular discs of a metal.may be placed at right angles ,to the h 1 = Surface cocflicient on the hot side, W/n�2·K.
tubes {Figure 5-16a). Lon.gitudinal fins are also employed (Figure 5� h2 = Su'rfocc cocl'licicnt on th•.! cold side, W/m2 ·K.
"'.4
16b). Spiral fins i:nay be attached to the tubes (Figure. 5- I 6c). · km = Mean proportionality COllStant, Wim·K.
L = Thickness of the heating surface, n1.
c' Uses : Fins g'reatly reduce the size of the apparatus. They; .also N = Length of the hollow cylinder. m:
increase' the -surface· area of contact. This in turn enhances the� rate of. q = Rate of heat transfer; W (J/s).
-� I'\ ;
142 PHARMACEUTICAL ENGINEERING

r = R;.id:.1s of the thin cylinder for heat transfer, m. Ch-5 Fl.OW OE HEAT
rm =- 1.,,e,1i i1hmic mean radius, m. 143
l:. :\l�..:u,c tcnip:�rature; K. 18. Differentiate log mean radiu"s anJ arithmetic mean radius in conduction of
t 1 " :..:m:•.:1;.:11:n: at the hot surface, K. ,h11at. Whal ,ire its applications?
t:i ,.,. ·1 l·,,1;·...;r;.1tl:rC at the cold surface. K.
i 9. \\'h::it- is meant, by overall heat transfer co..:ifo:icnt? \Vh::it is its significance?
\1,,, \• :.:,, .. ..:ii�· a\'.:ragc tcmpcrutur.: Jitkrcncc. K.
20. Di ITcn:ntiatc hetwccn a heat interchanger and heat exchanger .
.�t · i ,'t'.lj'�·;·..nu:-i: Jii'li:rcnce. K.
l ·, 1 h ·:, .,i! h,·�11 transkr col!l'licieni rn1 hot side, Wim.:! ·K. Each question carries 5 marks
t: .. lh,·1.,lU1.:at tran\ti:,r cocfli�il:nt l'll ,·nlJ s.idc. W/m'·K.
I. Comp::in: anJ contrust heat tr:111smission following countcr-·currcnt and
a ·- Ah:-,•rpti, it�
paralleh:urrl·111 fi:ed techniques with relevant equations.
p "- H.dkdi,ity
t =- · 1 r; .111'1ni:;�ivity
7 lkri\'c .in cquation for heat tra,nsfer· by l':,mduction through co.mpound
c·, l'mi·.si,i:�- n::sistances in series.
3. Draw a nca, ,md labelleµ diagram of a shell-and-tube .heat exchanger and
exrfain. its wnstruction.
QUESTIOl'i BANK . .
-1. Dcscrihc linn..:J tube heat exchanger and its specific advantages.
Each qut'sJion carries 2 marks_
I. I),·�,,\,.. :n�·- °
1:, p..:-. ,,J ..:,llldcnsati_un f,ir �aturntcJ \ ap,llir fr..:..: frnm n, 1 11-
5: Describ.: th..: rnnJuction of heat through a circular pip�. Give suitable
-equations for ratc ur hcal transfer and explain h:rms.
.
"·,,ihh:n:--i:,;, . :=�1,..::,;.
6. Describe the conduction or hcat through compound. resistances in series.
... L>iff,·rc'm:.;::b·:l\\CCn a ·Black body' und '(ircy hody". uiw charactcristi..:�
,,r
I . ''f• , ,• I ' 1' • '

;1 1,1;,.-1. :,,, J�.

7. Dcri\ c an c.,ifrc:.siun for Ilic lugarilhmic mcan temperature diff<!r.!11e
c.
1 (ii\..: ,lu:·,:.-t,·ri:.tics llf Jrop!..\\jse 'and lilm tvncs condensation. 8. Describe liquid heat interchangers..· What arc its advantages?

�- · D�,,1H, is.: l,r tilm type cond�nsation gives. superior value of overall he:lt 9. Explain the wor�ing or a heat exchanger \\ilh a labell�d diagram.
, .
tronsfrr cocflicienl and wh)? r
5. List the characteristics of heat transfer by radiation.
E.ach question carries 10 marks -dl'>
6. What an: ·Grey bodies'? How do. they radiate heat?
I. \Vith•the help of a neat diagram, explain the concept of film and 0\'erall
7. Give th�· ti��y �quation for h'eat transfer by conduction through resistances
heat· transfer toefficicntS- in forced con,·cctionJ Deduce rclev;rnt :,
in scrb and explain the terms. mathematical equations.
1
.
8. \\;hat arc "o\'era!I heat transfer COe fficient' and 'individual film coefficient'? 2 . . Dc-rive an C\!Uation for heat tran·sm"ission through· a circular pipe from
.
9. Explai11 the tcm1s 'Black body' and 'Grey body'. Fourier's. law.
10. Dit1:;:r�i1tiatc between Jilm coefficient and overall heat transfer coefficient. 3. Describe 'the construction. 01w:.ition, ad, antagcs and . di�:!dYantagcs or a
J { State thi: rdatit,nship bctw�en individual film coefficients and o�era11 hea'.t_ multipass. h,!�lcr.
transfer codtkicnt. .. ...,
12. Define conductivity with a suitable example
t'3. State· ·and explain Stcfen Boltzmann's law of'heat radiation.
14. Sta.le and explain Fourier's law of heat transmission with equation.
15. Explairi ·nucleate boiling' and 'film boiling'.
16. Define radiation. Explain �tefan �oltzmann's law.
17. Writ'e the final equation for- heat transfer by conduction through resistances
in parallel and explain the terms.
 Ch-6 SIZE REDUCTION . 145

In the mechanical process, the substance is subject�d to mechanical

forces using grincling equipment (ball mill, roller mill, coiloid mill etc.).
6 In general, dry grinding or milling is used in the production of tablets
and capsules, while wet grinding is used in the preparation of suspe_n­
sions, emulsions and ointments. The method of milling is applied either
Size Reduction in the production of raw materials or as a� part of the production
.

· the manufacture of dosage forms. ,

.
.
cycle . ·in
.
Size reduction of substances offers several advantages. These are as
Mechanisms of Size Reduction
follows.
Modes o� Stress Ap plied in Size Reduction Content uniformity : Mixing of dif(er�nt ihgredicnts can be effec­
Classification of Size Reducti·on Equipment
Size Reduction-Equipment
tive, if the particle size is uniform and small.. Size reduction .ens!Jrcs t�s
Selection of a Mill objective .• Particles of optimum size are desirable for effective mixing.
Theories of Comminution
Energy for Comminution.
As the size of particles is .. small, the number of j>articles per unit
weight (d'ose) is large. The larger the number of particles, the better fs
·c'
the mixing. Thus, better content uni.folinity can be obtained for a given
Size redz_iction· is a process of reducing large solid unit masses (vege dose. This is particularly important in form,ulations containing potent·.
tr.blc
or chem:c
_ al substances) into small unit masses, co;rse particles or and lo� dose drug�..
fine ;; r1:;
particles.
Uniform flow': Smaller particle sizj! and controlled size distribution
�ormally, _pharmac�utical powd�rs are polyclisperse, i.e., consisting promote the flow of the.powder into dies dur(ng compression of tablets..
p�rt1cles of different sizes. Polyd1spersc powders create considerable
_ _
d1fficult1es The same principles are used in the production of capsules.
in the production of dosage forms. Part
icles of monosize
(equ�I siz�) may be ideal for pharmaceutical purposes. In practi
ce, Effective extra'.ction of drugs·: Smaller particles\ allow rapid pen­
�owder� \�1th narrow range of size distribution can obviate the problems etration of menstruum or solvent into the tissue or cells of vegetable and
in processing them further. Size reduction alone is
not sufficient to ·animal origin (live'r and pancreas). · As a result, extraction or leaching ·of
� bt�in mon o-siz�
_ or n ,rrow size range powder. Th;re fore, size reduc­ active constituent; becomes effective and complete in preparation of
�
t10� and size separation should be combined to· obtain powders galcnicals. The time required for exfraction can be shortened. For
. of
desired size. (The fundamental aspects on powder,· their characteristic example, pancreas is subjected to grinding' action for the extraction of
s
and methods of evaluation are given in the book, "Textbook of Physic insulin.
al
Pharmaceutics" by C.V.S. Subrahmanyam, Vallabh Prakashan, Delhi). Normally, fine powders are preferred for compound powders, while
Size reduction process is also termed as comminution or diminution' moderately, coarse powders are. used for the. preparation of tinctures.
. or pulverisation. Normally, size reduction may be achieved by two Coarse powder without fines is employed in percolation process.
methods, namely preci'pitation or mechanical process.
Effective drying : Drying of a granular mass can be· rapid and
In the precipitation method, the substance is dissolved iri an appro­ effective, if the size of granules is small aqd uniform .. Such techniques
.
pnate solvent. Subsequently, it is finely precipitated by the addition of are used in the production of tablets. Similar.ly drying of medici.nal plant
another solvent, which is miscible with the · first, but in the later the parts can be quick and fast after size reduction. ., ·
substance is insolu.ble; This method is suitable for the production of r:aw
materials and bulk drugs. Inorganic chemicals, such as calcium carbon­ Improved physical stability : In case of suspensions and emulsions,
ate, magnesium carbonate and· yellow mercuric oxide, are prepared bv the rate of sedimentation decreases to a large extent if p�rticle size is
precipitation 111ethod. small.
144

,·
146 PHARMACEUTICAL ENGINEERING Ch-6 SIZE REDUCTION 147.
Improved dissolution rate : Size reduction increases surface area, type of mills should be avoided, 'when drugs �f high purity'�
which facilitates intimate contact of solid particles and gastric o.r intesti­ reql!ired.
.
na?' juices. Thus, the rate of dissolution enhances. For example, size Th_e importance of size reduction is so profound thaJ it is used in the'
redu"ction of griseofulvin led to the development of oral dosage regimen production of all dosage forms' such as tablets, capsules, suspensions,
with a dose half that of the originally marketed product. In case of emulsions, injections and galenicals. The principles of size reductio�,
insuff1ations (preparations inhaled directly into the· lungs), the drug construction and working of equipment ..are discussed in this chapter.
should be usually smaller . than about 5 µm. Micronized powder of The equfpment, which are used ijJ:t; pharmaceutical industry, are ·given
aspirin is used in the preparation of tablets, microfined aspro (analgesic importance_.
and anti-inflammatory agent). ' .
Improved rate of absorption : The small�r the particle size, the MECHANISMS OF SIZE REDUCTION . .
faster is the absorption, because of enhanced dissolution. Chlorampheni­ . The mechanism of size reduction may vary �ith the nature of mate­
col has been shown to absorb faster when given with particle size of rial. Therefote, each _drug may require a sep.arate treatment. However,
50 µm compared to· particle size of 400 µm. Keeping in view of the th� general mechanism may be described as follows.
advantages, pharmacopoeia specifies particle size :!S. a quality control
Flay.'S in Crack Smaller particle and
tool. For ex;imple; griseofulvin (antifungal antibiotic) should have additiona-l surface
particle
surface area of not less than. 1300 to 1700 metre square per kilogram (as . ./.
per IP). If it is less, the absorption of the drug decreases. Sulphona- , Further
Impact
midt:s attain their antibacterial activity at powder sizes of about I �1m or impact
> >
belo IV. lnc'reased antiseptic action has been demonstrated when the
particle size of calomel has been reduced..
' .
The disadvantages of size reduction process are as follow�.
(I) Dri,g degradation: Drug decomposition is possible due to the Un milled Flaws develop Cleavage of particle
particle to cracks
heat produced,· during milling. Thermo-labile substancrs are the . .
to smaller size
. .
most affected. The incre�sed surface area also facilitates drug (a) Mechanism of size reduction when impact type of stres_s is applied.
decompo$ition owing to enhanced dissolution.
.
·. 1
' Smaller particles
Cooling support systems are provided to decrease the heat in
milling equipment. Drugs containing waxy materials become.
soft due to heat generated during milling. Therefore the feed is Attrition �-
chilled before milling. . . >
(2) 'Poor mixing : Normally, very small particles possess strong .
· · cohesive forces, hence, aggregation of particles is possible.
Aggregation inhibits the effective blending of different addi­ Unmilled Edges break
tives. An increase in surface area may promote the adsorption of particle
ai�," which may inhiliit wettability of the drug during production. • (b) Mechanism of size reduction when attrition type of stress is applied.
T.herefore, optimum· particle size is "desfrable to improve blend-
·. i\)g and to avoid poor mixjng. Figure 6-1. Mechanisms of size reduction.
(3) Contamination : During millii:ig and grinding. the grinding sur­ Particles, be it aniorphous or crystalline, will have flaws to a definite
faces· wsar off (examples are ceramic or iron equipment), the · degree. These constitute weak parts in the particles. Wh�n ,sufficient
particles of which are present as impurities in the powder. Such stresses such as impact, shear and compression are applied, the weak
148 PHARMACEUTICAL ENGINEER!Nf, Ch-6 SIZE REDUCTION

flaws develop into cracks, which eventually lead to cleavage (Figure 6- (3) Attrition mills, example is attrition mill.
1a). Thus, smaller paiticles arc obtained with additional surface area .. (4) Tumbling mills, example is ball mill.
. When stress in the form of attrition is applied, the particle surfaces C. Ultrafine grinder, example is fluid. energy mi IL
chip and produce small particles (Figure 6-1b). D. C�tting machine, example is cutter mill.
Some of them are discussed individually in the foliowing sections.
t �
MODES OF STRESS APPLIED .IN SIZ.E REDUCTION
The mechar:iisms have demonstrated that stresses of varied nature are
required to achieve size reduction. The common modes of size reduc­
· SIZE REDUCTiON-EQUIPMENT
..
The equipinc;1t described in .this chapt�r- 4re used. in small-scale
tion are explained as follows. plants. The basic principles qnd working remai. n· same. even in large­
1. Cutting : The material is cut by means of a sharp blade(s). scale operations.. Other v_ariants are also i i;icluded in brief.
! 'Example is cutter mi.II.
General Parts of Size Reduction Equipment
, 2. Compression : In this mode, the material is crush�d between
rollers by the application of pressure. Example is roller ·mill. The milling or grinding equipment· c�nsi�ts· of three basic compo-
nents. These are shown in Figure 6-2.
3. Impact :. This involves the op'eration of hammers or bars at high °
speeds. When a lump· of material strikes the rotating hammers, (I) A structure for feeding material to the '!lill. It is called hopper.
· the material splits apart. This action continues until particles of (2) The miliing chamber is the one in �hich actual si;e-reduction '.
requir�d size are obtained. Exa�ple 'is hammer mill. tali.cs place. It consists of a rotor and a stat.or.
Impact also occurs when moving particles strike against a sta­ (3) A discharge chute or. receiver in which the 'milled product is·
tionary surface: In the same way, particles moving at high collected.-
speeds· collide each other and produce smaller particles. Exam­ Feedstock
ple is fluid energy mill>
4. Attrition : This process involves breaking down of the material
by rubbing action between two surfaces, i.e., surface phenomena.
Example is fluid energy ·mill.
·c: Although the predominant mode with one examp'te of equipment is Mill chamber
discussed above, normally more than one of these modes ar� exhibjted to
some extent.
Different types of size reduc'tion equipment are available, since mate­
rials have their own distinctive properties. For example, a powder
· produced by ball mill differs from that produced by hammer mill, ev�n
though both powders may be screened to the same fineness. The
differences may be in· terms of� shape, roughness and their internal pore-
stru_cture �f a particle:
Figure 6-2. General parts of size. reduc­
'tion equipment. "I;hrc,c basic com.poncnts.
CLASS!FI_CATION OF SIZE REDUCTION EQUIPMENT . ""'......
A. Crushers, exa111plcs are edge runner mill, end runner mill. Other Accessories
· B. Grinders: (1) .Impact mill," example is ham'mer mill. (I) Sieves �r screens arc enclosed in the milling chambs:r to ciassify
the particles by size. . ·
(2) Rolling-compression, example is roller mill.
 I • PHARMACEUTICAL ENGINEERING
Ch-6 SIZE REDUCTION 151.,
150
to the Construction : The construction of a cutter mill is shown in Figure,_
(2) Cyclone separator or centrifugation equipment is fitted 6-3. Tl;e milling chamber consists of two types of knives, n�mely''
mills for separation of particles' by their sizes. rotatin g knives and stationar y knives. ' A horizontall y .mounte4 rotor disc .
(3) Dust 6ollectors are employed in order to collect the fine powder
' ' ·_. Jf .
consists of 2 to i'2 knives spaced uniforml . The casing ;:\!so_ has sever:a_l '.:
• ,,.,
y
and dust that may arise during milling process.
' .
stationary knives. The hopper is placed above it. The bottom of'casing ::
holds a screen that c0nfrols the size of th� material.· Discharge
.

· chute is
Sp�ci?3l Featur�s attached at the· bottom of the mill. "·-
( 1) Cooling devices are fitted to the chamber to reduce the heat
\Yorkin� :· The 'ro�or 1.is�, is aH9wed to :oi�te �t sp·e�ds from 2po t�;'.
. produced during milling. - · - 900 revolutions per minute. The feed matenal is loaded mto.the hopper,-­
(2) · A clos;d environment is ·desirabl� �or mi�li?g hygrnscopic sub­ which flows down by the force of gravity. Durfog 'the rotation df disc;':
stances:· For this purpose, dehum1d1fied air ts necessary. the material. comes very close rotating k�ives/·1
. . . between the stationary
-. ' . . and
' .' ,
(3) Closed system with inert �tmosphere (nitrogen or carbon diox� thereby the material is cut into small pieces. Smaller particles pass ·
ide) is desirable for milling of drugs, which_ are oxidisa?le or through· the screen. The knives lift the coarser particles up while
combustible. Similarly, material to be used m the production of ' rotating and promote further size reduction. , The· product is collected
parenterals should be mi-lied under sterile environment. ., "'
·i:[
into a receiver.
Though general parts of the equipment are identical, several modifi­ _ The particle size and. ;hape are determined 15y the rotor size, gap
cations have· been incorporated in ord,er to make the process easy
to between the rotating and stati�nary knivc:; ·ari. d· qpening_ of-- the sieve. ..,,-;-,
,..._- ,.· .-,... .
handle _and to provide desired discharge.
.

Uses : Cutter mills are used 'for the size; reduction (fi,ner than 80 to
. ·.· ;

I 00 mesh) of tough and fibrous materials. Medicinal plcfnts , plant parts

ROTA�Y CUTrER MILL •. • t
and animal tissue are normally converted into small parts. Soft materials
Pri.nciple : In the cutter mill, size reduction involves successive such as roots, peels and wood are cut befor-e extraction. It is also used in
cutting or shearing the feed material with the help of sharp knives. the manufacture of rubber, plastics, recycling of' paper waste and plastic
materials. ii,,::;
Variant$ : Double-runner disc J?!_i!L-j-It consists of two-vertical discs,
each rotating in opposite directions.. Single runner disc mi/1--only one
disc may rotate and the other is -stationary. The disc may '.be provided
with cutting (aces, teeth qr knives. 'Clearance ·.between the discs may be
Milling Stationary
chamber knives adjusted to optain the d<;!sirable particl� size.
.i .. 1! 1 1-1• •

Rotor disc MORT°XR AND PESTLE. 'I

This. is the classical and the simplest equjpment for g.ri[1ding .. In this
I • • • ' I

.method, the material is crushed . by th� application of attrition and

Rotating pressure.,_ The apothec�ries used an array of metal.,1 wooden and ceramic
knives mortars and pestles for the prod4ction o;f'pills. 'In' this equipment, both
Product
mor_ta·r and pestle are rotating , wh�reas �·' scraper is. statte. Heavy pestles
\ , , ,
•.s:..,:;:,.- -
...:-<. R .
provide the force. of compression, which is an efficient process for wet.
,� � -
- _,,.
ece1ver grinding. This equipment cannot· be provided with a. sieve · for' continu-
ous removal of fines. ,,
Figure 6-3. The constru::tion of cutter mill.

/
152 PHARMACEUTICAL ENGINEERING .
Ch-6 SIZE REDUCTION 153
ROLLER MILL HAMMER MILL . �· ·. :=·. .
Principle : The material is crushed (compressed) by the application Principle .: The hammer mill operates 'on the principle· of impact
of stress, though· attrition· also· influences. Stress is �pplied by rotatini between . rapidly rnoving hammers mounted on a rotor and· the powder1
heavy wheels, niulle�s 'or rollers.. material.
' I ' ' \! i

Construction : Th� construction of a roller mill is shown in Figufe Construction"� The construction of a hammer mill is shown in
6-4. Roller m,ill consists or' two cylindrical. rollers, made of stone ot, Figure 6-5. The hammer,mill can be either the horizontal or the-vertical
metal, which ar� mounted., horizontally. Rollers can have a diameter shaft ty.pe. Hammers are usually-made of hardened steel: stainless steel
ranging froin a few 'millim'etr�s. up to a m�tre. Rollers are c;tpable o_f • \vith impact surface made of an· extn:meiy abrasive resistant material
ro.t,11ting on 'their longit,udinal axes. Generally, one �f the_J?ll.ers . i� such as haystellite and carbaloy. Stainless steel hammers are sufficient
driven ,directly using a motor, whiie the second one runs freely. The. �a� �
for pharmaceutical purposes.
between the rollers cin· be c'ontrolled.1to obtain the desired particle size.
> • ./ ' •
/
0
I I , >: !,
,}' 1l
..
Fe�d

•
Feed

't
,, !' ('' .l.

Q. "
I,'
,, j , L
Product

- l;;J- -
(j,,

oo· ·.o e> Receiver

• , .o ,,: • 0
•• Q-._"'
Receiver .o : ... i,
.,.
, r
,I' !� ·
. . Figure 6-5. The: construct.ion of I-lammc:r·mill.
� -.
f, '6, , 1
l 1··

Hammers may take several shapes. \wo b��lc shapes:·a�e th�\tirrup ,

It

F.ig�.re �-4. The- construction, of. roll�r mill.

1 1 and the bar. Bar-shaped hatnmers are used extensively in "tablet 'granula­
Wo rking : The rollers �re allo;ed tci rotate: 'The material 'is fed tion. The hammer blades can be with flat c_dges oi- 'sh�rp �edges or both
from the hopper into the gap between the twq ,r91le�s. ,: .Jhe :�ai1erial i� on .each side. Ha1)1mers. may be ei_ther r_igid or''swing-type. Free
crushc.c,l whilt! paJS\1'£,, through the rollers., under: hig� .pr�ssure.,, ,T,he swinging typci has. art' advantage tH�t'ihe�·e �ii( bf in,��i��i�� 'clearance
. ,
'Clearance (gap) betw�en the roUets cari'be adjusted to control the degr�e . between hammers and scre�n, if excessive build occurs .'ii'l' the mi 11.
.
of si�e.,reduction; The �roduct·:is' collected
' i�to a receiver. · This unit is enclosed with a chamber coritainin'g � grid or ,removable
• . . . . . ' . . . ' I'<!. :
;•
Us�s : Roller mil} /s use � tor cr�1shin� a�d c,racking of seeds ��fore screen through which the, m_aterial must pass. · These screens are not of
, _ woven type. ScreeQs are prepared using metal sheet of varying thickness .
ex�raction of .fixed oils. It is' also used to crush soft. t1ssui: to h�lp W tho
. ,�with' perforated hoies or ,s,loJs.. -- . ' . ,,
perietratio' n ofls?lvent d,uring extraction process ..1 , , •
. Working : The hammers are allowed to be in· co�tinuou� 'motion··
. ' •· . 1, ' ' • .

. : Vari�nts : Multiple �.riooth rollers or corrugated, ribbed or saw-

toothed rollers can provide· cutting action alsq. (SOOO to I 5000 revolutions per minute). The feed material is. placed into
the hopper, wnich. flows vertically down and then. ho"rizontally., while.
hammers are in: continuous motion: These rotating ;hammers bear4he.

J
 , I
154 I l'I IARMACEUTICAL ENGINEERING. Ch-6 SIZE REDUCTION 155
:'.

Advantages : (1) Hammer mill' is easy to setupJinstall); dismantle·

'; l

material lo yie!d smaller particles. Then, these pass through the screen.,·
. . . ' f,'.)

· ·
Due lo th� tangential exit, the siz� of the pro�uct is considerably sni.iller ., and clean up. .. . . ., .
thar the: aperture of the screen as seen in Figure 6-6a. (2) Scale-up' problems are minimal provided Jame type. �/\nil! i�· .·
I
I
I
, used..
(3) VarioL!s types of feed stoc� can be 'handled using screen of
� ; ;,� '1
�. !

�,'/;di:.
I I ,

--: different sizes.

High speed'-.;;l ,
� b.'-:.:} ,,.lowspee
· d (4)' Hammer mill occup.ies small space.

.H
I

(5) It is versafile, i.e., speed and screen can be changed:'rapidly.

H Mesh size of
the sieve (6) As it is operated in a closed environment, dust can. be reduced
and explosion hazards can be prevented.
(a) Influence of the speed on parti�le size.
. Disadvantages : (I) The screens may get clogged.
(2) Heat buildup during milling is more, therefore. \·p�c;,puct degrada�
tion is possible. , · ;. :i i' i:. y·,
' ,1, . •

'•,';::'
• ,,

ii ; . ,f
(3) Wearing of mill and screen is mot�·with abrasive materials.
(4} Hammer mills cannot be employed to mtll ·sticky.· fibrous and
hard materials.
Variants : The examples of hammer mills used., in. pharmace· (n;cal
(b) Influence of the thickness of the screen on particle size. industry arc:
(a) Fitzpatrick com'r:ninuting machine (Fitz mill)
Figure 6-6. Size reduction modes in the hammer mill.
(b) Stokes torn�do mill
The screens are interchangeable,. so that any grade of fineness can be
. '

achieved. The hammers act as a centrifugal fan, so that large amount·of
air is drawn through the !l)i!L ln· most cases, this, is sufficient to
counteract th!! heat generated quring milling.
The finene.ss of the product can. be regul�ted by allerin�:
_rotor ·speed,
j ::-
Fitz mill is used for drugs, roots, herbs, glands, livers, soaps etc.
Micropulveriser·: Micropulve�iser has been used 'for -sugar; chemi�
cals, pharmaceuticals .and cosmetics. T,he: conJtructiorH s, almost same as
shown in Figure 6-5. The liner of the' mil\ hous.ing:is-n:iade .of mu!J,iple
serration,s. which promote the breakage of particles :thrown· against the
'c;:an

wall by the _rotating hamme�. s. An airi,nj�ction fe,S,<ler be used, to ,

ll

··reed rate, ., .
'·
'"'"7,

' 'clearimce between hammers and. gr,inding plates,

' t

project the · feed directly . in ,front . of the hammer. tips, . which a_re fitted
'' • • '

:;-. • t
'- number and type of hammers, with tungsten carbide insc::rts. This. arrangement . increases mill effi-
.ciency. · ,.
'"i '

- size of the discharge opening (screen).

• ' • : I
•

,· _::;\,i.;.' .
' � ' '

o,n·
\ l • I /• I •
J '

Uses. : Fine to ·moderate grinding of. powders may be obtained, !-l�1111mer crus�1er dnd vertiqf{J:, impacrpu/veriser;�YC!fk the prin��pj�.
dependin� on the speeds of the hammer. The· expected particle size may of impact for s+te reduction. �;y-'' ·• ·:·
·,
vary from IO to 400 mm. Non abrasive to moderately· abrasive, brittle
materials can be used as feed ..stock. BALL M,ILL QR PE'BBLE MILL '\
These are also known as turnhling mills. · · , .,
.

. It is used to mill dry matcr'ials, wet filter press cakes, ointments,

'

• ' '
slurries': etc. Brittle material is best fractured by· impact from blunt Principle: The ball mill works on the principle'qf irnpaat, : o�tween the
; • . � ' ' - : '' '� ' f Y"._• J • '

hammers; fibrou; material is best reduced in size by cutting edges. ·• rapidly rnoving balls and the powder material. both' enclosed in' a 'hollow'!-..'-
,
 156 5
SIZE REDUCTION
.,J 7 )
l'I IARMACEUTICAL ENGINEERING Ch-6
I

· cylinder. At low speeds, the balls roll over each other and attrition (rub­ At still higher speeds. ,the balls· ar'e· tnrown out to' the >waI' I' by j
bing actioh')' will be the predomin.ant mqde of action. Thus, in the ball centrifugal force. Hence, grinding will not occur. khe compressiomby ., '· ·.•
mill, impact or attrition or both arc responsible for the size reduction. the balls against the wall will not be sufficieqt fo(effective comminution
of the substance. (Fig�re 6-�B) ··;·, ; , i .
Construction : The construction of <3: ball mill is shown in Figure , • ... :.

Q'
6-7. Ball mill c onsists of a hollo,v cylinder, which is mounted on a

'"00'..-=- ,.·
; ·�� ·,
- metallic frarne in such a way that it can be rotated on its longitudin�I
axis. The length of the cylinder is slightly greater than its diameter.
The cyli�der is made of a metal and is usually lined with chrome� In
pharmac!!utical industry, sqmcti111es the cylinder is line·d with rubber or
,' ' ' ,'. \ H)J, J , ·;:;,'
porcelain.. A
, 1! ·
. 'B ' •
t) I� 1 t t: •
, C, ri ., ,,
Low speed High sp�ed Correct speed
• )j I ' r l I

Figure 6r8. The modes<;>( roll in� of balls in tihc. ball mill operations.
. I.''

Uses: Fine grind'ing,with a particle.size<:of IOO'to'.1 5 mm or.'less can

be obt.ained,t'particularly for hard •and· a-orasive materra'l's.' 11 Stainless steel
\,
balls are prefe.rred in the production of ophtlialm1c: 1 and'par;enteral prod-
. . ' ' . '

ucts, as there is a· less chance of111ontamihatiot1 d�e to weaf 13,fll mill, at

Steel balls
IOW Speeds is USed for milling dyes, pigments' and inSeCtletdeS. I
Feed material
Advantages :' Ball mill ·�ffers several ad�antages arffi is widely ilsed·.
Figure 6-7. The construction of ball niill. · These are: · 1•11 . ; '

· ( 1) It can produce very fine powder. : ,1

I • H ) •
The cylinder .contains balls tha.t occupy 30 to 50 % of the mill I,• '' I ' j • ' i; • •
volume. The weight of the bal Is is kept constant. The ball size depends (2) t · i� 4sed f9r I ba�ch . �pe!ation,.; . It, can be , made. continuous
on the size of the feed and the diameter of the mill. Balls are made of operation by including a chamber next to the cyJinder. The' se
·
steel, iron or stoneware. These act as the grinding medium. are separated' � using a sievei · , ' ,� , . ,
' , i : i ' '. , ' I f j � • l <l
. (3) Ball mi�l"is .sfta?le \or ?oth:,�i' an? d,ry g�i,ndi�g.w�cesses.. ' ·
iI I { t '•·.'

Working : The drug to be ground is put into the cylinder of the mill :
in such a quantity that it is filled to about 60% of the volume (material , (4) Toxic substances. can)�� grpu�q. c1s th�1Gy;p11��r1is a· clo�ed .syst�m.
to void ratio).· A fixed nuJnber ofbalfs are introduced <_lnd the cylinder is (i): Since the rniH is a,.dosed 1system, stel'ility·can be acnie�ed� · i . .,
closed. The mill is allowed to rotate ori its longitudinal axis. (6) Milling' operation ·�an be accoinpl' ished t,ii,finert �-t�osphere';' if
.,, .
The speed bf' rotation'is very important. At low speeds, the balls roll
.
' I OXygen Sensitive• SUbSfanCCS are to''be ll}illed.''\' {' '. ' 'I _''"

over each' other and attr.ition will' be a predominant mode of stress <1 I � -> l • : l•
• •
(7) .Balls can be of various shapes :and sizes." Rods. or bars may. b�
,i") ... ;• •' '

(Figure 6--SA). The use 'of small bal.ls (or glass pebbles) is recom­
.. used inste�d of b.a}ls .. �?j m)H 1sJpartJc.u)�rlyd1s�r�t,.t�r1 milling
mended so .that the surface is the greatest. Tl1is mode of attrition is used · 6f sticky materials.' . -- :. .,,..• . .. .·. ·, · o1,,1;11
( · .,t_i.· ·,. - lo-:·. \ , ! . r·, • ,.
for we,t grjnding. It 1113y be useful to add surface active agents to
• ff"
)
(9 In ball t:1ill, installation ,. <?Pe. ratiory and 1 la?o�r. �osts . a\'e _ I9w.
prevent agglomeration. ' l ' -4• • ..

.,

,. GJ
At correct speed, the centrifugal force just occurs, as a result "the balls
are picked Jlp by the mi_ll w:111 and carried nearly to the top, where they
break contact with the. ,,;all and fall to· the bottom . to be picked up J .•I ...,.,.,
L. ' I ! �: � '

(Figure 6�8C}. In this manner, irripact stress will also be induced and the Roun9 ball Banded·ball :·.,;.; Cube. . .G,ylinder1(rods}
· size reduction is made �ffectivc. · ':s: •·
. • ' . 'IC I

· Corr:nqnly used balls' °I · \ ,;,:·

J �.
 @ Disa�vantages : Some.of the disadvantages ar�. :
.
(I) The ball mill is a very noisy machine.
Pl1ARMACEUTICAL ENGINEERING

(2) Wear occurs fro1'n the balls 'as weli as from the casing, which
may result in contamination of the product.
(3) Bali' milling is a slow process. The rate at which energy can be
app'lied is limited, because it depends on the acceleration of the
�al'ls; Which is influenc;ed by the gravitational .. force.
(4) Sqft, ta�ky, fibrous material can�ot be miliei by\ail mill.
.� .,.. � � � >·" . . ' ''J. '' ' '
Variants :. (a) Hanlinge mill: Usually, Hardinge mill consists of
·� .

hollow cylinder with a conical certral section. Different sized balls are
used. The small balls are placed near the discharge end, where they can
peiform the finest grinding. The largest b�I'Is �erpain in the cylindrical
· f!!�d-e�? wi�h £?9.ual de�r.ease. in s,if'e of balls. As_,tbe charge rotates,
?if�erential/�
, !!. At�j(�g�I, fore� ,,S�u. ses tbe. finer _particles to· move towards
the <;lisc\l_ �rge end. In thi� eqtiipment, .remova,,�. of discharg� -can be d?ne
from, the side" covers. So the mill operates simultaneously for size
reduc'tio� as;.w�II as classi ficati9n.,
'' �- ' ·�

(b) Continuous ball mills.: In the simp\e type;of ball mill, it is not
possible to.remove tines witl�;ut emptying the mi)l. Sieving of.po�der
should be done separately. In continuously .operating b.all mills, a series
of cha1nb_ers are separated by siev�s of successively finer.mesh size. The
equipment is positioned under a •s'ma11 ·slope so th�\ the powder can pass
to·thc next chamber. :_ ': "'
.

(c) Vibrating ball mills : In vibrating ball n1ills, ;the metallic cylin-
).

• der is supported on ,a spring base and subjected' to forc�d vibrations

induced. b>y electromaghetfo· means. l ,These": have several ·advantages:
(I) Mi(! ;is.free from-fotating ,parts,.J2) It is easy to integrate the 1nills by
.classjpers a°i,dlott:�'. ,a9e;il!�r�JY,St�m11 (3) Y,ibr,ating mill grinds at rates
often� as .high as 20 ,tq �;O times ,t�at qf the;jconven,tional mill�
(4) Grinding efficiency is also high: .. ,. . .
;L�·m ··iN�R;� .MILL;oR J�T·M.ILL o� · 'NI1cR01,hzERs
·: . .- .
/OR ULTRA:FINE GRINDERS
· '// Pr.inci'�:le:.: Pfui,d energy m.ilfop�rat�� o� the principle.of i�1pact and
/ attrition�..., 'in this equipment, the feedstock is suspended· within a high
velocity air stream. Milling ··takes place betause of· high 1veloc. ty colli-
sions bet\.veen ' the suspended particle�.. ·
•..

Constructfon : 'fhe construction of a· fluid energy mill is shown in

Figure,6-9. Flui� energ;y., mill consists of an elliptical pipe. which has a
Ch-6 !ilZE REDUCTION 159
height of about 2 merres and dia.met er may be ranging from 20 to 200
millimetres. The mill surface ,nay be made of eirher soft stainless s teel
or tough ceramics. Usually, 1nills are c o-nstructcd such that the c onrnct
surfaces are merely linings, which c,:1n be removed or replaced, If
excessively erGdcd after use.
Oauffier
(<crten) Outlet (rluid and
fine particl•s)
Elliptical -
loop plr,e
Fluid noulc.s
Fleure 6-9. The con!truction 1lf nuid cnerg) mill.
Grinding nozzles (usually two to six).1nay be pl:iced mogcntisl andlor­
'-flJl9Set! te !he iitilie/ Ao_. J>Blh ofa:powder. Normally. cornpressed air
is used at 600 kilopascals IQ l.O megap11Scals. lnert gases <'..1tbe used 10
minimize or eliminate the oxidotion of susceptible con1polmds.
Venturi feeder is provided in the path of the ai r flow. An our!et with
a classifier (cyclone separator or bag filler) is lined to all-0w thP. ('�Cllpe
of ai.r.
Working: Po,,-der is introduced through the inlet of ven turi. The air
entering ihrough the grinding noules transport lhe powder in. the ellipti­
cal or circular track of rhe mill. In the turbulent strean, of air, the
suspended particles collide \Vith each other and break. Thus. impact and
aurition forces operate in size reduction. The resul,ant small particles
(by entrapment of air) are carried to . outlet and removed by cyclbne or
fihers.
'
The coarser particles undergo re-clicula1ion in t he chamber on a c -
coun1 of its own weighL These re-dn:ulated particles collid� again wilh
new in-coming feed stock particles. The powder remains in the n1ill.
until its size is reduced sufficicnily. Later it leaves via the sieve.
Hence, fluid energy inill p roduc es particles with narrow size disrribulion
• stationary. \Vhen the material is passed through these discs, t hey get
160 PHI\RMI\CEUTICi\I. F.NCilNEERING
Some 1in1cs the particlcs, which are enrrapped by lhc drag of gas,
.
leave the mfll and ear ned our to a cyclone sepnrator or bag collector fior
. .
size scpnra11on.
Uses : Fluid energy mill is used to reduce the particle size of most of
1J1e drugs such as antibiotics ;ind vi tamins. Wh�n srricr quality '.onirol is
desirable for the purpose of bener absorplion (bioavaii:ibilit) ), this rnill
is rhe pn:ferred one. Ultrafine grinding can be achiev-,d 'lloderafely
hnrd marcrials can be processed for size reduction.
Advantages: (I) It has no moving parts. hence, heal is not produced
during nlilling. There.fore, heat-labile substances can be mi lled.
Examples are sulphnr,a-mides, vita,nins and antibiorics. Due 10
the expansion of gas.t, under pressure cooling clTect ;-, producer!
during milling.
"') �I is a rapid and , i cfficiem method for reducin;; powders to
{-
JO min or less.
(3) Since there is ii1.. wear of the mill, contan1ina1ion is not possible.
Disadvantag�s : (I) Fluid energy mill is not suitable Jor milling of
son. lac�, and Iibrous materials.
(2) The �,,u1 pn1en1 is expensive, because it needs additional accesso­
ries pMtic•Jfarly fluid energy source and dust collection equiprnen!.
V1rlanls : Cenrrifagal-itnpacl pulverizer-In ceatrifugal impac1
pulverizers. a ro1or is spinned to induce higr centrifugal force on rhe
feed pariicl�s. The particles move towards the impactors, which are sci
at the periphery of the rot or. O n striking these impactors, the material is
further hurled a�ainst the outer casing where final reduction is achieved.
The material i:s removed from t he conical discharge a t the bottom.
Puticle Sile reduction i n the range of IO to 325 meshes can be
obtained with !his type of mill with minimum fines. Centrifugal impacr
pulverizers have been used for rhe size reducrion of a variety of mare-ri­
als ranging. from soft organic molecules to hard abrasive materials. I! is
also well suit ed for t he size reduction of heat sensitive materials.
(:OLL.01 IJ �11LL
Principle: CoflolJ mill consisrs of two steel discs having very small
clearance between them. One disc is rotating, ....·hile the other one is
sheared. Thus, coarse particles are broken down into small particles due
to she.sr.
Ch-6 SIZE REDUCTION 161_

Construction : The construction ofa colloid mill is shown in Figure

6-10. The colloid. mill consists of. high-speed rotor·' and·· stator '\vith ·•
conical milling surface. The milling surfaces may be s.:n·ooth surfaced_'''
or rough surfaced. Rough surfaced mills· are used for'fibr<ilus material'
i
because fibres tend to interlock and clog' smooth surfaced mills. The.,
. ckarance between rotor jlnd stator c�11:.1J,e adjuste� from ,9.05, to. 0..75
millimetres. During milling, the heat generated may dse the ternpcratu(e
up to 40 °C. l lencc, cold water circulation is provided tc, reduce the
te�peraturc as much as 20°C' The. discharg� pipe! is. also cqnne' cted to
hopper, so that discharge can be' recyctdd.'
\•J

rotor

Outlet
ti�
.,... Figure 6-IO. Construction of coi'.oid mill. ;.

Working : Mater.iais such as suspensions and emutsions arc placed

in the hopper. Usually, the solids are pre-milkd to prevent the damage
· of colloi� mill. The solids are mixl!d with the liquid vehicle before
being introduced into the colloid mill. The di�persion tlows down c3:nd
adheres to· the rotor. During the movement of rotor (3000 to 20000
- revolutions per minute), centrifugal forc��throws a part of the dispersion
on to the stator. Depending otj the clearance, t:\e_. dispersion is sheared
between rotor and stator. Thus; size ·reduction ciio· be achieved. The
milled liquid may be recycled. Aft�r"·achieviqg: the desired size, the
discharge is collected from the outlet in·'the·pe,riphery ·of the housing.
Normally, the size of mjlled particies ·may· be smaller than the
clearance; because of the force of high sh�ar. In emulsification, a
c.learance of 75 µm may produce dispersion with an average particl� size
of 3 µm.
The capacities of colloid mills range from 2 to 3 L/min for, small
.
mills to 440 L/min for the larger mills. · ,: ' · · · · '
 163
C:h-6 SIZI::. RED,UCTION

r.cvolve on _it s ax is , and. at the sa111e time trav!,!1 r9und the

l'IIARMACEUTIC/\1, ENGINITRING
,�
s hallow st�ne
�cs,:; .·c;olloid: miit is used for _greparin� colloidal dispersions, sus- ·. �ed.. The outc� - part1
of the .\�,1�cel has fo travel a grcaier. �!is t�,n��- tl�an the
.
inner, SO that SIZ� rCQL!Cli<'n is nchievJd by shearing .. aS, Jc'
pens ion.�;, cmu\s ions a.nd ointm�11 ts. It is not us ed for dry milling. :i . ,·•h.;mg ·
l
· · · , · t ,, , . , . •. , ·11 as � crus
Partick siz.� <1,s smal) as 3 µm can be obtained. Fibrous material can be Thc _n��t ena 1 IS gr,ou,ndJ:)r a d e finite ' period, The po�vaW'.\s
'-��hcctcci'
and passed through a sieve to get po,vder
rniUcd usjrig rough surfa'cca rotor and stator.
. ·· , . , " ,. · ., ' .• . of he
, ·
t . ·requ'
• are'
d �1· z'
.,·,. ..., ..· '1. ·.'Us
e '· :•.,i,·-,,a, , ·.
.,_ate
b h process . '''.''.
· /'�: Colloid 1�ill c�1} _be sl_E.dlised. So it can be used in the
.
' 1• • �1•''.\, . ·..;,�"I
.
·-�1·,,--i)�r,:'
.

production of' stenle products. Uses :. E�g_e �upncr mill is 1,1sed for,grindi�g to�gh· �;t�·
. ;i;l� ·t� fine
powder. h _1s-.st11l .uscd fqr �lant-l?ased products , while
. more sophisti.,.·
I .
9is:tdvanta1;cs:( l) C9ll�id _!!,1)\1 te_n_��--t-�jn_c_��P�!?te a,ir into th,e ,
t, 1 T .

eated m Ills ;i:\rC useP. for ·chen:11cals and drng.s i · >: , , , . , r: .. :.; , ;
nn_ishcd product.· Ther�Jore, the product should-6cattm,--ed tP.;
rest for some time for deaeration. Advan . tagc�·: Edge·r�n-p er mill does:not r · · ; · ,:,•.,· ·.•.
e a e t
. , operation. . "" ! ' .,,,, , �! 9�g !Ji ri ,:�/LA�,1 �i�, g
i� generi,!!Cd-dui:ing.-
.P-fl·kat �-······--··-·· .mi 11 ing. Hence. \ya t c r circulation
, I
facility around th, e milling chamber can be provided.
I .,,.. ·.·
Disadvant.;gcs : (I) Edge runner mp! oc::upies more
, , . I .. : ·'l,

space than. o•her

$ Colloid mill is not usefulJor dry milling. comm • only used mil l s. · . ·
1
. ' l'I, l " , _/ ' 1 '
. , (2) Contammat1on ·of the "p1'odoct�with�t'ollc('rrf"a t ···a ,�;is.· ....:p_' -. - .....
• • .\ i ,, _;: �

EDGE RUNNER MILL �- _ .'?t s

o s. ) b1e.
j.
(.>)
�
·n1 e rrnllmg process is time c9�sumihg.
• • •.\ 1 , ,•, .
.
Principle: The size r��h1ction is don� by crushing (domprc;ss ion) due (4) .· It 1s not used for sticky materia1s: ·
to heavy weight of stones.1 Shearing force is a,lso involved during the
cs) _E.nergy, s·on�.urnption is"'quite hi gh'.
movement of the stones. . ' If. .
Construction. .: The construction of an edge r�1nner mill is shown in , END �µNNE�_.M.�L,L
( (
�: \ 1

;,_, ,. ,,, r.
•• • �

.
gh several
I
Figure 6-1 I. It consists of two heavy rollers and may w ei
Principle : Size r eduction is done by crushing (com
tons. The rol_ l ers move on a bed� which is made of stone o r g ranite. pressi. on) du 1.
· h:::avy weight of steel pestle. Shearing ; stress i�; als
Each roller has a central shaft and revolve o n its axis. Further. the o·involved during�th�
n,,>vcment of mortar and pestle.
a horizonta l shaft and move. around the bed.
' mounted on
rollers an; . �. ' ··. ' ) ·,1

.
,..
I
('� It ]....,,.J .•·1�·,..,.l,.J. (;,

Rollers ,

'\
.,-
). - q • l J\ $ i I � '' • '�t , . !
1

.....: ;.
Slialt
- _t),_t.. , Ste� �odr
··., :,
·.,

-·-· ........ �..� ..... _._,.... ..........- -.

v , _i,,,fl
,
Bed Material Bed
Connected
�-- to motor· ',1{ �·. :1�,::'
\

Figure 6-11. Construction of edge runner mill.

I ·.:,: ,i·, :/

. B�velcd-cog �\ting ' ·' '. ..

l ,., ,,
'Working : The material to b e grou9d is p laced on the bed.
y

help of a scrapper. it is kept in the path of the stone wheel. The sfones
r

I,
 Ch-6 SIZE REDUCTION
164 165
Construction·: The constructio'n of an end runner mill is shown in Uses : [::nd runner mill is suitable forfi�e grindin_g. Now a days,4.his
Figur,e 6-12. it is �onsidered,as a;'tl;').$Chanicul mortar and pestle. ,It consists
ofo'ste�I mortar, \vhich is. fixed to a llangcd plate. Upderncath the flanged
.
mill is replaced by more efficient and .sophisticated milling equipment. .
Disadvantage : End· runner mill ls not suitable fJr drug's, which a�e
plat!!, a bevelled cog fitting is aft?ched t? a h?rizontal s.hafl bearing a ., ·
in unbroken pr slightly broken con9it�o.ns.· · · ,• ' , .;•; •::,·:···,r i , · •
pulley. Hence, the plate with mortar can be rotated at a high speed. .
In summary, several size reduction equipment are. described.. Some
The pestle is dumb-bell shaped so that ba!.ancing and el�cient grind­
. ·gcncri}I characteristics of various types. of mills arc given in Tabli6-I.'
ing by.its weight ca:, be achieved. The bottom of pest,lc 1s !ht rath:r. � . C·
tha:.t round.. The pestle ear.rics an arm; w!iich' is hinged. · By this lt
OPEN CIRCUfl' AND CLO.SEO CJRCOJT MILL . .. .. '· · '1 ,.,
arrangement, the pestle can\ be: raised from the mortar to faci.lit'l�e • ( c , ! •:; 'I ' ,
The size reduction process may be achieved iii open circuit.or closed
emptying and cleaning. The t�a�row central i portion of th� pestle. is .
circuit conditions. r · _· • _; ,, ·.�1 ·., · ' .
longer than the band or the arm arouml it. I le1.1<:c, iJ�stle can rise and tall 1. · .

over the mater ia! in the mortar. An ope11-circ:ui1 mill is one In whi�h n.1illing operation' is carried out
·
' . 1-'I. '
in one atiempt, i.e., by passing the feed m:i.teria! through the mill to
T;\BLE (,.J · · ·
obtain the desired size.
General Characteristic� of Vario'us Types of Mills
.J A closed-circuit mill is one i� v,h'ich the dis�h��gc, fr�·ni the millirig
SI. Na,ne of Actioh P/'oduct Uses Not 11jed
process is passed through a siz;c· 'separation device or .tlassifier, and
no. the. mill si:e " for the
over\ize particles are returned ,, ;, .. :. , . .
I. Cutt..;r mill Cutting 20 l� 80 rm:�h Fibrous, �rude 1-'.fiablc to the grinding chamber for · '> '.. .. ; :. '
., ·· 1
'.,lf
(animal and ·material further ·size reduction.. Mechanical air
vegetable
._ ,.. � ,1
dru
I
0)
e'
cla�sifier
2. Roller mill C0111 press- 20 to 200 mt:sh Soff matt:rial Abrasive
' · ion ' r(J ' ., ,, material
,. ( I
3 .. 1.!Jmm_cr 111,ill 1lmp:11:t I · � :o 325 rne�h ·I All most 1\brasi,·c
:111 drugs ·rnatt·rial
Fines
4. Ball mill ,\tlritiL\11 20 to 200 mesh Brittle drugs Soft mate·
. & impact rial
5. Fluid energy Attrilitm to 30 mm Moderatdy Soft and
mill & impa�t hard and fri· . stil:ky
•abie material material
5. Edge runner Crushing Alrnoft all Sticky.
.
20 to 80 mesh I

milt & shearing drugs material Finished product

6. End ·runner . Crushi 10"' 20 ro SO mesh Alq,ost all Sticky bin
'� ... Figure 6-13._Closcd
mitr & she ring .\
�' I dr�1gs n1aterial r:
· circuii'�il(.i1i>systcm
i i �1
.i \
'I l_
7. Colloid Sheari g 3. 75 llnl Alrno�t all Dry with hammer rnjll.
'\
mill drugs milling
The prjnciple of closed circuit grinding is widely .used ·in the pharma-
j;, •

.' j ·• .. t . ' � . .
Working : T,he. ma�ena:I to be grQpnd rs placed 111 the mortar. The 0ceut_ical industry. It has the advantages: ,· ;: · .
scraper puts the. material in the path of the pestle. �he niortar re'\'ol:es · fa). h provides fine a�d ultra-fine sizes�
at a high speed. The pestle is placeq in the mortar. .The· revolving (b) It eliminates dust. •./. ' · \
:..
'lr+
mortar �auses the pes,tle to revolve. During tliis process, size reduct.ion (c) It eliminates 'ov,��hca•ting. . ,, . . ' .
is ach.ie'ved by· sh.ear1;ng as wey .a� crushing.-·. The 1:1ateri_al is collected , .I
(d) It produces a produ�t that is free (rcim' oversize,�t I"or
\ � ''' •. I', ' • I'

and passed through a sieve to get the powder o,f desired size. .
·.
undersize.
,'fl'f)i1".:';:,:,·,;_;:-.: )

. ' �.: ,,• .

... '. . ··. \ ·, ); ��. jii_�.: ·\, ..

)
166 1'11/\RMACEUTICAL ENGINEl:RINC,
. A cl��ed cir�uit �ith an air classifier is shown in 17igure 6- l 3. In this
type, size rcdu�tion i. s combined with �izc classification. The working oi"
hammer mill is illustrated in Figure 6-1'3. The coarse material returning
.to the mill bv a classifier is known as circulatin�
' ' load.
�. .
Dry and Wet Grinding
The �se of a product and subsequent steps mainly decide the type of
equir,r11ent used. In the preparation of'colloidal dispersioi1s, suspensions,
emulsions and ointments, \Vet grinding _offorsadvantagcs. In the produc­
tion of suspensions and emulsions, �vet grinding has become an integral
- and plastic during milling. These low-melting substances should be
part of the processing. for example. rnill can be used as mixing
equipm�nt. Triple roller mill, colloid mill arc used for such a purp.osc.
Ch-6 SIZ£ REDUCTION 167
_:. Fibrous materials : Glycyrrhiza, rauwolfia, ging�r etc., arc fibrous
'ir 1· nature and cannot be crushed by pressure or impact. _Fibrous materi-
. als ·are tough in nature. They ·must be teared by a cutter. Nux vomica.
and ipecacuanha arc processed -in two stages'to get fine p9wders.
Friable materials : Sucrose and dried tilter-cake are friable.'and tend
fracture along_ well-defined planes. Brittle substances' can be easily- '
· <;onverted to smaller .particles. Such,materials are milled by the mecha­
nisms �ucl1_ _as attriti�n. i111pact or pr·i��ure.· For 'exarriple, sugar is . milled
· using hammer and fluid energy 1�ills.
1_ .:i.
Elastic materials : Synthetic gums, waxc;, and resins become soft
chilled before milling. Such materfrils arc milled using hamme'r,'collo'Ri
•
or fluid energy mill. 1

In practice, it is found that liner size can be achicvei.l by \\;ct grinding . . . � '
than l>y dry grinding. Wet griilding is used in ihc .. production of Hygros_copic matcri'als : .Substances. such. as potassium carbonate 1
• I:

flocculated suspc�sions: In wet gri1Jding, surl"actants arc added to attain absorb moisture rapidly. This wet m��s sticks and clogs the n,1ill. They
particle size of 0.5 �un. The advantages of wet grinding arc that: arc 'prcparcJ in a ·clos9d system .such as pors;�lain ball mill.
•
.,o ,, , '
• . \,, I
1

(I) · it eliminates the dust hazards. . · Solvatcd materials : Sodi�J'i\} sulphate (Na2S04• I OH20) and other
..
.
liyclr,1tcs Iibcratc,.water during milfing and cause clogging of the· mill.
(2) \\'.el grinding is usually done al low speed. therefore. it consumes ·
less power. l\.lclting point.: Solids with low ·melting points ·often become soft
/>) · grinding aids can be incorporated. and 111elt owing to the heat generated during milling.' Such --�atcrials are
' · • . · ·· · · . ' ·
1
chiiled ·before milling. .
Co\loid and ball mills arc best suitcu l<.)r wet grinding. II" the prnd11ct \ • • ' ,. t' ·• ' I,

undcrgc'.les physical or chemical changes i11 w:itcr, dry milling is recom­ Thermolability : Certain subst_an�es underg� pegradation reactiot;1s
mended. Thc fineness is limited .t0 \ 00 pm. ,\ll the mills reported ·such ils hydrolysis and oxidation· due to the presence of_ mois�ure and
earlier 'e�ccpt collo-id mill can be used for dry grinding. almospher.ic oxygen. Such reactions proceed faster owing to the heat
produced during milling. They should be mille{.i11 ·� closed system .'\�ith
SELECTION OF A MILL ,an 'inert atmosphere of carbon dioxide or nitrogen. Vitamins and antibi-
··
otics ;re milled using fluid energy and ball mills. :
The selection of a particular cqt;ipmcnt for size rcd.uction tkpcnds 011 •• ' • .. •l: : • ) •• •• • .•

a numb'er factors. These arc related to the feel milled pruuuct. safety,
and economics.
F:1dors Relaied to the Nature of Raw l\latcrials
. Th� properties of a solid determine its ability to resist size reduction
and innucnce the choice of c.qu1p111ent used for milling. Some physical
properties of the feed arc as follows.
Flammability :. Almost any fine dust, such ,as .dextrin, starch -and
sulphur, is. a potential explosive_.mixt_ure. unqer 'ce.rtain conditions� All
. : clectri�al s�itches should' be explo:;ive' proof· and · the 'mill shouid
· ·· be
. , properly grounded (earthed): .. '. ,.
Particle size of the feed : For a mill to operate satisfactorily: the feed
: . should be of proper size. For exampl�/ pretreatment of fibrous materials
·,\vith ·high pressure rollers ·or cutters facilitates further comminution. ·
' ·. ' .· ·. ..,·;_;, �: .. ,,.... :� ... ·1 · j • �_,.-:��

Hard materials : Iodine and' pumi�e arc hard and abrasive. 111
• •• •• 'l"'\ •'

· Moisture .content : Presence of more than 5% water. hi��fors -..the

gcner�I. hard materi�ls arc most di fticult to con1.mi11utc. For iodinc. milling process and produces a sticky mass:· The effect is morc .. pro­
hammer-mill or.fluid energy mill is used. Sizl' reduction process of such nouncc·d, when the concentration of water is more.· ln:gen.eral, materials
materials .can. lead to abrasivl:! wear of 111illi11,,; parts, which then cause '. :., ·r:.: :··.
;.,.,; ::1·,:
contamination. I·.
 /'

!•:r·'.,,r
168 1.
PHARMACEUTICAL ENGINEl:.RING
Ch-6 SIZE llEOIJC:TION 169
with moisture content below 5% ar� suitable for dry grinding and above ' �
under certain conditions. Explosi. on hazards of non-rnctailic materials,
' 50% are suitable for wet grinding.
. . . . ,,, (. ... such as sulphur. starch and. wood floor, arc often appreciable.. . Metal
· Pretreatment : For the mill to operate satisfactorily, the feed should powders pose a hazard ·because'' of their . flam1�ability: .. "Th� useful
be �f a proper size ,and enter the' f.�1uipment at a fairly uniform rate. precautions· arc: ',.. . !
Therefore, a pretreatment step shoul.d be included. For example, fibrous (a) ·isol�tc the mill.
material should be treated with cutter or roller, which can facilitate' (b) use of non�spark ing material of construction. ,:, · ·
..
further comminution..
Stainlcss steel has less sparking "tendency than· �rdin::iry '.steel or
forging.
I..
Factors Related to the Nature of Finished' Product
The nature of finished: (milled) ,product also influences the · selection
1:,
.• ...... ::.:·,::.
Facto.rs Related to the E�onomy
of the equipment. . . · '. : . .
Cost. power consumption, space occupied and lab.our costs ,ire some
Particle size : l f extreme size control is necessary, it may be essen­ of the economic factors that determine the selection of a mill ·(
tial to recycle the larger part,tlcs. rhis can be achieved by screening the
1 '
I �

Cost : Where the particle siz� control is not critical. thc'tost dc�ides
,, ' ' ,•

discharge material and returning the over size particles for a second time
milling. Moderately coarse or coarse powders with a minimuin of fine the type of equipment. In general, the cdst of the size., reduction
powder arc easily obtained by using a high-speed impact mill. for i_ncrcases, as the particle size decreases. · Th'erefore, it -is economically
example, cascara, liquorice, belladonna leaves and roots are easily bro- undcsirnblc to reduce the particle size to a 'finer degree than neccss;frv.'
. .
.. .
ken dc,'wn by impact �ill. • 7
',., ,,· ,':
For; cxample.. 'partic!c size of gri,seofulvin ;s critical in the production.
:
THEORIES OF COMMINUTlON
' �. iJ i \. ! I
Similarly the particle size is also critical in the stispcnsion of pcAicillin Mechanical 13clrnviour of Solids
I ' /)

. . . ' ..d
G procaine for ·intra-muscular injection due to its s)·rrngeability. When various modes of str�ss arc applied on.a powder., the particl��
Ease of sterilisation : \\'hen pr.cpurations are intended for parenteral get strained. This stress-strain relationship is.shown in Figt1re 6-14.
, • • •
and; ophthalmic uses. c;ize reduction should be conducted in. a sterile
,1 ,. ,. ,, : L ..

,.
e11vlronment. The eq�1ipmcnt should be stcrili'sable. Ball mill s and fluiJ
'1.... ' ..I i·: . '
: -Pla�tic. ·. · ,'
emi�gy mills arc suitable for this purpose.
i
deformation
Contaminatiol) of milled nrn,erials : In case of potent drugs and j
. low'dose· prooucts, contamination of the product should be avoided. Use
of equipment that is frc� from �·caring of mill parts is preferred. Fluid
energy mill is suitable for this purpose.
·in addition to the end use of a produc.t. subsequent.processing steps
111ainly determine the choice of wet or dry milling. In the preparation of
� I ) ' ) : i ·�

-�· Ct)lloidal dispersions, suspension�. emulsions and ointments, wet grind- . ____ ___
..,.. _..;._ ___• f �'.

i11g offers advantages in terms of siz.<; reduction of materials. elimination
of. dust hazards. Thus, wet grind'fng has become an- integral part··;)f the
processing of the above dosage- fo�ms. Th.e "same 1�ill can also be used
as 'mixing equipment. Examples are triple- roller mill and colloid mill.
F�ctors Related to Safety
The factors related to safety are cxplosivity, irritability and toxicity.
During milling, fine dust of drug arises which may become flammabl •
Strain.
Figure 6-14. Spcss�strain curve fo�_·a .solid.
- ln Figure 6-14, the initial- linear· portion ·is defined bv Hooke's
law. It states that stress is propo11ional to strain. Tl;e slbpe of
linear portion represents -Young's .modulus,. It expresses the
·
stiffncss or softness in m�gapascals. . :
- If the force o.f impact (stre.ss) docs_ n�t exceed the �lastic limit
(r·�gion of Hooke's law), the material i'� reversibly deformed.
 170 PHARMACEUTICAL EN(ilNEERIN<.i
171
· When the force is removed, the particle returns. to original Ch-6 SI7.E REDUCTlON

condition. The elastic limit 'is.known as yield value. The str�ss
energy in the deformed particle appears as · heat. ·' Example is
plastic material such as polyrfrcrY' ·
-· Th<:. strcs;�strain curve bc.:c0i'ncs nonlinear at the yieid point.
·c: l�his is a n,casure of the rcsista11c� to permanent d�fon11ation.
Beyond the yield point, the region represents irreversible plastk
dc{nnnation.
, - The area under the curve represents the f racture toughness (or
modulus of toughness). This is an approximate measure of the
length of new crack formed. The"mechanism of creating hew _flaws in a ..
particle is a s follo\'is. '
Usuallv. the surface of particles is irregular. . The applied force is
initially tiken on the high portion or'thc s(rrface. As a result, high stress
and increased ternpcrati:1rc may be' set up locally in �he .r a.rti�le. The
·bonds at this pla ce bccorhe weak. \vbich may be respo�si9le for creating
flaws. The particle further absorbs applied. strain,:,ei�e,rgy and is .9c­
formcd. The strain energy required to extend .the �rac�
,. to .fracture is
propo.rtional to the length of the crack formed. This energy is supplied
by the now of the residual strain energy to the cr�ck.
1

impact strength of the material. Fracture of a particle can be

obt_aincd when the force.: exceeds the elastic limit.
Theories.of Si·zc Rcµuction
(I), Ac.cording to Griffith· theory, :all solids contain flaws and micro­
scopic cracks. A jlaw is any structura.l,\�Cakncss that may develop into a
crack under strain. The w�akest naw.·_jil a particle determines its frncture
3. Not· ::di materials exhibit this typ� ·� f brittie·, b�h��i��r.. They
resist fracture even at much iarger stresses. because these are tougher .
Thcv undergo plastic f1ow, which al·lows strain energy relaxation without
cra:k propagation. When:pras.tic flow occurs. atoms or molc,cul�s _slip
over one a,wther and this process of deformation require� ..energy.
·.

strength. It.controls the number of particles prodU1.:ed·by frnctu'n:. The

particles \\ith the weakest flaw fractures most casi ly and prudul:e laruest ENERGY FOR COMI\-HNUTION ',
. (' . .
1wssiblc picces. lf1 the next step, another weakest flaw fractures. This Size rcdllction begins with the opei,ing .of small flaws that were
process continues until all flaws arc fractured. The pa11ick size pro- • initially present. Based on the' probabilit)':, larger part.ides .m::i::,,: have
duced in. this process may not be the· desirable one. However. Griffith nu1m:rnus !laws and readily fracture whe'ri compared'to ·sJn},1ller pat1icles
theory is: simple and explains the size 'reduction process ·reasonably. with fe'\ver flaws. The supplied cnergy'is. used to: ,· ' .·.. . ,
Acco:rJing to Griffith theory. tl;c ainount of force to be applied lrn.:rcase new ;;urfacc area from lla\\s. , : ,,. ·, · / .. >, · · ·,�
depends o'n the crack length and focus o f stress at the atomic bo11J of the Initiate tlaws._or crad.s in the P?l1i7)c-. . : ,, :·:' . ,
crack apc>i:·. This relationship may be mathematically expressc�I as: This phenomenon is observed generally in- fine gri11ding._ · ', · ,· ...
•I 0
1'
· ' ', .. , ·�· .,,' /!j , '.· f 1, .'>·I *t

. tv!ost efticicnt mills utilise less th::in l % of the ·energy input to

•{'.( (I) fracture particles or create new surfaces. The rest of energy fs dissipated
in: � .''
where T= tensile strength. MPa
I. Elastic deformation of �111 fr�.�\µf7·� p��{isle.�.. :: .. _'.'
Y"' Young's modulus, MP�
'2. Transport of mat_erial jwithit�.,the. millin_g,..ch , �rnber., ,
·c-;: surface energy of the wall of crack, J/m2 3. Friction between• th'e'particlcs. · ' 1 •·', ·.,' . l , � ,
·r '= critical <;rack path requjr�d for fracture: m · ·
4. Friction between the particles and mil!.
(' , '. , , I'· , - , 1 I , (

.
A' linear n:lationship (equation I) between the squan.: or tensile 5. Heat. , , .,,· ·,; :,i-"'' ·'. ,': ·,.•.·i)·\• :,: ''
strength of minerals and the critical· height for drop weight impact 6. Vibration and Boise. · ·
.,;::,
-suggests that the square of,tensile strength is a useful criterion of impact 7. Inefficiency of transmission arid motor.· ;·Hi:J"l; ._. 1 ,,1
· fracture. ,: . · . .
. Fncrgy input and utilisation arc important faJtors, �o estim�tc, th�
(2) _If tlaws are not present in' a particle: tl\c force 0f milling etlic.ic11cy of a mill for a give� n1:1�crial. . A numben.of theories has been
produc�s riew flaws. The useful work in milling is proportiimal to the proposed to establish a rdationshiµ,.hdwecn cnerg)1 input: ttnJ _the dcg�ec
.
· of size r�duction produced.

.•
 172 l'I IARMACEUTICAL ENGJNEERING 173
.. ,
Ch·6 SIZE REDlJCHON '
The cnerg)'. required to reduce the .size of the pa11iclcs is inversely shape is proportional to the change in particle dimcnsion_s. Accor<ling to
proporii0nal lo lb' !size· raised to sonJc'·powcr. This may be expressed Bond's theory. the equation can be written as:
mathematically as; ,
:JE I :-C I I
! -- -- -�-1 (2) E � 2Kn. ( fT -. ---) ,,','
I
(5)
lei;
•

di) IY \ d,,
..
'.
where E' :, amount of energy (work .'clone) when!. Ku -= Bond's work index. energ/ per unit n�a�lkW '. {'Jµm'
' required to produce a change.
.

kW·h- ., d; = initial diameter of particles. µm : ·• "· .

,-�:., . '·�.,;I :, .
;U "' size 01 unn mass, �1111
1('./
d11 ,,: new diameter of particles; µm .. ';
C '-" co11stant. W·h
11 = constant
!1011d's work index i; the work required to red.t.icc··a:·u.nit.weight from.
�\ th•:oretical infinite. size to 80% passing I 00 �1m .. According' to this
Equ;ition
.
(2) . may be written (when n '" I) as: theory. the enc.:rgy used in crack propagation is proportiona.l to the new
. •)
';
,,,. . �rack length produced. This law 1 is usefHI for rough mill .s1zing. The
1:
£0:(/11(�---) work index is us.eful for comparing the ernciency of mining. operations.
t

(3)
•

Q
cln ·,:·,· ,_.
. I

Kick's Theory
"", '-� ,' 1?:'·'\

• ' where dj't-=. size of the feed. pm , . : .' :.. ; v,�f .·

d,; =- size of th� product, run · According to the Kick's theory, the energy usect'.in deforming or
fracturing a set of particl�s of e,quival�nt shap\! is proporti9nal · to the
In cq�1ation (3). (�//d,,) is known ;t0 redudion ratio .. Tlrn .us1:fulncs� ratio of the change. in size.. rt niay bt; ·�xprcssed as:
of �qu.:iticm (3) is that it satisfies ,·arit1us la,vs proposed. These· an�:
� ·� . ', . d;' °
\',e . .-· -·:··
E = KK In -­ '/ ., ... •·.
.FOr n·\; 1.0 .. equation (3) hcco111e's Kick's la,v (6)
For n �. 1.5. c,iu::ition (3) bl!comc's Bond's law
For n ·"- 2:0. equation (3) becomes Rittingcr's law ' .·
dn
,·
where KK:: Kick's constant, energy per unit mass,. kW·h·
J ',, ..
Rittinger's Theory ·ie.•
. d; == diameter of the p�uticJe-in the initial s.tage, µm; ,:
d,, .= diarnetcr of the· new parti�le, pm ,,,.,,if,' . '' ·!''
Acc(lrding to the Ritti,igcr's hypc�thcsis. energy. E required for size
'.
reducti1)il of rl\nil mas� is dirct;tly proportional to the new surface area The Kick's proposal wau��cveloped on a"·sfr�ss.:.strain' diagram for
produced.' It is''cxpressed
. as: ·. cubes .under c�1ipression. It assumes that, the material' has flaws distribr
,,., 1t,. ·.•
uted throughout its internal structure. For crushing' (compression) of
E ..., K1dSn -- S;) (4) large particles, Kick's' equation (equation 6°)ds more usefuL· .w
where S; =- initial specific surface area, µm 2i11m 3 . 'the ,cbnd,ition that all
Equations ( J, to 6) apply preciselio!1iY ":Inder
S11 = new specific surface area;' µm2/µm 3 the energy is transferred into surface energy': ' .. . ,, ' : ::,•·. " '
. K; = Rittinger's constant, energy per unit
. area, k W·h./�1m
3 I
• ''< I •! ' '� I 1 ' :i '• .r .f . • I ', '· • ' ' ' , _I • ' �• J ••

Size reduction of a material is· alone not sufficie.pttq'_ obtain powder

f

E= I
amount :of energy (work done), kW·h,
,· ' ' .] .. of desired size. It is followed· by separation.,., Sev�(al . equipment
It is mostly applicable to brittle material� undergoing fine milling. described earlier also include . sieves or: screens as inf' ogral parti. How­
Rittinger's theory ignores particle d1.:'formation before fracture.
I
ever, size separation is discussed sepa;�te ly' in the follo,�iilg chapter.
• I' I

. . I I
', . ' I '
'
fl; • •. .'J/
.1 .
'o ' • •

Bond's Theor)· . Glossary of Symbols

'
'•

According to the Bond's theory� the cne'rgy used in crack, propaga­ C = Constant or coefficient.
c = �ritical crack path required for fracture·, rn: ,,
1
tion is proportional to the new crack length produced. It states that the
energy t1sed for deforming or fractlirir\g a set of particle of equivalent
174 1'1 IARMACEUTIC:i\L ENGINEERIN(i
SIZE RFDlJCTlON 175
q --=-'Size of unit mass, �un .
.E :' -·� mount ol �nergy required to.yroduee a change in unit mass. kW·h. 15. Powders of �amc particle size thft 'arc· ohtaincd by different equipment
.
di = Size of the Iced or initial diameter of partides. ·�1111 . have s;m1e physicochcmical di:mictcristics. True or false. Justify.
d11 "'. Size llf the product or new diametl·r of thl.! parti�ks, pm. 1 (>. l.i�t 1h..: areus in which size reduction cguipmenl. is used in tablet production.
i; Surfa.:e energy of thl.! wall of"cr�1d;, .1/m::'.
17. 1\ large number of size reduction equipmcn_t is";vailable currently. Wl'!bdo
.aa

Ku � l�'.mt�· s \\' ork. indl.!x, energy pe_r uni' t lllass, k W·h·-Jµm.

Ki.;. == Kick s constant, kW·h. . · · "c rcqu ire so many types of mills?
KR,= Rjtting.er's const�nt,·k\\'·h/11mi2. 18. Size ;eduction or powders is� not possible, if particlcs;<lo not contain flaws:: ,
· · · � ·.
n = Constant. or cr;a:ks. E,plain.
•(

·,�
.
Si =- _Initial spl.!cilic surface _i.m.:a. 11�12/11111 3. 19. The classical equipment mortar anu p�stlc uses the mechanism of impact in
s 11· = Ne,{· spccilic surface· area pn\2/�rn3. size reduction. True or Fal�.c. Explain.
T, � Tensile strength, MPa. ' '
:w. FruiJ energy mill is m1:ant for ltr,·•
wet grinding. True or false. Explain.
\: =. Young·s mod4lus, Ml'a.. ·/ · '
21. [�cJucing th'.:, si1.i.: or the particles to lines leads to particle aggregation.
' . ; True or false. Explain.
.
�.

QUESTION BANK 22. Sizi.: reduction mill can also be used as mixinC!� ·or dispersion' equipment.
Each ques.tion carries 2 marks ti!' Trui.: 11r folsc. Explain.
I. It is._essential to include a sieve itr the size reduction equipment. \Vh\''!
_J. I IOI\ <locs stickiness affect the process or size n:duction?
')'

2 . 1� a hammer mill, the particle size ·of the powders is far k:ss than the �111.:sh I low docs the pr1:sence or moisture interfere with the process or. size
. size 6f
the screen. · How is it poss' ibl c.? · · redul"tion?
3. Sc��cn iype of sicv.cs gives morJf·tinc. powder than the wire 111h en sieves
25. Dir!�ri.:ntiate the mechanisms, attrition and impact in size reduction.
Why? . . . It'' .

4. Size reduction of vegetable matter is essential for the extraction of crude Each question carries 5 marks
drugs�' Explain. I. l)cscribe fo·e factors that influence thi.: sclei.:tinn of milling equip111ent for
5. It is-idiflicult to obt.1in uniform sized product during millino without the siie reduction.
. · · · • · . ". use
of:sii,:,ves. Why? . ·2. Exrlain w ' ith the ht:lp of a µiagrar� the construction and working of a hall
'
· 6 .• Fl,�id energy mill' is helter equipment for size reduction of thermo- mi 11. '
labile
suhsianccs eo�1pareJ lo hammer 1rnill. Substaniiate. 3. l::,.;plain \\'ith the help o � diagritm the construction and working of a
7. B�H_ n1ill js �ot u�eli.JI for size rcd.liciion of fi brous material. Explain hammer mill.
8. It is· possible to prevent the heat generated during milling using colloid 4. Describe the mechanisms of size. reduction. with suitable examples of
mill. How'! "1 ti.,
9. Size reduction of� mafcrial enh;}ri.ces the action of drugs. Explain.
equipmc'nt.
,,
5. What is ultra-tine grinder'? Explain the co�cept of ultra-fine grinding.
I 0. When. ,ball 111il1. is used.• size .. reduction is not obtained. Under whal 6. Dcscrib� 'micronizcr'. Describe aseptic grinding process of antibiotics.
co_r:1dition size reduction is not effective. 7. Lisi 1he laws governing. size reduction. What is work index?-
Ir l!O\\' do )'�U prCM!=nt the pfohJems of sticking and dogging of si�vcs in the 8. I lo\\' is size reduction affected in ultra-line grinders'? Describe the
size reduction? � . ,, mi:chan ism.
: ')�· .
12. List .. speci�I precautions to be· taken while thermolahilc substances arc 9. I low is energy utilised in size rcduciion accounted for?
�'

subjected to size reduction proec;;, s_.

13. The powder inust contain frwer amounts of lines when il is meant for Each question carries 10 marks
percolation process of extraction. Why? I. l:\rl�in the factors related to feed-material influencing size reduction.
14. Wha_t are the advantages of swinging type of hammer compared to rigid . 2. Describe the construction. working. adva:1tages and disadvantages of fluid
hammers? energy mill.

�:· .'
 176 PHARMACEUTICAL ENGINEE�INO

3. Describe the milling. cquipmc�,t wilh the heir,. of a ncJl diagram that �s1cs
; '' · · the principle of shear .aiHt"i' 1t1i\�t:
·'·:'lt,
4. Explain the theqrics relat1:d to' ·"1(,lbc size redu1.:tion
' , 1 • '
-t '
of a powder.
5. F:\plai!l the advantages and di ���vantagcs of si1.c rcd�clion process. ·
.
6.• State ur1d explain the laws govc'rning size reduction..
7. l)cscribc the mechanisms and i,"1 odcs of size reduction of solid drugs.
 f'Ht\RMACEUTICAL f:NGJNffRl;\{;
3. To test the efficiency of a size reduction equipment or process.
4. To optimise the pro�ess conditions such as method of agitation.
time of screening, feed rate etc.
7 The testing of a powder and equipment used for classifying has been
discussed in the chapter. Mainly this chapter is purported to provide

Size Separation adequate support to the size reduction process discussed earlier.

OFFICIAL STANDARDS FOR POWDERS

In general, powders are vaguely described as coarse and fine pow­
Official Standards for Powders
Sieves
ders. However, it is essential to identify with some guiding specifications.
Modes of Motion in Size Separation lndian Pharmacopa:ia has prescribed standards for powders for phar­
Sieve Analysis - Testing of Powder .
Equipment for Size Separatir.n maceutical purposes. Accordingly, degree of coarseness or fineness is
cx�ressed with refc;.rence to the nominal aperture size of sie·,e through
.
which powder ,s able to pass. The relevant grades of powders and sieve
Size reduction of a solid material never gives particles of same size, but number along with nominal aperture size are shown in Table 7-1. · The
gives pa,ticles of varying sizes, i . e., distributes in different sizes. Thc5e IP 1996 specifies five grades of powder.
materials must be subjected to a separation technique to obtain narrow
size ranges. As far as possible size separation is included as an integral TABLE 7-1
part of the size reduction process. When particle size distribution is to Grades of Powders and Sieve Number
be controlled for the official specifications, size separation assumes along with Nominal Aperture Size as per IP
greater importance and has to be handled independent of the size reduc­
Sieve 1hro11g'1 Non1.:·w/ Sieve lhrough Nominal
tion.
SI. Grade of which all mesh which 40% mesh
Size separation is a unit operation that involves the separation of a :Vu. powder particles uperture particles aperture
mixture of various sizes of particles into two or more portions by means must pass size pass size
of screening surfaces.
I. Coarse pm\'d�r 10 I. 7 nun 44 355 pm
Size separation is also known as sieving, sifting. classifying or screen­
ing. This technique is based on physical differences between the pnrticies 2. ivfoderatcly coarse 22 710 µm 60 250 �tm
po\\dcr
s.uch as size, shape and density.
1. 1\loderately fine H 355 pm 85 180 µrn
Screening is a method of separating particles according to size alone. powder \
Particles can be separated into individual sizes using sieves. The final
4. Fin� pO\\dcr 85 180 µm
portion consists of a more uniform size. The material that remains on
the given screening surface is known as oversize or plus material. The 5. Ver:, line po\\ Jcr 120 125 i11n
matetbl passing through the screening surface is known as undersize or
minus material. Size separation process (or sieves) can be used: Coa�sc pow?er : A powder, all the particles of which pass through a
. \\rth nominal mesh aperture of 1..70 mm (No. 10 sieve) and not
C't!n'.
s1ev;;
I. As a method to determine particle size and size distribution,
1 ,1'.o:e th:tn 40.0 p�r through a sieve with non,1inal mesh aperture of
which arc useful in the production of tablets and capsules.
.i)) �m1 (No. 0M sreve) 1s c::ilkd co,mc powder.
2. As a quality control tool for the analysis of raw materials such
In a simi lnr \\:l)'. ntlier definitions can be wdtten for the contents of
as griseofulvin and aspirin.
il1·? lark 7-1. When fineness of a powder is described by means of a
-12 177
 il'l

Ch· 7 SIZE SEPARATION 179

number, it is an indication that all the particles of thC? pa°wder shall pass
through the sieve of which the ndniinal mesh aperture •
in µm, is equal to
1 • •
that numbc.r.
Normally, for compound powders, fine powders are preferred, while
moderately coarse powder is .used fodhe preparation of tinctures. Coarse
powder without fines is employed in ''percolation process. · ·

Tht; above mentioned terminology has applicatio.ns in the production

of galanicals. A few. examples are given in the Tab1e 7-2.
The. pharmacopa:ia has prescribed upper and lower - limits for the
three coars�. grades of po-.vder. ·. For· two fine grades, the pharmacopreia
has presc';ibed only the upper limit. 1 • • ' I
• •
.

· TABLE 7-2
Some Examples of Crude Drugs a,nd Nature of Powder Required
Li£111id ex/rads Usefi'�/ parrs q·ade of powder
"�... '
{
Ashoka 1 S}C!Tl bark coarse ..
Nux vomirn seeds moder,atcly coarse
' \ '
Rauwollia rqpts · modcratelY. coarse
Ergot sclcrotia ' moderately fine
lpccac root fine
Ephcilr� stein fine

SIEVES
Sieves arc _the simplest and sieving is the most frequcn.tly used
1ncthod .for size separa'tion. , '1
). '

Constructi6n.
Sieves for pharmaceutical testing· are constructed from wir!! · cloth
with square meshes, woven from �ire ,of brass, l;ronze, 'stainiesS''steel or
any suitabl� materials: Sieves should not be coated or plated. .There
must be 'no reaction between the matc,dal of th�. .sieve a�d the substance
to be sieved.

Types of Sieves
The primary considerations for sieves"'are given to the size and . shape.
.
(
of .aperture op�ning. Square meshes 'arc arranged as per th� 1 �peciri.ca-
tions. Sieves commonly- used in .oharmaceutical
• I'\.: •. ' • I
processing include:
(
Woven. wire sieves .�
 PHARMACEUTICAL ENGINEERING Ch·7 SIZE SEPARATION 181
.'
'180
B olt ing cloth s iev es
Closely spaced bars (screens)
Punched plates
ves ar e . general-pur.pose· s ie ves
�;: Woven wire sieves : W ire woven' sie
· ractice. The types o f woven wire
. and wide ly· used in the· pha�macy ·p

,moo·.
sieves are :
,,, ,, · - Plai n weave "- Twilled weave
Figure 7-1. For line s i e ving,
. j

The nat ure o f sieve surfaces is shown in ieves.

ommon e xamples are hand s
metal wire woven ·sie ve s are u sed. C Figure 7-2. The configurations of punched plates or pc;f�ratcd �crcen.
mill etc., during milling: In case
Thes e are in cluded in roller mill, ball
;giv en a double crimp to preserve round perforations is preferred o ver a wire screen. The applicat ions of
of c oarse sieves. the wire is generally .. ·
screen configurations arc given in Table 7-3. ·
the alignment o f the wire. •. ' r
i
TABLE 7�3 " . . .
I Applications of Various Mfll Screen Configuratio�s
. of Perforated Screens
f'e,foration shape
Round holes ·
.
Recommended USC
Fibrous materials
Com1Jie11ts
Clogs 1:1o�c quickly; lower
(a) Plair. weave sieve .
(b) Twilled weave sieve

of sieve surfa�cs.
hole size is limited, because
of structural strength.
. Figure 7-.t. The nature
Hcrringbu11l'. /\morph&u:} and Slightly coarse powder than
n a nd cotton arc generally woven
' Bolting cloth sicv�s : Silk, nylo screen ( slols ).c .. ,ryslallinc materials equal-diameter round
cloths a re generally designated
fro m twisted multi-str and fibres. · Nylon rerforations
in different grades. Th7se a re
by the ir microme\er opening and. available Cross-slots ,\morrhous materials Same grind size as or equal
Hum-mer screen uses this type
used for the separation of fi ne p�w.de rs'. and slurri�s with sized round perforation;
o f scree ns. coarse particles· finer slot size attainable than
nerally used in handling
large. a1id round perforations.
· Bar screens : Bar screens are ge I p on and
bars arc fixed in . para. lie
heavy pieces o f materials. The
ositi
. from one
which taper m thickne Herringbone design : Herringbone. design consi sts o f a s eries of
·)leld by cross bars and spacers. Bars
ss

, because they tend to avoid bl�fi ng. � slotted holes repeated across the surface o f the scr�en. Th�se are mad e
e" n d to the other are recommended
i

s .. · .:·. at a !1 angle of 45 degrees to the length of the screen. It is prefe rred for
Gri1.zlies use this type of screen
grinding crystalline materials and for continuous 6peration. If the width
'sc�eens).: These 'are used for coa�sc
::·: p��chc�I plates (P�rfor�tcd'
0 0

l o f va rying of the slot is equal to the diamete r of a round _ho le , .it gri nds the particles
d by using a sheet meta
si.zing. The screens are prep�r� coarser than the round hole. -TJ1is design shouid no t be' used for fibrous
holes may be round, oval, squar e,
· thi ckness with perforated holes.. The materials; as. it is possible for fibres to align themselves along the sl ots
in a hamme r
o r re ctangular (Figure
7-2). These types o f screens arc used and pass through with inadequate size reduction.
mil). , ·, . .
sidual
e num be f h les a nd a s� all amou�r o f re Cross-slot scn:cns : In. this type, openings arc at right angles to the
. A plate with a larg r o o
vice vers a. l n path travelled by.milling mechanism. Th ese arc used for milling slurries,
will wear rapidly and
metal ,viii have a large capacity, but dia , a p
_
wit h
h ver 25 m lim tres in r late but not used for tine grinding in hammer mills as it clog s r eadily.
general. fo� o penings muc
il e mete
o
 182 PHARMACEUTICAi. ENGINEERING �·h-7 SI/F SU'ARATION
183
Standards of Sieves, Dimensions and Notations According to IP I 996. a sieve must conr,,or
111 to the specifications
Common standards used for sieves are: given in Table 7--L
(a) Tyler standard sieve series (in USA)
T1\J�j .I-: 7--l
(b) US standard. sieve series (in USA) Sta ncla rds for SicH'�-:-Spccifi�ations
(c) British standard sieve series (in UK)
(d) German DIN (Deutsche lndustrienormein) (in Germany"and . l11111·vxi11u,rc : i/ •pr<1.,· i,iwte /\\imiJl(i/ mesh Tolcra11"e
Europe) /1L'f( 'l'/i{i/g('
,\'{ .Iii '\:L, ·.,
aperture si=e ,11·ei·:1.�,
'fl

(e) IP standard sieve series (in India) I/ti. /Jlllllh1'/' si, ·, ·ing ·, 1rea aperfl,re s1:e
---------------------------
(f) International test sieve series (ISO) (World wide) (inm) (t mm)
Tyler and US standards can be interchangeable, since the difference
-l.O (l.13
between the two standards is less than th.e allowable tolerance in weav­ 2
ing of the screens. These are also known as l'!st sie,ves. Sie,·es used for 2.8 O.OIJ
8· -IX 2.0
· pharrriacopreial testing must match with the following specifications: 0.07
IO - H, 1.7
1. Nu�be.r ofsine: Sieve number indicates the number of meshes (),()(,

. per' linear length of 25.4 millimetres. 12 ,11 1.4 •I 0 .05

2. Nominal size of. 1perture : Nominal' size· Qf aperture indicates Ih 1.0 (l.03"
the distance between the two adjacent wires. It represents the 7
Jim 11m
side of a square aperture. IP 1996 gives the nominal mesh
aperture size for majority of sieves in mm or in pm.
37 710 ., .
-='
<)
3(, 600 21
3. Nomina1 diameter of the wire·: Wire mesh sieYes arc made I()
5CH) IR
. from the wire having the specified diameter in order to give a
II
suitable aperture size and sufficient strength to avoid distortion -125 15
12 .18
of t,he sieve. 355 13
4. Approximate percentage sieving area : lhis �tandard expresses 37 250 13 l').9)
the area of. the mesh as' a percentage of the total area of the 14 8) I RO I I (7.(,)
sieve. It depends on the size of 'the wire used for any particular 15 I 00 3<i rsp '1),4 ((,,/,)
sieve.. Generally, the sieving area is kept within the range of 35 I (, I 20 125 R.I (5.l()
. t9 40 per cent in order to give 'suitable strength to the sieve.· 17 15!1 I 0(, 7..t(5.:')
<i&>

5. Aperture ·tolerance a',·erage size : Some variation in the aper­

. I 70
:...: : '\ '.�.ture size';'"is unavoidable.-:; This variation is expressed :as II 9()

t
6.(1 (·l.<•)
1"' 1·
perc�ntage and is. known as !he aperture 1ulera11c(! average; In :no 75 Cl.I {-I. I )
.
di' , ' fact, it is a limit given by pharmacopreia within which a particu· .:'-lo - .; I .,
;() 3-1 · 63
;,· ! · ).•, (.,.7)
1

lar dimension or average aperture size can be allowed to vary ·.:>

r 300
.�;., · .53 ·U! 13.-1)
and still be acceptable".for the ·purpose for which it is used. Fine
;• :. . meshes cannot b� WOV( n With the same :tccuracy as C�arSI: •4.!i '(3.1:,
meshes. Hence, the aperture tolerance average i,s lower for
· coarse sieves than the fine sieves.
""··' )l

...... '".
184 Pl IARMACEUTICAL ENGINEERING,
Ch-7 SIZE SEPJ\RATION 185
Comparison of Ideal and Actual Screens
material may roll on the surface of the sieve. The motion is parallel to
An ideal screen would sharply separates the feed mixture in such a ·
the plane of the sieve. The sieves· can be. slightly inclined.. The
wav that the smallest particle in t.he oversize would be just larger than
reciprocating motion is induced by means 'of ari ordinary eccentric on a
the. largest particle in the. undersize.
rotating shaft. ·
· ·such an ideal separation defines a cut diameter, Dpc that makes the
point of s�parhtion between the fractions. 'Usually, D1ic is �hosen to be
equal to tile mesh opening of the screen.
An act11a/ screen is the one, which does not give perfect separation,
Figure 7-3. Motion of �,n:l!n. shaking (osi:il\ations).
about th� cut diameter.
In an ::i'ctual screen, the overlap between the smallest particle in Vibration : The sieve is vibr.atcd at high speed by me?ns of an
oversize and the largest particle in undersizc is more prono\mccd. when eccentric device (Figure 7-4) either electrically or mechanic�lly. Rapid
particles: 1 vibration is imparted to the particles that helps the powder· to pass
are needle like, fibrq_us. through the sieve. Electrically vibrated screens are particularly useful in
- tend to aggregate. the chemical industry. Example is hum-me'r screen. They handle light.
tend to strike t.hc screen surface cndwisc and pass through. tine and dry materials successfully. lnduci �g vibrations also pn:ven �
tend to strike the screen sidewise and retained. hlinding ol" meshes.
Comn1ercial . screens usually give poorer separations than fosting.
screens of the same mesh opening when operated on the same mixture.

/ MODES OF MOTION IN SIZF. SF.P.ARATION

Sc;e�ning is a method of separating particles according to si,e alone . Ele.ctric
·:vibrator
The basic technique involved is passing the particles through a series of
(a) Mechanically vibrated (bl Electrically vibrated
sieves of uniform size. In this, the particks urop through the openings .
due to gravity. Coarse particles can drop easily through large openings. Figure 7-4. Motion or screl!n� \ ib1ating motion."
but it is difficult to .screen the line powders. This process can he • I
Gyration : In this method. a sys1em is made so that sieve is on
hastened by. inducing some type (mode) of motion (movement) to the
rubber mounting and connected to a11 ect·-:ntric flywheel (Figure 7-5).
p;,\rtiilcs. Size separation is basically assisted by three methods.
This gives a rotary movement of small amplitude to the sieve, which in
'L Agitation turn gives spinning motion to the particles that helps to pass them
2. Brushing through the sieve.
3. · Centrifugal force
These modes of shaking help to shake the material so that sieving
will be quick and entire sieving area can be utilised.
} ·:
1¢>
'
I

. Agitation· Method .........

:::: Sieves are agitated in a number of ,vay"s. Some of them·are discusscu
belo\v. ,, ' · ·, � �
· '- Eccentric
Oscillation : The sieve is mounted in a frame that oscillatds back .�nu (a) Gyrations in (b) Gyrations in (c) Gyration at one end.
forth. i.� .. reciprocal motion (Figure 7-3 ). It is a simple method. but thc horizontal plane vertical plane and shaking at other end
Figure 7-S. C.yratory motions of screens or sieves.
186 I PIIARMACEUTICAI. EN<..ilNEERINCi
Gyrator)' screens arc box like equipment, either round or square. with
a series' of screen cloths nc!-.ted attlp one a_nothcr (figure 7-5). M.ost
gyratory screens ha\'c auxili.uy , ihrations caw,cd · hy balls bouncing
aga_inst tl;e lower si1rfal·e of the scrcl'll. · ·
Agitation· methods arc not contin11ou� methods. l lo,,evn, these 1:an
be madt: continuous by inclination of the sieves. Separate outlets arl'
made for undersizc and oversize partklc�. Normally. all the tlm:c moJcs
of agitati6'n arc used s"imultancousl) for an cnil'i...:111 size Sl'paratio11.
Rotex .screen works on this' principle. ..
Advantages : (I) Agitation mcthods;are incx pensive. , · ,., ·
t2) Sitnplc and rapid ..
Disad)·antagcs : (I) Agitation mcthq�s have lower limit ·or the
par1,iclc size.
C2).· lf:thc powder is not dried. apcri11rcs become d�1ggcd with parti­
cles lending to impropcr sie\'ing.
(3) During �gitarion, attrition (particles colliding with each othcr)
occurs causing. size rrduction.
Brushing Method
In this case, a bru::,h is 11�cd to 1110, l' the parti�Jes on the !-.urfacc of
the sieve and to kt:�'P the nh.·shes dcar. The brush i,s rotated in the
mkldlc in the.case of a cirl·ul;-ir skvc. but spiral brn�h is rotated on the
lont!itudinal ;-ixis in· ci:;.: <if lwri,ontal ,ylindrical sieve. One cxa111pk is
bru�h sifter (Figure 7-6). Tl;i-. is ll�l·d for size separation of J!rl',hY or
sticky powders such as waxes and ·!'IO:\p�.
Triangular
Sieve mesh
Fii,:11rl' 7-6. Brnsh sifter
Ch·7 Sl/.r SEPARATION 187
CentrifuJ!:tl Method r
In thi'.> inethod. a high-speed rotor is fix.ed inside a vertical cylindi­
cal sie•;r: so that on rotation the particles are thnzwn outwards by
centrifu!!al force. The current� of air can be generated' by means of a jd
of air into the equipment. which helps i_n srparating ·,he partides. A few
exampks nf equipment that work on this principle ar� cyclone srparator.
ai1d air :separ'ator.
• 1;,,:-
Adv;1n tag cs ;..(I) Centrifugal in ethods are extremely useful in cases
"here conventional sieving tends to block tht' sicn•s.
(2) 1:,tremely useful for fine powder. because sieves. h;-i, e ,the lirni­
t;1tinn of mesh size.
SIEVE ANALYSIS-TESTING OF POWOER
Thl' 111illed material is subjected to size separation in orclt-r to ,obtain
the pow(l:r of Ol'sircJ sizr or size distribution. Size distribution analysis
is import;rnt in different areas as mentioned below.
()nality control tool for the analysis of raw 111aterial').
·, ,·�ting the rflicicncy of a si�c rt>duction equipmt>nt or process.
I lptirnising the prOCl!SS C,:Onditions SUCp as method llr :ll!itation
� '
i1111_c of screening. etc.
"il·lc'cting the sic,·e system for commercial equipllll'11l.
F.rrn?, ,·;in arise if 1111.· ':'ievcs ,ll'l' o,·crloaJed or if insuffil.:ient time is
allowed ,·nr the particles to pass through.
Sieve Shaker Machine
Prinriple.: lhe pmvclercd drug is-separated according IP its particle
size usi1:1• a numhl'r of sieves in a nest. These are subjected
. to diffcrent
types 01 agitation, so that size separation is rapid. "
Con'\truction : Standard sieves of different mesh numhers arc. avail­
able comn,l'rcially :is p1:r the specifications of IP and USP. 'I hese sieves
arc 1i:wd in a mechanical ..;haker apparatus (Figure ' 7-7).
Working : Sieves arc imangcd in a nest with the coarsest at the top.
A sampk (50 g) or the• l'(lwdcr is placc:d on the top sievr (Figure 7-7).
'This sil.'1�· set is fixed In 1!1e mechanical shaker apparatus and shaken for
a l·crtain perioJ of tim<: 12() minutes). The powder retained on each
sicvc i� wcighed.
Pral'liral considerations Care should be taken in. 'o�der to get
rcprod1Kihlc n:sult<.. · The type of motion int1uences sie ..·ing; vibratory
 ·.:...a .

188 I PHARMACEUTICI\L ENGINEERING

C'h-7 SIZI: SEPARATION 189
(3) During shaking, attrition (particles colliding with each other)
occurs causing size rcduction of particles. This leads to error in
0

0
r_ ,
.
estimation.
Sieve No. .i-.-+-+-'- Coarest sieve
Va ri�rnt� : Electro111agnet!·c sieve -shaker-It is useful for analysing
Sieve No. powders ui1der co.ntrolled conditions. Sonic sifter - This apparatus
Sieve No.
utilises sonic oscillations: A mechanical pulse action is used to reduce
blinding and agglomeration in the sub-sieve sizes.
4c.. ... Sieve No:
· Alpine Airjct Sieve
Sieve No..''·
Principle : In the Alpine ni.rjct sieve, sicNing action involves the
Sieve No. application. of' a jct of air on one side of the sieve and suction on the
Sieve No. other side. The material is maintained in a fluidised state on the screen
Sieve No. Finest sieve by a stre:1111 of air. · Vacuum is applied below the screen. so that the
undersized powder is sucked through the sieve.
�-+-+-- Receiving pan
Construction : The construction of a Alpine a.irjet �icvl' is shown in
Figure 7-8. It consists of a metal housing into which the sic\e mesh is
• '"J fitted. Sic:,·c" cover is placed in such a way. that :m air-tic.� ht. seal is·
'

On/Off obtained. /\ slit is providl'd such that its upper edge is in level with the
0 upper cc.lrl' of the housing. Provision is made to pass. airjct below the·
slit. Suclion line is provided below the sieve, which can he controlled
with the help of a manometer.
Coarse powder
Figure 7-7. Laboratory si�vc shaka machine.
motion is most efficient, followed by side-tap motion, b0ttorn�pat Sieve mesh
motion ' rotarv� motion with tap and finally rotary motion. Th1.: type . or r '
motion and i11tensitv of the shaker arc fixed and standardized. Shakers
are commercially a�aiJable. .
Other factors arc weight of the sample and duration of shaking.
Siev.es produced by photo-etching and electro-forming tedmiques ar" Fines
· US!!P to get a better estimate of the size distribution analysis with a lower
limit of estimation of p�rticle diameter 5 µm.
Vacuum
Advan.tagcs : . It is inexpensive, simple and rapid with rcproduciblo connection air flow
to manometer
result�/·
, Disadvantag'cs : (1) Lower limit of pa,ticle size is 50 �1m. Figurl' 7-8. Coris1ructio11 of Alpine ai�jct sieve.
(2) If powder is not dry. apertures get clogged with partidcs, lead• Working : A small amount of po\vder (about 10' g) is spread on the
ing t,� improper sievint:. sieve. Tl1e ·cover is placed in position. The slit is set into rotation by
sending a jct of air from bcloh•:1 .The powder is fluidised in the upward
 190 I
PIIARMACEUTICAL EN< ,INl'l:RIN(J
jet of air. The suction is adjusted until the manometer rl!ads abou\ Ch· 7 SIZE SEP,\lv\ TION 191
27 kPa. The vacuum (in the interior of. housing) sucks the undersized
material of constniction. The modes of size separation are discussed
powder through the sieve. The material is rccover.ed.
earlier. Some factors to be considered arc:
Sicvi11g is continue.ct for two minutes and the residual powder is (a) wear of the sieves.
weighed. This powder is transferred to the next sized mesh "ith a tin" (b) blinding.
brush. This process is continued until all fractions arc collcctcJ from the (c) machine noise.
sample, by changing the sieve meshes as wet! as magnitude of th..: suction.
General· Classification of Screening Equipment
. I . I t

Uses : Alpine sieve method is used for the anal)'Sis of powd..:r for ill
size dist�ib1ition. This method is particularly useful in ca:,cs where
conventional· sieving tends to block the sieves below
� .. . . about. . 80 �ml.
Ad,'.antagcs : (I ) In Alpine airjet' sieve, tluidisation of lllmJe� pre•
vents blocking of the mesh.
(2) It is a rapid method.and gives reproducible results.
(3) It is very useful for line powJers.
Disad,·antages : (I) The capacity of Alpine aitjet sieve is
Therefore, it is not useful for large.scale separations.
(2) This method is tedious. bt:cause each time only ·one particle size
powJcr js obtained.
. Data Presen.tation
Frequently a pov,der is assigned by a mesh number of the scree
through which it passes or on which it is retained. It is expressed I
terms of arithmetic or geometric mean of thc: two sic:ves, i.e.. a powd
passing through a.36 mesh and retained on 44 mesh sieve is assigned
a_ri'thmetic mean diameter' 0((425 + 325)/2· cir 375 µm. This is report
. 'as undersize.
The screcning or sieving machines· may be divided into difl'erent
cl.isses.
(I) Ciri::lcs : For coarse matcrials above 50 mm - large lumps.
(2) Re\•bfring screens : Separations above 13 l"':m ·- trommels.
(3) Shaking .k.,.l't.!11.1· .: Separation from 13 mm Jown \�:ards to tines.
(4) Vihratin;.: scrcn1s : Coarse size ( 13 mm) to tines.
(5) Oscillutin� scr<!ens : Fine mesh size.
(6) F/11iJiseJ systemv : For vcry fine pow1krs.
Some important equipment ar� d�scribcd bclow.
Shaking Screen
PrinciplJ: : Particles of different siz�s are scparate·d by pas�inl! the.a,
through a sieve. which oscillates to and fro continuously. · · ' �
:· Hanger
,
�/ rods 1'
i

.m
Sieve
Data Analysis
The ·weight of sample retained on each sieve is consid�r�d
analysis. The_ data are analysed for normal, log·normal, .:umulatl
percent frequency distribution and probability curves. Along with th ·. · · Discharge
, .different mathematical expressions are also used such as ave.rage partl Figure 7.9, Construction ofshaking scr�cn i�· i�dincd position.
diameter. gcometric mean weight diameter etc.. For, further anaiysis ns ·,

Construction : The construction of a shaking ·screen is shown in

the book, ''Textbc)()k (�[ Physical Pharmaceutics" by C.V
Subrahmanyam, Vallabh Pr!,ikashan, Delhi.
EQUIPMENT FOR SIZE SEPARATION
A wide variety of equipment.have been developed differing in
scale of operation, ruggedne. ss, method of movement of material
Q • ..,
Figure 7·9. Shaking screen consists of metal frame to·which a screen is
fi�ed at the bottom. The screen cloth may be· riveted directly or fitted
us1�g a remov�bl� b?lted fra °:e. The metal fra.me can be arranged
.
horizontally or in inclined pos1t1on.
_ It is suspended by means of hangt:r
rods, so that 1t can move freely. · The side of the metal frame is
.
connected to an ordinary eccehtric on a rotating shaft. The entire frame
can experience reciprocating motion.
r
192 I Pl IARMACEUTICAL ENGINELRING • Ch,7 SIZE SEPARATION

Working : The screen is allowed to shake in a reciprocating motion. arc col lccted separately at: the outlet p9int.
193

The feed (material to be screened) is introduced on to the screen from a

side. Therefore, fii1e particks get screened off initially. The remaining, Screen of certain size
material moves forward during the motion of the frame and gets sepa­
I.

�- l
I

rated. Thus. the desired size particles can be obtained from the material. Wooden -.r-\;--�::::= -;::; . ·s·ingte
The ad\'antagcs of shaker scree1i arc that it requires low head-room block _L..l'Q__...r\ lf'Q � Rubber J· screen
L-.1.� .--- .. ' b; a ll
and low power requirement.. T · =:::::-:
- =r=. �-.... := ··system
Supporting screen· · · •.
•
1·

Th/iisadvantagcs are that shaker screen ..requires high. cost of (Coarser than above screen)
maintenance ofscreens and supporting structures. Its capacity is low..
Variants : The ·above s�rccn system may be vibrated to keep _the
(a), Unit sieve system
Feed
"" 1: '" 1t,'( · , , . , · j

particles ·movmg and to prevent blind mg. It is used when larg\.! capacity'
and high efficiency is desired.
Rotex �crccn
Principle : Rotex screen works on oscillating agitation (back and Eccentric bearing
forth) by means of an eccentric n,echanism. Further, vibrations arc ...-.
caused by balls bouncing against ·the lower surface of the screen cloth. Sliding bearing
This rapid motion helps the particles to roll on the surface of the sc1wn Fir.e screen .....
and separate out.
Construction : The construction of a Rotcx screen is shown in
Fi�ure 7-10. The screen is slightly inclined at 5 dcgi'ees. A coarser
surporting screen is placed hdow a coarse screen (Figure J-.!Oa).
Between the screens, wooden blocks are placed at di ffcrent interval!:>. "Fine Coarse
siz:,e size
Between the wooden blocks. a number llf ru_bbcr balls an: placed. This,
two�sieve system represents one ur'1it. Several such units arc arranged il.1 (b) Assembly .,;r;

the descnding order, i.e.• sieve of larger size at the top arid smalkr one at Figure 7-10. Cgnstruction of R9tcx sc�cc
the bottom (Figure 7-lOb) .. Uses : Rotex screen is used for handling a ·variet
n.

. y of chemicals
If more number ofsicvc sizes are desired. 11 screens arc flrrangcd in a usually dry materials . G�anular matrices and powdered· foods are
_ also
simila� manner to obtain (n + I) fractions. This asscmblY;' is supported size separat.e� by R�tex sc_reen.. T erefore, these are,
_ � tised exte.nsively as
on sliding contacts at the low�1 end. The upper end of scrccn system is standard eq�1pment m p1any c�em1cal �nd pr�cessi
r;ig plants for
connected to an. eccentric pin on a tlywhccl. fine separations. • •· · ' - " · · · ·. ·· hand
· ling

. Working : The screen sy::;tcm is allowed to �gitate with the help of Cyclone Separator
eccentric. The shaking motion of the �crcc11 cau�es ball� to fly bctwcen Pri�ciple : In cyclone separator, centrifugal force
the screens. As they strike the inclini.:d sides of the wooden blocks, the _ is used .to separate
the �0!1d� from fluid s. The separation process depends not only
balls deflect upward and strike the underside of the screening cloth and part1cle on the
_ size, but also on the density of particles. Depending on the fluid
thus prevent the blocking of the mesh (Figure 7- I Oa). The feed· is vcloc.1ty, the cyclone separat or can be used to separate all types of
_ _ . _
introduced at the . elevated end of the screen. Th'c material passes pa1 t 1cles. It 1s also possible to allow fine particles
fl UI_ d • ·to be carried by the
through the upper screen and reaches the next screi.:n. This process
continues uritil a\l the material is separated into fractions. Th1.r fractions . ... I I •

I
194 I PHARMACEUTICAL ENGINEERING
•Construction : The construction of a cyclone separator is shown in
Figure 7-11, It consists of a short vertical, cylindrical vessel with a
conica� base. The upper part of the vessel is fitted with a tangential
inlet. The outlet (solid outlet) is arranged at the base. Fluid outlet is
provided at the centre of the top portion. w.hich �xtends inwardly into
the separator. Sµch an arrangement" prevents the air short-circuiting
directly from the inlet to the outlet of . the fluid.
Solids
outlet
Figure 7-11.• Construction of cyclo!1C scrarator.
Working : The solids to be separated are suspended in a stream of
gas (usually air). Such a feed is introduced tangentially at a very high
velocity. so that rotary movement takes place within the vessel. The
centrifugal force and vortexing throws the solids to the walls. As the
speed of air. diminishes, the particles fall to the conical base and arc
discharged through the solid outlet. The fluid (air) can esc.ape from the
central outlet at the top'.
\:Jscs : (1) Cyclone separator is used to separate the solids from gases.
(2) 'It i.s also' us�d for size separation. of solids in liquids.
(3) It is used for separating the heavy or coarse fraction from fine
dust.
Variants : Cyclone separators are also used for size separation or
1rsolids suspended .in a liquid such. as water. Such separators are known
. a:s we(.!or liquid cyclone. One· such apparatus used ·for this purpose Is
:vorfclone. ·,
··· .. • '·
·.Air Separator
Principle : In air separator, centrifugal force is used 'to se�arot
solids. The air environment is obtained by means of rotating disc an
Cl,-7 SIZE Sl:l':\RATION 195
bl:idcs. To improve the separ'i1t\on, stationary blades are used. By
controlling thesc""bladcs and the speed of the rotation, it is possible to
vary the size at which separation occurs.
Constrnction : The construction of an air separator is shown in
1-'igurc 7-1 ::?..• It consists cf a cyli,;drical vessel with a conical base. The
foed inkt is titted to _thi.: upper p.:111.of tho vi:sscl. The rotating disc and
rotatin� blades an: att;1ched to the central shaft to produce air envirot�­
lll<:lll. At the ba:,c of the vcsSl'I, two· outlets are provided; one for fine
particks and the other for heavy particles.
Feed inlet
Rotating clisc
Rotating bl.?c!e,
Outlet for
fine r,articles heavy particles
Figure 7-1 ::?. Construction of air separator.
Working : The disc an(] blades are allowed to rotate by means of a
motor. These produce a current of air as shown by the arrows. The
sample po\.vder is introduced through the feed inlet: The feed foils on'
the rotating disc. The tine particles are picked up and carried in.to space,
where air velocity is sufficiently reduced. The fine particles are dropped
and arc ultim�tely, collected at the outlet mea.nt Jor the fine particles.
The heavy particl�s·, which, fall downward, ari �emoved at .the outlet
meant for heavy particles.
Uses : Air separators are often ·attached t6 the ball mill or hammer
mill to separate and return over sized particles for further size reduction .
Bag Filter
Principle : In a bag tilter, size separation of tines (or dust) from\ the
milled powder is achieved in two steps. In the tir:.i step, the milled
powder is passed through a bag filter. (cloth) by applying the suction
. on
,.
 I
C'h-7 SIZE SEPAR.t,.TION 197
I
196 PHARMACEUTICAL ENGINEERfNG .
bags. In the subsequent, s' tep, the bags are shaken to collect the fines 'that
the opposite side of the feed entry. This facilitates the separation. I� ,the arc adhered to ,the bags. These two steps follow in succession and are
next step, pressure is appli�d in order to snake the bags so that powder controlled. at different intervals, with the: help of a beW'crank lever
adhering to the bag falls off, which is collected from the conical base. arrangement..
.is shown i n Figure .7·-
, . I .
.
°
Con�Jruction .: The construction of a bag filter
_
Bdl crank lever urrcmgtJmc.•111 : in this mechanism, 'a sh"afi ��ith a cam
13. It,consists of a number of bags ·made ot cotton,or wool fabric. 1 is allowed to rotate at a lo,w speed. Durmg rotation, the.cam can either
These are suspended in a sheet metal container. I' press the bell crank lever or does not come into co11tact. Depending on
this mechanism, the damper changes its position. The damper is a useful
Discharge
Low speed Damper ·· manifold mechanism, which allows the two steps to occur as_ shown below.
shaft
Movem�nt of damper
Step · A-lechanism "Contact between (:on/act b{!tween
bags and suction. bags a.nd atmosphere
Filtering Cam docs not press opens closes
period the bell crank lever ·
(Figure 7-13a) ' . ·, . ,•I',.
Shaking Cam presses the closes opens
period hell crank lever
. Filter bags (Figure 7- l 3b)

Thet;e changes occur at intervals of a few minut�s.

C> ··�· . -..·,
Filtering period : The exhaust fan positioned at .the top �ecps the
bags under les's pressure t1;1an atmospheric pressure. 'The gas containing
fine particles ( or dust) enters the hopper, as shown with· am;)\�S in· Figure ·
Oust hopper 7- I 3a, and passes up. The gas feed pass es through the fabric of bag.
. During this process, the fines (or dust) arc retained in 'toe· bags, whil� the
gas reaches the ·top·of the casing. Because of air, the bag' remains taut
during filtering operation. ,, :.,: ·.. ·.i, , ..:'-

Discharge Product Sh:1kif1g period : Since vacuum is cut 'off i� the chamber, ;air from
· manifold dis�harg.ed outside enters the casing and passes through the bags.• This results in
(b) Shaking period violent shaking of the bags: sp that the dust and fine particles ar�
(a) Filtering period displaced from the bags and falls into ·the :conica\:.base. '1 It is·· then
Figure 7-13. Construction of bag filter. removed at intervals. • . ' . . • f )I � .
Such devices are entirely automatic in· their action. and can· be "'de-
,

A '110ppe.r is arranged at the bottom of the filter to receive the feed.• signed t6 affect very large filtering surface per unit floor space.,,. ,
At the top of the metal container, a provision is made for the exhaust. .
'l 1
.., •J
Adj�ccnt to this, a bell crank lever arrangement is made . to bring the Uses : Bag filters arc used along with other size separation e'quip-
filte�s to normal atmosphe'.ic conditions. · ment, for example, a cyclone separator. Bag filters, are used to remove
_ _the fines from cyclone discharge. Bag filter i s connected to the dis:.
· Working : The wor.�ing of the bag filter consists of two steps. In the charge end of the flu idized energy mill.
first step, the feed is separated from air by passing it through the cloth i
1) I '!_�; I'
198 PHARMACEUTICAL ENGINEERING

Advantages : ( I) Bag tilter is extremc)y useful for removing fir1es,

which cannot be sep::m1tcd hy other methods.
(2). These can be used even to remove dust. The ordinary household
vacuum cleaner is a simple_ bag filter.
Dis:idvan;age : Bag filter is not size separation equipment as such. '
Mixing··
QUESTION BANK

Each qucs .tion carries. 2 marks

t. Name the standa�ds of screens used in pha1maceutica! practice. Section I-MIXING OF SOLIDS·,···
2. What are standard sieves? lnterparticle Interactions-Segregation
Mechanism of Mixing in Solids
3. Diffrrentiatc ideal and actual screens. Mixing Process-Steps
•i_ List th<.' spcci!icatiotis aml standards for siev<.'S. Degree of'Mixing and Statistical Evaluation
5. 'Explain the term blinding of screen. How is it prevented'? Factors Influencing Mixing
Classification of Equipment for Solids Mixing
6. What arc varil,uS grades of coarse powders'! Dc(ine them. Equipment
0 . - • .
7. Give the dassi!ication of fine pom.lers with del11111tons.
8. What :m.: the advant ages of cxpr1:ssing sieves by a sieve number over the .. .
I Mixing is .defined as a process that tends to result in a randomization ·of
nomin::1 size of ap•:rture'? dissimilar particles within a sy�tcm.f,
9. Diffrrcntiate t.he t.:nninnlogy, nominal size of aperture and nominal diameter ,: ,'. :
of the wire. (Ihe term mix means . to put -togeth�r ·in one mass or as�cmblage with
more or less thorough diffusion of tht: constituent eleme!'lts amon!k,one
Io�· \\'hat are the uses of screen analysis? How is it exprL·ssed'?
� ..,.. another.) Thi! term blending means · to 1nix smoothly and · inseparably
11. List th·.: methods of sieve analy:;is used for tt:�ting the powds:rs. Ciivt: their togc;hc'r. During blending a minimum energy is iJnpa�,ed �o the bed..,
n:l,1tivc advantages.
These terms arc commonly ,i:1scd interchangeablyjn�the indust ry. '
• ' • • f. ·l ., '
Each question carri-:s 5 marks Some of the mixing operations io·the dispensing,practice are spatula­
I: E:-:olain the working of a cyclone separator and its uscfulnt:ss. tion, tritµration, tumbling, geometric dilutio� etc. How-�ver, 'industrial
2. De.scribe the mc1hod of -:;ize scp.1ration using a Rotex shaker screen. pharrnaceuticar'mixing involves large-scale'tquipment. A major 'compli­
J. Explain various grades of powders oflicial in pharm�c�paaia. cation i;i· the intimatt: mixing 1Hf';particles· is 'the segregati�n·of part.iculate
'4. Give details about t_he various standards fixed ·by the pharmacopa:ia for
sol ids that res.u'tts from gravitational 'effect on· the agitated° bed. Mixing ..,
can also be achieved· by millfog. kneading etC':\··, :, ',, 1 '. ·" 1 ••, ·• :
l
sieves. •
,1
... . •
I
.: •• f ·: .:,,• ti ,

The diverse characteristics of pa�icle�, such as. si:2e, shape; v9l�me,

,·
j

·, S. Describe the spedficalions of standard sieves as per IP. .

surface .;irea, density,. porosity, flow . and
' charge,
� contrib' ute to the ' solid.
Each question carries 10 marks mixing. It is difficul t to predict .the inter-;particle · .
• interact ions: .There;.
I. Describe one industrial method for size separation of a. powJcr. and its
,
fore, some empirical correlations are possible. In. practice,
· l :.1 ·• , , • ,� ' J•
..

optimum·
applications. mixing is considered satisfactory. · '· 1
' ,,
Depending on their floy,: proper ties, solid� ar_e. diyided · into
twC'
cla�scs; cohesive and ....wmcohesive. Noncohes[ve mater: als s��h
J as
gr�i.p.'. d..1)\.3.�.Dcl.and .pl.!stic .chips readily flow ·out of a bin or
.._�
' '
,. I• o'
silo.
,..,.. • ' I '

199
 Mixing··.,

··section I-MIXING OF·SOLIDS· ·'.,"'·:., ,.,;; :d

��·--���-·��-'--��������--,-,-���-,-�-·�
! ·_, ��-

lnterparticl� lr;i!eractions-Segregation .
Mechanism of Mixing in Solids
Mixing, Process-Steps
· Degree of' Mixing and Statistical Evaluation <'
·•· · ''Factors Influencing Mixing
.. _ Classification of Equipment for Solids Mixing
· Equipl')1�nt

I Afixin'g is :defined as a process.that tends to result in :a rai:idomization,·,of

.Ji '

dissimi!ar1particles within a sy$tCm.,{ , .·.

(.rhe teri11 mix means to put 'togeth�r 'in one mass or as�c'inblagc with
more or lcs�. thorough diffus ion .of tht:: constituent �lem�!lts..:aiJ10n�ne
another) The term blending means· to rnix smoothly a.ndi. il}separably
togqhc'r. ' During blending. a minimu� en�rgy. is ynp�rt,eq_!o, the bed.,.
These terms arc commonly .ihcd interchangt!a,b.ly,,in th.e ipdu�t ry . . T'·•
'
, '. ' •.. •' . . I ' \(. � • • ,.'.,',. , ;•,

. Some of the 1:1i.xing operations' ,�Q:the, dispc.n�jng'. prac::t_i,ce,?.�� spatula­

tion, trituration, tumbling; gyometric dilution etc. However, industrial
pharmac�utica(rnfx i�g' invo 1,,es large-scale iquipment:. ·. A 'majo� 'compli­
0

1
cation f1�:the inti111ntc mixing 'Hr�pa�ticles· is 'the s'eg1'egati�n·of particulate ·
so) i1s tl;at res·� ts froril°'gr�vi�atio'n al, ',ef�ect, on''t,1�e ag! t��l� ''�ed l� i�i�g"
. . . . , :, :
can also be achieve� �y m11lmg, kneading etC':\' · ·i · :. ·· "• • '',' .";

.' . ;,i'.Ji . -j ,";_11\i-11,·�· I 1•·· ':;q_ ··.· · ),\; II,>";.:·' ·, : • 11i

: ,, '.

The diyersc chara�tcri�tics ·of parti.cle�, .sucjl, as srz.e,;.shape; v9lume,

,

surface . .:.ir�a, dl!nsity, porosity; flow_.a11,d ch�rge, .cqi:1trf9ute �� t�e· splid

mixing. His difficuit �o. predicLthe inter�particle ,int��a�tions:'' .'The. re;,
fore, some empirical correlations are possible: In .practice,' ·o,piirri�-m ·
· · ' ·i
rni:d'ng is considered satisfactory: ·'
" •

. , , Depending, on their fl o.� properties,' solids . ar.e di�id�d: ,;t� c­ ,tw

clas.ses; cohesive �l/,9 �ncohesive. , ·,\�o;�c�/1es[,•e. --�za/�r:J�fs .S�(?h, as
gra. 1. <:l_cy
- in, -�-
. .
,,. sanq_.,�nd p l::!stic.. cJ 1ips0_.,r.cadily flov,', ·out ,.of, a bin or silo.
' " ·• . ' ,i,'li -�····'· ! ( ...�.'� , :;i:·· · • . .. 1

, , I) ;'; \? .J\ I

199
 .I

200 PIIARMACEUTICAL ENGINEERING Ch-8 MIXING 201

, l

Cohesiv� materials such�-�et cl_ay are cha,racte�ised by their resistance INTERPARTICLE INTERACTIONS-SEGREGATION
to flow through openings. The particle characteristics such as size,. size distribution, shape and
! \ '

There are significant differences between solid mixing and liquid surface in0uence the interparticle interactions in a powde.r bed.
·
�These are given below. Inertial Forces
•• i- '

�-liquid mixing Solid mixing

P.:'.w currents arc responsible for
transporting unmixed material to the
·· mixing zone adjacent to impeller.
Truly homogeneous liquid phase can
be observed
�
'_.,/'5 mall sample size is sufficient to
study degree of mixing
tixing requires low power
Flow currents arc not possible.
Product often consists of two or
more easily identifiable phases.
,, Large sample size is req.uircd
Mixing requires high power
Inertial forces 'tend to IJ.gJd nei�hbouring partkle� in a 'fixed relative
position. These are van der Waals, electrostatic and surface 'forces. A
special mention of surface forces is relevant._ , ·,., ·, :.,ii·.' ; . :'.:····:,_:,.
Surface (�� interfac�f fo.�ccs : The ·cohesive forces pre�ent intimate
mixi'ng O\.'r:ing to iriteractioi1 of their stirfaccs (or :interfaces))•'Frictional
forces also resist'ihe tnovement of particles so that' they tend to form
lumps. These dep.end on sur:face area, surface roughness,. surface polar­
ity, surface �harge and adsorb.ed substances such as moisture. During
I

mixing, the particles develop surface charges. Surface charge; produce

r··
Mplications .
•Mixing is one of the most common pharmaceutical operations. It is
involved in the preparation of many types of formulations. Mixing is
particle-particle repulsion�, which make random mixing impossible. For
• �ffective mixing, surface to· surface interactions should .be minimal.
whi_2 can b� achieved by surface treat�ent. ' � -
0

.,
also an intermediate stage in the production of several dosage forms. #gat1011 occurs due to the following reasons.
- . Wet mixing in the granulation ..step in the·production of tabl.-!ts �.)/Poor flow properties of the powder bed inside a·blender.
. and capsules. / .
� Wide differences!� parti���i'zes·in a ?ry mixture. '.· -
- . ' ' .

Dry mixing of several ingredients ready for direct compression (3 }/Differences in the mobilities o(indfviciiiaritfgredi�ots.
as in tablets. (
Differences in particle d�nsit7 ��� :shap_e to a lesser ex.tent.
0

- Dry blending of powders in capsules, dry syrups and compound �

powders (insuffiations). (5) Tu111Sp.o.rt.in.g-s-tage, pouring the powder from one container to
/ another (hopper' or drums), or emptying . the container: ·
Production of pellets for capsules.
(6) Dusting sta ,e; fine particles beco:Jle air borne and separate froi_n
In the manufacture of tablets, normally a number of additives arc t e u k of the powder. . .,..,.,,-:,-./,:.. . ·. · .
added. Therefore mixing of powders becomes an essential part of the .,
Segregation may occur even after the mixing.
'

proce�s. Whcrl the dose of the active substance is high (for example
parac�tamol tablets) mixing is not a problem. But in case of potent .Gravitational Forces
drugs and low dose drugs, high amounts of adjuvants (for example
ii'l.'

Gravitational forces tend to improve the movement. of two adjacent

lactose) ate added. Therefore, mixing is considered as a critical factor.·
particles or groups.· of particles. Tumbling action promotes, the. intt;r-
Otherwise, content uniformity of tablets does not confirm to the
particulate movement due to gravitational forces.
. p!iarmacopreial specifications. �similarly weight variati6n increases.
Motion of particles can resu.lt fro;,, d1�·ect contact �ith the n�i�er
Mixing of cohesive materials is even more difficult du.e to for:mation
surface or/and from contact with .o�e an.other. These. proc.esses <1�eler­
of aggregates and lumps. Wet �ixing is also encountered iri pharn;acy
ate the movement of translational and rotational modes of sing16 particle
as an individual operation or as a subsequent step after dry blending. In
or .groups of particles. Wl�en particle-particle coll i,sions occur, exchange
. several situations, these operations are carried out in a vessel and by
(transfer) of momentum i� achieved. · Continuous� exchange or distrit,-�.
some mixing element. Hence, this section describes some aspects of
•. t.. '
tion of momenturn between translational and rotational modes is necessary
theoretical considerations and equipment for dry as well as wet mixing.
 202 ·• l'I IARMACUJTICAL ENGINEERl�G
203
for effective mixJng. The efficiency of momentum transfe r depends on:
Ch-8 MIXING , ·. '· . : .(.!' . ·

(I) Elasticity of the collision.s-lf collisions are elastic, effective The motion of particleS, to achieve random distritiution assumes that
transfer of momentum docs not take place. The l oss due to no other 'factor" influences the distribution. · This is rar¢1y the case.·
inclasticity· should' be minimal. Instead ,. a, number of pro'pertics of the powders influemfo the approach to..,
.randomAess. Flow characteristics ofpowders largely cfetermine the ease:
(2) Coefficient of friction-:-Particlcs with high coefficient of friction ..,
. will be like!.,: to exchange rotational momentum 'more readily. with which the p rimary partiot.cs ca� be mixed.·· . ,,. ·
c·
- S ur f'ace area of contact-The larger the swfacc area of cont;Jct,
(3)
J't· ",, .... ' .
. ' � ' :· . ' .
' .
'
greater the exchange of momentum.
(4) Surface roughncss--Thc surface 'roughness' of the partic!es in­ ,*11w 1olid11�,IW :.1x��;�P.::'���=���:J;i��91v�{ �he�:' al:'
volved ill coliisions determines the distribution of the transferred t··!I Expa�s1�!)..Pf .�he-bed �f-sol'.ds�. ·: . ""'-
'.

\ ,·.? vder
momentum bet\vecn translational and rotational modes. ((" · 7. .
Appilcat190 ot threc,..d1mens1 · n�I shear:>·,fo rc
o
,
:',:� t�
�
_ t10;n.�
; . t�e_P.
- .:
: ,. bed.,,
. f .e_�i:t_i_el!!s . .,.a, .
(5) Centrifuga l forces-These act on rotating aggregates. to break ·.} Mi� lo�! e�-�h. to P,.':�!Tl_it.. J�ue_ r�i:id.�).!li:za :
th · 4 ., M;u:ntain ran.QQ!W,Zat,or (ru>:s!!gr� , gat1_011 ?fter m.J.�1,n.g). 1 • /
· miler units und aid in mi,ing process.
_ .
4 · When' dry mate�ials arc l oaded· �nto a 'ini1<e�. th�y.;form ·a 'static bed: ,, ·
This bed expands sufficiently.\vhen mixing is initia.tecl. ·Therefore� there·
(' � CHANISMS OF MIXING IN SOLIDS
- should be enough void space ip the 1.nixcr after it i.s charged with the
Segregarioi) of' pas_ti�li.:s occurs due to a number or reasons. :'vlixing
_
can prevent 1t. Tht'. · rincipal mechanisms in solid-solil.L.i.1,'\.i.:,jJJ " are·
�n grcdients.v >'.:;]:�:.>/: .:'.:
_
,rl . : ;,_.:·,<:
. The shear force proqucc;s' movement of particle�: This is a<;compa­
--,:·":=r:·�
.
nicd by expansi.�·of po�per.Be�. The str,�s�.ind�'.ces"'.'the, movement of
I
-

Convective Mitj,ng
·t:,�,•-

. . ··
_,. ------- �·- --- •- ------·-

/ �achieved by the inversion of the eov.:der b�using blades or particles in three gircctions·.· This turbulenfonoveincrit "of particles can "°
achieve randomizafiort , [f ihe forces are inadeq.uate, 'pa�icle agglomer­
paddles' or scr�"· element. 2w1 o"'Y1
ates mov,� together leading, to poor rn ix ing.
A lar��-1�. !�ss of materi,11 mo-;cs f'rom one part to another. Convec­
----- (;"('!. y

Mixin g is expected ,to prodt1ce r�ndon1' distribution of pa1ticles. It

tive mixing is ref ffed fo' as 11i?rc;,·011:ixiilg7-·- --·-·-· ..,- .
c
depends on ·the probability that ari event happens in a given time./rhe
· law of mixing app\!a(S .to follow a first order. ,_. , ; · ·.,·,.
/ fil1£1tr �ing
., ,.
�- �···i................... .... .

In this type,. the forces o( attraction arc broken down so that ead·, 1,· / M':'":1�'
.e-!'1
1) -
. (1)
particle lllO\'CS Oll! iS-OWn between regiuns_Q_f different COITI_p§itio.n...a'nu
wh7r� AI� �egree �f mixi'ri.g ·aft'er 'time i' · :
P·�!all.:=_ �_!� �heir surface�/ · , · ,.. '"·
t = time, mm
In___a parti_ culate mass, the .9rc.�s. o.f att a.c.t.' n. are-pr�d-0mina·tmg, . ,: ' \ , ..
•• ,·,.'· · J

_ A and k = constants
f

\�h!._cl!..�:�ke Mt�la�!_jp _over �'1.C..:1.i����.;!··�· uch types of attraction

I '' , I '

. forces are predom1·11ant �;:1�--��,}:1!�9.,.J)'.l?S�� '.� es.�jps�fo:.'...'rc� es , The co.nsfants A and k d�pend on .the aj,s..�L,&_�9.l1:tetr_ y, physical char�
. l . • ' . .

. � i?.---:7'-,,I•
rcd�l.il�e.J!!!.rn£!t()11s- .
and reduce the scctle of �cgri;!g�t1o ac�eris�ics,)rrhe'l)H'!�!S;,·'1'��- P}'OP;?;�r?rT qf_ �fJnat�rhil, be)ng ',�_ix�d�f
.
...,

. ·' y
Initially tlie rate of mix1ng ,is. rapid. ·,At: a later ,.stage the rate
1>
IL__i rrus.b:'.�ain "b\.· . ·
decreases.. · .Since the r.ate. process· j. s. first o rc!er· (asymptotic), perfect
It ._!.!!Y�J.��s Jhc r���-?21� . .!::2l!2E1• 9
. .C. l?.iiJ��SJ�s "":i�hi \1 thc. ,r9wc_t_ sib.e.d. mixing is no't attainahle. i.e., it t, ·es infinite tittle. Empiricall.y the' best
thcr<;, QX. .P��cl5� ;han?c th_elr .r�siti.Q!lS_ rela.tb'.�J . g__<:>_IJ!!. �J.Qthcr. 11 1ixing time wquld be 30 to 35 minutes. Once the desired mixture· has
I ·
Diffu�j. e mixini; oc�urs .�t the int�rfaces of. dis.simitanc., been achieved, tl�e process should DI! stopped:. ! • · : .. . · " ·
· --o-ions.
· - Dif-
,I I.,.! ,. �t �' .
• I I . .......__ _. I i.
v

fusion is 'sometimes referred to as micrumi."t.:ing · ,S Once mixing. is,stowpeq, the, bl�nd should exisf in static 1 equilibriu
. m:J
• • .r ·I . . . .. " ', :1". ,.)

Subsequent handling of the mixture should be so as not to· disturb the

static c9uilibrium.
 204 PHARMACEUTICAL ENGINEEH.11',!G

DEGREE OF MIXING AND STATISTICAL EVALUATION Ch-8 MIXING 205

Degree of mixing, is also known as .degree of homoge,wity. After
mixing, the best possible degree of mi.xing can be. achieved provided
·each particl.e moves. freely to every spot of the equipment. · It requ
. ires
the nioveruent of particles in three. dir�ctions. The ·degree of mixing
must be 'considered for the purpose of econom.ics. Time of mixing·
should be long enough to obtain an acceptable randomisation.
I , . ingredient is ·divided and recombined a nurnber of times in the powdered
. Ideal Mixing or Perfect Mixing
As illustrated by equation (I), the mixing process will never yield an
ideal or · perfect mixture. Ideal degree .9f ll)ixing is represc;ntcd I
schematically in Figure 8-1 a by a c-hessboard with .black .and white
It will be �early identical in �omposition to all other ordered units in· the. ,
.
mix.
Ordered mixing probably yields the closest situation of the perfe�t
mix. This can b� achie::ved by a number of ways. , :·
(1) ·Meehan ical means of ordered !lli�irig' : . The mass of each
bed (Figure 8-2)_-, The· smaller the Uttits, the .�ore, unjfonn· the mix .
Since no particulate adhesion is present, segregationv of the. mix easily
takes place on fu�her handling.
! ... ':'
·;

squares representing two compor:ients (equal quantities). It indicates that .

' ... ·'
, > ....
each particle of one component is lying nearly adjacent to ·a particle of
another componeat. · In practice, dcgre�. of mixing is indicated by its
Combine-1
standard. deviation.

,.� ""'. ..,;, I

.,,._. .L "-"'r+ n;; t il{1I
· Oivide-2
.,

(a) Perfect mix (b) Ranc;lomized mix

Figure 8-1. Types· of binary mixtures.

Acceptable Mixing I

I
• I

Since perfect mixing can not be achieved, other alternatives for

obtaining an acceptable mix must be considered.· Combine-3
Random mixing : It is indicated by. random distribution of particles
as shown in Figure 8� I b. Random mixing means same ratio of compo­
nents in. the entire mixture. Artificial randomization in the Figure 8-1 b Divide-3
is based on random numbers in statistical tables. However, it should be
noted that the use of random motion to achieve random distribution
assumes that no other factor influences the distribution. This is rarely

j
thc 1 :c�se. Instead a nu'llber of propci;ties o_f the powders being mixed ., Figure 8-2. Ordered mechanical mixing. .:..'
.
influence this <1,pproach tQ randomness ..
(2) Adhesian means of ordered mixing: These forces of p�rticles
· Ordered mixing : Ordered mixing is described ,.
as the use
• 1· ,,,
of me- · may create ordered units of nearly ·identical composition depending on
chanical, adhesional and coating forces. Ordered units in the mix should the process (Figure 8-3a). Partial solubilisation or ·the us� of a bindi�g
be suc..h that ordered unit will be the smallest possible sample to the mix. agent during wet · granulation approximates. the .s�.me effect as shown m
' ·· ·
Figure 8-,3a.
206
PilAK;,\ACEUTICAl. ENGINEERING Ch·S MIXINO 207
.. , i· \

(3) c�ating means of ord�rcd 1�1ixing: P�rtidcs in an ass�• n�.lagc · Ideally, the degree of mixirt!tbegins rapidly up to a partic,.ular ,Iev�l
.
may also be coated with other mgrcd1c11ts to gi :·c an ordered mix either and sl?ws d,owrtgradually. Uniform degree of mixing c�n be; r.esulted by ..
_
as individual or coated particle agglomerate:; .(f 1gure 8-3 b). , continuing mixing for. some more time._ The practical defipition of
mixing uniformity is selected to relate as closely. as ·possible· to the
.desired properties of the mix. , The sampling technique largely deter-
Adhesion mines the'·validity and inter·pretation of the derived mix... · i "· '"
Solubifoation · Statistical Parameters . .· . . .. ,, :•-'. ,,. , ,·
Th� analysis ofsamptes bef�rc a�4 �fter mixi�g pr�vld.es:_inf�r�ation
about the degree of mixing. Solid mixing with sqme 'kind of tracer
mate�ial is used for easy analysis. Some impo1tan! method{o'r analysis
are the particle siz� distribution and' the· assay. pr6cedures for _different
ingredients in the sample. ,•'.. . i :,r;: : '. 1

Arithmetic mean : The me.an (assay value' or size �istributi°on an.,ily·�

sis) value . of' a. group of random samples is a. 'measure''·or .the central
Ordered-unit tendency· of the batch population. The arithmetic mean is· expressed as:
agglomerate .
..
.. h :

or granule 'n y·1

(a) Adhesio.n
Arithmetic mean, y = I- (2)
n
Taking a number of samples (n), _the true me..n, y, is estimated.
I f .'

Mean may be attributed to concentration of a component or particle size

'· · · · ·
of a particular component.
-Coating StarJdard deviation : The spread <?f dispersion of individual samples
,a Coating
is important, because it is impracticable to obtain the sarr,ie true m'ean for
�� Particle the same product mix obtained by another lot. 9r .by anqther mixer.
· Ordered-unit Therefore, standard deviatibn is used. It is_ express�d as: . . . :r, ; ;- , .
single coated
� . .- .;· r
particle n _ 2 ':' '.'., . ,.. 1 ·

0
.. �(y; - y)'.._-. . •,' '1. ,· . () · .

Standard deviation, cr = I
" .' .,�.,,:.:�: . (3)
'
·\ . iJn.:- J) ,,,;:·, .!l):� �,.\ ., T
'
Variance, which is a square term of standard· deviation; can also be
.. .,. / � I ,� \, � , : I � .il .".. :', '; ' .•

Coating used for characterisation of powder mix;•, Standard dev,iation ;is- applica-:
Coating
� ble for a specific material and·a specific·mixer., •,·,,. q · 1 : ; !

Particle
� Ordered-unit Mixing of pharmaceutical p�wders'.'should .be c��tin��d �ntil the
single coated amount of the active drug that· is required in a dose is 'within i±' )3 .SD ·
particle units of that found by assay in a representative number�f sa,�ple d�ses.
(b) Coating
To achieve this objective, n sh_o· uld be 'large. 'This'is l)OSsible''by. rnilli�g
' ·
Figure 8�3. Ordered mi;in'g based o� the the ingredients to fipeness. 1' · 1· 1 ·

. principles of (a) adhesion and (b) coaling. ., .

208 PHARMACEUTICAL ENGINEERING C:h-8 MIXIN<i 209
Relative standard devia tion : One may follow the mixing 9peration ao :..: --.Ja(I - a) (7)
in ca given process by plotting the standard deviations as a function of
time. The relative st.:indard deviation (RSD) should replace the stanclard where u �- overall fraction of tracer in the mixture.
dcvi.atio'n as a measure of sample uniformity, which is expressed as:
Statistical Evaluation
Pt.:rC�I/( retaiive standard = ,standard deviation (CJ)
.. i.,r.•r,

x JOO (4) Mixi::r scb:tion depends on the degree of mixing or th,:: powdC'r in
. . 11 (RS'D1I
clev10t10 .· mean (y) the final product The procedtire invoh�cs s�mpling �pcf.a1�alysis� The .
sequence of !;\cps involved in the evaluation of the degree of mixing or
Equatjon (4) is useful for comparing·the efficiency of two or more del.!rec of homogeneity is given in th� Table s:1. \ ·. : ··.·. ;J,1 .'., ..,;:;,
mixing operations or different sample sizes or �iffere11t compositions.
._ 1, , , '; ,4 , :-· ,•• 1,, \.
i • �

. . Thc•objectives have been specif ed· in· the Table s:.t>_, .The sampling
Mixing Indices technique largely dctermin�s the· v�lidity
· , t;1tion o_f� the, de-''·,
·and inte�rc_
The selection of a mixer depends on the mixing index or degree of rived mix.
mixing. The above mentioned statistical p�rameters are useful for Criteria of sampling : · While sampling a bed of powder, there
evaluating the mixing indices. should he assurance that the qed is sampled uniformly. It is assumed that
Mixing index. involves . the comparison of standard deviation of sam­ the powder b1::9 consists of ti 1t;umber .of.zones. Within·ca�h- zone. the
ple of a mixture under study with the estimated standard deviation of a, composition is uniform, but among zones, the compo�ition is different�
completely random mixture. Therefore. method of sampling is ve�y _i'1�1po·rt;nt. For thi�'purpbse, two
concepts arc important.
Mixing index is expressed by Lacey. Two of them are:
standard deviation Sca/11. r�f segregation': It is a furJction: of size of the zor�e·: fr assumes
of random blend that zones arc having uniform b<;d, but differing in composition. Good
. i\,{ixing index, M = ( 5) mixing should yield more riurriber of zones· with small size. The�. the
standard deviation of cr sample reflects the true character of the powder bed..
the sample blend .
.• ,, ·: .
ao - a lmemity <f segregation : lt.. is a function of composition differences
Mixing index, M = --- (6) among zones. Generally the process of mixi11g tends to reduce the
o-o .- 0-R intcr�sity of segregation.
where o-o = standard deviation of unmixed powder. Sample size guidelines :, The 11umber of samples re.quired.should be
The r;atio will be less than I. The higher the M value, the greater the not less lhan 20. preferably 30' and more ideally I 00. Analysis qf these
homoge�eity. Equations (5) and (6) are used to determine homogeneity samples is t.irnc ct)11su111ing and kdi' o�s. · Therefore, economic c�nsidera-
tions suggest 20 samples.. ' · · .,; ' · ' . '·f1
in a mixture depending on the objectives at hand.· The selection of a
particular equation is essential when the mechanism of mix.ing is being Random sampling is the mctl1od of cl19i�e for stu,die�/ S��ple size;
Result� of practical use can be achieved by using statistical analysis.. in most cases, should approximate the unit dose siie,p_f,�!l _ e fin�) product.
The differences may indicate poor or inadequate sampling, inappro­ Collection of samples : Some golden rules of sampling are:
priate. mixing operation, improper handling• of the powder · sample, I. A powder should be sampled when' it.is iii motion.·".,
1

unsuitability of the mixer, operational conditions etc, ;1- • . ,, 1

..., The whole of the .stream uf powder should be taken for many
' • ,. • ' ' I : • • ·., I

'Blf�re mixing has begl!n, the m,aterial in the mixer exists in two short increments of time in preference to a part of thc'>stream
layer�, one of which contains no tracer material and one of which is
taken for the whole time.
tracer ·only. Under these conditic>ns, the standard deviation at zero time
(o-o) may be expressed as: 3. Sampling after completion of the mixing. ·,

/
210 .PHAltMACEUTICAL ENGINEERING.
TABLE 8-1
Statistical Evaluation Procedure for the
Blending or Mixing of Powders
Objectives
I ..'fo compare the cflicicncy of two or more mi:dng operations.
2. ·To, compare' the cf!icicncy of two or mun: cquipmcn't.
3. To follow the mixing process with time.
4. 1'o optimis� processing parameters.
5. To investigate the mcchunism of mixing in a gi,·en piece of equipment.
Sample �izc guidelines: (a) Random sampling
(b) Number of sampks
Number or samples: Requin'd -- 30; l<.h:al - IUO;
Econoinic:.il s:unpling ··-- 20 (pre1��rrcd).
.
Sample size - :.ipproximatcly a unit dose of the !inal product.
c;J,
Sample c:ollcction: (a) At different intervals \\hen the -bknd is in motion.
(b) After blending is co111r.letcd (prefcm:<l).
S�_mple utilizati�n: (a) Scooping sampling
(b) Thief probing (prcfi:rn:cl)
Sampling methods: (a) Returning the sample tu the bu:lk, for example,
after completion of partich: size nnalysis (non-
· inserted in the powder bed, it' 'ca'.rries' material .from. th7 surface _o'f t: .... '
dcstructi ve evaluation). ·
(b) Not returning the sample to the bulk, for example,
due to soluoilisation for assay pruccdurc (destruc-
.
tive method).
Statistical Analysis
Determination of arithmetic mean and standard deviation of the ran-·
do�ly mixed sample (standard).
Determination. of arithmetic mean and standard deviation of the un- '
mixed blend of sample (initial stage).
Determination of arithmetic mea� and standard deviation of the sample ·
after blending (test sample). · ·
· .
C�mparing mean values (sample) with target value (true mean).
- If they arc compara._ble, s\andard deviation should be calcul�ted (indi­
cates uniformity _of the sample): High standard deviation indicates less
,1.miformity.
Determination of mixing indices:
- Scattering of sample about mean or standard deviation (plo(.-of standard
deviation vs. time). . ·
Accuracy and precision assessments of these estimates.
Ch-8 MIXING
211
Some times,' powder sample cannot be �amplcd from a moving
stream. because:
(I) confi!'.!:uration of the mixer·'- for example the ·shape' bf the bowl
does·;ot lend itself to du1�1ping. . , . . , · . ·
(2), size of the batch - large v�lumci arc n<.1t conducive to1 , routine
transfer from the blen'der to ilntm or '
larger collectors. •
I .
(3) possibility of mixture segregation biasing ti�� sample. .:.,
Therefore, it is always preferable to collect th�_samplc once mixing is
completed. .'·:, ! . ,ai;. ·l \ ·,:,
· Method of collecting samples . : Sa;,�'plcs should be 'c�il��tcd at
selected points or serially as the powder is discharged frot� 'the mixer.·
Two type!> of sampling methods arc adopted.
(I) Scoop sampling of the bulk mixture
·�
(2) Thief probing of the bulk mifturc ... r·
Scoop sample : This 1nethod has some drawbacks. (A) Surface layer
sample may represent scgregafod mixture·.r '' (B) Sain pies can not be
removed from the bottom an<J middle' o'f .the blender or container..,;::,
. Thi4probe : This method has some dra�vbacks'. (i) o·�rfog sampling,
some comvaclion takes pli,lce around 'the thief. J (ii) As the. t)li_ef i,s..
mixtur..! down into chc mixture. ' . ,
rhicf. probe is prci�rrcd over. the sc.oop, b-:caus'e sampks- can' be
taken front deep within tlloi dlowder bed and a fair· degree ·of random
·
sampling catr"'be achieved.
Sample utilizati�n : If th; .�ethod, �f.analys(�'.is,-,n��;sdc-structive, for
example, particle size analysis1 the sample ·can bv,retlf�nedto th_e mixture
after analysis. If the method is des;ructive�: for··· example
·· ,, 1
assay, the
.
sample can not be returned.
Analysis of data : Several statistical parameters and mixing indices
are calculated. The comp;·rison ·af the- mean value of the sample under
.
analysis and the};rg;l val�e.. If the :mean value of the sample under
analysis is on or near the target value, calcufation of the standard
deviation (and Of variance) wjll give an indication of the un_iformity of
the sample. Oth'er det'aiJs· are g\y.en in the.,T�ble 8�1. . · \·.
I",,·
 ' I 213
212 l'J IARMACTUTIC'AL ENGINEERING Ch-8 MIXING

. �CTORS INFLUENCING MIXING - there is a ·l�rgc diff�rence in the pr.opo•rti�n- of.two p o wders, mixing-e,:>is
n g or der o f the1� weights.
·c· Particle and powder characteristics innucncc the n1ixing process. always
· · in the ascendi
done · · . . . :
. The fundamental aspects qf t I1c �art1c · and' p o �ers
· I ��·1 . .1> "Crd
� . . , are d1scuss
Aggregation inhibits p;oper mixing. Therefore,. higher sheari;;g."forces , -
.IIl (he Texthook' <�l Physical •P!1prmace11tic� by C. V .S.
��b��.h1;:a �yam
are applied. Hence, co rrect mixing of o ne cqmponent does not imply , .· . . · ,
( Vallabh Prakashan, Delhi).
v • , . . . · ..

go�d mixing of-0!�1e� components. Therefore, adding dye to the mixture .

. "'
is often misleading. The dye may n ot aggregate, but active substance A ·�! . ,. : ; .. ·� ·1 . . .

inay aggregate'. �L·lsslfICA�ION. ?F EQ�IPME�f ·� OR SO���S � IX� N �

. ; .
A single factor can in no way be considered as a unique indication of . . ', l3 ascd on tl'i� ��w.'. _ero p�rtic�<�_f ;lhe p:owders, ..app�?f{1atc mixer .
sh ould be selected. v,..rfC·,· ,.· ;., _,· ·'.·; ,,,; ,,·,_·:
o

mixing. However, flow properties of the components is the mo st impor­

tant consideration which is agai n influenced by a number or factors. "(/ Free fl owmg so lids - V con� 1bleJ'\dfr • ;!":''"t , ''!>'-:C::f',1" 'b l�"dt..1..,1.
(JI'. !)
• •

.../N�t�rf .�f_ !h.( $r_rfacc : Rough surface of one of the components X' lfl_ O oubfe co ne ble.nder . · _ ..,
<'!!)- t,.Mbe,J �. · ·<:.;(\.H t.J -' CfA� f,.l-iiie .
docs nof-1n uce satisfacto ry mixin�. This can be due to the entry of lf):r
·. .
Cohesivc solid� _Pl::mctaQ' mixer . . ,. , . , r:,. , ,'1/l4f · �i;1l< rv
active substance into the pores _ of the other ingred ients.
Ad d ing a substance, wliich · will\ be adsorbed o n its surface, can
;. . fa19- Sigma blender. , _;,1,,. ,.r.
(._�
··.•· ''(tl,:..·(�"
� f.N\C:• V�
u
·-c'· ·· ,.. ·
,_ 11 �.}""
C'I-VL
. Bas9d. <;)11 . the �Gi.}lc ot mi'�Wr�g':YJi,:<l'ng equi ment;may. be c lassificd as
i
decrc;1se aggreg<\tion. Example,.is the add ition of aerosil (cQ]lcidal . ' 1-·-
give1� in 1 ab lc s ·- :
.
. .•' "·.,· · ,'
silico i� di o xide) to;.inc oxi.Ge. Thus, a strongly aggregating zinc o xide
bzcp11?es a fine dusting powder. which can be mixed easily. · ,·, TABJ,E 8-2 . . ,
_))ens_l!_LQfJlu:...par'ticle-s : It is of min or importance.. Demix Cl�ssificati on of Mixliig'Equip'�cnt >.
ing is �����..,......�· �� �"'��.�.,:-:��- 7-..-��.....:._.-����:,a:,:11�:,,1�:o:7:11:1 ,:x7.i,:::
acceforafc when the den sity of th,e smaller partii;.I� is higher or whe11
the m:x 1ng p-�oc'es� is stopped.abrupt!�. This is.. due to the lac th
..- <; · 1 .·of mi:o. er. i.1 Exampl_es, ..;
• • No . Nat�. 1i·e.
.'
., !vfe..cl s f 1g ..',
at dense
t
1·. "
material always moves dow nward and settles at the bottom. I Batch type'
./.J"I . Small scak
J�ilJ:fi5Jc:size : It is e,as_y _1.2i]_�"':_o po�9ers having approxin{atel 'N ·, �.f • ' '·
y
I • •

. the same particle size:' The variatio--;--ot "' ? Tumbling ri1i:,.;.crs or Doubk cone blender., .rl!mbling rction
p
parficfesTie-can··1e-rialo . .. . :� . r:- :' ..
separatrOA,.-bec_ause the small particles move downward thro ugh
the . ) · ,2yl.indricul 'mix�rs· v-cone 1u.1xers "' � Ci • I ( '4' )

spaces between the bigger particles. As the particle size inc:reascs, flo 1,iihout mixing hlac.k ;�·ill��� bafOes
pro perties also increase due to the in fluence of gravitatio nal force o
w
Cube blcnpcr
n the . . . ...
size, Bey o nd ·.a' particular po int, flow property decreases. The powd TumBling•\nixcr with · v ·cone blendc'r \vilh . Tumbling -a�liofr us we ll
ers
with /mean particle size ·of less than iOO µm are free fl owing,
facilitates mixing.
which ,) 'a mixing bl.rdc r a' mixi11g b·lacle ·
•

· ,. D,ouble cQn�jblc'rtder .....--- 1: • . ' . ..

a� shearinu:�b�bladc
.
,.
with a mixing blade
,'

·'Parti_�_le. �h»e : The- ide. at particle is sphe}ical in shape for

,. y
c·

' ......- the

>!
--�·..;:;::.l'---- --
-- ) ·�.
Static ·n'.ixcrs , · Ribbon.. blender -· , stationa& shell and
p,ur.e_o se of,, u·lll[�rm m�p�. The irregul
• •�'!'"--- ·-·. . ,_
• .... .
ar shapes can · b-e-co me inter-
,r.· rotal ing· btat:!c ..
t

lockett'1tr(cf thereareTess chances of separation of particles once '"§Ii�,;� bl.en�cr

these
are mixed together. " I .
...� -Planetary
---- . paddk. ' ·•

- ··�· - i: '
........

5 Air m·�crs or 'Flt:1idiscd mi'.\er Air supported blct1ding

. ..P_�n�J�:-c;b:}.r.g.e :: "S o'me parti�Jes exect. ,attrac;iyf forces due _to eJ_sc/
I
.,(luf<li�ed mixers· - ,�.' � •. J >· \
tr o static charges on them. This can lead to separation o r segregation.
Propo r:tion,, Qf .mate.Pia ls : The best results can be obtained if two
(: Continuous type
Large scale
Barrel --type
------
Zigzag type
. · Rotating shell....with

Jotating blade
. "-... .-
powders· are mixed in equal proportion by weight and by volume. ! f
�-:---· ···
� . -�- - . \...,.._, ,,

/ ,!

__..,.
I
Ch·M MIXINU 215
214 Pl IA RMACElJTICAL FNGINEERIN< ·
E.dgc of' 27 degrees is good for mixing. Special:rollcrs arc available
EQUIPMENT ·so thnt ai1y vessel cai1 be placed on it at t'J1e optimal condition. lt is very
A mixer that promotes the randomness in ·mixing should be selected. handv since the vcss!!I can be used every" where· in the ·process. 'When
I� should_,als?. �revcnt tf1¢·c·onditions resp�nsible for segregation. Th,erc­ mixc�I, cohcsiye po':"'ders tend- fo ball up and aggregate. Therefore,
_
fore, opttm1zat1on of operati61i'al conditions is critical. tumbler type is not si1itablc., · ;' '·.
Th� etfo:icncy of a tumhli;1g mix�r �1ighly depends on the speed of
Mixing Equipment-Criteria .i·, rotatfon. ll should be critical.
I. 'The ·powder bed may expand s�fficicntly, th.erefore, equipment ;
'· ( J) Slow rotation - No intense tumbling, .no .cascade1 motion. Not
��.ould never be fille9 for more than about 60% so as to le�ve
enough shear rates .is applie�.._ · .. .·:·:.. . ·'
sufficient mixing volume. .
2.. �he particles sh,;>UJ.cl b�}ubjcctccl, �o movem�nt m three direc- (2) l\apid· rotation - Sufficien.t e('ntrifogal action to hold the J�owder
. t,ons. tn the sicks or the mixer, more dusting an.d segregation of fines
. . ' .. is po�sible.
3. The s! c ring or cc should b� su�ficient't'6 ,w_�vcnt aggregation.
! � � _ Thcr;forc, the rate of ro·tation should be optimal, which dcpe;1ds on
Appro . rdate m1x111
� � mech.anism sllould be s��cted and allowed 1
!he size, shnpe of 1he tumhkr and the ·nature of material to be ·mixed.
�o contmue for P,gt1mum tiinc..
Common rang<.: is 30 to ll)O rpm. . ·' '· '· ·
·i:;:.1.
4. There should b',:' -�o centrifug;I effect,. so that the powder does
.
no� get separated according to their weights. , · ,. . . �or cube· mixers
Neither ·cvlindrical . are used to a -great c�tent in the
5. The fo ces should not cause breakage of the particles, which industry. For simple blending of dry mixers, 'y c,one an.d double cone
� hki1(.krs wi!hout baffles arc used. The tumbling 'rnotion is 'accentuated
· c: may brm� �b_o�t delll!�!ng du�. t,o ciiff:reryces in particle· size.
by rnenns of baffles or s'impiy by virtue of the shape of the co'ntainer.
6. The mi�ing process sh0uld-be stopped abruptly,. because slc)\v'
or ·
:dit�inishin� forces in o_ne c!irection might cause demixing. There TWlN��rnELL 1n., ENDER OR v CON� �L�NDER. .
­
fore handhng of po�vd�r blend a�pr mixing is equally. impor
tant. Thi.! construt:tion 0L1 twin shell blcndc/is ih�wn in' Figurt�:.:5','' It i�
Some n�'.xing equi m ent arc disct:�sed below. ..
I
111ad1.: or cith1.:r �tainkss steel or trai1sp'a'rent plastic. Smaller models .take
� . . a chare;c ·of 20 kg arid rotat..:: at 35 rcvolution�pcr minute, whiic larger
TUMBLERS OR c, LINDRICAL BLENDERS WITH NO MIXIN - ones t;kc a char;e of about I to1111e''.and rotate at 15 . revo.lutions per
G
BLADE minute.· The material is loaded through ·either of the shell tfalcnes.
._,,

··
This, is a genc al class of equipment meant for blending of Emr,tying of the blend is normally dbne'through an ariex por(
: dry • ', I
::J
powders Th� equipment consists o�;� container of one;:: of the
••
• , , '•a ' �, I : �! t ·: f

; several Shell
ge mctnc form. ·These are mounted so that it can he rc;,tated about •'·.Sha fl
? an 'drive
axis. These do not have.packing glands.(.seals) round the shaft. i]f(
Cubes ,tr•

or hexagonal cylinders may be· rotated' in any axis· depending on the "

manufa�t�re (figure 8-4). Such a cylindr,ical vessel is not. suitable for

mixing since one-dimensional mov. ement �ould be obtained. ........ \ .
"�· \.... "• :'
,0

Figure 8-5. V -:,111.: bkmk·r. Rotating shell \\ i,hout bMnc�.'

-@- The material (to be blended),is loaded approximately 50 to 60 % of

it,s lol:11 v6lume. :'\s the blender rotates, the 1natcrial undergoes tumbling
motion. When th� V is· invcrtcc!,· the materiai splits into two portions.
(a} Cylindrical blender. (b) Cube blender. ·This process of dividing and rccon1bining continuously yields: ordered
Figure 8-4. Tumbler blcnd.crs without agitator blade. 111ixing by mechanical means. The powder mass 1s converted shock-
 I
216 1'111\RMI\C'l:lJTll'i\L l:'s(ill)IEL'.IUN(i Ch-8 MIXl�Ci . 217,
,} .
11. I
wise. so that no dcmixing due to density c.)itTcrences will oc<.:u�. �··1i is TUMBLING BLENDERS WITH AGITATOR MIXING llLADE �-.
rotated so that the material alternatively is collected in the bottom of,Jhc
.\
The Y-cone blender a!)d .double �one blender with ag.itator. b ; l.;tdei
v. (baffles) are-shown in figures 8-7 .and s.:s, respectively., The g�,rteNI
. '·' '·

,_'/.' .
consfructi�m and \Vorking is same as meqtioned above.. Agitator blades,
11knJcr speed is the key for mixing dliciency At high speeds. more,
dusting or segn:g�1tion of fines. is possible. \vhile at low speeds. ll(il ,,.
are added which have several advantages. .... .

enough shear may be applied.

Advantages : (I) If fragile granules arc t.o be blended. twin shell·,
hlcni.Icr is suitable because of minimum attrition. • 1 I

(2) They handle large capac\tics.

. 1. <

{3) Easy to clc'an. load and unload.

(4) 'i'his equipment requires minimum maintenance. I,
'
Disad\'antagcs : (I) Twin shell blcnckr needs high hcadspace for
'' L
'installation.
Agitator blades
(2) . It is rwt sui!able lor tine par1iculatc system or ingredients of
lar�c differences in the' p:uticle •iize distribution, because .not
I
Blender shaft
enough shear is applied';· · drive
-·�·
v ......
.
(3) If powders are free flowing .. serial dil.ution ts required for .the .,
\i. 1,

addition of low dl)Se active ingredients. .-I . . .. 1 I

, ' • \' Ag1tat�1
7" . . · · shaft drive
,r .ifa ··· · :
Lr. coN·E BLE,NDER . .
The construction. of a doubk cone blender is shown in Figuie 8-6. It Figu rl' 8-8. l>nuhh: ·cone blcnckr.
is usually charged and di�charged through }he same port. It is an l{11.lati1H! sh..:11 1, ith rotati1111. hartks. •
effici�nt ,design for mixing powders of d\fferent densities. These are.
used ·,n�stly Jor small amounts -of powders. The rate of rotation should' �nta�es: (I) B,tll:s ·:,c useful fo, �oth wit :nd dcy mixing.
be optiinum depending on the .size and 'shape of the tumbler. nature of� / . . (�) Wide range or shearing force. can be applied \Vitt/agitator ba. rs
material to be mixed. Commonly the range is 3'0 to 100 revolutions per. perrnitting' the intimate mixing of very fine �s well' as c�arse
minute. The method retmins same as that of the Y-cone blender. pov-,ders. . ';; it:;
·:.•; ,, � . , . .L
(3) Serial dilutior� is no� needsdwhen incorporating IO\":·dp�e �ctivc .,,
Shaft
drive
ingredients. '' '\)) ;

---0�---,-___.• �an��gcs_: (I) Attritiop is largc. size, reduction -off. riable parti·
cks u:sults. ,
.
1 . •· ,. . •: .
· �. 2) Scale-up can prove a problem, because general principles· of
Figure 8-6. Double cone bkmkr. ,scale up do not. \\Ork. . ·. · . 1 :
Rotati!ig shell witl�out baf11cs.. (3) Cleaning may be a problem, because ·the agitator assembly-,must
be removed and ttic I packirig should be replaced for a ·prod wet
. , he advantages.and dis;Jdvantages for double cone blenda are same
T
changeover. •. , . · ,, ·
as given in Twin shell blender (or V cone blender).
(4) Potential packing (sealing)' problems. ''' · .
. (
 218 1 1'11/dtMACHJTIL\I. EN(jJ�LU'.INCi
. . .. Ch-8 MIXING 219
�;N BLENDER
. · · · ��ii>lc : 'Th� 'mechanism ·of mixing i:, shear....Sb.car is' tr�nsfcrr:c·d Uses : Ribbon blender is used to �ix finely divided solids, wet solid
mass, sticky and plastic_�Q.Li.ds- Uniform size and density material ca.n be
• I
.... , ..,r<_ .......-...,..._,_,.
....
� .. �"�

to'. lhc PO\\'cter_ b�_d. by- moY.ing,-blac.Ic's··{r1bbo.n shaped) i�- � · ri'xcd (non-
·1
• \ mo-i/abi�X ��.:1�: "Tffg h shc�r rates arc effective in breaking fl�mps an_d '
_ .
easi+y--m,xca.Tt1t�d
.
for l.iquid-solid
,,
and solid-solid. mixing
.
.
aggrcga_tcs. Convective mixing also occurs as the powder bed is l,i--1,:ted.:, �ntagcs : High shear can be applied by using perforated baffles,
r and allowed to cascade to th:.: bottom ofthc container. An equ:librium 6ich bring about a ruhbing, and break down aggregates. Headroom
state ofmixing can be achieved.,/'
�
requirement is less. ·1 • ·

Construction : The constructionI of a ribbon blender is sho�vn in ' �s : {I) It is a poor mi��r. betau,se movement ofpa;ti�
I ,

D�antag
'
l

Figure 8-9. It :consists of a non-movable horizontal cylindrical trough ,,,.,,.- cles is two-dimensional. ·
.

(shell) usually open at the top.. _ It is .fi.tt_ei t with _tw

_ o helical blades, which
.
)21, S)1cari11g action is less than in planetary mixer.
\ ' ) �·

arc mounted on the same. �haft through. the loi1g axis of the trough. The (3) 1)ead sp0t\Jarcas thpt .rcmain 111n1uiwd) ,115 observed 111 the
blades have both right am! left hand twists. The blades arc connected to 111i..;,:r. though they arc mi11i11111111.
a fixed speed drive. Ribbon. blender is top loading with a bottom
It i? having fix�d speed drive:,
discharge.port. The trough ca!1.be �loscd1 with a lid. '

,. .•
, 'I

51GMA BLADE MIXER

Principle : Jhc mechanisi, n
_ of.mixing is shearing. The inter-meshing
. ' q t . �1 1j 11'·" \,,,,. ,� .j .. . ' ,.,
Helical blades

or �:igm:1 shaped bl�dcs creates high shear a'nd kneading actions. Con� ·•
( vcctivc mixing is achieved by cascading the'material. : · '.·. · · '-
Construction : The construction of a sigma b'lade bk:nq�r is shovvn
in Tigurc'18-10. i It tonsists of}bublc trough sl_1ap�d, stationary bowl.
Two sigma (indicating the shape ·of the Greek let'ter) shaped blades are
fitted horizontally _in each trough -of the bowl. These ,arc connccte.d to a
fixed speed drive. The mixer is' loaded from the top and unl.f)aded by, ·?
Discharge spout
Side view
tilting the entire bowl by means of a rack-and-pinion drive. ' , ··., Y ..-'
Figure 8-9. Rihbon mixer. �t.ilionltry shell and rotaling blade.\..
Working : Through, the fixed speed drive, ribbons arc al 10\vcd to
Intermes'hing blad
' e design A
' ' Blades

ioiate.
.
d11y
·'
blade m,o�·�s the .solids slowly in one direction
,-
and the .other
mo�es them quickly in oppo�itc direction. Different powders arc intro- ' ''
duced from the top of the trough. The body is covered because
considefoble 'dust may be evolved d(1ring dry blending and gra1�ulating
SOlUtfOn may evaporate during WCt granulation.
The powders are lifted' by a cc11trally locakd vertical scrC\', and Cross�section A � '.
'; Top View ' \
,

allowed' to cascade to ·the bottom of tl�c containcr"(twnbling action): The Mixing tro:igh
'

Direction of rotation
cou1Jtcracting blades set up high shcai and arc effective in breaking up I
lun�ps or aggregates. He! ical l)_la�es _n!oyc the powders. from one end to Figun• 8-10. Sigma hliHk mix..:r. Slation�ry shell .and rl�lati1w. b Iadcs.
, 'I

. another as .�hown in, Fi_gi.1r� 8-9. The final stage of mix represents an Working : Different powd�ts arc introduced froni the top of, the
, equilibriu1;n state. , Tht!',:,Opdating conditions 'of a given rnix1:r can mark­ trtH1gh, The body ;is covered because considerable dust' may be evolved
edly effect the steady state and thus the quality of the mixing. The during dry bl::nding and granulating solution may cvaroratc during. wet
, blend is disc;harged from the bottom opening.· granulation. /
 220 ,I Pl IA RI\IA(HiTIC'AL EN(i!NEERIN<i
Through the fixed speed drivl!. the sigm� blades arc allowed to
rotate' .. The blades inovc at di'fferent speeds,. 01ie· usually about twicr.! the
speed 0! ,,other. rcsuhing in lateral pulling of the rnateria!. They turn
1 It rotates on its ow11, apd around the central. axis ·so that it
towards each other so that the powders move' from the 'sides to !he' centre
of the bowl:' The matcri-a! further moves from the top to downwards
over th� point and then sheared bctwel.!n the b!adcs··and the \V,t!I of the
trough. ihus cascading action (convective) as well as shear action can
be acl_1icvcd. The perforated blades hdp in breaking lumps anJ aggre­
gates. Thus high shear forces are set up:· ··rt:ic final" stage· o'f- mix
represents .an equilibrium state. The opcrating··\�onditions"of a given
mixer can 111arkedly effect the stcudy state and 'thus the quality of the
mixing. By means of a rack-and-pinion drive· the bowl is tilted to empty
the blend.
llses : Sigma blade inixcr · is· commonly .L\�cd for' mixing of dough
221
,ing : In the planetary mixer. •th�· agi'tator has· a plar\ctary
reaches all part.':i, 6f the vessel. , B'cater is shaped to pass with close
-'r.\..
clearance over the side and bottom of the· mixing bowl. Therefore, "
literally there arc no de'ad spaces in the mixing bowl: The blade tears
!he mass apart anfhshear;is applied between the 1.nov.ing blade and the
stat io11ary ·wal 1. , The plates i,n: tf1e blade a.re sloped so that th.e.. powd�r
makes an upward movement. The.rcfore, tumbling (convective) motion
·is also obtained. Since it is a v.iriahle speed driVb1. initial)� the biade
1110\'es sloi.vly for prtmixing and 'finally at increased sp, ced'for active
mixing. Thus hi'gh sh�ar can be applied _ for 'mixing.
Planetary
.
•'

ingredients in thl.! bal-dng industry. !t is usl.!d in wet granul�tio1� process in _gear ;

the manufacture of tablets, pill massl.!s and oinuni.:n(s. h_is primarily used
for liqi1id-so!il.l tnixing. al'though it can be used (or solid-solid mixing. 1
.

Advanta�cs: (I) Si_g1�1a pladc.mixer creates a minimum dead space

' .' ,1 •r !
I ' 1 • ·�·

· · Beater
during mixing. · or, blade
., '·' (:::!f ;It h;s clos/�:l'era�c�s- bct\V,C,CI; the b(adC-: and the sidc-w�lls as
• \veil as bottom of the mixer'shell. .
.
,I
I
• . -
•, , . .

,, · Disadva·ntagc : Sigma blade mi:-1cr works at a fixed sp1:cd. Shell or bo�l

J: � P,J�..r;J;:-.�\t ; MI x ER ,'.
VV.c·i�:lc : In a plan1:tary mi:-:er, tile blade ,.tears the mass apart and
shear. is applied. b�twe' cn a moving blade ano a station;ry watl. The
mi., ing arm moves· in two ways, around: its O\Vn axis and around. the
central axis,' so-thai it reaches every spot of the vessel. The plates in t�.c
'
blade are -�:19���.. -.'s.? that the powder makes an upward · movement.
..
.
Figure 8-11. !'J;rnt'lary nli:,;er.
Emptying. .t,he .bowl may be done by hanc;l (scooping) or by dumping
mechanism.
E,1Pl:inelary mi:xer produces precise blends .i!1 .ad�itio;� to br�ak-
.
.
111g down of agglomerates rapidly. Low speeds are used' for drv blending,
�nd_ faster speeds for the kneading actiou. required in· wet g;·anulatio;.

Thcrefore.�tumbling ('conv�ctive).'motion is al'so obtained .. Steam j:icketed bowls are us�d in. the manufacture of sustai�1ed release
Construction : The construction of a planetary mixt!r is shown in products and ointments. .'
Figure 8-11. It consists of a vertical cylindrical shell, which can be �ntages : Speed of the rolo,t101� c.on· be varied at will, so it is
0

removed either by lowering it beneath the blade. or raising the blade a�:rnia;eous O\'er sigm:i bbde 01:·�,'ibl;on "type blciJders.' This is more
q,bove the bowl. The. mixing b!adl.! is mounted rron1 the top of the bowl. useful for wet granul;1tion process. There are nof packing olands in
. ·
� t:,
contact "ith !he product.
•
The 111ixing shnlt is dl'iven ,b.y a plandai·y g·ear train. as indicatc�d .in the
figure-8-11. It rotates around the ring gca!·, which furth�r r"otates �ound
the·mixer blade. Jt is normally built with a variable speed drive. --,
�1d\' antages : ( l) Mechanical 'he<1t is bLi'11t up within the po\\'der
1111X.
.
_./

(2) II. requires high power.

� , .,,.-::,

(�) ll h:is limited size :ind,is useful for hatch wor.:i only,
222 I
Pl IARMAC:.:ElJTICAL Q�Gl!\!EERIN(i
. Ch-8 MIXIN(i
AIR l\,�x�R OR FLUIQIZED MIXE� . �-,.
'\,,� ,. ,··�
: 1,
to. rota.le using electric power. Side openings are provided on. each side
Principle :,,,The air movement is used for m1x1.ig powders. 1'hc
for charging and discharging of materials.
powders arc mixed in a stationary. cylindrical vessel. Air is admitted at
its base atran angle. This gives tumbling action and spiral movements. to Working : The mixer is allowed to rotate. Along with it the baffles
the.powder. Thus mixing is achieved. also rotate. The ingredients are introduced into the shell through the
Thi! constructio.n and working of an air mixc� or!· fluidised 'r'i:iixer inlet. They begin moving towards the, opposite end of the blcrider due to
remains sa111e as shown in fluidised bed dryer in the Chapter Drying. tumbling action. Bartles furti1c:' r ci1hance tl1,e mi_;<ing. As the material'
I 1; 1 ; · ( • ....1 -� 1 '·' . •'. ,
,.
.• ••� }_ ·. :, · 1 -�· ! :; • ·, '· •. '•, · ' • , •. t • ; approaches the mid-point of the mixer shc.JL the b"artlcs are so positioned
.Advaptagcs' : Alr,.ti)ixer. shortens_ .�he mi.�ing time. It_ is �?eful AS �
to cause the feedback of part of the material in the direction of the inlet,..
throµgh-oyt'p�t,·, Mi�ing-is intimat�_ and e_fti�Jcnt.
, _ .
is �� so use d for w�t
_
J end. The n10vemrnts are shown in. Figure 8-12 using arrow markings.
oranulation in tablets. With add1t1onar attaehnients, thi. s equipment 1s
The feedback action continues l!P to the discharge enc!} where another,
:seful for rnixing, wet massi11g and drying in the wet gra'nulatio,n method.
set of bafn.:s guides the mnteria1 to the discharge port. The overflow of ·
This method is also used for coating witl.1 some modifications.
,, ...... ·-· .. -:.. material causes tin: blended solids t(i discharge. Since charging and
lk;dia?·g.i11g ar.:. simultaneousiy done. the proce�s becomes continuous.
IlARREL TYPE CONTINUOUS MIXER
',. .. �

.•
Principle : In a barrel type continµous mixer, the rotating shell keeps
\ '•

ZIGZAG CONTl1� lJOUS BLEN[);f.R

the material under tumbling rnotion. The presence of baft1c.s further Princi11lc: Zigzag continuous blender is a rotating shell type having
enhances the mixing dction'. When the material approach the mid-point several V shaped bkndcrs' connected in <;erics. · The material ·undergoes
of the shdl: another set or'baffl�{- causes part of the nrnterial to move tumbling motion. When the IV section is in\'ertec.L the rr;aterial 'splits
towards the <lirc�tion of:inlet end, .�llowing the remaining part to move
inio two portions; one-ha! f of matci·ial moves. b;1ck ward (iiito the 'preced­
forward. Such a mechanisri:l provides intense mixing of ingreJicnts.
ing section). ,,llile another-half or material moves forward. Due to
Thi:- pro .;ess continues up to disch;rgc end, \�here ,mother set of baffles
inclined axis of the shell tow.irds the discharged end, the material gets
1

�uide the inatcrial to the discharge port. The blenJ.':d material at an ·

1 discharged. /\s the lirst V section clears the 1:harge'. a Tresh feed enters.
�quilibrium State O\'t.:r0ows from the discharge e1;d.
Thus, it is used for co�tinuous blending of so!ids:
. . ,, ' • ,! �·
l:onstruction : The construct:on of a barrel type: mi'x�r is shown in Con5truction : The construction of a zigzag continuous blender is
Figure 8-12. ' 1 It re'sembles a: large cement mixer.. Baffles are fitted�to.,th� shown in. Figun: 8- I 3.. The shell takes the shape of. several Y shaped
inner surface of the shell. The shell is fixed to a shaft, which is allowed
Inlet hopper-ingredients
metered in

: �r\l' _.;-q�. �' .

./
., I \ L,

Direction of material 1 Material inlet

J
flow : , , ' 1
, .

r \
� �\ v�(!
/l:?{;C,�
•, �
__ _
Charge
cham!J.er

t:l
180 ° rotation
M;w shell

'/ '
Mixer baffles
Mixed-material
discharge 350 ° rotation
. Fig�r,e 8-12. Construction of barrel type continuous mixer. Figure 8- 13. Construction of zigzag continuous .blender.
 224 J
1'111\RMACEl lllCAL ENCilNE°l:RIN<i Ch·M MIXING 225
blenders connected in series. A chamber for charging is attached to r>r1e
end of the shell. The other end allows the discharge of material. The
shell is inclined towards the discharge end.. · Section-II MIXING OF LIQUIDS
}�'.�r�ing : A single pre-weighed charge is introduced into the chan.?,c
cham\:>c\., As. �he' shell rot�\cs, at 'one p�11icular angle (Figure 8-13)� a Mechanisms of Mixing
mcte:ed m��ff!HI. :�·1.1tcrs the V-shaped section by gravity. With each Mixing Vessels or Tanks
, Mixing Devices - rlow Pattern
rotation,. �nc�haY,( of the blend matcrial moves downward back to the
Mixing Equipment
preccdins.leg'and..anothcr-l1alf of ihc material moves forward to the next
leg.ofth,e blender. lri'each rotation,' a p:frt of the material moves t�\\;ards
· ' : ·· :
the' discl1argc 'en.,cl.· .· :<·' · ·•. · · · : · ·. /Liquid-liquid m1x111g is considered as a simple operation compared to
that of solid-liquid mixing.lJ't in�olves the formation of a homogeneous
. ' : .

As the fi�st :�harge clears the first V section. which may take only a
fc�· minutes, the next charge is added. The uniformity system. Similar to solid-solid mixing, fluid (or li'quidJ ·mixing also
. of blending
depends on the flow properties of the ingredients. � ·., . involves the a�pl- ication ofshear. Agitation and mixing are not synony-
mous.
Glossary of Symbols Agitation refers __to. the ind'uoed motion of, a material in a spccifi'ed
/\ "' Constant.
way. llSOaUy Tn' a circu!atory pattern. inside a container.
a = On:rall rraction or trac..:r in the mi:.;turc.
t = Time." min. � /,rfi�ing refers to the ran.do"m distribution into _or through one another
·
k = C:onstur.t. of two or more separate phase�
M,·r=:O�g�e:c,ofmi,ing or mixing ind,·,at time. t.
The nature or'liq�1ids mainly determines the ease of mixing'.I G:\ccord- .
n � Number of samples., ;��=--:::>
. ---..._,__�----.
RSD = Relative standard d..:viation. ing lorries of sqlutions, liquid mixtures are c lassified as follows.:-
<7 = ·standard deYiation � Miscible liguids : \�c are _rniscible__. in,all_prqp. . ortions. For
�; ·=-- Standard' deviation of unmixed powder. c;,alnplc, e..!E-yl alco�.o.d...wa��.n:..mis:" all.w.portions. These
<7R. = Stundard dc,·iation of random t-ih:nd. ..
y = Arithmetic mean (particle size or concentration). ··
liquids can be mixed easily by employing the· mecb�.isms\ of bulk
. ,,
t1·anspott and shear: Cosmeucs � (. flftcr-shave lot_io,n).· elixi'rs etc.. belong
y = True mean of the sta11dard. to this class.
Yi,· = The value of a given sample:
(2( P ar�qu:ds : T�e�� a.r�...misci.bte�i-n.. <Jne,.a,nether-cat
_ _ _
one particular proport1011. Their m1sc1b1hty depends on temperature and
QllESTIO� B,(NK
pressure:--For example, P;:SJ�soLruid· ,wat.e,r.-are misci�ttaib...�
· §_�ion. Mixing poses certain difficulties in the p7e.pa�atio_n o(disin-
Each question carries 2 marks
I. Me�tion the equipment used for solid-solid mixing. fectant solutions. . ·· ,
2. Li�t the equipment uscp for powder mi,ing in pharmaceutical' industrv.
. \
, ' I •
•
(3/1.l)UIHiciblc liq.uids .: As the na1�in.9.Lsi�S... 1ltes.e...ar� .not..misci­
l
.
C2(JJ.D1p.le.,.. vegetable oil� �vater are riot miscible gr the·
Each question carri�s 5 marks.
1
ble.�· .... For
- ...... � .. .� ..
mi?.1;i, ,blli.ty.. is-:v.err low:·
,..,_..,._ _, '
· .. Normally,
·� -�
they· form emulsions, . Mixing of
L E:,.plain the ,,orking of a mixer used for 1111, mg dry powder..; he fore
granulation. these liquids is very difficult. . A homogeneous dispersion may · b\
obt:1ined by adding e1nulsifying a�el)lS. Mixinp.,them requires high shea.!)
2. Explain the eonslruc1ion and worhing
. uf a ribbon bkndcr 1·or mixing soliJs.
'
3. Draw the neat sketch of the sigma blade blender and giw its "ork ing. The mixing of immiscible liquids i's discussed as ·a separate section.
. : .
In pharmacy, one of the liquids normally ·used is water .. A nurnbefof
Each �uistion carries 10 marks ll lid and liquid ingredients are added in t�e for'.nulat!?n of �o�?ge _'forms.
L Describe the equipment for solid-solid mixing ofpharmaceutical materials. Onsed on the shear stress-sh.ear rate rclat1onsh1p, fllilds ar� cJass1fied.as
·'
,:
 Ch-8 MIXING
PHARMACEUTICAL ENGINEERING 227
In the turbulent flow, fluid velocity at a giycn point fluctuates
'!)jewto.nian and non-Newtonian systems. _The general flow characteris­
continuously in���s; x·; Y: and z. · However, the.liquid moves
./tics of the fluids have been discussed in the Texibook of Ph;isicu't"·...,
. in one ·ai1·cc"G61'i'"dcpending o'11 thc-domin t component. In genera
.... P�maceutics. by C.V.S. Subrahmanyam (V�llabh Prakashan, Delhi). l, the
liquid has different velocities at different loca�ions at the sal'nc ne.
:Y
��ications of Liquid Mixing
. .{Jurbulent (ll)\�i.L;Lbj_ghly cffec_tive mechc;1J,1ism--for- · ··n . Turbu­
Giquid mixing promotes heat transfer bct�·een. liquid and a heating. ��t ·f1_o�!1-�C SC - ;ltt.COi�"pW_lC Of cgdtCS Of various SIZes.' �eddy
source. This step is essential in the crystallization of drug substances. A.sle+rrrcd as a portion .
of fluid moving as a u.nit in a dircction:JLarge
Uniform heat transfer in the solution yields crystals of same size. for cdd ies "kncl to hreaktip fon:nirig eddies of sihaller size: u�1ff f1Tic�� are
no
example agitated batch crystallizer works on this principle. longer distinguishable. An additional characteristic of turbu!cni flow
is
Liquid mixing process is essential in the manufacture of a number of ) s intensity, which is related to, the velocities with which eddies
dosage forms. Some of them are listed below.
,. move.
Laminar Mixing:
\1

I Preparations

/ Suspensions
Phases mixing
���Lquid
Examples
��iocJotion
-lu,a-'.1�r ''.ifyin._,,_ is U.1'.' !)Jixin� o(..Jw� ..dissj_milac li_q11ids through
�ntnar flow, _1..c., the @Hl1�!2ear stretches the intcr!ai;> ' between thew.
Emulsions Liquid-liquid �!!rgxL.h..er_ wuite �n this _111cch�ismr··la��!��l �.E�E-J � .:_lvcs . Thus the
J� �
(immiscible) emulsion num�cr of laycr�.1ncr,9�se� �en :c, the ,interfac1al arc� betwee .
n them
� _ _
/Solutions Soluble solid-liquid 13 Compl�L��ir also 111creascs cxponent1aliy 'Nlth time. M1xin£ may·aiso result in simpl�
1S�.u.ti. ons · Soluble lig�id-liquid Alcohol-water (elixir) stretching of the fluid 1�,yers without any significnn, folding action.
T.his
_._.....-.
I Chloroform-water is also suit:iblc for liquids, which require moderate mixing. .
(preservative) -�-'-'---+-''--'-.;c...:..;.=.::c.:.:_::.:.=...:.:.;:.
....,, �

Sal�utamol inhaler 1U:ol�la.r.Djff�3.!orf'..

f Aerosols · 1
Liquid-gas
h (Mo._Tecul'!� diJJusion is the mixing at molecular level. in which ..
' •

. ..t{ mol-
�!i_f��� due /0 th';rmar rriotioni, . . . 'J ,. ,
"" + .
� _1\1.ECHANISMS OF MIXING Molecular diffusi?.!!)��xpla'in.ed by the Fick's la� which depends on
of liquid m1xing can be studied under four_ classes.
.1:he mech�isms .the con_<:_�n_tr�ti�i'(g���nt it q1fferen_L,[.�g1ons-(:ffhf �o�centration
,,

_ grad,i­
They are: �nt decr��es_ with t1�� and it reaches.zero w�en ?1ixmg 1s c�mplet�
.Bulk transport 1.e., equ1hbnum condition. When molecular diffusion and laminar flow
•Turbulent mixing occur simult aneously, molec ular diffus ion reduce s the sharp
, Laminar mixing discontinui�iJs at the interface;' between the two layers! .
'
I Molecular diffusion Simultaneously more than one me�hanism may· operate during mix-
. B k Trans u! ing.
1 ·
: ' J]ulk. transport is defined as the movem�nt of a large porti�a
•:;? materia,1 ffom"one io�ation to another"locatioriin a given system./ �xfr;i:� VESSE�S
frhe n1ixing apparatus consists of. a container (tank) and a mixing
��-,. · Fo� this purpose, mixing �vices such as r_?tating.JiJ�Q.£��.W.�•.p,addl
..
·•
dc�e. :'hese are asscrnblcd and used for a batch proce�s. � �,nll
� · arc u�d. which moves' the material in differne t dir�ction�.' - ___..,. ,.,,.
' ,,
c��truct101=1 of the mixing tari'Rcrr contaiRs'f is sli�1c "8=14
·
1 · · ire· o . 1..m.i�ck.Yic,e is
nlled _imp::llcr, which is· mounted with the help of a shaft. )"he shaft is
, tlrivcn by a motor.
I
 Ch-8 MIXING
228
.
PHARMACEUTICAL ENGINEERING'
MIXING DEVICES-FLOW PAITERN
_( Mixing devices are USC� !9 su�plt.:��o the s stem so long as to
\_ Motor Lidt. , _
bring about r�as�r;ibly r�p1d 1111xmg. Flow currents are· responsible for
,· I
transportJJJg unm1xed materials to the mixing zone. ·
.,
!'..:i�1g C::YJ&c_s . '.'ue.chiii.cgU_y-eaJfod<--a·s-•1mpellers .. IIT'pcllcrs arc
• .
classified on the baSJS of the shape �nd pitch of the blades that are
-..Jacket
attached to the central shaft. 'Three main types of impellc"rs arc used
Baffle namely, propellers, turbines --··and
---paddles.
----- These are discus·sed below.
· .
\

Impeller {i:o rs {"'

ro eller norm�ll con 1_;1in? a number _g.(bladcs (Figure 8-15). A
_
I � _ cd ·.dc�1gn 1s the nf'ost common for I�guids. � marine type
lad
'... p_ropcllcr 1s similar to the blades of a table fan or a ceiling fan.

- n/_:_ .
..
/ Shaft
' outle�_,,/·t.._
I . \.
Figullt 8�1�. Mixing vessd o � tank. �
, The tank is mad� up of stainless steel. The toA of the tank may_ be (a) Side view . (b). Top view
open or closed. It is constructed with tank diameter to liquid height· ..
Figu re 8-15 ...J;ropdlcr type oi"rifixing devices.· A three bladed design.
ratio� T!1e .size of t?e tank depends o� the p�t�r�.-�Lthe. agitation_ _
m_!tl10d. The tank bottom J.S"-roup_ded (not flat} to el111}(n�te sh__arp comers,' (t_r?pellcrs may be ,either right or left handed, depending on the ..
.
or regions into which fluid �vould penetr6te. · It a<so carries an d�1ll¥ d1rcc�,o� ofsl nt ftheir blad�i) Four bladed or toothed dr similar design
: �
coils, jackets, tci;n pcrature measurin_g devi_ce etc., '\h:reyer n�cess�ry. propt:1 lci-s a1 _ t: us1:. d fo r special. purposes. In a deep tank, push-pull
_ .. _
p,opcllcr 1s used 1n which two or mo're propellers may be ;ittachcd to the
Baffles : Containers can: be .either. baffled �unb<}.ffled. Baffled
same shaft. Thes� work in opposite directions to create a zone of high
<r_p'ntainers are those in which metal strips1baf{lesLa.te.i.plac.�al'ly ·
turbulence. he size of the ro eller is small, i.e., the ratio of diameters
to the in�eE11�.L�_µ.rf°'ce. When bulk transport is impo.rtant 1n mixing, -
between pro eller and container �nt or Jow viscous
baffles.aie used. Thes1! are particularly }fesip!,le 'in the iriitiat s'tag'<!s of
mixing when segregation is present on � forge scale.· ,Baffles facilitate. �qui s. _However.
. for Jar e tanks the maximum s.ize of O. es
interming1ing of the liquids eveq from remote regions of the mixer. propeller 1s used. Small . ers turn at full motor s eed u to 8000
��lJl�
-·-j. ·- . ..baffies
In· most of the cases four are sufficien1.. Even one or two .
TJ}e ro eller produc�longitudinal) movement of th · uid.
baffles provi_de a strong effect on mixing. The widttr6f the baffle may T hc flo �v u rrents leavmg t e propeller continue through the liquid in a
be from j£J.01h to 1/! 81h of thf? tank diameter., If solids are pr� in the . . _
given d1rcct1oh until deflected by the floor or wall of the tank.
liquid to be mixed, the baffles are fixed with � gap or abouLn-..
, . ) ·. . jUses : Propellers are used when high mixing ca�acity is ncedea.
0

· �ill��Jr��-1etween the baffle and the tank surf�ce. .

_ '.., .
· The above discµssion ·,ncludes contaLners in. which the Ji quids mov_�.
One
. In some cases, the container, itself moves to mix the liquids. .
example is �mi�i:,>y::oscillatory movement l:; applicable:on a small
scale whereas rotary mov'emcnt is applicable on a large scale., Shaker
mixers are r?,rely used in'pharmat�/
rhesc arc effective in handling liquids having..a maximum visco;ity of
abouU.O paS£als·!;econd and slurries up to lOo/v;olids of fine mesh si.ze.
�he� ca n_ be .use� upt�J.1_me!f.�- cube (or 3500 litres). Effective gas­
liqu1d d1spcrs1on 1s possible at the laboratory scale. Multivitamin elixir
disinfectant solutions are manufactured using propellers. . '
I.
.
 ri'tARMACEUTICAL ENGINEERING
Ch-8 Ml:\ING 231
. . or slotted ring; which surrounds the turbine. It increases shear forc.!;:,S.
Disadvantage : Prope llers are not nonnally effective with liquids of
.. .vi9cosity greater than 5. pascal·sccond, for example,· glycerin, castor oil The liqui9 pa'sses through the perforations rcduci!lg rotational swirli_ng_
. etc. and vortcxing. J .- • , . •: ...
(' .
�ses : Turbines 'arc cffecti°vc for. high viscous s'ofutions with. a very, .,
J.lurbints
O
.
, • • .
wide range of viscosities upto l.o-0-pa'scal·seconds. A few examples ar�
�..
f. A turbine consists of a circular disc to whi��--n�n}���-rt
. bladesare attached. <Eigm6 s;�-.- The·ar--·er of the turbine ranges syrups, liquid paraffin, glycerin c�_r;:. In low ·viscosity materials of large
\:-Olumcs, turbines generate 'sfro�1i;currC!}}S (intense shear) whjch spre�d
· frd 0-50 · ercent of the diameter of the vessel. It ro ates at a lower
throuehout the ·rank dt:stroying stagnant pockets. The/ can handle ,,
·..c__::�..._th'""an propeller (50-200_ tion r minute). Different orms of slurri�s with 6.Q%doliqs. Turbines are suitable for liquids .or lacge·,
terbines are s wn in Figure 8-16. Th�e� �b�la�d;!_le�[llilµ�����LUicU.,
volume and high viscosity, if the tank is baH)e.d.· · ' ,, ',
.... ., )

ty·· ''�£h,ft
� Advantages : Turbines give 'greater sh�aring forces· than propcl.lers,
Circular disc though the pumping rate is less. Therefore, turbines are suitable for
.emulsification.
/'/
f.f>actdlcs f' '
/_A paddle· consists of. a hub centrally- �vith�wo long� �
Top view Side. view ·. att�hed to it vertically '· igurc 8-E7.);. . _ · : ,·
I '

(a) G.:ncral assembly of blade disc turbine or flat bladed turbine.

'*1
· Flat blade
I__,·
..----r-,...:__. � 1@:::::J .
� ··� . ' '

cb.
Hub I'

(a) Side view (b) Top view �1

• I 'j I
!
<
r· 1

:; . Fig4re·8-17. Paddle type of agit.ator. or impeller. I !� . :

� � ..,,
' � ·" •' ' 1 ' I

ddks with 'two b'lad s or four s are mmon. Sometimes, the

• .\ ' ! ;', ·1

· Open straight Vertical curved Pitched blade

•blade turbine blade t1.frbine turbine blades arc pit;he . In some ,paddles, the ,9l'ades. are dished.,.or.;- c_mi­
sphcric;il in sha c and 'have a large surface area in relation to the iank in
·(b) Various. types'.of turbines
p __,,. whicli'ihey.. arc used. li$cause of .!_his shape, paddles pass .�·to_the
Figur/8-16. Turbine impdlcr (or mixing element). tank walls and effectively rtiix viscous liquids, avoiding dead spots and
.,____ '-
ids. ·.•·
<--
-:_..,.i,
.• '

A.. .J flat bladed turbi dial and �- flQi'w', . but as �

•
spec increases, radial flow dominates. f,. pitched blade JW:b!oe Q_ro- . A shaft' carr in hub-blades rotates at a low speed of aI 00
!
QllCCS axialfl_ow� rev.,Q.luti-0il&-
_ -pcr_miuu�e. us 1 . 1qu1d radially and tangentt T y
� · �i:notion unless the.blades are pitched.. In deep tanks.
.
:, 1,'it�IJ isec;,fi�,..a���Jit'lSl:.J�� i�d moye throu_gh lhe several paddles- arc attached one above the other on the,same.shaft. At
Q,ui�,per 1:e\'olut1on, 1f_sltp�age doc�. .n�t occ�. very low speeds it gives mild agitation in an unbaffled t�nk,w�ere as for
.
, Near 'the impeller,. the wne of rapid curre!)tS, high turpule�cc and higher speeds baffles ��e nec;es�ary. · Otherwise, the l,iquid .is swir,led
i�tense shear is observed. The shear produced by turbine� can be further l\round the vessel with little mixing.
enhanced using a dif!user ring'. A diffuser ring is a stationary perfo�ated
I
 - .,.

232 . PJ:IARMACEUTl<;:AL ENGINEERING 233

.
· Ch-K MIXING

· J.Iffs : Paddles are. used in the' manuf�cture, of ari��_uspeosions

(

(aluminium hydroxide gel and magncsium_hydroxide), agar.and pectin

related purgatives, an;tidiarroheal J'l')ixtures such ,as b\smuth-kaplin. ,,
· J�vatrtage : Vortex fonnation.·is not possible with paddle impellers
because of low speed mjxing.
. . -Disadva:ntage : 'Mixing
' of the suspension is '.P.QQr, therefore, baffied
· · · ·· · --
tanks are required: ,,
(a) Tangential or (b) Radial flow (c) Axial or longitudinal. flow•' -<1 <"
�attcr� Durin��ixing circular flow (top view) (top view) (Side view)i
�iq�ids are m,ixed usually by impell�rs, which ·produce shear forces..�
for inducing nece�sary flow pattern i11 the container.. Mixing takes place Tangential flow
due to the resultant eff�Gt ,of three components acting on the liquid.. (circular flow)
These are radl�J_�qmponent, longitudinal_fomponcnt and tangeritial
· · '' com- .. ··
ponent (Figure 8-18). . Strip of·
f liquid in
. Tang.cnil:!,!i.£..q_!nponei:i,t ((>r circular-).: It ac'ts in o_.di1Tct1on taogent\ a vessel
to the.-cTfcf� of rot.rt i91) a-i-c:i und the .impe4 ler shaft ( Figure 8-1 Sa). If shaft Radial
is placed vert-ically ai1d·ce11trally. tangential flow. f6llows a circular path· flow --4
around the shaft and creates a vortex i.n t.he liquid.
.fuul.i.u.Lc.o.m.1HHt�Q.t : 1t acfs i� a. direc.tion' vCillraL.10...lb.e :...imp.dl.er.­
I
I -4- Shaft axis
I
shaft (Figure s:18b).,, Excessive· radial ·now takes-the material to the
cont;incr wall. then material falls to the-bottom1 and rotate as a mass
beneath;thc impeller. Lorigitudinal flow
i·
(axial)
.,\{ial component r(or 1dngitu�i�:3�l or.. ".cr:tjcn.i{ It acts in a_ 9.ir.£��
Ji£riJf�i:.ill�..!Q.f'c;·unp.<;Jkr..,sb.aJi.(,Etgttr�Nk7:-···ln:fdeq't�te I ong fti.1dinaI (d) Diff�rent components of flow at a horizontal strip of liquid section.

componen! c�uses .th� liquid a_nd solid tbrotate in ,layer�. ,�i�hout 1�1.ixing. Figure 8-18. Diagrammatic representation of a cylindric· al tank
.,., Adequate lon'�itudit1al pattern ,� bq! used lb generate strong. vcrfttal with tangential. radial and· axial flow. Each diagram represents ·
currcnts'p:;iiticularly when''s'uspcndin!.! solids arc p;·esent in a liquid.
one type of flow (a, b. and c). ln usual sit�ations, one or more or
a combination of these flow patt�;ns occur simultaneo�sly (d).
', ;,··1 .. "1j. r I j•, - . ,I
-., · Thesj: m�y ,OC!,:Ur. singly or in va· rj9us_combinations. A satisfactory
j ·\ .. r ,l) .
.
/
{'I"
Uortex- Formation
flow :pattern-:-.ilepends on· the--balance,of the c�mponents. The flow
patterns of different impellers'are given in Table 8-3. :>.' ..
/
A strong circulatory flo\Y pattern sometirnes maiifests into formdtio;
.
---
of a vortex near the irri.pclle'r shaft (l:igurc 8-19).'
I .
--·

Vortex can be formed when:

•.±· . • -� ..•I"'__.;_"'.. .... -.... � ....-,... •
,

/'- The shaft is mounteri,.\vertically in the centre of th<; �tank, i.e.,

• l

sym1;:;;t"ry.-Sucham�tfnfing "te11d· ro·-i· ncfiTctbnge�tial flow. ,,

I•

Impeller type· Flow component

-rro�llcrs
. /'
� �ia1'
1
,, r_ Bbdcs in the' turbines
· are arranged perpendict.lar
'

· to the central
\ '

Turbirles-,_ shaft.
. 1 '

axial or tange�(ial o'r both

,,
� At high impeller speeds.
,. \,\(
Pa�les ..... radial' and tangential not mdal
,:""..

- In unbaffied tanks.
·: I ' ,' .(.J.
Padd!lswith pitcn radial, tangential and axial
V I
 234 PHARMACEUTICAL ENGINEERING
Ch-8 MIXING
235

" ; •·'
. �t '
: ' Propeller sh�ft

'o/
�

�1.��
•. \
.

L J '· ! :. i-'',.

.figure 8-19. Vortex formation with a turbine type impeller

Si�ilar pall� is hservcd ith ropdler type also).
��� m t / .�
/ 1:fu.�t�·: Vortex form;i.tion. Jeduces the. mixing int!!nsity by
. l, :'.I! ,t..J
reducing the velocity of the impeller r�Jative to the surrounding fluid/ 1
(a) Off center 1 ' ,l, ..
When · vortex reaches· the i�1_1_J2e]ler, air from1 surface of the liqu_id is 1
: (b) Inclined
. , (c) Side entry
drawn. Thi�fs-antfo-desirabl.e sit:uation, peca'i. se air bubbles �-��.difficult 7Positio ns of prope llers with'flow pattern'in a'v�ssef,.to preve�t vortex
.
'fo remove. The entrapped air causes oxidation of the substances in ';, .. :',·, . ). . i.1 •\ . J. ;.··
, cerf�i11 cases. Ttie air'bubbles in the 'Quid can cr�ate uneven loading ·o�
the impeller blades;·. ·· . .. J , . • •
© . .. ,
, , ; ., , l A�
� �rey_�n_t!<?� ?f__v_��-�<:�__for_mi!lion : Vortex formation can be pre­
wnted b ny one of the following methods (Figure 8-20).
7.
�npeller 0should be moun_ted m a�y one of the positions lo :!void
symmetry (Figure 8�20:•1 ). At the same time, it should be deep in the
•
'•'° I .,, ··1 ;·.

liquid. •
(i) �� ri'trally pl.aced propell' i' ,, (ii') Centr
When the propeller is placed off centrally, a small amount of tangen- · � ally-,;raced propeller ·· , ' __.
. in a baffled ta[lk, side v1e,w . in· a baffle I W, · · 1 i"<i,l,
,d tank., top· v·e ,
tial flow is induced. This discharge stream will offset the swirl induced .
· ·_,, ;;.. farfan ger11e fllt of baffle s' and flow patter n i�;ia 'veilsel to· preverit vortei)(i . \
by its .rotation (Figure 8-20. la). ,
'CA similar. effect can be observed by placing the impeller in an I

inc!inediposition (Figure 8-20. lb). � ..,

In side ·ehte'ring propeller, swirl is seldom a problem. This geometry
, ., ti)
provides\{'..'6,affling effect and 'results in circulation of material- from t:ic
top to botto;n 'in' a vessel (Figure 8-20.1 c). The disadvantage for this
position is lt:akagc, there fort!, the packing round the shaft must be secured.
'1
I 1;:ritr is also a source of contamination .. which is difficult to clean.
Side
Qf Baftle·d- containers should be. uscp (Fig_ur� 8:20.2i). .In such a
case, inipel!cr can bl! mounted vertically_ at the center.
(3. Two, or p1or�. irripellers flre m,ounted on same shaft in a tank
where g,reater dcp_th· '. i� desir�d. This system1 _is known as push-pi1ll .J f

(;1) Propeller in an unbaffled tank(:: '(b) ·Turbine in a baffle'd tank "

mechanism. With 'such an arrangement c?.ch impeiler acts as a separate
mixer. Two types of flow ar_e· produced from impellers. The bottom 3. Arrangement of pu.sh-pull mecha..nism with
.
flow patterns 'in a tank t�' prevent vortex: . f'
impeller is placed about one impeller diameter above the bottom of the .
.j

tank (Figur� 8-20.3a and b). It creates a zone of high turbulence: Figure 8-20. Po�iti�ns of impellers 'with flow p�tterri in a
l'csscl to prevent. vorlcx formation and gas entrapment.
 236 P,1-IARMACEUTICAL ENGINEERING
Ch-8 MIXING 237
- '' Return Flow with Draft Tubes
Draft tubes are. placed to control the direction and velocity of the Position of the impeller : Central� off-center, side entry, vertical or.
flow to t�e impeller. I ' inclined et�.
'•I
Th'e return flow to an impeller of any type approaches from all Shape and size of the container Cylindrical or other geometric
directions, because it is not under the control of solid surface. Draft forms. Presence or absence of baffles.
· tubes can control at. These arc moui1ted around the propeller (Figure 8- Cost of equipment and its mai11te11011ce.
21 a). In case ofi turb.ines, draft tubes· are mounted
· imme4iateJy above the
·· ' C. Process Related Factors
• impeller (Figure
. 8 ;- 21 b).
'
Speed of rotation of the impeller
i� :� •I
..·. .c_....L....
I
Baffles-':)
I
Time rl!qtiired for mixing
,,,, Amount of power that can be expended
Ease_ of operation
. Draft " .., Batch size •
j
· tube
The general mixing apparatus are disc�ssed earli�r. · Tl)ese are used
for batch operations, which involve assembling �f different ' parts. It is

)•
. . , _ · {at}�ropeller _ {b) Turbi�. e 1,\, • • ,_
Fig�re 8-21. Fl�\\ ,pattern of liquid in a baffled 't�nk vJi!h 'draft tubes
'Uses: Draft1 tub$!�-?lre,f!ti�d to: equipment _used in the manufacture of
certain emulsio'ns. When solid particles terid to1. float on the' surface of
the li�-:i1. id, ·ther an; dispersed :using draft tubes. -Airjet mixers for
continuous mixing of liquids employ draft tubes.
s ''. . .
, Di_�advant�ge : pr�� tub�s add to the fluid frictJ�)n in the system.
These reduce the rate offlow. So these are used only when required.
i. J'
also possible to develop con_tinuous mixing equipment. Some of thern
i
are discussed below._
' " i : .
AIRJET MIXER
Principle : When compressed air jets are pqssed from the bottom of
a vessel, air bubbh!s arc formed in the' liquid phase. The buoyancy of
the bubbles lifts the liquids, which are confined to the central portion
due to the presence of draft tupes. The liquids flow down fr�i'\1 the
periphery of the vessel and enter from the bottom due to suction e'ffect.
. Thus mixing is achi�ved.
Working.: The assembly of an airjet mixer is shown in Figure 8:i2.
The liquid is placed in the ve��el. Draft tubes are played S\Jrtounding �ir

l \ �/
j � .• -
jet as shown in· Figure 8-22. Compressed air or a suitable gas is allowed • 1,

j,• EQUIPMENT
The followr g factors1i'nt1uence the mixing of liquids in tanks. These
also help in sel�cting the equipment.
'., ... 'i! I .
"':••
,Q n.
A. Material R�lated 1 Factors
Tank
\\

.
Properties of .nq�ids : Physical properties of the materials to be
mixed. Examples are density, viscosity (Newtonia:n antl non-Newtonian)
and miscibiHty (intermolecular attractions). ·_
'ti Draft tubes'

Inlet
B. £quipl}'lent Related F2ctod for air L---�:::::::_..,,,,.
_ Shape. of ti(_� /;,peller : Propeller type, straight, vertical, curved or
pitched. .: Figure 8-22" Vertical tank with centrally located
· , · ., airjct and <lraf\ tube. Mechanism of mixing.
238 Pl 1/\RM,\CEUTIC/\l. ENGINEERING j
• �
Ch-8 MIXING 239 l

to pa ss at hig h pressure from the inlet provided at the bottom of the tank.
This causes buoyancy of the bubbles, which lifts the liquids from bottom _ When .a rapidly rn�ving liquid .comes in contact with slow moving
to the top of the vessel. ( or almost stationary) liquid,. high velocit); gradient w,ill be developed �t
the boundnry.. As a result, �fKrng shear stresses. exist at the. boundary'·
Draft tubes serve to confine the cxranding bubbles. and entrained
wh ich induce foixing in two ways. , '
-:
liqufus to the central portion. This results in· a more efficicn't lifting . . · ·· · · ' •..'
.
action by the hubbies. T h e liquid mixture flows down from the periph­ (I) The st esses tear off portions of th e fast movin_s stream and send
�
ery of the vessel. The ov erall circulation brings liquids from all parts of it off mto the ,slower moving areas as vortexes or eddies. The
the vessel to the region of the jet itself. Thus mixing is achieved. . shear stresses tear off eddies and generates considerable turbu-
lence. which contributes to the.mixing action. .
Uses : Liquids of low viscosity, non-foaming, non-reactive with gas (2) :Y hen a slow moving · l.iq�id �nters ;he jet, the volu�_e of. jet
are mixed by using airjct mixer. _ decreases.
mcr�ases and velocity This decreasing velocity catJses .
lhe Jet to expand. Thus shear develops which aids \n mixing.
JET MIXER
Principle : The liquids to be mixed are pumped sep..rately into a jct ..Enough time and space must be provided for. .
the strea�·
thornug hly into the mass of fluid b)' the mec�ani'sm of entr�inment.
to blend
mixer at diffe rent velocities. The. high velocity fluid has a lower static
pre ssure than surrounding liquid (higher static pressure). During mixing, AdY ntagt· : The power_ required for. pumping is ofien su.fficient to
� ·· ·
the slow moving liquid will be drawn in.to the high velocity jct. This accomplish the mixing operati'on. . . '
increases the volume of the jct and dccn:ascs velocity, which causes the
' /1,1 I
I

jet to expand. Thus shear is dcvciopcd and aids in mixing. \Pf.OW MIXER OR LINE· MJXER OR PIPE MIXER ·' ·...
Th e constructions of � baffled pipe mixer and a chamber. mixer are
.Working : The construction of a jct mixer is shown in Figure 8-23. shown in Figure &-24 and b, r spectively .•Liquids to be rn.ixed are
Two liquids arc introduced into the mixing tank at different velocities . � . �
One liquid is pumped through a small nozzle at uniform high velocity. passed through he pipe. M•xmg takes place �tainly through bulk
. �
The second qquid ente rs the tank at a low velocity. The fast moving transport 111 the direction of flow. Placing certain devices, such as vanes
liquid impinges on the slow moving liquid at high velocity. As the jet baffl�s, screw , grids d a combinati?n -of them, enhances ,th�.:.rnixin�
� ��
emc,ency. L,t le add1tron al -p:>wer .supplied to pump' the liquid itself
moves away from the orifice, the area of its influence dec reases. The _ � _
acco1:1phshes m1x111g - ,. . ·, . , . . . , .· '.,
core of.the jet is surroµnded by an expanding turbulent jet, in which the v
For an effective mixing, controlling the feed rate is' �ssenti. al.' Suit­

.rr · ;,·
radial velocity decreases with distance from the center-line of the jet:
able metering devices are employed. If input
�ate .i s. difficult to control
Nominal boundary
of the jet

<·>
Feed���'�
vf v �
' "" :�
� � �
--.. Outlet
--,.- \JI• ·, �

Constant
velocity core {b)

Feed

Figure 8�23. Mechanism.of mixing in submerged circular jct mixer.

'Figure 8-24. flow P�itcrn of continuous mixer yr line

mixer. ..., .
'- , •·
 Pl IARMACEUTICAL ENGINEERING
' .
and fluctuations in the added proportions of the liquids arc unavoidable,
continuous mixing equipment of tank type is preferable, because hold-up
.of the liquids and back flow or recircula�ion is possible.
Uses : When large volume of liquids are to be mixed, flow mix�rs . :·
··./Equipment . 1· · ' · ,', :d
an:. used... ·
(a) Baffled pipe mixer with little back flow.,
,)

(b) .Chamber mixer with flow induced recirculation and hold up. Mi>.ing of immiscible liquids is carried 'in pharm'acy inainly 'in· the
mar,ufactu,ring of emulsions .. The equipment used for the preparation of
an a!����� _:o�.Fler�V� a· fine_·e�n�!sion ·can .. be­
ob:arned and, . thcrcfore,. cquipmcnt 'j,; �.ts'o krio:\�itas ho1noge1iizer;:::. ':
QUESTION BANK
.
. ·····- ··�--j;

· Fine em.u-lsion'·1.s·-preparcd in tv.·o. stages.' :·1n· .the' �fst �ta ge,�co'a'�e

Each question carries 2 marks . , ·., '. �,-r-·�··� • .. :·..1: ; . ·;·��-)(-,"!�""" ..�......--;

I. Define and differentiate mixing and agitation. cm'..llsion is .£!:Cpared by usi��l_!c]!'\"q'e [Qjk,wing.: · ., . · - : · · ·� ·
2. Classify liquids based on their miscibility. Give one example in each case. · - wedge wood ' . porcelain mor'-ilr and pestle ; : ,•.. ' .
3. Enumerate. the applications of liquid mixing. mechanical blender milk-shake mixer ·
.
4.,,,:Describc
. the mechanisms for liquid mixing. _ - hand homogenizer ;- · propeller in a'baflled tank.
, s
5. What arc the factors affecting selection of a m ixcr'? Someti1i1cs, the above eguipment directly gives fine emulsion. Oth­
6. How are pipe mixers advantageous in liquid mixing? erwise, coarse emulsion is sJbf�cted to homogenization in the sc�
7. What do you mean by vo11cx? How is it pre.vented'? stage to get fofc emulsion by using one of the following. · .•
. . ···7·� s1Tversoi1 emulsifier .. ·. . . . -
Eacl: qu�stion carries _5 marks < Colloid mil ,.\ .
I. Give the characteristics. or mixing impellers. - Rapiso�ic)1omogeAizcr
2. Descr.ibe the operation of agitator mixers. .
.

HcnG ti1csc equipment arc also k 1ow.n as homoge,;izers.

3. Describe the turbine mixer with flow pattern.
,..
.

L
' .,

4. Suggest a suitable mixer and its operation for mixing of viscous liquids.
'

EQUIP�l!ENT ·.t
5. Draw a ncat-labdcd diagram of mixing tank with accessories for efficient Factors._l�Q-�cncillg t.hc Sclcciion � an_Erriuls_i_f��
Hquid mixing.
£Qu��J.fil9J!..��w:&l�--� B,i\cl1fj�� 0 p._i:::�on�inuous
. --·--· ··-
. '·�;

6. Dt:sci'ibe the principle, working and advantages of jet mixer. . . op,eratton. . · ., ·

· , ; •i.
7. What arc flow components for liquids? Explain their role during mixing.
·

F�ow eropcrt!!��.ids : 'Ne,1t,9_niEn, plastic, .P�C_l!9?.P)�stie:.::�

� I ., :I l �
,

8. What arc the reasons for vortex formation? What arc the drawbacks of ·· • -r ·' ·"·' ·
.dilatant. .;
vortex? Suggest solutions for the problems of vortex formation.
• .. · ';'·

T.£!Uperatnre maintcna,ncc : Mix.;ng will be effective at high tem . ­

, LJ..l · • -. ·'

Each question carries IQ marks pcraturcs provided the material s stable.

t. Discuss the devices used for liquid-liquid mixing.
��'ll..£2.Qli!l&...:Jf cleva\;:d ten,;1eratures arc applied.

L -· . ,.....
Some equip'm,::nt used for the prernration of . :nulsions arc described

- ·�
(Y'1Lf�=�N MIXER-EMULSIF{m�(··
: <l,

P·;inciplc : SiIverson n.1ixer-einulsij .e� p;;du·�es i:itens'c .��e.aring_forces

and t�1rbulence by the .usc-ofhigJ.,.-sp ,ed.,.rot-Ofs.,- This tu,·bulence
0
• .,t
causes
.

24'' ../
 'Ch-8 MIXING 243,
.
242 J 1'11/\RMACEUTICAL ENGINEERiNG
intense mixing action. Centrit:ugal forces expel"the contents of the head.
the liquids to pass through fine interstices formed by closely placed with great force through the mesh and onto the cover (Figure 8-25b). As.
perforated metal sheets. Circulat1on of material takes place through the a result a fine emulsion emerges through the openings of the outer cove�..,
head by the suction produced in the inlet at the bottom o!' the head. The .intake anq expulsion of the mixture set" up a pattern of circulation to·'
Circulati.on uf the material ensures rapid breakdown of the dispersed ensure rapid breakdown of the bigger globules into smaller globules.
. . . .
liquid into smaller globuks. Uses_; _Sjlv.c.rs.on...mixc.r_i.s_us.cd.-f-Of--ilie'!preparat-i-on of e111ulsions and.
. .. . . . . . .
creams of fine particle size.
/ Construction : The construction of a Si Iverson emulsifier is shoym
. in the Figure 8-25. It consists of long supp01ting colu11:11s connected to ��anta�c�
. �-- 0) Silverson mixer is available i� diffe;e��\[��s; to:
a motor which give support to the head. The central portion contains a handle the liquids ranging from a few. mii!iJ.itre�,sev.c::ril
shaft. one end of which is connected to the motor and the other end is thousand litres.-
connected to the head. The head carries turbine blades. The blades are
,�
(2}--Jt..can be used for batch ope��!i�ns_. It is als'o used for continu­
surrounded by a mesh, which is further enclosed by a cover having ...-:- OLIS Opefafto11-by- -inc-orporating into a pipcli�e, through which
openings: the immiscible liquids flov,·. . : · · .. ·
Motor /.
. pisadvantagc : Occasionally. there is a chance of clogging of pores
of the mesh. (' /

Central ��Q�'\\l·H:::l::.
rotating , . (rrinciplc : Colloid_ mill .is b«.s5!d .on the prLncipl� t)1at th.e. coarse�
sha�
cmul� i �l S i tcn ely shear d i � � U3lrr<;>W �p�CC between. thc .fast oving
: � .: n _s �_ '. _;:i · ·
rotDr_ arid staro tor a sho1t perrod· to get a very fine _
emuls1on.;9'
- Elecric
f
.,..-· . • ' ' \r
motor' Colloid mill is a mixer as well as milling· equipment because size
" reduction is also si:nultaneouslv involv.ed .. The construction. w0rkir1-<>• �'
_, I I4

advantages and disadvantages arc discussed in the Chapter 6, Sizl!

Shaft
Reductio:) J
Circular
Stand covering ULTRASONIC EMULSIFIERS-RAPISONIC HOMOGENIZER
of the head
· Principle : When a liquid is. subjected to ultrasonic· vibrations,
Emulsifying alternate regions of compressil)Il,' and rarefacti�n are produced iri the
head
Immiscible
liquid. Cavities··«rc fonned in'the regions of rarefaction, which subse-
quently collapse in the regions of compression. This results in the
..
liquids
generation of great forces for emulsification. ·
(a) (b)
Constr�ction : The ·constructiori. of � Rapisonic homogenizer is
Figure 8-25. Construction
� of Silverson emulsifier.
� shown in Figure 8-26. It consists of a pump driven by a motor. It is
W�g : The emulsjfier head is placed_ in the ve�sel containing .connected with an inlet tube and o·utlet tube for the discharge of a, fine
immiscible liquids (or coatse emulsion) in such a way that it should get emulsion. The homogenizer ·head consists of a flat jet for liquid inlet.
completely dipped l� the liquid-.--When the motor is started; the c�-�� facing the jet;' a thin blade is present with edges facing �ach other. This
rotating sh'att rotates the head, which in turn rotates turbine blades at a blade vibrates at itsnatural frequency of about 30 kilohertz.'
· · very high speed. This creates a pressure difference. As a result, liquids
are sucked into the head from the center of the base and subjected to
 Ch-8 MIXING · ills .
1
24J PIIAR-'VIACEUTICAL ENGINEERING
(3) As th;s method is ... �ighly efficient to d�rease. glo,'·�.iz/."' · . «:i
. � 'o

· Working : Coarse emulsion is pumped into Rapisonic homogenizer reduced concentration of �mulgents is su�ficicnt, . , . / , , i. :·
through one end of a tube. A powerful stream of liquid is forced (4) Its capacity of mixing liquids ranges from 2q. t�- .5.00 litres per
through. the jet. Liquid impinges on the blade causing it to vibrate. The minute.
streaming liquid deflects on either side alternatively with the result that (5) In Rapispnic homog�Jrti;.ze�, heat. is not g!!nerated during mixing
1
_\.. . 1 J '1 ' )
, ' '( ,; �

oscillatioos above the sonic range are produced in the liquic;I. During I unlike'"colloid mill. Hence thts' is suitable for' thennolabile>
this process, the emulsion experiences alternate regions of compression substances.
. . /

and rat<:!faction. . In the regions of rarefaction, cavities are formed.

'; · i .. )
.
; .I .' .. � I
',
Because of exterl1al pressure, the cavities collapse violently afterwards. Disadvantage : Rapisonic homogenizer is. u��ful '.�mly� \V'!th,.1!'lui.9s ,o°f'.\ •
. ' . - '·:' �' ' .n.:.. ..... '·, ,;··.\tf ;, . .
Thus sufficient turbulence is created which is capable of causing disper­ low visc.osity. .
.�·,>! .. ·.·. .· �· ··,:.·.... -,�.. ·,;j� :J!!1' . .'. · .. 11.'1,' �,,
sion of phases: Thus a coarse emulsion is converted into a fine emulsion.

Section IV-MIXING OF SEMISOLIDS

.f '·Equipment ' .;·'\'•

. ' � '1 .

Scm isolid dosage for.ms_ i�clude; ointments:. pastes, creams, jellies · etc.
While mfxing such dosage for-ms, the material must .betbrought-to.the
agitator Qr 'the agitator must move the material throughout the mixer.
Jet of
The mixing.. action includes·combination of lov"...1.P��h.e.ar��:smearing,
liquid wipin1.7
... _.,..._ ,;...
JQJ.gjng,�--s,ti:�t.clung. and...,,.........
cqID-1?£�§.�ing. ... A large amounio me-
chanical energy ,is applied to the material by moving parts. Sometimes,
: ,·. �'1
inlet
a part of the supplied energy_ appears as heat. The forces required for
efficient mixing are high a9d cons,�mpti.on of power is als� high. Hence,
the equipment t'l'!USt be ruggedly constructe4 to. tolerate these forces.
Vibrating
blade Mixing equipm_cnt are. also used for prepari�g tooth:��tes; pill masses
and wet m_as�.for ·granulation., ..
I ,

· ,, ; •
'.',;) j • �....,._;.� �

So,ne semisolids exhibit dilatant property, i.e., viscosity rncreases

---- ----
-·--i�-
----- ---
-------·--
�
Immiscible
liquids
with increase in shear rates, Ther�f�f�.' inixi_n_
1
speeds. The speed must be· changed accordingly to thixotropic, plastic
and pseudoplastic materials.
g i;n�s,t be done at lower

., " '. l, . ,·: '. ·: ·';:j.1 · �,, · ·

Figure 8-26. Construction of Rapisonic_,hornogcnizcr.
. EQUiPMENT' 1 ·... · ·� . ·····.·.,. ,: " -.·...•
Ad.�antages: (1) Rapisonic homogeni�er can be �sed either for batch assificatioli o'f Equipment · · . .. ): /. . · .. , . ·: _' ..: :'
•
•· • " ·,. , ••, .,. ,.· •• • ·.,-,;., '·. ,J ,.., '

process by placing it� in a tank or for continuous process by · ... ·.,r- ·

�itator mixers : Exa�1ples are sigma mixer a!1d planetary mixer.
keeping in � pipeline. In a pipeline, the time of exposure is less
. for a gfven sample of liquid in one pass. So, mixing may be �}?" mixers : Exampl�s a,re; tdple· roller: m_ill: an� :c�llo_id�I n�i.il_ ;.
incomplete. To ensure complete mixing, liquids must be
recirculated. "-"'Sigma blade mixe· r and planetary mixer are disc�ssed, in the :solid­
solid mixing. Co"lloidal mill is ai1�_cuss�d in_t\1� Chapt�r 'Size lled�ction'.
('2) It has. the capacity to produce dispersed globules of one micron
Triple roller mill is discussed here. ..,..--.
size.
 /
247
t�ction
Ch-8 MIXING
, ;:IAl"1.ACl'l!TJCAL ENGINEISRINc'
i�� . . . Between second and third roller. the gap is small and produces a thinner
of M1xmg Equipment. for Scm1sohds
,, film of iced. The speed of the third roller is increased to compensate the '
�ysical 'prnperties of the materials - density, viscosity and reduction 0f cross sectional area. In the thinning filin, more crushi.ng .
� · · iniscibility. 1 and more abrasion arc developed.
�conomic considerations regarding processing - time required
. • · ,

· f-inally the scr�pper removes the material complct�ly from the last ·
' ixing and po,icr c6nsumptio�. · .· roller which can be collected immediately into the receiver or trans-.
ported through a suitable conveyor. .' � .
�
<:U:::• nt an d its ffi� intcnance .
Advantag/: Triple roli'�r ;nil! i�c;· suitable for continuous processes.
11
Extremely uniform dispersion i� obt�in 9
;1,{R:PL::;��::
-)7( Principle : The differential speed and the narrow space between the. - �- -
rollers develop high shear over tile material. This shear causes crushing ·.· ,'l"
of aggregates, particles and also QUESTION. BANK
· distributes the drug_ uni(Qqnly_ through
·. :

· ·
·'

oiet the semisolid base.

•,··. .. '.:� ;_ ..
. -
1. Each question carries 2 marks ,. · . ·
I. Sul!l!cst suitable mixing equiprnent for s�'inisolids.
I • -�. •' I ' • � •
i. - .

Construction : The construction of a triple roller mill is sliow11 in

2. Describe the diffen:nl fac�ors influencing the sclecti6n of an cmulsi tier.. ' ·
..__ •

Figure 8-27. It consists of three parallel rollers of equal diameters.

·\ , 1 1·.;.-1•'): ,·I .

These arc made up of hard abrasion resistant· material, normally stainless Each quc�.tion carries 5 marks·
steel. ,The .rollers are mounted in a rigid framework horh.ontaliy. The 1. Describe th� constructi,;n and working of a Silverson mixer-emulsifier with
pressure and gap between the rolle· rs are independently adjustable. A ·tht.: help of a i,cat diagram.ii,· , .. .': ..
hopper is arranged between the first ;two· rollers. A scrapper is attached _ :
to the last roller. , ' Each qucstior."�arries JO marks ..,
.� I. With a neat sketch; describe the construction arid working of cquip�cnt for
mi.,ing pastes and plastic masses. What· arc tli'cir pharmaceutical
app)ications?

'
Low
speed
Medium
speed
High
speed LIJ ,. Receiver

Fig'u·re 8-27. Con;truction of triple roller mill. ../"

�I� •

1Wo�king : The ga� between the last two rnllers is adjusted t· o be l·ess
than the gap between the first two rollers. The rollers a�e rotated at
�,• "' 1 '\.. ''.l
,; '

different speeds. In practice, the. first roller (receiving-roller) rotates at a

..
• "�
• I

slower speed compared to the second' roller.. Similarly second r�lle� , l.·.

. ,speed is less than that of third roller (discharge roller). ' � (I

"

· The feed·, is· passed through the gap between' the first and second
rollers.. The aggregates and particles arc crushed and then abra�cd by
the rubbing action of the rollers, which is developed due to different
· speeds of rotation. A. film of appr��iable. thickne�s of the feed is
produced. The material passes from �lo\v rotatirrg to fast rotating rollcr.
 Ch-9 F_ILTRATION 249
, :,I•';;.,:!
Once the prclimiriary layer of particles is deposited, further
•. .
filtration
'l .
.
is brought about wherein the �lter n1edium serves only as a: support.
The filter will work efficiently ·only after ari initial, depo.sit. . In an
9 industrial scale, large quantities of suspensions ar_e mechani�ally :han­
dled. After a particular pain! o"ftime, the resistance offered,by 1 the filter
cake is high . that virtually filtration is stopped. . For this r�ason, a
Filtration positive pressure is applied on the filter cake (upstreamtor negative
pressure (suction) is applied be1ow the filter medium (downstream).
I ' ,{ ,,}; ' J

·JI
Feed :. .:
i
\ ,•
Mechanisms .of Filtration
Theories .of Filtration
Factors Influencing Filtration
Filter Media and Filter Aids 'v
Slurry
Classification of Filtration Equipment
Equipment . ,
Filter medium

"1
Filt,'·atfo11 may be defined as a process of scparatio1{ of solids from a
11uid by passing the same through a porous medium that retains the
solids. but allows the t1uid to pass.throughI
/The suspension to be filtered is known as sluny. The porous ·r
medium used to retain the solids is known as filter medium. The ·
accumulated solids on the filter are referred to as filter cake, while the i I1 � >

clear liquid passing through the filter is filtrate./

/when solids arc present in a very low concentration, i.e., not e�c�ed­ Figure 9-l. Principle of ti!trati'on. · ,..,
ing 1.0% w/v, th!.! process of its separation from liquid is carted
clarification:./
�,/
({;'plications
. (

. ii ·.:, ,
'
d ): J

Production of sterile products : Air is filtered through i:J:EPA filters

Clarification is generally employed when contaminating material is
(high efficiency partkulate air·, filters) or laminar aii1bench .to 'obtain,
finely subdivided, amorphous or colloidal in nature. These solids tend
sterile air, which maintains good envi_ronment p�ior to' and duri.�g njanu-
to plug the filter medium. Several other processes having similar
facture of sterile products. 1 ,> · . <·: •
·· ·· · y.z�:r:·
mechanisms are decolouration, decantation, colation, expression etc. .
. . . : .:. ;��fl}
· A sqlution· is passed through·a bacteria proof filter in order' to ·obtain
Process of Filtration .
sterile solution, paDicularly whilm� heat stcri.(b�tion ,is, no,t suitabl� ,o� · . 1
A typical filtration operation is shown in Figure 9-1. The pores of account of thenn6labile nature of the contents. In case of. steriie
the filter medium are smaller than the size of particles to be separated. products, particles as si;nall as 0.2 µm sh9uld be .. r�moved,.cwhich
· Filter medium (for example filter paper or muslin cloth) is placed on a includes the bio-burden of fungi, bacteria etc ..
support (a sieve). When slurry (feed) is passed over the filter medium. · Similar 'facilities are required for the production of antibiotics by fer­
the fluid flows through the filter medium by virtue of a pressure difTcr­ mentation. recombinant technologies of biological products and vacci�'es.
ential across the filter. Gravity is acting on the liquid column. Therefore.
solids are trapped on the surface of the filter medium. · · Production of bulk dr�gs : S�lids of intermediates 0 and 'finished
products are separated from the reactio·n mixture by filtratior. t��hniques.
By this met�od. impurities can be removed.
. 248
 250 Pl l:\R�1i\CU;TJCi\L ENGJNEEIUNG
Ch-9 fl l.TRA T!ON 25!
Production of liquid oral formulations : Filtration is an essential '
" ' .
,> '··' ,' . . '
step in the production of liquid orals (or obtaining clear solutions v-l5cpth filtration : In this process, .slurry penetrates to a point where
(clarification). the diameter
.
.of solid particles is greater than .that of the. tortuous void qr·
(a) Dewaxing of oils. channel . . � iw
(b) Removing suspended oils from aqueous solutions. Examples are Depth filtrath.,n is aided by the'mechanism. entanglemeryt,., T�c sqlids
aromatic ,,;aters. syrups, elixirs, eye drops etc. arc retained with a gradient density structure by physical restriction or .•
(c) Removing of undesirable solids, which interfere with the trans­ by adsorption properties of the medium (Figure 9-2). I} is extensively
parency of the liquids. Examples are honey and fruit juices. used for the removal of small amounts of contaminants from relatively
(d) Clarifying the potable water. Jarg� volumes ofliquids (clarific�tion). These arc also used for roughing
or prcfiltcring pharmaceutical solu.tions. Examples arc c'eramic �rs;
Affiucnt and waste water treatment : Waste solids must be sl!pn­ - . . . . "'
sintered (bed) filters. . , . ,, • . . . :
rall!d fron1 the \\'ask liquid prior to iis disposal. Somctimu_s. the soluble
comr ..:nts arc pri:cipitat.:d and then scparatl?d by liltratiof..

Screen filter wi!h direct

. MECHANISMS OF FILTRATION/ passage of the tarrier
The mechanism whereby particles arc r�tained by a filter is signifi­ molecule£
cant only in the initial stages of filtration. Some of the m echanisms arc:
Straining : Similar to sieving. i.e .. the pa11icks of larger si?.e cannot . · qg o o �S!� Depth fil;er : Greater

. .'Iii � °".
pass through the smaller pore size of tile filter medium. � Sl O � O �� thickness and mo,1�/
. "rt""'

L
, oiQ • liq•id pathwa y
ln1pingemcnt : Solids having the momentum move along the path of .
•
streamline flow and strike (impinge) the filter medium. Thus. the solids
are re.rained on the filter medium. Figure 9-2. Types of filtration.

. · Entanglement : Particks become entwined (entangled) in the mass

of fibres (of cloth with a fine hairy surface or porous felt) due tb smalJcr
size of particles than the pore size. 'Thus the solids arc retained on 'the
@ TABLE 9-1
Differences Between Surface and Depth Filtration
Surface filtration Depth filtratipn
filter medium. .
The size of the particles retained is The size of the particks.·retained
Attractive forces·: Solids are retained· on the filter medium as a
slightly higher than the mean pore is much smaller th:in the pores
result of attractive forces between parti<;°lcs �nd filter medium. ·as in case'
'of·electrostatic prccipitatior..- �;( .// ·
size of the mediu� '-v..
through which Ouid. ' ''.l'.>Ses.'
tvlcchanical strength of the filter �chanical strength is high..
In practi e, filtratio1 1 y ��ne various mechanisms. : medium is less, unless it is
_ : ! 1f'
� y"ypes of Filtration .JJ . ·made of stainless steel. ·
. Aas low capacity )rhas high capacity
\ �chanism, two types offiltrati'on arc broadly identilied.1 The size of the particles retained The size of the particles retained is
�urfacc filtration (Screen filtration) : It is a screening action by, is more predictable. 1.£.,Ss predictable
which pores or holes of the medium prevent the pas�age of solids. Equipment is expensive because it Che«pcr because ancillary equipment
. The mechanisms, straining and impingement are rcspo1isiblc for sur­ should require ancillary equipm<;nt is not required.
1
(( such as edgc damps. whi9h should
face f!Itration. For this purpose, plates with holes or woven· si'!vcs are
f fie much liner tolerances.
used (Figure 9-2). Its ef iciency is defined in terms of m<:an or maxi-,
E-;arnplc is cellulose membrane Examples arc ceramic filters, and,;:,
mum pore size.
ti her. sintered (bed) liltt•rs. -------
252
253
/
Pl IARMACl:lJTICAL ENGINEEl{:NG

A special c.ase of depth filtration is the sliee/ filtration, in which thl! Ch-9 FILTRATION
slurry is passed through a series of pads mounted endwise to .the flow 9f Surface area . .
fluids. The pads commonly consist of a· mixture of asbestos fibres. Powder of grarnile bed visualized
as a bundle of capillaries
embedded in cellulose.
· Do'wnstream
The differences bl!lwcen surface and deplh filtration are given Upstream ---+ -
- >_ pressure, P2 ''
111
Table 9-1. Pressure, P1 ����������� t_ ,,,.:·. '
''' !·.:

Cake filtration : A tilter consists of a. coarse woven cloth through ---- L -�--,.
Flow rate·: m3/unit time...-:,
'which a concentrated suspension of rigid particles is passed so that they Viscosity
bridge th� holes and for.m a bed.
.,
'
�scuillc's Equation :J · · . · ·· . · ,
The,cloth may be ineffective when'· the holes are likely to be much 'filtra tion is similar to. the streamlm. e flow·
·
·. u1
V �·p 01se 11,
e cons idere d that . . , . .
larger.than the ·particles to be removed. Therefore, the cloth is presented c'api·Ilaries. Po1se u11le s equation . is:,
of a liquid under press ure throu gh . _
with a concentrat.::d suspension of rigiq particles that bridge the holes
and form a bed. The particles will be held back, while liquid pas.ses . 1rtJPr4
through the small interstices. Example i.s tilter cake made from diatomitc
(3)
Ji ,"e·-· --�
;:

( I 00 pm). This cake can remove submicrometc,r colloidal particlc_s with

8LTJ

flowing in unit_ time,

.

rate of flo�, i.e., volume of liquid

.'

high etJiciency. v "'" _

. . J where

L1J =
m /s (1/s)
3

pressure difference .across _the filter, Pa

�HEORIES OF FILTRATION m
>

r'= radius of the capillary in the filter bed,

h). m
The flow of" a liquid through_ a filter follows the basic rules that L = thickness of the filter.cake (capillary lengt
govern the flow of any liquid through the medium offering resistance. '7 =· viscosity of the filtrate,. Pa·s /.
The rate of !low may be expressed as: of part!cl� . and the !!quid
s
If the cake is composed of a bulky mass
drivirn� force a mult1phc1ty of capillary_
Rate = -----­ flows through the interstices (correspond to
) ,(I) h these may be expressed by
resistance tubes), then the flow of liquids throug
.tThe rate of filtration may be expressed as volume {litres) p1;:r ' nit'U
Poiseuille's equation.
time (dvldt)._y The driving force is the p:essur � diffcr�ntial between the lnrcy's Equation_· · • .
_ : . ·
found_. m th�, _fihe_r are
upstream and downstream of the tilter. 1 he resistance 1s n�t constant. It v .. Poiseuille's law assumes that the c_apillanes _
if t?eJength of a �a�11l�
increases witl1 an increase in the deposition of solids on the filter hi hly irregular and nonuniform. Therefore,
g correction factor for. rad1�s 1s
medium.· Therefore filtration is not a steady state. is taken ·as the thickness 'of the bed, a _
approx1mate�·and s1mp!1�ed.
The rate of flow will be greatest at the beginning of the filtration applied so that t�e rate equ�tion is close!�
has been incorporated mto
process-, since the resistance is minimum. Once the fil.tcr cake is formed, The factors i�fluencing the rate of filtration
an equation by Darcy, which is: ' ' '
its surface acts as filter medium and solids continuously deposit adding
to the thickness of the cake. The resistance to flow is related to several KA&'
V=---
factors as mentioned below. \ (4)
TJL
I
cake, m
..'

where' K = perme�bility coefficient of the

.

.
2

pre:ssure upstream - m), m2 .

pressure downstream A = surface are� of the porous bed (filter mediu
Resistance to movement � --------- (2)
length of capillaries
/

-...:.. -.. .
 254 1'11/\RMACU!TICAL. E:--:C,ISl:f:RIN(i
Other terms arc same as shown in equation (3 ). The term K depends
on the characteristics of the cake, such as porosity, specific surface area
and compressibility.
Pcrmeubility may be defined quantitatively as the flow rate of a
liquid of unit ·viscosity across a unit area of cake having unit thickness
under a pressure gradient of unity.
This model rclatc:s not only to filter beds or cakes but also applies to
other types of depth filter. Equation (4) is valid for liquids flowing
through sand, glass beads and various porous media. Darcy's equation is
further modified by including characteristics of K by Kozcny-Carman.,it
yKozcny-Carman Equation
f!oiseuille's equation is made applicabk to porous bc<l, based on a
capillary type structure by induding additional parameters. Thus the
resultant equation. which is ,videly us1:d for filtration is Kozcny-Carman
cquatiun.
v � ----
.l
• ---- • ---
.J
.JI' {,
(S)
,7.\'1 KL (1 - l/
\\h1;:c =- porosity of the cake (bed)
t,·
S I.I-= specifit: surface area of the particles comprising the cake,
0
? '
m�m l
: K = Kozeny constant
Other terms are same as shown in �quations (3) and (4). The Kozcny
constant is usually taken as 5. The effect of compressibility of the. cake
on flow rate can be appreciated from equation (I), since the flow rate ) s
proportional to r}/(I-c) 2 . A 10 per cent chan,ge in porosity can_produce
almost 3-fold change in V.
�imitations of Kozeny Carman equation : Kozeny Carman equa­
tion <loes not take into account of the fact that the depth of the granular
bed is lesser than the actual path traversed by the fluid. The actual path
is not straight thr hout the bed, but it is sinuous or tortuous.
/ · pressure difterence is app!ying pressure on the· surface of the slurry, i.e,,(
V �TORS INFLUENCING FILTRATION
. A simple straining process does not provide a co!'nplcte .description
�f how· particles are removed from a suspension. The particles are
exposed to a number of forces· including gravity or electrical fields.
Some of the factors influencing the filtration are:
Ch-9 FILTRATION 255
(I) Prupcrtics of the liquids-density, viscosity and corrosiveness.
(2) Properties. of the solids--particle shape, particle size. particle
char ge. density, particle size distribution, rigidity or.
compressibility of the solid under pressure and tendency of
particle to flocculate or adhere together.
(3) Proportion of solids in the slurry-rate at which the filter cake is
formed, especially in the early stages of the tiltr�tion.
t4) . Objectivcs---whethcr the sol ids or the liquid or· both arc to be
coikctcd.
<yemperature of the suspension. / ·
�tee Arca of the Filter Medium
According to equation (5), rate of flow of filtrate flowing through the·
filter is inversely propo11ional to the specitic ·surface of the tilter bed.
On the other hand, if the surface area of the filter medium is considered.
the rate of filtration· is directly proportional to the surface area of the
filter medium (equation 4). Hcncc .. the rate can be increased either using
a larger tilter or connecting a n'umber· o( sm�ll units in parallel. For
exampk, filter press works on the pri1�ciple of connecting the units in·
parallel. Pleating the filter paper or using a. pleated funnel increases tl.�e
effective .-;urfoce area for filtration.
J
Pressure Drop Across the Fiitcr Medium
According to equation (5), rate of _filtration is dire,ctly proportional to
t.he overall pressure drop across filter medium and filter cake. The
pressure dro.p can be achieved in a number of ways:
(J'-0'.
Gravity : !� simple method, of obtaining a pressure difference is
maintaining a head of slurry above the filter medium. T�e- pressure
developed depends on 'the density of the slurry.· As a. rough guide, a·
,head of IO metres. of water ,creates a pressure difference of I 00
kilopascals.
Applying pressure : The most common method of obtaining· a
pumping the slurry onto the filter. · '
'. ,,
The pressure difference obtained by, this method is greater thari that'\
is achieved by reduced pr�ssure. Industrial plan! may be operated at
pressure up to 1500 kilopascals. However, in the early' stages of
filtr::it1nn, pressure difTerence should 'be less. This is to prevent the p9res
of the filter medium from c!.ogging or plugging, which sub_sequently
incrcnscs resistance to the flow.
 256 l'IIARM,\(TlJ rtC/\1. l:NCill\l:ERl�(.i
R�d��ing pressure: The pressure underneath the filter medium may
be reduced below atmospheric pressure by connecting the liltrate re­
ceiver to a vacuum pump. This creates a pressure di ffcrl.!ntial �cross the
filter. This factor has limited applications, because the prcssurl.! differ-
• ence of about I 00 kilopascals may 'be achieved. Reduction of pressure
lowers the boiling point of liquids so that it is possible for the filtrate to
boil in the receiver. Apart from the loss of liquid. the vapour may
damage the vacuum pump.
Advantage of this method is that it is safe. If a par1 of the equipment
fails, it will collapse and not explode. Therefore. this method is__c(),m·
manly applied in a laboratory, where the apparatus is usually made of
glass. However, in the in<lus\rjal scale, the p!ant is usually constructed ·
with a metal that is able to wiihstand high pressure.
Centrifugal force : Centrifug�I force could replace the gravitationa(
force and is used to increase the rate of filtration. The principle behind
centrifugation is discussed separately in the chapter I 0.
Viscosity of Filtrate
According to equation (5), rate of filtration is inversely proportional
to the viscosit)' of the fluid. The viscosity of the liquid, not the slurry is
important, since the resistance to flow occurs as the filtrate flows through
the filter cake.
Raising the temperature of the liquid, which lowers the viscosity,
may increase the rate of filtration.. This is not practicable. if thermola-'
bile materials are involved or if filtrate is volatile. Another alternative to
decrease the viscosity is to dilute the filtrate. In this case, it is important
to ensure that by doubling the volumes, the rate must be more than
double, which should indicate the advantage.
In brief, surface area and pressure differences are the two factors,
which are applied, in industrial practice. According to equation ·(5),
other factors such as porosity also influences the rate of filtration. These
are discussed below with filte aids.
vfr:Mcdia . · ··.
The filter medium acts as a mechanical support for the filter cake and
is also responsible for the collection of solids.
#aracteristics : Filter m�dium sh�uld have the following chara�tcr-
.
1st1cs.
Ch-9 F!LTR/\TION 257
(I) It should have sufficient mechanical strength.
(2) It must be im:rt, for eGrnplc: it should not show ch�mical or
physical intt:raction.
(3) It should not absorb the dissolved material.
(4) It shoulJ allow thl! maximum passage ?f liquid, while retaining
the sol id,V" It means that it must offer low resistance to flow.
The resistai1ce offered b,/the filter ' medium is not si1......mificant in
large scak operations and can be. negleqtcd.
.. ...
\
, .,.
The 111:1gn ituJe of the resistance of the tilter medium will change due·'\
to thl! layers of solids deposited earlier, whii::h may block the pores or
may i'orrn bridges over the entrances of the channe�. Therefore, _the
pressure should be. kept low at the peginning to avoid the plugging of
the pores.· The usual procedure is to filter at constan( rate by increasing.
tile pressure as necessary. When i1ormal working pressure is reached, it
h, maintained. On.continued fittr..'.;tion, the thickness of the cake further
builds up and lrcm:e the rate of filtration decreases. Whl!n the rate is
uneconomical. filtration is stopped.· The filter c·ake is· remqved and
Ii It rat ion is resta11cd. . '
Vl\l:ltcrials
·. : The following materials arc.. used as filter.. media.
(I) IVon.'11 matc:riuls such us felt or cloth. Woven material is made
of wool, cotton. silk, glass, metal or synthetic fibres (rayon,
nylon etc.). Synthetic fibres have greater chemical resistance
than wool or cotton, which are affected by alkali and acid,
respectively. The choicc of the fibre depends on the chemical
rcactivity with the slurr)·.
(2) Perforated sheel metal. For .example stainless steel plates have
.
pores which act as channels as in case 'of 1netafilter (edge filter).
. .
(3) Bed of gnmular solid built up on a supporting medium. In some
processes. a bed of graded solids may be formed to reduce the
resistance to the flow.• Typical examples of granular solip. s are
gravel, sand, asbestos, paper, pulp and keiselguhr. ·The choke of
solids depends on the size of the solids in the process.
(4) Prefabricated porous solid unit. Porous solids prefabricated into
a single unit arc being increasingly used for its convenience and
effectiveness. Sintered glnss, sintered metal, earthenware and
porous plastics arc some of the materials used for the fabrication..
(5) ',\le111hrat1t.: jilil'r media. Cartridge units arc economical ancl avail­
able in pore size of I 00 µm to even less than 0.2 µm. These can
be usi.:d e: thcr as s,urfacc cartridges or depth type cartridges.
f
 j

< 'h-9 Fl I :mATION

259
258 ; I
Pll:\RMACl:UTICAI.. ENGINt:F.RING

(a) Surface f.ipe cartridges These arc corrugated and resin
treated p�pcrs. These. are used- in hydraulic lines. Ceramic
cartridges arc advantageous in cleaning for reuse by back
flushing or firing. Porcelain filter candles are used for
sterile filtration.
(b) Depth type cartridges : These are made ,�f cotton, asbestos
. ·or cellulose. These are disposable items.'since cleaning is
/' /' . not feasihl.e�
. 1
�terAids
· Filter aid forms a surface deposit which screens out the solids and
:·_also prevents the �lugging of the suppo11ing filter medium.
. ti It rate.
· Justification : The object of the. filter aid is to prevent the medium
from becoming blocked and to form an open. porous_ cake, hence,
: reduc.ing the- resistance to flow of the filtrate. •
• (a) Usually. low resistance is offered by the filtc.r medium itself,"but
as the layers of solid built up the resistance will be increa�ed.
The caj-e may become impervious by blocking of the pore in the
medium. Flow rate is inversely proportional fo the resistance. of
I k1s a porous structure ·and filtration can be eflici�nt.. The filter
the solid cake. ' · ·
(b) Slimy or gelatinous material and higl1ly compressible substances
forlil impe_rmeable cakes. The filter medium gets plugged and
·' . the flow of filtrate stops. · _
':. /
'jcharacteristics : The important .characteristics of the filter a-ids.., arc:
(a) Chemically inert to the liquid being filtered and free from impu­
rities.
(b) . Low specific gravity. so that filter aids remain suspended in liquid.
· Activated· charcoal is used for removal ·of organic and inorganic
impurities. Kicselg11lu is a su0c;ssful filter aid arid ·as little as 0.1
pcr1.;cnt c:in be aC-ckd to the slurry. The rate of filtration is increased by ..
� times or m0;·c. at th.: above concentration, �hough the slurry contains
20% sol"Js
lir:ig-of filter aids:' Filter aids arc _mostly used for clarification
pr cesses, i.e .. where solids arc discardc�. Different flow rates can b�
achieved dcpend}ng on the grade of the aids.
Low now ratc,'(fine solids)--Fine ·grade tilter aids-mainly intended
for cl:i.rity.
F:is_t now ratc (coarse solids)--coarse grade filter aids---acccptablc
The til\cr .iid can be employed in either one or both ways.
( 1) Firstly. a pre-coat is for;11cd over the medium . Fort'i1is purpose,
a stlsp�nsion 01: the filtei ain· is !iltcrcd to give a coaling up to
0.5 kg per metre squ.arc.
(2) Secondly, a small propo1tion of tilter aid (0.1 to 0.5% of total
batch weight) is purposely added to the slurry. �o the filter cake
i1id cf I to 2- parts per each part of contaminant is mixed in the
feed, t�111i k. This slurry is recirculated through the filter until a
clear f ltrate is obtained. F,iltration then proceeds to completion.
The body° 1 mix method minimizes equipment requirements and
)t , mination potentials.
.1
'SIFICATION OF FILTRATION EQUIPMENT

.· J;:;
.·\·

, (c) Porous rather tl�an dense. so that pervious cake can be formed . Et1uipmcnt ar� .dassilicd based on �he application of externa_l force.
Reco�erable . .
; : _is �d,;antages ·: The filter .. aids remove the coloured substances by (I) J'n:s.rnre fllters�--Plate and frame filter press and mctafilter.
.
a orbing them. Sometimes active principles such as alkaloids arc ('.!) l'ac1111111 fllters---Filter leaf.
. adsorbed on the filte.r aid. Rarely, filter aids are a source of contami­ (3) Ce111riji1gal jilters-Thcsc arc discussed in the centrifugation
: naqts such· as soluble iron salts, which can provoke degradation of chapter
�. sen�itive ingredients. Liquid retained in the pores of the filter cake is
; lost in the manufacturing process. Classitication based on the operation of the filtration.
(a) Cont i1111011s fi/1ra1 iun--Disch:irg� and filtrate are separated st-;:ad-;i
I . Examples of filter aids llrc: ily. and uninterrupt�d.
,,;·
Keisclguhr Talc Charcoal Asbestos
Paper pulp Bentonite Fullers earth r
V
'·
260 ·
I
I Pl JAR:-.IA(Tlll lC,\I. l:NGINEERIN(i Ch·'J FILTRt\TION 261
(b) Disco11ti1111011sfi/traticm-Dischargc of liltcrcJ s0liJs is intermit­ plates are used so that surface area increases and consequently large vol-•
tent. Filtrate is removed continuously. The opl!.ration should be l1tncs of slurry can be processed simultaneously with or without ,...-ashing.·
stopped to collect the solids.
Construction : The construction of a plate and frame filter press is
Classi ticati(,n based on the nature of filtrat1on; shown in .Figure 9-3. The frlter press is made of two types of units,
, (a)' Cake filt<!rs--Rcmove large amounts of solids' (sludg'c or crystals). ' '

Slurry inlet Filter medium "

(b) Clarifyi11gfilters-Remove small a111ounts of solids. '· , . , :·'.(.
(c) Cross-flow filters-Feed of suspension flows under pressure at a l Through channel

fairly high velocity acros·s the tilter medium�

/ .____
. �IPl\1ENT
In the bulk drug industry, solid is the desired r'.roduct. Its size,
physical propet1iec; and purity are important. These factors· should b'e
considered. while selecting the equipment and operating cornfaions. (a)
Filtrate outlet·
Some of them are: Handle to
rest on rod
.J'1'atctials related:
·
(a) Properties of tht: fluid-viscosity.
(b) Nature. of the solids-particle size. shape. size distribution
and p::icking characteristics. Clear filtrate Solids collect
outlet
(c) Con·centration of solids 'in suspcn�ion..
(d) Quantity of material to be handled.
..
(c) Whether it is necessary to wash the filtered solids
(t) · Whether any form of pretreatment will be helpful
r-{uipment and process related:
Vqu
(a) Flow rate. ·. \\\ -\
\ \ 1
(b) It should be absolute in the sense, the limit' tD lsize of
particles passing through the tilter should be known.
(c) It should be sterilisable by heat, radiatioh or gas (examples
Material
are ethylene oxide, formaldehyde etc.). enters
(d) Independently checking the efficiency of' filter.. · It should be under
economical.
' '

Different forms· of equipment are employed for filtration. Some of .

'

(d)
them are discussed below. (a) Frame-Maintains. the slurry reservoir, inlet (eye) for' slurry.
(b) Filter medium. •.
�TE ND. FRAME FI T R PRESS . ., :. .
� � � . (c) Plate along with sectiori-supports the filter medium. receiv·
.
·. Principle : The mecharnsm is surface filtration. ing the filtrate and outlet (eye).
The slurry enters the
(d) Assembly of plate and- frame filter press.
frame by pressure and flows through the filter medium. The filtrate is
colli;cte(on the plates and sent to the outlet. A number or frames and Figure 9-3. Plate and. 'rramc filter prc�s.
 { h·'I 1·11. rn. .-\TION 263
/ I .
Pl lt\RMi\('l�TIC,\I. ENGINEi:RtN(j
u
Slurry
.,. ;,
plates and frames. These are usually made of aluminium alloy. Some-
times. these are also lacquered for protection �gainst corrosive chemicals • •• • ·•• •
and m:.idc suitable for steam sterilisation.
j�
· Frame contains an open space inside wherein the slurry reservoir (
t
is maintained for filtration and. an inlet to n.:cciv1.• the slurry. It is Jr!�
Plate Plate
indicated _by two dots in the description (Figure 9-3a). The plate h:.is a
studded.or grooved surface to support the filter cloth and an outkt. It is
indicated by one dot in the description (Figure 9-3c). The tilter medium
�
.al"
(usually cloth) is. interposed bet\veen plate and frame.
Fr�mcs of-different thicknesses are available. It is selected bast:d on .
the thickness of the cake formed during filtration. Oµtimum thickness or
the frame should be· chosen.. Plate, ·filter medium. frame. filter medium Filter medium
(filter cloth)
and plate are arranged· in the sequence and clamped lo a supporting .,.;»

structure. It is normally describL-<l hy dots as 1.2.1.2. l so on. A number•
of plates and frames arc employed so th:ll f:ltration area is as large :is
necessary. In other words. a number of filtration units arc operated in
paralkl. C'hannds for the slurry inlet and tiltratc butkt can .be arranged
by fitting •:yes to the rlates and frames. these join together to Corm :1
channel.
In some types. 011Jy one inlet channel is formed. \\>hik each plate is
having inJividu�I outlets controlled by val\'cs.
Working : The working of the fraine and plate process can be
described in two steps. namely filtration and washing of the cal,.;c tif
desirable).
· Filtrc;tion opera:io11 : Th� working of a plate and· frame press is
shown, i'n Figure 9-4. s:Iurry �nters the frame (marked- by 2 dots) from
the feed channel and passes through the filter medium on to the surface
of the plate (marked by 1 dot). The, sol.ids form a tilter cake and rcmain
in the frame. The thickness of the cake is half of the frame thicknps.
because on each side of ·,e frame filtr:1tion occur. Thus. two filter cakes
arc formed, which 1111.:d ev�ntually in the q:11tre of the fran�c. In
general. there will be an optimum thickness of filter �akc ,for any slurry.
depending on the solid content in the slurry and the resistance of the
� dots) an.: closed.
tilter cake.
The filtrate i:lrains between the projections on the surface of the plate
and escapes from the outlet. As {iltration proceeds, the r�sis�ance of the
cake increases 'and the tiltrati<J n rate decreases. At a ccrtai1,1 point. it is
preferable to stop the procc�s rather than continuing at very low flow
rates. The press is emptied and the cycle is restarted.
-�·
Figure, 9--t. Plat.: and rramc lil11:/pr'Jss, prim.='ipk,or operation (filtering).·
Washing operat ion : l f it ,''is necessary to wash ._tf1c ti ltcr cake. th'e
ordinary pl:.ltc and frame press is unsati.sJactory. ·�a�cs arc built up
in the frame meeting c\'entuall_y in the middle. , This means that flow is·
brought virtually to a stand still. Hence. water wash .using the same
ch:rnnels of' the filtrate is very ii�oJicient. if' not impossible. A modifica­
tion of the plat..:··Jnd frame prl!ss is used. For this purpose, an additional ·•
.,.....__
channel is included (Figure 9-5). These wa�h plates are identified by
three dots. In half the wash plate.-therc is a connection• . from the wash
water channel to the surface of tbc.p!ate.
The sequence of arrangement ot' plat�� ai1d frames can be represented .
by dots as 1.2.3.2.1.2.3.2.1.2.3.2.1 so on (between l and I, 2.3.2 must be
arranged). Such an arrangement is shov,:n in Figure 9-6 (a) and (b) for
the operations of filtration and water washing, respectively.
The procedure for washing th/ ' ;ress is show.n in figure 9-6.. The
steps are as follows. .
.
' : ...: .·. ' .
(I ) Filtration proceeds in the ordinary way i.mti_l the frames arc tilled
with. cake.. ·� '
.
(2) To wash the tilter cake, the outlets of the washing plates (thr.ee
-
(3) Wash water is P,um'pcd into the washing channel. The water
enters thro.ugh the ,inlets on to the surface of the washing (three
dots) plates.
(4) Water passes through the tilter cloth_ and enters frame (two dots)
which, contains. the cake.. Thc-n water washes the cake, ,Pas�es _.
264 l'I IARMACEUTICAI. El':<ilNEERING Ch-9 . HI lRATIClN 265
through the filter cloth' and enters' the plate (one dot) do(vn the ' so that the flow resistance of the ca�e is equal to all points. Hence, the
surface. entire cake is washed with eqva) efficiency.
(5) Finally washed wat�r escapes through the outlet of that plate.
· Slurry. -..--,---.--,--....,p,-�--.-
. .
'I

'.
Plate --. _ Wash plate
(1 dot) (3 dots)

.
. ,· ;;
j
- E Frame Filter medium

-
.r: �
:::,O c....
O'I
C
lllnfllll!lllllllllllilllllft-: � E
(2 dots) r(cloth)
.r:"'
,· • • ' \ , ,I .• '1 !"'
.r:
I- u (a) Principles of filtration operation using the three types of plate and 'rrame.
.'
-�--.----'I�--.....
�. t

Water for
wa�hing

.. . . • .•
,o
�
"'
. �Wa'sh p(ate
E
!., ·I
.•

Plate
(1 dot) (3 dots) :

1
----------- Wash outlet
JI·
. (filJate)
Q ggggggggco
Frame
channel
j .. ,
filter medium
•

ocgg�gg���gg.
DQOOQDODODDO
'":c.,,' ·e·
(2 dots) (cloth)

-
QDllDDDDDDOD
�1;11J01IDDDDIHID
CDOIIIIDQDIIIID (b) Principles ofcake washi�g ysing three types of plate and frame.
....
"'Cl
0 0

.... c
QQIJDIIDIUUIIIU! 0
DCDOIIDIIDDCDD . . ' '-'�'·
,
J

'o O DCDOC:IIU:IDDDIUI
CDDDIDDIIDDIID. -·• Figure 9-6. Plate .ind frame filler press. ·
O
c ....
"' "' QODDDDOCIIJO
Principles of fihr;ition and washing. ..

____,
:x: e! "
.
"' . -
i

\.._ It should be noted that water-wash· is efficient only if ti;� frames are
'; ,·, . l full with f]lter cake. If the solids do not fill the frame complet�ly, the
·;"' ·Figure 9-S.-Platc and franic filter wash water c,rnscs the cake to break (on the washing plat� side ,of ti.le,)
press with water wash facility. .frame). then washing will be less· effective. Hence, it. is essential to
.1 'Thus wfth the help of spt!cial washing"pl::itcs. it is possible for the
allow the frames become completely filled with the cake. This helps not
wash�water'to flow over tne entire surface of washing (three dots) plate, only in emptying the frames but also helps in washing the cake correctly.
 266 J>I IARM:\CElJTICAL ENGINl:l'H IN<i
. I Ch-'l 1·11.TllA TION
··. .SJJec:ia/ 1wm·isiu11s : (I) Any possible' contamination can be observed
by passing lite liltrate t_hrough a glass tube or sight glass front the outlet (2)· The filter press is an expensive filter. The, .�1;,_P�>'.ing time, th,e
labour involved a11d the wear and tear of 1Hc cloth rcsult111g in
on each plate. ·-This permits the inspcctior} of quality of the filtrate. The
_,., filtrate goes through lhe control valve to an outlet channel. -
hiQh COStS.
. Ii'
.
' I

(:!) The filtration process from each plate cai{be seen. In the event (3) Operation is critical.·, as the frames should be · full, otherwise
washing is inefficient and .the cakc i:; Jifticult to. remove. :,
of a broken cloth; the faulty. plate can be isolated and filtration can be
..
I ' . "
j J,
continucJ with one plate less. · (4) Ti,c filter press is used for slurries cpntaining less than' 5%
solids. So high costs make it imperative that ti* filter press is
Uses : Filter
.
she.:ts composed ·,
of asbestos
I
and cellulose are capable used for expensive materials. Examples include the cel�ection of
of retaining bacte1Ja. so tha(steri'f 1i·ftra�e can be obtained. provided that precipitated antito,in and removal of precipitated proteins from
the \\'hole filter press arid filter 1�1e?itim have �!',!en previously sterilized. insulin liquors.
• Usually steam is passed th�ough the;a�sembled unit'for stcrilizati(in.
Examples indudc collection of precipitated antitoxin, rl!moval of �ILTER LEAF -
precipitated proteins from insulin l'iquors and removal of cell broth from Principle : filter leaf is an apparatus· consisting of a longitudinal
the fermentation medium. drainage 'screl!n covered with a filter cloth. The me�tianism is surface
.;.,,

l�eating/cooling coils arc inco'rporated in the press so as to 111:\};.•.!.,it

filtration and
applieJ to increase the r:ite. of liltratioQ.
.
. acts as sieve ()r strainer. Vacuum or press�1re can be
suitable f he filtration of viscous liquids.
Construction : The gcncr-al arrangement. of a filter leaf is shown in,
• '

j .;,. ,, ••

vantages : (I) Construction or filh!r pr\!SS IS Vl.!ry simpk anJ a

1\nurc· 9-7 ..It consists of a narrow frame enclosing a drairiage screen· o·r·
variety of materials can be used. :::- . ,·.• •

groovcJ pbtc..)'he framc m;y bc of any shape. �ircular, square or ..

t •'\:.-''
)
Cast iron for handlinl! c:ommon ,. substances. rectanQular. The whole unit is covered with filter cloth. The putlet for
- Hronzl.' for sm�ller u;its.
- Stainless steel is used ther�by contamination on be avniJ.:d.
the filtrate connects to the interior of the lbme throuuh
. suctio11. ·
. ; -
Hard rq�pcr or p\astics v.l1erc metal must be avoided. Filtrate
Wood i'or lightnc�s' though it must b.e kept \Vet. t
(2). It provides a largi:: filt.::ring area in a relatively small floor sp,1c1:.
It is v·ersatile, the capacity being yariable according to the Frame Frame
thickness of frames and the number used. Surface area can be
increased by eii1ploy·i'r1g chambers up to 60. Drainage
(3) The sturdy construction permits the use of considerable pressure canal Filter cloth
difference. About 2000 kilopascals can be normally us1:d.
(4) J;::fficient washing of the cake is possible. Filter Filte.r
cloth
(5) Operation and mainknance is strafght forward, because th,::re arc.
1 cake
no moving parts, filter. cloths are easily rcne\vahk. Since all
joints are external, a plate, can be disconnected ir any'leaks are
visible. Thus �ontamination of the filtrate can be avoided. (a) F[lter leaf (b) Filler leaf during filtration.
(6)�: '.(produces d� cake in the form of ,slab. Figure 9-7. Assembly of Ii ltcr lcJf.
\(f>isadvantagcs· � (f)· It is a batch filter,· so .there is a good d1:al of Working,: The filter leaf is immerscd'in the slurry .. Vacuum system
'down-time·. which is non-productive. is connected to the filtrate outlet. The slurry passes through the filter
; • :T 1
cloth. Finally filtrate enters the drainage canal and goes througlf''tli�
,1
/
268 Cli-'1 FII.TR,\TION �269

outl�t into the receiver. Air is passed to flow in reverse direction· which This channel offers rcsistarce (strainer) to the flJw of solids (cqarsc .
Pl IARMACElJTICAL ENGINEERING

facilit;ite's r_emoval of cake. � . .,
Uses : The filter leaf is satisfactory, if the solid content of the slurry
is not too,.high,. abou_t 5%, ,i.e., dilute suspensioi1s.
Advantages: (I) Filtcr'leaf is a versatile piece of equipment. Filter leaf
is probably the simpl:st form of tilter used for b�tch processes.
(2) · A number ,of units can be connected in parallel to increase the
sµrface area for ti ltration.
(3) Pressure difference can be obtained either with vacuum or using
pressure up to the order of 800 kilopascals.
(4) Labour costs for operating the ·filter leaf arc fai_r)y moderate.
(5) The effici�ncy of washing is high.
(6) Slurry can be filtered from. any vessel. Simply immersing the
particles). The clear liquid is collected into a receiver from the top.·
Construction : The cor.structioi1 and asscmb'ly of a metafilkr. is
· shown in Figure 9-9. The mctafiltcr consists of a series of metal rings.
These arc threaded so that a c:l��nncl is formed on the edges. It contains
a grooved dra:,�agc column on which a series of metal rings· are packect,
These rings are usually made of stainless steel and have dimensions of
about 15.0 millimctn:s internal diameter ,;n<l 22.0 millimetres external
diameter.
Each' metal ring has a number of scn1icircular projections (0.8 milli-
11:iefres in thickness) on one side·of the surface as shown in Figure 9-9a.
The projections arc arranged the same way up. These rings arc tightened
Outlet

· · 'ti!'ier in a vessel of water can wash t_hc cake.

Raised
Variants : Sll'eetland jilter : A variation is to enclose the filter leaf
in a special vessel into which the slurry is pumped. under pressure. In
this form, · a number of leaves are connected to a common· outlet to Grooved�
provide a large area for filtration., A typical example of this ki.nd is the rod.
' .. '

�I
' !

Sweetland_ filter shown in- Figure I 0-8. The vessel is cylindrical and R.1119 Endcap
filter leaves are arranged so that they arc supported by the uppcr par:t.
The lower part can be swung away. This permits the cake to be
,
· v
•
discharged by compressed air while removing the filter leaves from _the
vessel. Figure 9-9. i\ktalilter.
(a) Surface view of a ring. (b) Assembly of rings on column.

.. I Filter leaf
Slurry
/ ent'1'
pre�sure ..
1

• ap�li�d Slurry

Cylindrical
vessel
Cake Cake

Figure 9-8. Sweetland tiller

· �
Principle: Metatilter funct1o_ns as a stramer (surface filtration) for the · Groovedrod
-�- . -· . .
sepfiration of particles.. In this method, metal rings contain semicir.cular
projec;tion�, which are arranged as a nest to form chann�ls on the edges. Figure 9-10. tvk.:hanism uf q1tratio11 through m.:tafiltcr.

�.,
 270 l'I IARJ\1/\CE!J r;�.'AL FNGINFERIN(i Ch·9 1·11.TR/\TIO� 271
on the drainage column with a nut. Therefore, mctafiltcr is also known Construction : The construction or a cartridge filter is shown in Fig­
as edge filters. lll'e 9-i I a. Ca�tridge 'filter has a cylinclrical :.configuration made with
disposable or changeable f:lter media. These arc made of either plastic or
Working : The working principle of a mctafilter is shown in Figure
9-10. · -These filters arc placed in a vessel and may be operated by metal. It consists two membrane filters (sieve-like) made of polyprop);lcne:
pumping the slurry under pn.:ssure or occasionally by the application of a rrefilter and an actual filtct for filtration: A protective layer s11rrounds
them .. Tlic cartridges arc housed in a holder. A number of cartridges
reduced pressure· to the outlet side. The slurry passes through thl�
channels fanned on the edges between the rings. The clear liquid rises
up and collected from the 'outlet into the receiver. Mctatilter functions
as a straine,_- (surface filtration).
Slurry --4£.:� Filtrate
For the separati.cln of fo11.: particles. a bed of suitable material such as inlrt outlet
kicsclguhr is first built up. The pack of rings serves essentially as a base
on \Vhich the true filter medium is supported.
Vi.cs : Metafiltcr can be used for:
·j C�rtridge ''
- clarification of syrups Cartridge -+ A . -+ .-
-- filtr;,tion of injection solutions holder -. I .._ - t
- clarifo:;1tion of insulin liquo1s t 't
- filtration of, iscous liquids can be achieved by applying
pressure. Discharge cake
Advantages : (I) Metafiltt.:r can be used .under high pressures, �vith­
:.· out any danger of bursting the filter medium. . (a) Filter assembly.
(2) ·Running costs are low, as separate filter medium is not used.
Filtrate outlet
The volume of residual hold. up in the filter is less.
' ,· 'p ;,;, .

(3) · It can be constructt:d from .a material that can provide excellent

resistance to corrosion and avoid contamination of sensitive
products. Polypropylene
(4) It is an extremely versatile filter. It can be used for the filtrati0n
of very fine particles using filter aids. Large particles can be
protective layer___,
Prefilter ---1� t
._..,
,t
separated by building up of a bed of same particles: Membrane
.;,• \/\

[
. '<'
(5) Removal of cake is carried out effectively, by simply hi'�k­ filter (0.2 µn'l)
flushing with water. 4-'

(6) <:;:hange over .from one batch to another or one product to Inner
another is easy. support core
(7) Sterile products can be handled. End cap
metal seal
Non-fibrous
,vCARTRl,DGE FILTER support net
' Principle : Cartridge-filter 1s a thin porous membrane in which pre­
(b) Cartridge filter unit.
filter and ,nembra.ne filter are combined into a single unit. The filtration
action is mainl'y sieve-like and the particles arc retained on the surface. Figure 9-1 I. Cartridge filter.
 2l2 l'I IARMAC'ElJTIC'i\L ENCilNEERl!';G
Ch·'l FII.TRATION 27:5'
can be placed in the same housing. The housing is closed 'with a lief. . '
As it dips, vacuum .is applied in this segment so that the �olid is build up
The housing has provisions for slurry inlct and filtrate outlet.
011the surface. The liquid passes through the filter cloth into an internal
··
Working : The slurry is pumped into the cartridgt.: holckr. It passes pipe and'valve. Finally the filtrate reaches the collecting tank.
through c<!-qridge tilter unit by the mechanism of straining. The clear As the -drum leaves the slur�y section," it ent�rs the drainage zone.
liquid passb to the centre and moves .
UR to collect through the outlet. I lcre excess of the liquid is drawn inside. Special cake compression
.
Us�s : Cartridge filter is particularly useful for the prcparatio1� of rollers may be included at this stage, so -that the cake is consolidated by
particulate free solutions for parenteral and ophthalmic uses. This Jilter the compression of the cake. This improves the efficiency· of washing
holde_rwill process I 000 to 15000 litres �f sto;:rilc solution per hour. and 'tlrying process.
Vacuum is applied to carry the slurry° along ,vith the d rnm
Advantages : (I) Stainless skel construction permits autoclaving for· - . Drainage zone
stcri!.! operations. Water washing arrangement
(2) ¢"artridgcs with self-cleaning devices are advantageous. - Drying zone - dry air supply
(3) Rapid disasscmbling as \veil as reusing or filter media is possi- · - Cake removal wne
bic. Washing
(4) Cartridges are not brittle; wh..::n they arc dry.
(5) Th..::y arc usl.':d as in-line continuous filtration. which reduces
handling of solutions. It minimizes the chances of contamina­
tion.
I;'isadvantagcs (I) Cost of disposable elements offsets the· labour
Dr;:inage Cake removal
saving in terms of asscmhly and ckaning of cartridge clarifier:: zone zone
(2) A number of manufacturers provide the components. which are
generally not interchangeable between· suppliers.

DRUM FILTER
-�tary drum filter functions on the principle of filtering Connections to Scraper
the slurry through sieve-like mechanism on a rotating drum surface, · rotating valve knife
under the conditions of vacuum. In addition, co1ripress1on, drying (using Pick·up zone Slurry troug!1
hot air) and removing the filter cake (using a knife) arc possibk.
Figure 9-12. Drum filter.
Construction : The construction _of a rotary drum filter is shown in
As the drum leaves the d�ainage zo�e,' it enters the water. wash
Figure 9_-12. It consists of a metal cylinder mounted. horizontally. The
section. Water is sprayed on the cake. A sei;a�ate system of vacuum is
drum may be up to 3 metres in diameter and 3.5 metres in length and ;1pplie<l on the panel in order to suck (he wash liquid and air through the
gives a surface area of 20 metre square. The curved surface is a cake of solids. Wash liquid is drawn thrqugh the filter into a sepa1�te
perforated plate, which supports a tilter cloth. The Jrum is radially colkctirag tank. . · .. ..
partitioned dividing the annular space.into separatc compart111c11ts. Each
of it is connected, by an internal pipe to the centre of the drum through a Thcn the cake cnicrs the."drying zone, where ho(air is blown on'thc' ·
rotating v, alve. .cake. The cake may h:1ve the moistL!re content le?s th�n one percent.
Finally the cake is removed using a ·doctor knife and discharged. .
\Vorking : The drum is rotated at a speed less th:m one rev0lution
per minute. The drum just enters the slurry in the trough (Figt1rc 9-12). All these steps are completed in one rotation of tl1e dn'lm. Now the
· · ·•
drum is ready L<; receive a fre\'f lot of slurry.
 l.'h-'1 FILTRA flON
274 J> l l:\RM,\CEUTICAL ENGINEERINU 275
�p "' Pressure di !Terence across the n'tu:
·,· Uses.: Drum filter is used for continuous operation and is utilis.eJ to r , �a•
r Rauius of lhc capillary, 111. .'
'-=

filtt:r slt1rrics containing high proportion' of solids up to 15 to 30 percciit. S -= Speci(k :m:� ,if the particles comprisi
ng the cak.e in Kozen)·-C�rman
In the production of penicillins. the extract is separated from mycclium cquut1un. m"/m3.
(cell mass) by Jrum tilters. · These are used for colkcting calcium V ·"' R,itc or tiltrution. i·,e volumc or Jinu
J ·m unit· lime
'1 i<l tl l1 1�1ng ·
, m3Is. , · .
carbonat.e. starch and magnesium carbonate.
• .. :

Ad.vantages : (I) Cake is removed simultarn:ously during operation. QUESTl<>N BANK

Therefore. suitable for USC with conccntratcJ slurries. Each quL'slion carries 2 marks
I. l.bt lhi.: fac tnr� inllucni.:ingOn;::: l'�llC
(2) Tht.: labour costs arc very !ow on a.:rnunt of auto111aiic ;rnd _ or tiltrution.
continuous op'erntion of the rotary tilter. 2. Writ..: K,1J�ny�Carman equation .in<l gi\'c
its significance.
(3) The fi ltcr has large smfacc an.:a. 3. I.isl th..: functions cir lihcr aids.
(4) The speed of rotation can be varied and the cake thickness can be
controlled. F.or exa1nplc; if the solids form un impenetrab!C'
* 4. Gin.· the principle ot' filtration process.·
5. Dil'!i:rentiatc between prcssu�c tiltrution·
and vacuum filtration.
cake. the thickness may be limited to kss than 5 mi.llimetrt.:s. Ci. List 11 1..: properties of tilter aius.
_
On the other hand. if the solids an: coarse and form a �po'i"ous � 7. Distinguish filtration and c!arilic4tion.
cake. the thickness of 100 millimetres or more. can be obtained. 8. \\'hat ure tilter aids? Ciivc ti,·? examples
.
Disad\'antagcs: (I) Rotary drum filter i; expcn'.>iw equipment with Ea� h question carriL's 5 marks
.
complex functioning. lt contains moving parts and also rcquir.es !I(- I. Explain the m�chanisms of tiltrution:
a number of accessories such as vacuum pumps. vacuum receiv­ _
2. What arc fi lter aids'.) Name the, tilter
aids
ers. traps etc.
(2). The cake tends to crack due to the a_ir drawn through by the .
_
pracllcc. .
*'-3. D..:scribc the construction and wor
. . .
commonlv usc J in pharn1aC)'
, _ .. • . . .
(

vacuum system. This makes washing and drying processes king of a rotary continuous � l tcr..
Ii �. lkscrihc the constructi
ineffici�nt. in·and 1,wking of leaf' filters.
'.

(3) The rntary tilter is suitable only for straightforward slurries. It is Each q ucst.ion l'arriL's IO marks
less satisfactory, if the solids form an impcnneablc cake or it is I. Explain the 'construction, work.ing adva
ntag
difficult to remove the cake adequately. press. . · .. ' . . �s 'and disa
·. d\·�n..tage
, . s o. f. filI ter
1.
Variants : String discharge rotary filter: It is especially used for 2. Exp!aiq the theories of filtratio11 givm · cipl·e,··' mec
· · · · g-· t I1c ··· prin
factors affecting· the process. - ·hanism and
filtering the fermentation liquor in the manufacture of antibiotics, where ." ·
the mould is difficult to filter by ordinary methods, because it forms a 3. _With a_ nt.: t dia rarn, describe the �oni
� � tructi�;;· an · d ·working of a suitable
' felt-like ca\..:e. A number of loops of string are kept on the drum surface,
1 m�ustnul tilter for h..indling of high solid
�011taining slurries., . . , . .-
· :which pass round the drum. The cake is formed on the strings. These -t \V llh a � c at Ji gram, describc the cons
·;;;trings lift filter cake off the filter medium and is thus remo,ved.
fi I ter su11abk �lor
clari(ication of syrups. :in·
tn;�tion ·and \,:orking �f ' industri�I

Glossary of Symbols ...

/\ = Surface area of the porous bed (lilter m.:c..lium), m2 .
i: = Porosity of the cake.
ri = Viscosity of the filtrate, Pa·s.
K = Constant in Kozcny-Carman equation.
K = Permeability coefficient in Darcy's equation, m2.
L = Thickness of the cake (capillary kngth), m.

10
Centrifugation • Biopharmace '!tical &f!�lysis of_dJ:ugs : Drugs present in the blood,
Theory of Centrifugation
Classification of Centrifuges
Equipment
Centrifugation is a unit operation employed for separating the constitu- .
ents present in a dispersion with the aid of centrifugal force..
Centrifugal force is used to provide the driving force for the separa­
tion. It replaces gravitation forces in the sedimentation. Centrifugation
is particularly useful when separation by ordinary filtration, is difficult;;·
for example, separating highly viscous mixtures and colloidal disper- ·
sions (particle size less than 5 mm), in which difference in the densities
is less. In short, centrifugation provides a convenient method of separat­
ing either two immiscible liquids or a solid from a liquid. The equipment
used for the separation are known as centrifuges.
Process of Centrifugation . , ... ,, . . ..
The ce:itrifuge consists of essentially a container in_ which a mixtur:e
of solid and liquid or two liquids is placed and rotated at high speeds.
·
The mixture is separated into its constituent parts by the action of- · ·
centrifugal force on their densities. A solid or liquid of higher SJ>ecific
gradty is thrown outward with greater force. Therefore, it is retained at .
the l ,ottom of the container leaving a clear supernatant layer o.f pure .
liquid.
. . ..
Th.· �peed of a centrifuge is commonly. expressed in terms of the
nun,l:er of r�\'olutions per minute of the rotor.
J. prli.=ations
Production ·of balk drugs : Centrifugation technique is used to
separate crystalline drugs such as aspirin from the mother liquor. Free
flowing product results due to the removal of traces of mother liquor an
··avoidance of effervescence.
d
. 276
Ch·IO CENTRJFUGATION 277·
. Produ�tion of
biological p'roduc;ts : M�st of the proteinaceous drugs
3:nd _. macromolecules are present as colloidal dispersion in water. By ·
n.orma_l_ methods, it is difficult to produce them in large scale.· Centrifu­
gal methods are used for the separation of these constituents from water.
Insulin can be obtained in pure form by selectively precipitating other
fractions of proteins and subsequently separating them by ultracentrifu­
gation. · Centrifugation is employed for separating the blood cells from
blood.
tissue fluids and urine are normally present in the form of colloidaJ
dispersions. Centrifugation is used for separating the drugs. ..This
method is essential for the evaluation _of pharmacokinetic parameters and
bioequivalence studies. ·
. Evaluation of suspension� and emulsions : Centrifugation method
is used as a rapid empirical test parameter for the evaluation of suspen­
sions and emulsions. Normally, creaming is slow process in emulsions.
This process can be hastened by inducing stress condition (using a
centrifuge). A stable emulsion should not show any signs of separation
even after centrifuging at 2000-3000 revolutions per minute at room
temperature.
Det�rmination of molecula r weight of colloids : Determination of
molecular weight of a polymer is not possible by usual method. Ultra­
centrifugation methods are used for determination of molecular weight
of serum albumin, insulin, methylcellulose. Centrifugation (ultra-cen­
trifugation) is also used for ascertaining the degree of homogeneity of
the sample. For example, insulin is a monodisperse protein composed of
· two polypeptide chains, whereas gelatin is found to be polydisperse
protein with fractions of molecular weight I 0,000 to 1,00,000.
· This chapter deals with the principles of centrifugation, equipment
used ,and examples of the use of the methods in pharmacy practice,on
. '
commercial scale. .. , . . · .,
. ._ __ · ·
• - I • �
THEORY .OF CENTRIFUGATION
[n a colloidal dispersion, the diseersed phase may be either a solid .or
a liquid. Particles having a size�� S µm sediment at the bottom due
to grav_itation force. In such cases, · separation of solids is possible by
simple filtration:<ff 'particles are of *e order of s µm or less, they
undergo Brownian motion. Hence; they do not sediment under gravity.
Therefore, istronger force, centrifugal force is applied in order to
.
278 PHARMACEUTICAL ENGINEERING
Ch·IO CENTRJFUOATJON
279
se�e them. The sedimentation also d�pends 9n �e densiJi,:s 9f the
dispersed phase and dispersion ��i� - . 'If_the �iff¢rence in !'e cfe�si­ =-=-
ties of these phases is [� again separation is 'di�cult By apj,lyiilg mgr (3)
gr
centrifugal fore�. it is possible ·to facilitate
. - (in.crease the rate of sc:dimeii- ·B�t " = 2nm, -:V.h�e n == s� of rotation (rev
.tation) the separation p� olutions per second of
centrifuge). Substituting this in equation (3) yields
·
Centrifugal Effect or Relative Centrifugal Force (RCJ?
The centrifugal operation is described by equations including the
C= (2nrn}1
.
gr
,,.
4,,2,1 n1 4,,Jr ,,Z
o; --- (4)
gravitatiol)al constant. The derivation is as follows.
gr g
Since 2r = d, where d = �iameter,of the rotation Substituting the
Consider a body of mass m kg rotating in a circulat,path of radius r value
in equatlcm (4) giv�s: .
metres at a velocity of v metres per minute (Figure I 0-I). 'llhe force
2,,Zd ,i1
acting on the body .in a radial -direction is given by: C=---
(S)
g
Tb.e gravitational constant has� value of9.80
· 7 mJs2' so that equa1ion
(5) can be simplified as:
Centrifagpl effect = 2.013 ,Id (6)
In equatiqn (6), n is exprcs.1ed in s-1·- and d is in metres.
Whether the measuranent of d is made · from the free surface of
Figure 10-1. Principle of centrifuption. liquid or from the tip of the tube to·the centre of a centrifuge should be
. mv1 mentioned· while reporling the centrifugal effect.
Force acting in rpt/lal direction,. ·F = -. -. (I ) . Pf9m eq,-iatiqns (S) and (6), it can be inferred that
r -"'centrifugal effect cc diameter.
- Centrifugal effect or: (speed .of ;otation)2.
whese� F = centrifugal force, N . . . ""
The same body is exRCriencing gravitational fo� (newton). lt � .. ��uatioq (S) hell>$. in-th� selecticm . \ .of the tyf,e of centrifuge and other
� _expressed as:
· · ·• · · .
experimental
.. condidoiit"-
,.
. .

Gravitation/or:ce, G· = mg
- _If it is fequired to increase the centrifugal effect, it is o( �r
..:_,· ;,,· . (�)
advanfige to use a centrifup of the same siz.e ara-�pr speed
whe,c g = acceleration due to gravity, mJs2 rather than using a l!l(Pr centrifuge at the same specci olro�n.
�- cortrifogal e/fecl is expressed as a tafio of centrifugal force .to - lt i, •lways 'beUer:to..use the, smallest si:ze-of centrifuge � bas
gra\tftational force. ,In other words, centrifugal effect is• force, wbicfi'Js the appropriate capacitya since .the .centrifuge (eqd1�) is
a number of times glQter than the gravitation force.. subjected .to CO!J,1iderabl� Jtlffl in ,operation, larg,Jy due to....the
Separating power of a centrifuge is expressed • a ratio· of·� p�ure·of "1e· ,Ouid-.on ,tho '111.fs. ,lt � be s6oWJt ·dianhe
�fugal force to the gravitation accelerat.ion. This' ra�o may have •. .P..rrisw.r,. Js di� :J>�q"1 - to the sq�. of the s� and
Yalue as high as 1o4. .• _ tJie .diamet�r· .J'hi.sprin�_lple. is �eru, for ttie separationof>two
. ' liquids as .i�-�inulsions. · · · · · --...;,__.� ,,
The centrifugal etfect can be expressed �; - 'The, 'tentij��' is �iped ,to suit· the required purpose ,If. a
'_ .·- · · . . . f� acting.� radial_ di!f'C�� :.F_, ..··: . �: iifofllJ8fcrial �· to bo processed and a low ce'!tri.�aal
:c
. ..Centr.lfoga/ 4eet, Ci _ . . ,.. arilf;)Yi1 ·su,Ucimt to separlle,' then it is -eco�ical.
;
• • _ .•
graVitationaf force
.
•
---
- · ,· - . G. ·•• ·
� - • v.' .

\' ':· :· ,,,, ( . .

.dect
l {ll'go �c_entrit&,p �pcndio g at a lo w speed. .
_ tcf"Use a
-. .
'- �
., ..
....
\
--
280 PHARMACEUTICAL ENGINEERING
The centrifugal sedimentation of very small particles requires
_
high centrifugal effect. For this purpose, equipment of a small
diameter is used, but operated at very �igh �p�d. For example,
tubular bowl centrifuge functions on this prmc1ple.
The centrifuge is comparable to a pressu� vessel. Therefore, it must
be handled with the same care as that of a high-pressure autoclave.
CLASSIFICATION OF CENTRIFUGES
Centrifuges are classified based on their mechanism� of separation.
,
Sedimentation Centrifuge
· Sedimentation cen,;ifuge is a centrifyge that produces sedjmentation
of solids based on the differe(!�e in the densities of two or more phases
of the mixture.
The efficiency depends on the velocit)'. of rotation to w�ich the
mixture is subjected. Examples are horizcmtal continuo�� _ centrifuge,
supercentrifuge-mit!· conical disc centrifuge.
-ui���ntrifagation : When extremely fine solid ma�er is_ to be
separated from a liquid for example in colloid�! res�atch, ultracen_!rifuge
is used. In \his instrument, a relatively small rotor 1s operated at speeds
exceeding l ,00,000 revolutions per minute and with forces up to one
million times gravity.
- .
Centrifuges h�ve repl8':ed the �i� scpa�!� �o a co�sid�rable
extent in production operations because o��t1veness m separa-
tion.
-·
· ·· Uses�uspensions containing low concer1tration of solids can be
separated quickly.
� Lanolin is recov�red from the �oo.!J?Y_scoun�g p�ss.
�live and fish liver oils � putified by removmg dirt and water.
----
�- Jlie liquid/liquid phases are separated in-the e�tion of �rugs,
- for example, manufacture of antibiotics. ··
� Bacterial enzymes are prepiied by removing bacteria.
� Blood plasma is separated from whole blood.
� Starch is collected after washi� and purification � es.
-::!!>·
In the manufacture o� insuli� liquor is clarified so as to remove
- .
the precipitated l)N)lelns. • •
Ch· IO CENTRIFUGATION 281
Advantages� Centrifuges are C2!!!J)3Ct and occupy a very. small
space. · �
jJd- Treieparating efficiency is very high, so that the particles are
deposited very rapidly. It is suitable, if the stdiment is' a fluid ,..
depositorsfudge.
� Two immiscible liquids are easily separated on a conti�uous
process.
�By �ontrolling the speed of rotation and rate o� flow, C<>3!'5C
. .
particles are separated, while finer particles remain in the sus­
pension.
Disadvantages : (J.)A'he construction of sedimentation centrifuges is
complicated.
�ts capacity is limited.
Filtrati9n Centrifuge
Filtration centrifuge is a centrifuge in which solids pass through the
porous medium based on the difference in the densities of the solid and
liquid phases.
In this type the container contains a porous wall through which the
liquid phase may pass and on which the solid phase is retained. Exam­
ples are@rforated basket �_fuge an� .�mi-contin1:1C?us centrifyge.
The soligs that. fonn a porous cake· can be separated in the filtration
centrifuge. Normally· perforated wall is covered with a filter medium
such •as canvas or �eta! cloth.
-
Uses : (1) When solid recovery is the primB.!)'_goal, centrifugation
ml1$t . be considered as an alternative to simpie filtration.
.
(2) It is also used for removing unwanted solids ft9m a liquid. For
example, precipitated proteins are removed from insulin.
•
• Advaniages : ( l) It can handle slurrie-s with a. high proportion of
soli�s and even_ those having paste like consistency.
�-The final product has very low _moisture �onte_nt.
(3}-ln-this method, the dissolved solids are separated from the cake.
Disadvantages : �The entire cycle is compiicated resulting in
considerable labour costs.
. .(l-)--lt is a batch process or semi-continuous type.
�he solids may form a hard �e, due to the centrifugal force,
which is i:lifficult to remove.
 282 PHARMACEUTICAL ENOINEERJNo
Ch·IO CENTRJFUOATJON 283
Classincatioa Based on Sc•le of Us•ce
diameter of the pgforatlons should be selected based on the size of
Lalaor.atory. Horizontal �inning ann type
c.rystals to be separated. In case, the size-·of perforations is bigger-than
scale Angle centrifuge (45 to SO angle) that of the. particles, a �ltet cloth is employed.
High sp�ed centrifuge (10,000 revolutions per minute)
_ s per minute)
Ultracentrifuge (85,000 revolution lnterlodring switch Cover
.L /
Commerci•I sale
. Batch type :
--
Perforated basket centrifuge
Semi-continuous scale : Short-cycle batch centrifuge
-....
•
Continuous centrifuge : Super�ntrifuge Fflter Perforated
cloth t basket

EQUIPMENT Mounting
shaft
..,.- outlet
Centrifuges of different types are available· to meet the specific I
Liquid
requirements of the slurry and the end product. In addition, experimen­ Ill
tal conditions are established by considering the factors affecting the q:,
Motor
process. Some of them are:
• Nature of slurry • Densities of the materials to be separated Fi1ure 10-2. Construction of perforated basket centrifuge.

L
• Flow of feed or slurry • Bottle (centrifuge) size
trifuge dimensions • Centrifugation time
pharmaceutically important centrifuges are discussed below.
ERF RATED BASKET CENTRIFUGE
In this centrifuge, a basket is mounted above a driving shaft. Such
an arrangement is described as under-driven. CoDYerse(y,' if tfte ba5ket
is suspended from a shaft, it is described as over-driven. These are used
for batch processes. An under-driven bowl centrifuge is described below.
./
.-Lf'rindple : Perforated basket (bowl) centrifuge is a filtrttion .co�tri·
fugc. The separation is through a perforatcd wall based od the diff'orence
i� the densities of solid and liquid phases. The bowl conti;ns a
perforated side-wall. During centrifugation, the Jiquitl phase p�es
through the perforatcd wall,"whlle solid phase is retained in' tho bowl.
The solid is removed after cutting the sediment by a bt,de af.)or stopping
the centrifuge.
Coaatnettoa : The construction of a undcMtri.von perforatoc:fbuket
c:enirifuJe is shown in Fiaure I 0.2. It consists of i buket. mad• ohtool
(1omotimts covenid with vulcanite or lead) or ooppor br. monol or any
other suitable molal. The basket material of construction should � auch
that It offers the arcatest resistance to corrosion. The buket may
have a
diamoter of 0.90 motres and a capacity of 0.015 """' cubp. 11to
The basket is suspended on vertical shaft and is driven by a motor
using suitable power systems such as belt pull�ys, water turbines and
electric motors. The basket may require about 5 kilowatt power for
starting and 2 kilowatt power for running. Sometimes. steel hoops are
used, externally to strengthen the basket. Surrounding the basket, a
casing (stationary) is provided which collects .the filtrate and discharges
it at tlie outlet.
Working : The material is kept in the basket when the basket is
stationary. The amount of material should be optimum. otherwise,
during centrifugation it puts a great strain on the basket. The loading of
matorial must be done to give even ·1ttsmbutfon. Power is applied to
rotate tho bukct and maximum speed m�st be attained quickly. The
basket runs at !Q.QQ...rcvolutlons per minute.� p���cuaim! for
�
running is small om .ared to the power require or starting and bring-
· · · .· . ··
ing it to the full speo
�
- During centrl gatlon, the· U�ld_ passes t�rough the perforated wall:/ .
whllo the solid phuo retaliis"m tho bukot. The llquid leaves the baikct
ind Ti collectod at tho outlot. Tho cako is then spun- to dry as-muoh 115 ·
po11lb lc, Somotimn llt11for 1pood1 arc UIOd so · that the QUO wlff be
cornplotelx d.rlc.d. After a doftnlte period of time� tho power Is turned.
off: By applyIng a briko tlie
.centrifuge is· stopped..- The buket is
brou aht to rest. The solid cake.ls our using ·a blade and thon unloaded
�ually.
 284 PHARMACEUTICAL ENGINEERING

: �l) Perfora�ed basket centrifuge i� extensively used for sepa:.

.���� _
rating cry�talhne drugs_ (such as aspmn) from the mother liquor. �h-JO CENTRIFUGATION
·
Free flowing product can be obtained because mother"liqu or· is ...
.. 285
· removed completely. .· may be made .of steel.or any other suitable metal. .Th e. bask et .s
(2) It is also used for removing un;ant�d\olids from a liquid. F or sus pended . .
on vertical shaft and is driven by. a·· motor using . ·
.· · . . a su1· ta-.
bl•e
example, precipitated proteins are removed from insulin. pow er system. . _./
(3) Sugar crystals are separated using p_erforated basket centrifuge. �orki�g : Th� suspension is fed continuously into the basket.. During:
centnfugat1on,
·
solid phase is retained on the sides of the basket, Wh"II e
. Adva�tages: ( l) The centrifug�. is _very compact and it occupies very d re
I"1qu1'. � ams on th� top. The liquid is removed over a weir or through
little floor space. a sk1mmm� tube (F�gure 10-3). When a suitable depth of solids has
(2) It can handle slurries with a high proportio� of solids and even be�n deposited on the walls. of the basket, the operation is stopped. The
those having paste like consistency. solids are then scraped off �y,hand or using a scraper blade.
(3) The final product has very low moisture content. Uses : Non-perforated basket centrifuge is useful when the deposited
(4) In this method, the dissolved solids are separated from the cake. · solids offer high resistance �o the flow of liquid.
(5) The process is rapid.
Fe�d
Disad,•a ntages : ( 1) The entire cycle is complicated resulting in
considerable labour costs. ·� ..
1
(2) It is a batch process. · Skiming
tube
(3) If the machine is adapted for prolonged operation, there is
considerable wear and tear of the equipment. On prolonged Liquid
operation, the solids may form hard cake, due to the centrifugal
force, which is difficult to remove simultaneously.
Solid
· Variants : For the separation of fine crystals, the perforations of
I
3 millimetres in diameter are sufficient. But for finely ground mat�rials, I
the basket is lined with fine meshed gauze or with a cloth.supported on a
coarser gauge. When a mixture of liquids is to be separated, the denser Motor
liquid is collected near the walls and the lighter liquid forms an inner
layer. verflow weirs are arranged so that the two constituents are · Figure 10-3:_C��str��tio� _of non-perforated b�ket �e�trifuge. . ··,. : ;,·
conti ously removed. ·· ·.
SEMI-CONTINUQUS CENTRIFUGE OR SHORT CYCLE
ON-PERFORATED BASKET CENTRIFUGE .,.. AUTOMATIC BATCH CENTRIFUGE
. Principle : This is a sedimentation centrifuge. The separation is Principle : Semi�continuous centrifuge is a filtration centrifuge. The
· based on the difference in the densities of solid and liquid separation is through a perforated · wall based on the difference i� the
without a porous barrier. The bowl contains � non-perforated side-�all densities of solid. and liquid phases. The b_owl contains a perforated
I

During centrifugation, solid phase is retained on the sides of the side-wall. . During-centrifugation, the liquid phase passes through the . ·
while the liquid remains at: the top, which is removed by a skimm perforated wall, while solid phase retains in the bo\VI. The solid is :.
tube. . :-: ......·, washed and removed by cutting the sedifl!.ent
- using a blade.
. ' It is a short
·;�.·
cycle automatic batch centrifug e.
Construction The construction of a under-driven non-perf ·, ' . . : . . . . .- . '·
basket centrifuge is shown in Figure 10-3 . It tonsists of a b�ket, whic ConstrAction : The construction of a semi-continuous ceqtrifuge is · .
shown in Fi ure 10-4. It consis.ts of a vertical perforated basket, which
is supporte rfroin a �o�iz�nt�l shaft drivep, by a mot�r.. , From the _open
�
 216 PHARMACElTllCALENGINEERJNo
side ot the basket, provisions are made at the centre to introduce feed
and-wash pipe through horizontal tubes. /it,. feeler (not shown) ridiJs over
the feed. which is coMected to di hragm valve throu h air su
feeler controls the thickness of the feed. H draulic crtinder attac ent
is made in such a manner that the'discl\arge chute en ers ftom the sides
---
or.basket, when discharge of crystals is desirable.
...
�..�....... Dischirge
wembly
Flc•re IM. Construction of semi-continuous centrifuge.
Worldac : The perforated basket is allowed to rotate and sluny is
.
i.Jllroduced ftom the side pipe. Duri ng centrifugation, the sluny passes
through the perforated wall. The solids arc retained in the bas�et, while
filtrate leaves the basket, which is collected at outleL Further' the cake
.-- - - -
is washed with water. The wash escapes from lhe basket through the
tilttate outlet.
After achievil\8 the desired thickness (SO to 70 millimetres), the feeler
cuts off the air supply to a diaphragm valve.�,e tically shuts off
9 Worklnc : The bowl and the screw conveyht are allowed"to rotate
th� enny of s!urry. l'!'e hydraulic cylinder i/ �fui �hich lifts the
knife along watb the discharge chute. The ifc docs not cut the cake
�
complctety down to the screen, but leaves a la er of crystals that
acts as
a filter medium for further separation in the .xt cycle. The residual
crystals may be given • brief wash before starting- the next cyole.
Through • timer and air supply mechanisms, diaphragm i,atve con­
trols aJJ steps. Therefore, the entire cycle is semiautomatic. Tho
discharged crystals may contain 2 to 4% of moisture..
Ch-10 CEllrl'RIFUOATION 217
Advanta1es : Short-cycle automatic bakh centrifuge. is used when
soli ds can be drained fast from the bowl.
e
Oiijdrantage : During discharge, considerable breakage of crystals
is possible. Many moving parts are involved making the construction
and functioning complicated. ·
co�ORIZONTAL CENTRIFUGE
Principle : This is a sedimeni.tion centrifuge. The sc:�on is
based on the difference in th� densitics-«if solid and liquid-phases
without a porous barrier. When:Sturry is introduced through the shaft of
the screw elemeM into conicafbowl, sedimentation of solids talces place
due to centrifugal action. The solids are lifted up by �c screw element,
while the liquid phase is continuously drained..
Construction : The construction of a horizontal continuous centri­
fuge ii shown in Figure 10-S. It COJl5ists of a cylindrical or conical b9wl
mounted1 horizontally and capable of rotatin'g at SO to 65 revolutions per
second. The bowl has i diameter of about 0.5 metres. Within the bowl,
a scn:w conveyor is p\aced which �tatesjp. the same direction as the
bowl, but at a slightly 11ower spee.
d
Screw c:onveyor
. ( 1....1111._
- @·i��
Liq�utlet
Flaure 10-S. cynstruction of tJie horizontal co�tinuous cent rifuge.
using suitable power supply. The slurry is introduced through the shaft
as shown in Figure I 0-S. The liquid mov� s into tile w� der p�rti?n of the
bowl. Sedimentation of sollds takes place due to centrtfugal action The
:
solids are lifted by the sc�w element. while die liquid phase is continu­
ously drained. The solid materiai is carried tow.ards ouUet bJ. the
conveyor and is discftarged conlinuo�ly.• The �olids � conveyed· to a ,
dry"beacti' �where they get dried '
:
 Ch-10 C�RIFUOATION
219
288
zo....
PHARMACEUTICAL ENGINEERING
The liquid-liquid interface (the so,.alled __
Y•es : Horizontal continuous centrifuge is used when a high propor ­ . I'1c balance. These t'Wo layen •-·
by an. hYdrau
·- ...__, 4 IS . IDalntal
. n · ec1
. --
.:.. 11mu, ...- __,,...,_ly
··l y -..--
tion of solids is present in the slurry. �moveel-.:.....:..
nvm d�ffi,.,._ . ts throu modifi
• erent heigh h ed weirs (as shown- in
F11ure IO�). ThUi the supercentrifuge can work c-=-=:
Adv.ntages : (I) Continuous centrifuge is very flexible in operation. . n f.1mm1sc1.
t1o o . ble hquid · -1m·uous ...,...
,or con
. phases.
J

(2) It is capable of handling solids as large as 10 to 15 millimetres

or as small as a few microns. Motor
I
(3) It can be used for slurries with concentrations ranging from 0.5 I
to 50%.
0
Variants : The conical form as shown in Fig4re 10-5 is in common I
use, but some materials are difficult to convey when dry, for example, if
the material is soft and compressible. In such cases, a cylindrical bowl
is used with a short conical section near the outlet. As a result, the solid
is submerged in the' liquid for most of the time and is separated only light
phase =""
whe s near the discharge point. .�
�
/
�ERCENTR,IFUGE HHvy
ph1se
Supercentrifuge is a continuous centrifuge used for separating two
immiscible liquid phases.
Prindpl� : Supercentrifuge is a sedimentation centrifuge. The sepa­
ration is based on the difference in the densities between two immiscible
liquids. Centrifugation is done in the bowl of sniaGntrifuge. During
centrifugation. the heavier liquid is thrown against the wall. while the
lighter liquid remains as an inner la�er. The two layers are simultane­
ously separated using modified weirs.
Construction : The construction of a supercentrifuge is shown in
Figure I 0-6. It consists of a long hollow cylindrical bowl of small
diameter. It is suspended from a flexible spindle at the lop and guided a!
the bottom by loose-fit bushing. It can be 'rotated on its longitudinal
axis. Provision is mAde at the bonom for the feed inlet using pressure
system. Two liquid outlets arc provided at different heights at th� top of Fi1ure 10-6. Construction of superccntrifugc.
the bowl, for simultaneous recovery of the separated liquids using
modified �·eirs. Use : Supcrcentrifuge is used for separating liquid phases of emul­
sions in foods and pharmaceuticals.
Worki•C : The centrifuge is allowed to rotate on its longitudinal axis
at.• high frequency usually about 2000 revolutions per minute with the c VariHb : Tubular bowl centrifuge : It is used to separate solids llnd
help of drive-assembly. The feed is introduced from the bottom of the liquids, when the solid content is low. It is a cylindrical bowl and other
centrifuge using a pressure system. During centrifugation, two liquid facilities remain the same. During centrifugation, clear liquid overflows
phases separate based on the difference in their densities. The heavier from the weir at the top, solids are deposited on the wail and are
remo ved at intervals, if necessary. Capacity of this centrifuge is limited.
liquid is thrown against the wall, while the lighter liquid fonn� an inner
layer. Both liquids rise to the top of the vertical bowl.
 p}IARMACEUTICAL. ENGINEERING 291
290 Ch-10 CENTRIPUOATION
DE LAVAL CLARIFIE�
CONICAL DISC CENTRIFUGE OR Working : Centrifuge is all owed to rotate. Low speed and short
liquids, are Pres«:nt m !ow
As it is a clarifier, SQlids or immiscible poSSlble
time of"ce ntrifugation is sufficient to give high degree of cluific:ation.
· the �.a
concentrati·on an rilete clarification of the feed 1s
ac;,;111. Com,.,. The feed is introduced through the concentric tube SIDTOUnding the shaft.
by centrifugal means. The feed flows down and enters into the spaces between the discs
. The separation. i_s based (shown by the arro�). During centrifugation , the liquid flows into the
Principle : It is a sedimentation centrifuge
the phases under the influence chan nels (holes at the centre of the disc) and upward past the discs.
on-the difference in the densities between
ne-shaped plat4:5 are attached These substances move along the surfaces of the discs to the limits of
of centrifugal force. In this, a number of co
feed) at different eleva­ the in ner and outer layers. 1be solids and heavy liquids are thrown
to a central shaft (which bas the provision for
t wn o�ds � �e outward and move underside of the discs.
tions.· During centrifugation, the dense solids are �
the lighter clarified hqu1d
underside of the cone shaped casing, while Then the solids deposit at the bottom of the cone, which is n:moved
top of the cone.
passes over the bowl and recovered from the intcnnittently. The lighter liquid moves to the upper side of the discs.

----.
_.,.. Inlet The liquid raises to the top and escapes fiom the outlet.
1
� · Lighter liquid Uses : (I) Two immiscible liquids cm be easily scpmated br a·
.
1 · =�-�--
t
cunu nuous process _aner nqu1a111qu1a ex�on as in case ot
:�;.;.;.: Heavier liquid
manufacture of antibiotics.
(l) Suspensions co9:1taining low conccntra� of solids can be scpa­
.
�ted quickly. Solids �tare gelatinous or slimy can be sq,ualed
by �Use cone centrifuge. Such substances may plug -the filter i n
other methods.
V) :Starch is couectea aner wasnmg and puritlcation stages�
(4) I n the manufacture of insulin, the liquor is clarified to remove
Conic.al the precipitated proteins.
disa (S) eoncentration of one fluid phase as in th'e separation of cream
from milk, c.oncentration of �bber latex, removing solids from
lubricating oils, inks and beverages � possible.
Adv1nta1es : (I) Conical disc centrifuges are compact occupying a
very small space.
(2) The separating efficiency· is very high, so that the particles are
Hewitt deposited very rapidly. It is suitable, if the sediment is a fluid
tiquid + deposit or sludge.
solids
(3) By c0.ntrol_ling the speed of rotation and rate of flow, particles
F"11•re 10-7. CoMlruction of the conical disc centrifuge. are separated into two size fractions.
Co�stnctio• : The construction of a conical disc centrifbge is Dlaadv1nta1es : (I) The construction of a conical disc centrifu�e is
sJ10wn in FlJwe 10-7. It consists of a shallow form of bowl containing a . complicated.
series of conical discs attaehed to the ccntrc shaft at different elevations. (2) Its capacity is limited.
The cfiscs arc made up of a thin sheet of metal or plutlc separated by
narrow spaces. Mmdtina holes in the discs about half way between the (3) It is not suitable if the sediment of solids forms a hard CUie,
ui1 and the wall of the bowl fonn channel throuah which the liquid
puses. A concentric tube is pllced surroundina the central drive shaft.
 PHARMACEUTICAL �NGINEERINo
292
Glossary of Symbols 2•
C = Ce ntrif ugal eff ect, m/s
m.
d = Diameter of the ro tation,
F = Cen trifugal force, N.
G = Gravitation force, N.
m/s2 •
g = Acc eleration due to gravity,
m = Mass of the body, kg.
er second.
n = Speed of the rotation� revolutions p
body in a circular path, m.
r = Radius from the centre to the moving
v = Velocity of the moving body, mis

QUESTION BANK
Each question carries 2 marks
1. Write two pharmaceutical applications of centrifugal sedimentation.
2. What are basket centrifuges? Describe their applications.
3. Write the applications of perforated basket centrifuges.
4. Explain the principle behind centrifugal separation.

Each question carries S marks

1. Classify industrial centrifuges. W rite construction and working of a
· perforated basket centrifuge.
2. Give five pharmaceutical applications of industrial centrifug
es.
3. Describe continuous centrifuges, giving their adv
antages.
4. Describe the construction and working of a
Sharples supercentrifuge.
S. Describe the theory of centrifugation.

Eacb question carries IO mar�

J. Discuss construction and working
of a discontinuous centrifu
separation. ge for solid
2. Describe the construction
and working of a centrifu
of slurry containing high perc ge use d· for the separation
entage of solids.
3. Describe the construction
and working of a cent
of two liquid phases as rifuge used for the separation
in ·case of emulsion
s.
 I1 ..
•
Distillation

Theory
General Equipment for Distillation
Classification of Distillation Methods
Simple Distillation
Flash Distillation
Fractional Distillation
Azeotropic and Extractive Distillation
Distillation under Reduced Pressure
Steam Distillation
'Molecular Distillation

.
Destructive Distillation
Compression Distillation ;

Distillation is defined as the separation of the components of a liquid.

mixture by a process involving vaporization and subsequent condensa­
tion at another place.
The distillation process involves two steps; (a) converting a liquid
into vapour phase and (b) transferring the vapour to another place and
recovering the liquid. by condensation. The feed liquid is known as
distilland. The condensed liquid _is known as distillate or condensate.
If one component is volatile and others are !),On-volatile, it is possible
to separate volatile components from nqn-volatile components by distil­
lation. In such cases, distillation is considered as a separation ·or
purification method. When heat is supplied to a mixture, a more volatile
liquid evaporates readily than . the less volatile liquidJ As a result, th�
condensed liquid <:onsists of a high _proportion of highly volat_ile liquid
and less amount of less-volatile liquid·.· Therefore, distillation is said to .
be partial separation method. · The extent of separation is governed by
the properties of the component� ,i_rvolved and the physical.arrang\!ments
used for distillation'.
In pra�tice. it is di,fticult to distinguis� three process�s•. namely
evaporation, distillation and drying. Only workin·g definitions help m
differentiating them.
293
294
/
PllARMACEUTICAL ENGINEERING'
I. Distillation operation is used when condensed vapour is required
as a product.
.., E,·aporation operation is used when the concentr�ted liquid
residue is necd_ed as a product. The temperature of the liquid is
maintained below its boiling point. Further vapour is not c_on­
densed, unless recovery is essential.
3. Drying operation is used when dried solid residue is required as
a product.
Applications
Scpa'ration of volatile oils : Volatile oils are separated from cloves.
anise seeds and eucalyptus leaves by the method of steam distil lat.ion.
Purification of organic solvents : Normally, simple .distillation
. method is used for the purification of'liquids having single component
as a major fraction. Simple distillation method is also used for determin­
ing the boiling range of a liquid as per IP. 1996, as a me!hod to decide
the purity. Absolute alcohol ( I 00% ethanol) can be obtained by
azeotropic distillation.
Manufacture of official preparations : Spirit of nitrous ether and
aro111atic spiri("Of a1nrnonia are prepared by simple distillation. Distilled
water ai1d water for injection are prepared as per the specifications of
pharmacopoeia by simple and compression distillation methods.
Refining of petroleum products : In the petroleum industry. th.e
crude oil is refined into different.fractions using flash distillation. E;ich
Yracti�n is a multicomponent system. Examples are petroleum ether 60,
80 etc. � ...,,
-I
Recovery �f solvents : Solvents are· used for extraction of drugs
from plant parts and synthetic reaction mixtures. These solvents must be
recovered. in order to prevent er,vironmental contamination. The recov­
ered. solvent may be recycled for further use.
· Quality control methods :. Distillation method is used for determin­
ing alcohol content in liquid,. dosage forms _such as elixirs. as per IP.
I 996. Azeotropic distillation ·method is used for the determination of
water content _in a substance using toluene according to IP, I 996.
Separation of drugs obtained from plant and anim_?'I sources
Drugs of natural origin (such as plants) are_ non�ally extracted using
maceration. or percolation methods. The menstruum (s,;>Jvent) used for
extraction is distilled off and the active constituents are separated. For
Ch- I I DISTILLATION 295
example, vitamin A is separated from fish liver oil using the method of
molecular distillation.
Pur.ification of drugs obtained from chemical · process : Many
chemical processes involve the conversion of raw materials into prod­
ucts. The products are separated from th_c reactiol) mixture .and purified
using the methods of distillation. '
In order to handle distillation effectively and economically. it is
necessary to understand the theory _behind this process; Several vari­
abl.cs are ii1volved in the process, which arc often intcrr�late�. Theory
includes the understanding of different factors influencing the distillation
process. The laws of conservation of matter and conservation of energy
have to be applied. This chapter deals with the theory, methods and
types of equipment involved in the distillation process..
THEORY
Distilbtion is a process of separating and purifying the components
in a liquid mixture. The primary data required to solve any distillation
problem arc vapour-liquid equilibrium relationship. -Oistillation method
depends on the relative voiatilities of the components- present in the
mixture. Some of these aspects are discussed below:
When two liquids are mixed together, 'they may· be miscible with
each other in all proportions. ;B'lth miscible liquids arc known as binary
111Lr:lun:-s of liquids.
Ex:implcs of binary mixtures are ethyl alcohol and water, 'water and
acetone, benzene and carbon tetrachloride. It is essential to understand
· theories o_f ideal and real solutions (non-iqeal).
Ideal Solutions
Ideal solution is defined as the one in which there is no change in the
prope11ies of the componerrts other than dilution, when they are mixed to
form a solution.
Heat is neither absorbed nor evolved during mixing. The final
volume of the solution represents the additive property of the individual
constituents. Example is methanol 'and water, which have similar prop­
erties. Ideal. soluti.on theory provides a mod�I system to· which real or
non-ideal solutions can be compared. Ideal solutions arc characterised
by one of the important physicochemical properties of liquids namely
vapour pressure.
r
296 l'l li\RMi\CEUTICAL.ENGINEEll,.ING Ch-I I DISTILLi\TION 29.7
Raoult's Law· Dalton's law is mathematically expressed as:
Raoult's law expresses a quantitative �elationship betweer:i the con­ . . . ..,
Total vapollr presslire = partial press.ure of 'A + partial pressure of B
centration. and vapour
. pressure.
,: . . ;. . . . . '
Raoult's /aw�tates that the partial vapour . pressure of each volatile I' = P.-1 + Pn -"3)
constituent is equal to the vapour pressure of the pure 'constituent
multiplied by its inole fraction in the solution at a given temperat�re. .
Sub�tituting equations (I) and (2) ir; equation (3 ) ii,ve�
�
0
P = P A XA + P n Xn
0
(4)
. Since the .solution is homoseneous by definition, the relative num­
bers of components on the surface reflect the numbers of these Their properties .ire additive. i.e.: the total vapour pressure of the
compon�.nts. _in ,the. wnole of _solution: These num?ers can be expressed �ixture is the weighted average of the vapbur pressures of pure indi­
on mole fraction scale..· Thus RaouWs . . law is appropriately suited to vidual constituents. This behlt•(('our is shown in Figure 11-1 a. The
des.cribe an ideal �oluti��- . fol lowing concli'.i;ions can be drawn from Figure I 1-1 a.
Consider a mixture of miscible liquips A and B. In this mixt�re: · The partial pressure of the component varies linearly from zero to
· Let partial vapour pressure ·exerted by A= PA kPa. full vapour pressure as the mole fraction varies ffom zero to one.
Let partial vapour pressure exerted by _B = .PB kPa. -- Tl�.e total pressure exertco by the system at a parti�ular compqsi­
Let vapour pressure exerted by the pure. component of!\ ".' p0 kPa. A tion is equal to the sum of the partial pressui:es of its components.
, L�·t vapour pressure exe11ed by ihe pure co111pone11t of 8 = ,,a,; kPa.
Applications : According to an ic;leal solution, the compon�nt having
Let mole fraction concentration 'of liquid A = )(1 relatively greater vapour pressure will be distilled first. This principle is
Let
•·
mole frac.
J \J
tion concentration
· · · ·
of liquid 8 = Xn used in simple distillation.
.· 1 i
0
Raoult's law may be mathem�tically expressed as:
Partial vapour pressure vapour pressure x mole fraction
of a liquid. of pure liquid of the liql!id
PA
0
P A XA (I)
PB P O
IJ XIJ (2) 0

>"'
a.
0
A mixture of ethylene chloride and benzene obeys Raouk's ., law. "'
a.

When two liquids are mixed, the vapour pressure of each one ·is reduced 0% A Compositior_•1 100% A > 0% A Composition 100% A
100% B 0% B 0% A Composition 100% A 100% B 0%8
by the presence of other to the extent of dilution of each phase.
100% B 0% B
Ideal solution is defined as the one that obeys Raoult's, law. Raoult's
(a} Ideal .curve­ (b) Positive deviation (c} Negative deviation
law is obeyed by only a few solutions of liquid in liquids.. These Raoult's law . from Raoult's law from Rao�lt's law
solutions are also .known as 'perfect' solutions. The components of
Figure 11-1. Vapour-composition diagrams
these solutions have a similar structure. Examples are benzene and
for c.lifrcrcnt liquid-liquid systems.
toluene, n-hexane and n-heptane, ethyl bromi·dc and ethyl iodide. The
indivicjual components do not have interaction of any kind or complete Real Solutions
uniformity �f attractive forces- is observed. . Most systems show vhrying degree of deviation fr.om Raoult's law,
Dalton's Law depending on the nature of the liquids and the· temperature. ThE;se ·
Dalton's law of partial vapour pressures states that the total pressure solutions arc known as real solutions.
exerted by a mixture of ideal gases may be considered as sum of the . Deviations arc observed because solute-solute, s61vcntss'olut� and
partial vapour pressure exerted by eac h gas, if alone were present a1,1d solvent-solvent interactions arc unequal. Examples include carbon tetra- .
occupied the total volume. chloride and cyclohexane, and chloroform and· acetone:, Mutual
 299
198 PHARMACEUTICAL ENGINEERING Ch-I I DISTILLATION
·
interactions lead to either lowering or cnh�ncing of the vapour pressure Volatility . defined as the
, . y o f any substance 111 a solution may be
.
iv,"ded
of the mixture with respect to ideal behaviour.• . The volat1/1t
. . . um p art1. �I prcssure of the sub stance ·n i the vapour phase d'
. .
..

cqu1hbn
·,·)., l

These are described as follows. ution.

m ole frac tion o f the substance in the sol
Positive deviation : In some liquid systems, the vapour pressure is by the .
in � i qu1'd mixture
I' has partial pressure
ple, a sub stan c A
. m
For exa . mole fraction scale.
e
greater than the sum of the partial pressures of the individual compo-
con cent �at10
· n in the mixture 1s X'A on·•
nents. Such systems are said to e xhibit positive deviation from Rao ult 's PA and its ma y b e math ematicall
y expressed as:
y of A ( vA)
· Then volatilit
law. partial .vapour
· Examples include carbon tetrachloride _and cyclohexane, benzene and pressure of A PA (5)
ethanol. The typical behaviour of such a system i s shown in Figure I I- Volatility of c omp onen t 1· VA =
mole fracti�n of X A
I b. This type of behaviour occurs when the compone1its diffc.r in their A in solution
pctiarity, length of hydrocarbon
.
degree of deviation from _Raoult's law decreases as the tempe rature
�.
chain and· degree of association. The ·
The volatilit y· of a mate rial in the pure state is equal. to
the vapour

increases, since the difference s in the nature of components arc reduced pressure of the material.
at higher temperatures. Conversely a decrea·se in temperature may lead
to a decrease in mi scibility of two components and phase separation. Relative Volatili. ty . . g t '''O component� A· and B. ln
m1.'xtu r c nta inin
.
C onsider a l qui'd , essed in terms· o f t h
e
e o
Negative deviation : In some liquid s·yste rns, the vapour pres sure is of one c mp onentis expr
, the vola tility .
such a cas
o

atility may be defined as.

e
lower than that of the sum of the partial pressures of the individual
scconu..1' Relative vol
= V-.,_
components. Such systems are said t o exhibit negative deviation from
. volatility of component . A f
(6)
Raoulr's law. vola tilit y. =
1:1t B. vs .
a volatility of compon
Relativ e e
Examples in�lude .chlor9form and acetone . pyridine and acetic acid, . of the .t�o
water and nitric acid. The typical behaviour of such a system is shown in . . .is common ly ex
lity . I)ressed with the highe r
Relative vo lati . volat1ltty
Figure 11-1. c. This type of behaviour ·occurs', when ;nt eraction s such a s nu mer ato
, r · This m eans that the relativ�
volatilities in tl e .
erical value less tI1an l .o .
1
hydroge n bonding, salt fonnation ·and hydr�tion occur between the com­ er hav e a num . .
should nev .
ponents of a solution. As a result, the vapour pressure of each component . it may be substituted in equation (6)
. 5.
is lo_wered with respect to the behaviour. of an ide al solution. The total' . Since, v - PIX (equation )
vapour pressure curve shows a minimum in _the curve (Figure 11-1 c). · . p 1.JXA Pt1 X B (7) \
a=---- =
Raoult's law docs not apply ove r the entire concentration range in a P.elX B PeX A
non-ideal solution. If one liquid is present in high concentrations, it is · .,,· of A and B .
Dal ton' s, \aw, the p�rtial vapour pressures_. · �
consider�d as a solvent. The other liquid is very dilute. H enc;e, Raoult's According to
law is_ valid for that composition, though the liquid pair behaves non­ may be expre ssed as: . (8)
ideal m�,nner. PA = Yt1.P
J (9)
AppUcations .: The differences in the behaviour of a mixture influ­
ence the . method of di stillation. The areas include fractional distillation ion A in the .vapour state
where Y ,f = inol� fract e vapou'. state
. .
of inte rmediates and drugs, purification of alcohol and other organic Yu = mole fraction B in!,�ethvapo ur, kPa
solvents. Complete separation of the components of a rnixture by p. = tota.l pr. essure of ·-,
�os.
fractional. distillation n:iay not be achiev ed· if larg e positive or negativ e
. ' al so be expr essed b
y substituting �quatio
de�iations from Raoult's law are observed.. Su.ch solutions form so­ Relative ..
vo .. I a 1
t'_l'ty
1 may
.
callcd '.az�otropi� mixtures. There fore, the principles of real solutions and (9) in Equ atip n (7) g ives:
(8)
a�e 'important in d_istiliation.
II,
300 l'IIARMACEUTJCAL ENGINEERING

YAP.X11
YAXIJ 301.
------ (10)
Ch- I I DISTILLATION

CONDENSER
Equation (] 0) is often gives as the definitio Condenser helps in condensing the vapour. Con. denser is � heat
n of relative volatility.
Using equation ( I 0), the value of relative vola
tility can be calcula.ted cxchanger. It is kept cold by circulating water through .water .
Jacket.
directly from the vapour-liquid equilibrium The boiling point and volatility of a substan�e ar. e t I1e ma, n factor�
data: For example, a mix­
ture of methyl alco hol and water is having governing the choice of the condenser. The main pomts _ _ the construc-
1�
a total vapour pressure of
l O 1.31 kPa (76.0 mm Hg). This liquid contains 0tio11 of a condenser are as follows.
0.40 mole fraction of
methyl alcohol and the equilibrium vapour cont J. The condenser must be easy to clean.
ains 0.729 mole fraction.
The data may be written as: 2. The cooling surface must be large enough, because rate of con­
.
.x:.1 = 0.4; YA = 0.729; XIJ = 0.6; Y = 0.271 densation is proportional to the area of the condensing surface..
a
0.'.'729 x 0.60 3 The condensi ng surface must be reasonably a good conductor of
.
Relative volatility = . = 4,_ g35 · heat, because rate of c01idensation_ is P.fOport1onal to the rate �t
0.271 'X' 0.40 which the su:rface is cooled. For this reason, metal condenser 1s
·
Sometimes, relative volatility may change with concentration espe­ preferred over glass, if suitable:. .,;:,
cially if the binary solution do not obey Raoult's law. However, 4. T.he film of condensed liquid is a bad cond�ctor and must be
mixtures that. obey Raoult's law show only a slight change in relative .
removed quickly in order to avoid serious ·.:;tnpa1rme�t of tpe
volatility with �oncentration variation. · efficiency of condcns'er. For this reason, condenser is always
placed in an inclined position. -
'. .
GENERAL EQUIPMENT FOR DISTILLATION' 5. The warm water in contact with the condensing surface must be
Tbe construction of equipment for the distillation has been described quickly carried away a\)�1::its place shouid be taken by fresh cold
using several figures in subsequent .sections. The general equipment, water.
· :J:he cooling water .is arrange_d to move on _the cou,nter- .•
either for laboratory usJ or for industrial scale, consists of three parts. · current pnnc1p , 1. e ., its direction
· · le·· , of flow is opposite to that of
the flow of vapour to be condensed. '
STILL
It is a vaporizing chamber and used . to plac , The condenser is connected to the rccei�cr through a suitable ad�pter.
e. the material to be
distilled: The size of the still should be such ·.f cICJ/J/ t'r 1�-iav• be employed where the receiver cannot be convernently
. that only one-half to two­
thirds full of liqui d is filled. If the still is to supported at the end of the condenser. Som : times, · ti1e adapter has a
o large, superheating and . .
soine times1 dccompositioi1 of liquid may. occur.. · provision to connect to the vacuum �uinp as 111 case of :�cuum �1stilla­
The still is heated by a
suitable, mean s (example, steam) for the vapo tion Condensc'r is placed in an upright or oblique _ position. Different
risation of the volatile
. constituents,. The temperature at which the liquid typ�s of condensers are used (Figure 11-2). Three classes of condensers
boils is of consi. der­
able irnportance..... Tlierefore; provision is made to ;:ire described below.
place the thermometer . ' : . .
-·· in the stitL A cond enser is attached to the still using .
1. Si11g!e-s111fon: co11(/e11sers: �-:.xamp . I .1
I cs are ·ebio"' condenser (Fig-
appropriate joints. . . ..,
On lab·q�atory scale, round bottom flasks made ure I l -2a), spiral (gla?s-worm condcn;er) (F1gu1e 11-_b). .
of glass are used so . · .
that the progress of the distillation can be 'noticed: . .
2. Dn11!1/e-surface condensers . 1-11e c ffiic1··e ncy. of the con0ensat1on
At the same time� the . , .
feed � an_· be. adde d as and when required. Stills increases. (Figure I 1-2c).
are made of stainless .
steel, copper or suitable material to provide effic
ient heat transfer. In 3 Multi-tubular conden�ers : These are usually made _of_ metal and
j. these stills, an observation window is provided. ·
· used for large scale .work.. In the preparation of d1stilled water
Sbme liquids have a tendency to bump or· froth. which promo and wate� for injection, multi-tubular condense(s are used.
tes the
• carrying ··of liquid with vapour: To prevent this,
a· trap is inserted The basic differences in the construction show variation s i� the
between distillatioi1 flask ;:ind condenser.
efficiency of the condensation. Water-cooled condensers are not suitable
302 l'!IARMACclJT!CAL ENGINEERING Ch·! I DISTILLATION 303

for liquids, which boil above I 30 ° C. In such cases, air condenser may Some times, the receiver is immersed in an i��-ba�h or any .Q.lher
be used in place of water condenser. Air condenser is a straight tube freezing, mixture. This minimizes loss due to volat1Jizat1on.
with sufficient length ( 1-2 metres long), which is p.tssed through the J. ., '
bung of thG flask. The vapour rises in the air-cooled tube and gets
condensed.

Jacket -·
. Water (a) Conical flask as receiver • (b) Flat bottom round flask as receiver
outlet
Condense� outlet
�
� Globules of oil
, and water

Aqueous.)
Liquid out overflow
returned
°
Plain condenser Spiral .(y1ass-worm)
Liquid to still
' . · Liebig condenser
(a) Single surface condensers Oil �yer withdrawn
(b) Double surface condenser
from time to time
Figure 11-2. Different· types of condensers.
(c) Florentine receiver for oils heavier than waters
RECEIVER .
It is used to collect the distillate. It may be a simple flask (Figure
J 1-3a & b) or modifie<;i flasks such as FlorentirJe receivers (Figure I 1-3c
lt.:__-- Condenser outlet
� Globules of
& d).c, Some times, the receiver is immersed in an ice-bath' or any other O
oil and water
freezing mixture. This minimizes loss of volatilization. Florentine. r�­
ceivers ar_e 'used for the separation of oil and water. These are two types. Aqueous
. overflow
Type I : These are used for the separation of oil heavier than water. - returned
Type II::. These are used for the separation of oil lighter than water. Oily layer to still
ov.:!rflowi ng Mechanically
The receiver used for oil heavier than water has two taps (Figure I 1- to a receiver emulsified
3c). The .tap fitted near the bottom of vessel is used for collecting oil, layer of oil
while the ta'p fitted near the top of the vessel for water ;o overflow.
., and water
The receiver used for oil lighter than water is fitted with siphon at (d) Florentine receiver for oils lighter than water
the bottom;/which works when it gets filled with water (Figure I l-3d),
Figure 11-3. Di.fl�rcnt types of_reccivers.
while the tap fitted' n�ar the top .is an outlet for the flow of oil.
 305
Ch· I I l)JSTII.L/\TION
304. 1'11/\RM/\CEUTIC/\L ENGINEERING
is fitted" into the side arm_ by
CLASSIFICATI_QN OF DISTILLATION METHODS a side arm sloping downwards. Condenser 1·�··.
�neans of a cork. The cond enser is usually wat�r conden:;er.
/
. . r. The cond enser is. connected to a .
'
Simple distillation
J·acketed for .circu. lation of wate. I \\·l10 I e .
.· Flash distillation ' rv. scale. 11e
a. I aborato
Fractional distillation receiver tlask using an adaptc1. . 0 n
Azeotropic a.nd extractive distillation ipparatus is made of glass ..
Distillation under· reduced pressure
Steam distillation Thermometer
Molecular distillation
D�structive distillation
. . Compression distillation
Some of these methods are discussed in the following sections both ·
on laborato.ry scale and industrial scale along with the specific theories.
. ,;" , _,o •I j ' .

SIMPLE DISTILLATION
Simple distillation is a process of converting a single constit uent
from a liquid (or mixtur�) into its vapour, transferring the vapo ur to "Receiver
ano!.her place ,and recovering the liquid by condensin'g the .vapour,
usually by allowing it to come in contact with a cold surface.
c., ·�·

This process is known differential distillation, as distillation is based Figure 11-4. Apparatus !'or si1nplc dis1il\ation (on laboratory s'ca\c).
on the differences in volatilities and vapour pr<:ssures of the components
in the mixture. This method requires simple apparatus. Procedure : [n the laboratory scale, the liquid to be di�ti)l�d is fi_lled
1s avo1tjed
into the flask to one-half to t\vo.-third ?f its yolume. B.ump1?g. _
Principle : Liquid boils when its vapour pressure is equal to atmos­ by adding small pieces of porcel ain or porous pot be. fo re d1sttlla '.1on. A
pheric pressure. Simple distillation is conducted at its boiling point. �nd xed to the flask. T �c
thermometer is inserted into the cork p _ , atcr is
The higher the relative volatility of a liquid, the be tter is the separation the s1d an 1. \\
thermometer bulb must be just below the level of � :
by simpl\:! distillation. Heat is supplied to the liquid so 'that it boils. The circulated throug h the jacket of the conde nser as shown 111 Fig ure 11,,,,4 .
resulting vapour is transferred to a different place and condensed. If the il after
liquid of interest is volatile and remaining components are nonvolatile, Th� coi:itents arc heated gradually. The liquicj begins to b� •
and pass�:! dow.n the side a.rm ·; ,.
then simple distillat.ion is a useful means of purification and separation some time. The vapour begins to rise up
a constant
of liquids. into the condenser. The temperat ure rises rapidly and reac�es _
h 1 s eq ual to
value. The temperature of the distillate is n�ted do,>,in, wh1� .
Applications : (I) Simple distillation is used for
the preparation of ·the boiling point of the liquid. . ..
distilled _water and water for.injection. �1'>:� �oll cted i,nto the re�eiv er., The flame
Tl�e vapour is. condensed e
(2) Volatile and aromatic waters are prepared.
is adjusted so 'ihat the distillate is collect ed
_
at the ra � o( one· t? two ..
e
(3) Organic solvents are purified. drops per second. Disiillation should be coi:itrn ued until a .smaH volume
•
(4) A, few official compounds are prepared by distillation. Exam­ of liquid remains in the flask.
ples. are spirit of nitrous ether and aromatic spirit of an:imonia.
Large Stale Equipment for Simple Distillation
(5) N.on-volatile solids are separated from volatile liquids.
Construction : A simple still as shown in Fig me I I -:'i is used· for
Laboratory Scale Appan1tus for Oistilla.tion broc-scalc dislillation. It is made .up of stainless s�_cel, cop? er or any
1
' ' I •

Assembling of apparatus : The construction of a simple distillation otl�cr suitable niaterial. A still of this kind has a limited heating sur fac�
apparatus i� show� .in Figure I l-4. It consists of a distillation flask �vith

/
 307:·
Ch-I I
. ,,�
I DISTILLATION •
306 PHARMACEUTICAL ENGINEERING
Prcpa·ratio.n of Purified Water (BP) and Water for Injection (BP)
and functions perfectly with volatile solvents, but is not use ful for By Distillation
concentrating dilute solutions. Specially designed stills suite d to one The principle involved in the preparation of water for injection by
product or a group of produc. ts are used for frequent and continuous use. distillation is same as that of the simple ·distillation. However, it is a ·
special case for the following reaso'ns: · . · _ · ·
,,.· ··: ·•
• �

(I) Gases dissolved in the raw. water must be rel')Joved. These

•I .'•• :., �. •• . •
Condenser

c::i ' t:,•' should not be allowed to contaminate the distillate.' Such gases
include carbon dioxid�. A�monia'.... ''is the most important gas to
· · ., ·
be avoided. ,
(2) The carryover of soiubl�· •:materials i_n the droplets must be
circulation avoided, particularly if the pr�uct is required for use as water
for injection. · · ·
(3) Entrapment of liquid droplets by the vapour must be prevented.
Receiver

For this purpose, baffles are included in the path of the vapour
between boiler and condenser. ; .
· Figure 11-5. E;quipment for simple distillation on large scale operation.
(4) Contamination of the distillate by pyrogen from feed water must
A the rmometer i� fixed to the still to note the te mperatur e of the
boiling liquid. An observation window in the hood ·is helpful to the
be avoided. ,.
(5) The residue of solids musr not be concentrated to a point where
operator to see the progr�ss of the distillation and the level of the hydrolysis occurs.. Otherw. ise, the distillate may be conta�inated
contents to be distilled. The still is connected to a condenser and then to by volatile material produced during hydrolysis. For example,
a receiver. The still is heated using steam. Therefore, a ste am inltt at hydrolysis of chlqrides produces ·hydroc.11�?ric acid. " . ''·
the bottom of the still and an outlet for rernoving the condense d steam Construction : The arrangement of an apparatus for the continuous
are provided.
production of distilled water or ·water for irijectiori is.shown in Figure
\Vorking: A liquid to be distilled is filled into th� still to one-halfto _ I 1-6. The distillation apparatus consists of a boiler, which �ay b� made .
two-third ·of its volume . Bumping is avoided by adding small pieces of of cast iron. 8affles and c61'� enser tubes.are ,made_ l\P .of st.ainless steel or
porcelain o� porous Jiot _before distillation. ": thermometer is inserted _ monel met�t The top of the condenser jacket is ope n:· so that gases from
into the still. Water' is circulated through the· Jacket of the condenser as water can escape iqto atmosphere. The condenser tt,ibes are vertical ·· and
shown 'in Figure 11-5. • . .. . . open at both ends, as shown in Figure f 1-6. - '
. Ste.am i�· pass�d througt the inlet. . The cont�nts are hea\ed grad_ually. Working : Water (fet!d) 'enters· at the base or'th� stiit" ��d rises in the ..
The liquid begins to boil after some time. The v_apour �egms to nse up jacket� which contains a numl;>er of tubes.' In 'the condens�� t�bes, the
and ·passe� into the condenser. The temperature rises r�p1d!y and reaches condensed liquid descends, The rising feed 'water get;/he�t�d on ac­
the
a constal)t' value. The temperature is n?ted down, which 1s equal to count of condensate in the tubes: The i:ate of flow is adjusted in such a
boiling 'point of the liquid. way that the water gets heated to 90-95 °C, before' it enters the boiler.
·
Th e vapour is condensed atid collected into the receiver. The · pas- The dissolved gases in water escape to the atmosphere. The heated
is collect e �t a slo er
· sag e of ste am is regulated so that .the disti !late � :,v water then enters the boiler; in which steam is ;;irculatcd under\pressure •.
few drops p· r second). Oistillat on should be cont1n u �d until.a
rate (a e ! t through a copper coil. The stcaf):l that is obtained. by feed water cannot
·
sinall·volu. me of liquid remains in the still. :· escape except through the.c�mdenser tub�s• .whose .upp�r ends arc pro­
for
Water stills are used for producing distilled water including water truded· into the boiler head. The descending steam is .condensed into
tinuous basb. distilled, water,. which flows from the lower ends of the tubes.
. ' . n on a. con
inj�"ctio . '

0 .
 Ch- I I DISTILL/\TION 309
I

308 l'l li\RMi\CEUTICi\L ENGINEERING molecules of high boiling fraction get condensed,. while fow boiling
Baffles
fraction remains as_ vapour. This - pr�cess requires certain amount of
r' Escape"of gases time. Therefore, the liquid and· vapour is kept in intimate contact until
. . , .t, 1· I . • � 1 • t\ • •, •
I

equilibrium is achieved. The liquid fraction is collected separately.' -The'

vapour is separated' from the liquid and 'furthe'r all.owed t� condense. '�:.,t
' "
'•1
,I •
.� • I {,j: 0
: J. •

Uses : Flash distillation is used for' -separating compon��ts;,.w hich,

., •

boil at widely different temperatures. It is widely used. •in, petroleum

industry for refining crude oil.·_ . '
Heating ,., · _.,,:
coils Advantages : Flash distiLlati'on is a continuous process} If is i'used, fo/
obtaining a multi-component systems of narrow boiling range:,: especially'
·t: in oil refinery. �xamples arc petroleum ethe1 60, 80 etc.,,,:,,: 1,,-- . ,
t ' ,
• .

Disadva ntages : Flash distillation is not effective in 's�;pa;ti�g com:'

I

Overflow of
• : .
excess water ponents of comparable volatility. It is not suitable for two' componen!
· i• ' t fl' • ,· .i • ,
' ' '. · · 1
�
condenser
systems. lt'is not an efficient distillation when nea�ly ,pure c9mp9rien�s
arc required, because the condensed vapour and residual liquid arc far
from �ure.
Equipment
Construction : The sonstruction of a._ f,1ash.-distillatjon appara.tus· i�
shown inFigurc 11- 7. It consists ofa pump, which·is conne�ied_ t()_a,
· · Distillate
Figure 11-6. Construction of a distillation ·unit .••' r

for·the prej:>::ration of water for injection.

Advantages : T his process is economical as . th e amount of steam

.·· ..
ust:d in coils is reduced on account of preheating �: feed water by.,
counter-current flow Of the condensate T h is also facilitates the escape
of dissolved gases without any additional effort. Pressure'
. . :, __ Vapou�
separator.,
reducing' i-----l ·� I ' '

valve , °f'
FLASH DISTILLATION Feed
\ ,,
Flash distillation is �efined as a process i� which the entire liq�id - ..,;:, ,,
mixtllre is suddenly, vaporized (flash) by passing the feed from a �1gh ,_._____._.-··: 1. · ''·' Liquidj' ·'' · ·' ::,,· ...
' .. , J

pressure zone to a low pressure zone. Heater. ·,.

. ·
Flash distillation is also known as equilibrium distillat_ion, 1.�:' s�pa­ Figure 11-7. Appar�t. us for Hash distillation. :·· ';. '" :,:·'
ration is attempted when the liquid and vapour p�ases are in equilibrium.
.
. 'I:":· -, ·:.'�I : 1 � . . "

This method is frequently carried out as a contin,uous process and does

_i;' j; : ,
feed- reservoir. , Pump helps in pumping the feeq,, into __th� ,heating
not invoh..: rectification. chamber whichcontains_a suftff6le heating mecha.nism�- T�e-other\end ,of
·' - · le •. W hen. a hot liquid mixture is atlowed to �nter from ·a ' the pipe is dir�ctly introduced into. the, vap'o�-r-liquid separator. throug_h a·
Prmc1p _ · · · ' · is reducing valve. The \(apour outlet is provided at th_c' top of the separ.itor
h igh-·pressure. .zone ·nto
1 a low-pressure zone ' the entire liqu1• d mixture
D
twn. ur-
,
.
and liquid outlet is provided at the bottom..
. " \ ..
suddenly vaporise · 'd This process is kno.,vn as flash vapon.rn
. '. ' · __ . -� · ·
. · The individu al v:1pour p hase
mg this · process th e chamber gets cooled.
 1
,, :310 J>l iARMACEUTICi\L ENGINEERING Ch-I I DISTILLATION 311
· Working : The feed is pumped through a heater at a certain pressure. and reheating. the liquid repeatedly. ·equilibrium between liquid
and
The liquid gets heated, which enters the vapour-liquid separator through vapour is set up at each stage, \vhich ultimately results· in the separat
ion
· a pressure-reducing valve. Due to the orop in pressure, the hot liquid of a mor'e volatile component.
flashes, which further enhances the vaporisation process. The_ sudden .. . . ;J ' '
Applications : Fractional distillation is used .for the separat
vaporisation induces cooling. The individual vapour phase molecules of ion "of
miscible liquids such as acetone and y,;ater, chloroform and
high boiling fraction get condensed, while low boiling fraction remains J
•
benzene.• •

as vapou·r. The mixture is allowed for a sufficient time, so that vapour Disadvantage : Fractional distillation cannot be. used to.
separate
and liquid portions separate and achieve equilibrium. The vapour is· miscible liquids, ':"hich form �7,fi:,'._;)tropic mi tures. •. .
:"
.. ..
separated th
. rough a. pipe from above and liquid is collected from the Theory : According to the principles of colligative proper
ties, when .•
bottom of the separator. a substance is dissolved in a liquid, the.. vapour pressu
re of ·solvent · is
By continuqusly feeding into the still, it is possible to obtain continu- lowered. When two miscible liquids are mfxed; each m'
ay be considerd
·ous flash distillation. The operating conditions can be adjusted in such a · as a olu!ion of one in the other. The v�pour pressure
� of each compo­
way that the amount of· feed exactly equals the amount of material nent 1s lowered. · The pressure exerted by each one is known
as partial
removed., ' Therefore, vapour and · liquid concentrations at any point . pressure.
remain constant in the unit. According to Du/ton's law, the 'total pressure e·xerted.
by a gaseous·
mixture is the sum of the individual partial pressures
of the .co;ponent
FRACTIONAL DISTILLATION gases. If A and B are two niiscible liquids and, PA ·and
PB. rep�esent their
partial pressures, respectively, then Dalton's law 111ay be
Fractional distillation is a process in which vaporisa1ion of liquid · · mathematically
expressed as: · .· .. · . · · ·
mixture gives rise to a mixture of constituents from which the desired
one i ;; s�parated. in pure form. Total pr�ssure = PA -+; PB
This method is also known as rectification, because a part of' the Like other gas laws, Dalton's law holds strictly good
only when the
vapour is condensed and returned as a liquid. This method is used to partial pressures are not t�o ·high. Dalton's law is·
impo.rtant because it
separate miscibie volatile liquids, �hose boiling points are close. by
0

permits the _estimation of total vapour pressure, which

• means of a fractionating column. should be equal to
atmospheric pressure so as to reach the boiling p'oint.
At' boiling point,
Fractional distillation is different from simple distillation. In simple the vaporization is maximum. ·
.
distillation, vapour is directly passed through the condenser. In frac­
Based on the boiling point behaviour, the binarv mixtu
tional 'distillation the vapour must pass through a fractionating column in · . • res arc classi-
fied into thfoe classes.
whtch partial condensation of.vapour is allowed to occur. In ·simple
distillation, condensate is collected directly into the receiver, while ).n Boiling Point-Composition Curves of Mixtures
.
fractional distillation, condensation takes place in the fractionating col­
Since repeated vap.orisatiM and condensation processes are involved
umn. scr that a part of the condensing vapour returns to the still.
sinn ltancously, the composition of liquid, and vapour phases change
'.
Principle: From the operational point of view, fractional distillation continuously. Hence, boiling point-composition' c·urves are helpful in
.
is a mass transfer process involving counter-current diffusion of the predicting whether the separation is possib, l e or not, if possible, .whether .
components at each equilibrium stage. it is easy or difficult. These are helpful in designing the equipment for
When a liquid mixture is distilled, the partial condensation of the fractional distillation. · .· · . ·
· vapour 'is allowed to occur in a fractionating column. In tJie column. Boiling point-composition curves are constructed
as follows:
ascending vapour from the still is allowed to come in contact with the (I) Mixtures of liquid A and liquid B are prepa
condensing vapour returning to the still. This results in enrichment of red in different
propo rtions.
the vapour with the more volatile component. B:1 condensing the vapour . .
. . .. 1 ·
(2) Boiling point of each mixture is determined.
 312 c· PHARMACEUTICAL ENGINEERING Ch- I I DISTILLATION
313
(3) Liqui d
composition of each component is analysed at its boifing' Fracl iorq I Distil la tion_:__Azcotropic Mixtures
point.
Many liquid mixtures cannot be separated completely into· pure'
onen t is analysed at its boilin g
(4) Vap�ur composition of each comp components by simple distillation, because the v�Ia_t�lities of t�e cqmpo­
point. nents arc equal. Such a mixt1.,1re is known as an azeotrope· (Greek: boil
· ' · ·:
(5) The boilin g points arc plotted on y-axis against composition o f uncha n ged) ·
the mixt ure (x-axis ). Th e res.ultin g plot is shown
in Figure 11-8.
. A.:eotropic solution is a soluti on which distils un chan ged' a_t a con­
(6) The upper curve represents the vapour phase composition. stant temperature.
(7) The lower curve represe nts the liquid phase composition. Such so lutions are also known as constant boiling mixtures. · An
The different areas correspond to the existence of liquid. vapour . exampl e of t his type is 89.43 mol % mixt ure of ethanol and water
(8 ) at
and liquid plus va'pour phas es. atmospheric pressure. This mixture has a relative volatility
of .J .0.
. . further purification cannot be obtained by conve n tional distillation. These
The curves represent the equ ilibrium condition. Therefore , they are solutions deviate from the Raoult's· law to a laroe ex .
helpful in drawin g co nclusions regarding the composition of compon ents - . � tent. · , .'.
at any given temperature.
Minimum boiling point azcotropic sofutions--:-Type .II solutions (uon­
. . idcal solutions) : System that exhibits a minimum value in the boilin-8'
po 111 t-com!'JOS1t1 on curve i s shown i n Fi'gure 11-9. Such a svstem
.
Fractional Distillation-Type I Miscible Liquids (for Ideal Solutions)
• • . - b

is
Fractional d istillation is suitable for a system \vhen the boiling point known as azeotropic 111ix111re with a maximum vapo ur�ressure �or '
�1i·ni-,
of the mix. t' ure is .always intermed iate between tho s e o r pure co mponents . mum bo (ling po int. Examples include chloro form and acetone, pyridin
_ e
There is neither a maximum nor a minimum in the composit ion curves and acetic acid. and water and nitric ac1d. . · . ·
as shown , in Figure I J-8: These. systems arc known a s :eotrop ic
mixtures. Examples include benzen e and toluene. carbon tetrachlorid.e
· and cyclohexane, and water and methanol.
LJ D
The usefulness of F.igure 11-8 in the design of fraction al distillation
0

is illustrated in rigure 11-10.

V�pour + Liquid ic
E
I �
....,
c:
·ac.
0,
c:

T1
. ,, [.

I-
I.
100% C 0%(
Composition
0% D · 100% D

X1 X
Figure 11-9. Boiling poi'nt-composition curves. of a constant
.
0% A Xz 100% A
hoili�g azcotropic mixture having minimt;m boiling point.
' . 100"/o. B Co�position 0% B
The azeotropic inixture has a lower boil ing point tha� that of the com­
Figure 11-8. Boiling point-compo­
. sition diagram or miscibk liquids. ponent with the least boiling point. At the 'minimu.m boiling point temp­
erature. the liq:1id comrosit;on remains constant and is equal to tlie �apour
_ r
�·
314 PHARMACEUTICAL ENGINEERING
Ch-I I blSTILLATION
composition (ari sing from such a liquid system). This is indic ated by 315
coincide�ce at the trough (Figure 1 ·J -9). · C�nsider a hypothetical case (Figure
11-1O) in which the mixture
contains mo.re of A than B, which. is repre ·
A.11,�ixtures of compositions lying, between C and T (trough) can be . sente. d by L · If th'1s mixt ·
ure 1s
d'1 � 11·11c·d . the;. rn
, �11p?s1. t1,o'.1 ol. vapour 1·.is richer in A and
separated by continuous fractional distillation. In this proce ss , pure poorer in 8. At
this state. t�1e l1qu1d res i due in. the disti
liquid C is recovered from the still and .a mixture with const ant coinposi­ llation flask will be richer in B
and poorer 111 A. The Vapour'at vis cond
tion (as of T) is obtained as a distilla te from the condenser. In a similar . ..
ensed , the liqu i· d coinpOSI·t·1011 ·IS
way, all mixtures of compositions lying between T and D can· be
1_ep 1ese 1 ted b . Li.' If th i. s l i. quid is istilled,
. � � . � the composition of vapour
'I is fu1the1. 11cher 111 A and poorer 1n B. Thus on repeatod
s eparated by continuou s fractional distillation. In this process, pure . r . - d'is1·11
. I a t'ions
liquid. D is recovered from the still and mixture with constant composi­ (1.e., 1ract1onal d1sti.llat1o .
n). the liquid A in pure fonn can be obt
. .
a d'1st 1·11 ate. But the res idue re i ained in aine· d as
tion (as of T) as co.ndensate. _� the still is always the mixture .of·
A and� of cons ant co111pos1t1on. Sim
Since vapour gives constant. composition of mixture, liquid curve . '. . ilar arguments can·be proposed
for fractional d1stdlat1on of component B bv
(i.e., liquid pr�sent in the still) should be considered for the analysis , cons·ide i··ing Ie11-s
r.t 1'de curves
to r. . .
(Figure 11-9).
Cons ider a hypothetical case (Figure 11-9) in which the mixture
contains more of D than C, which is n�presented by M. If the mixture is
distilled,, the vapour has a composition of x. When this vapour is u
0

c9ndensed, the liquid composition is repre sented by M1 , which is richer

in D than C. When this liquid is redistilled, the vapour has composition ...,
:,

Q)
of � 1 . When this vapour is condensed, the liquid has the composit'i'bn of Cl.

M2. Thus on repeated distillation (fractional distillation), the liquid D ...,

Q)

...,
.
. ·a
will be in pure form and remains in still. Simil ar arguments can be
c:

Cl.
.
proposed for fractional distillation of component C by considering lcft­ 0,
c:

side curves to T (trough).

Maximum boiling point azcotropic sol.utions-Typc Ill solutions
(non-ideal solutions): System that exhibits a m;iximurn v al ue in the boiling
point�composition diagram is sh�wn in Figure 11-·I 0. Such a system is
known as a=eoJropic mixture with a minimum vapour pressure or maxi­ 0%A Composition
100% B 100% A
mum boiling point. Examples include benzene and ethanol, water and , p
0% B'
ethanol. Figure 11-10. Boiling point�compo
. sii'io11
The azeotropic rnixtur.e has .a higher boiling point than that of the curves of a constant boiling azeotropic
mix­
ture having m�ximum b:oiling point,
component with the higher boiling point. At the maximum boiling point
. � !\if i '
temperature, the liquid composition remains constant and is equa l to the General. Method-•for Fractional Distillatio
.r.
vapour composition (arising from such a liquid system). This is indi­ Construction : Th ,asse mbly of app�ratt1s
cated by coincidence at the peak, P (Figure I 1-10). � for fractional distillation ,.
on a laboratorv scale 1s shown in Fioure
. .
const1.uct1on .·of equ i pme nt fot 'fraction
"' 11 -11 .- o ,
n a rarge sea I e. the
All mixtures of compositions lying between P (pe ak) and A give a l distill ation IS
. . . ' · s h own in
pure liquid A as distillate and a mixture of A and B with constant f-.1"'o urc• 11 -'J -") · The fractiona ting column is ·inserted between the still
the cond� nser. A provision is made for the and
composition in the still. In a similar way, a ll mixtures of compositions supp ly. of heat (usualiy a
lying between B and P give pure B as distillate and· a mixture of .A and steam coil) at the bottom of the. c;�lumn.
. At the top of column.· a
B with co�stant composition in the still. conde nser 1s prov.1�c d. The column, has
. . a large arc.a for providin�
sufficient flow cond1t1ons. The broken lines acro
ss the colurnn
· ·. · · ··�s,· ent
repr -
the contact'ing devices.
316 Pl IARMACEUTICAL ENGINEERING
317
I
Ch· I I· DISTILL.ATION

- Thermomete� . fractionating column can be: illustrated usi�g the following general ex­
ample (Figure 11-13).

r
To condenser. . 11· . , 'I',- ..

Vapour of pure A formed from

Fractionating - ----;- liquid condensing only 98% A
column· . • ' � �. .' f ' i ! ..

Adaptor Condensed vapour

3rd condensation and containing 98% A
Miscible .,......,.�:?' partial revapourisation
liquids · Vapour c·ontaining 98% A formed
- Receiver from li.9uid ,contajning only 90% A

Condensed vapour
Figure 11-11. Assembly of apparatu� for 2nd condensation and containing 90% A
partial revapourisation
fractional distillation (on' laboratory scale). Vapo·ur containing 90% A formed
from liquid containing only 60%.A

Condenser Condensed vapour

containiQg 60% A .. . ... .
1st condensation and "·'1·· . ;·,;.

partial revapourisation Vapour containing 60 °/. A formed

from liquid'containing only'20% A

Vapour Product liquid containing 20% A

..
tl
Liquid Fractionating
Initial vapourisation
from distillation flask
column From distillation flask ... :' '1 lJ ;

Figure 11-13 •. Sequence of boiling point-composition .diagrams to "'

illustrate the fractional •distillation of a mixture of comp�ne_n.ts. ·! ·
Feed inlet Consider a P1ixture of two miscible liquids A and ,B cor:itaio.i_ng 20.% :
Steam inlet --fl--� Boiler
of A and 80% B. Liquid A (More Vola.tile Co1nponent.''MVC) is.)iaving
. a lower boiling point •than B (Less Yolat1 le Component� LVC).' 'These
Outlet liquids do not produce constant boiling point mixture. The boiling' point
. . composition curves of this mixture arc shown in Figure .11-)3, which is
Figure i 1-12. Fractional distillation
· �pp'aratus for la'rgc scale opcrati�1i. similar to Figure 11-8. but written several tfo,es so as to rcprcs�nt the
sters (i.e .. in fractions) in fractional distillation.. : '.·, 0-:, ·, _ ..: ·:·· '
"'"
Working ; The mixture to be distilled is fed' to the boiler and (I). When the boiling point of the mixture is reache'tl, the vapour­
heated usually, by steam. The sequence of events occurring· in the ·�omposition curves arc drawn as shown byJo\vest pair,of cu:ves_,.
:
318 PHARMACEUTICAL ENGINEERING
(Figure 11-13). These curves indicate that the vapour contains
. .:..•
60% of A .
(2) When this vapoui: is condensed, the resulting liquid is �a�in
heated to boiling point, this vapour gives the composition con­
taining 90% of A (second pair of cur�es from the bottom).
(3) This vapour impinging on a cool surface and gets condensed.
This fraction is revaporised by heating to its boiling point. This
boiling point curve of this distillate indicates 98% of A (Third
pair of curves from the bottom).
(4) This fraction of vapour impinges on a. cooling ..surface.
This gives fou11!{ pair of curves. Now this vapour contains
higher (m.ore. than 98%) proportion of A, i.e., vapour of pure
component.
(5) The vapour moves to a condenser at the top of the column and
gets condensed.
Thus, repetition of these processes yield pure A as shown in the ,
curves in Figure 11-13. The proportion of B in the ascending vapour
becomes progressively srnaller and entirely eliminated at .its upper most
point. The liquid B trickles downward to the distillation flask being
further freed from liquid A on its downward journey.
Once distillation is commenced, the size of the flame is adjusted so
that liquid passes over at a rate of one drop per every two or three
seconds. Once the Jo,v boiling point fraction has passed over, distil·la­
tion should be stopped. The liquid available in the still is pure B. It can
be collected as such or purified further by simple distillation (keeping
the fractionating column assembly).
The above process forms . the basis of the continuous method of
fractiona} distillation. Distillation is continued m1til all the MYC has
been distilled off from the top as the p·roduct and the L VC is left in the
still as.a separate product,
Efficiency of the Fractional Distillation
.
The efficiency of separation of a mixture may be expressed in several
ways.
.Length of the fractionating column : A state of dynamic e�uilib­
rium i� required for the separation. A maximum degree of separation of
the components is obtained along the length of the column.
0 tion. The obstruction also retards the downward flow of
Ch- I I DISTILLATION 319
.. . . . . . . .. ,· . • •. , ·. ,' 'f ,' ·.
Reflux ratio : Reflux rati; ,'is the quotient �f ·�h� lmo�rit of .liqu.id' ' .
returning through the column to the ampunt collected into the ·receiver
du_ring the same interval of time. A column operating undenotat reflux ·. ·
will not.yield distillate. The reflux ra,tio should be high.· It is controlled
by means of a suitable still. ije,::-,: · ., '· · ·. '.'. ::,� •. ,:,
Heat i�put : Heat input to the still should be controll�d.1 If it is too
little, the packing is insufficiently wetted. If it· is too high, velocity may
be too great for equilibrium to be attained. The size of the flame should
b� adjusted-so that liquid passes o'ver at a rate of one dr�p for every two
or three seconds.
Column temperature: For a column operating at a temperature above
60°C. heat loss should be prevented by insulation. Exa1npies ar� asbes­
tos cord and silver yacuum jacket. For temperature above I 00°C, the
column is surrounded by a heating jacket, which is generally adjusted to
the temperature of the vapour that emerges from the:top of the column.
Heat loss will cause excessive condensation within the column, which
may result i.n flooding. It will al!,o disturb the ,steady �tate tenJperature
.
gradient along the �olumn. , ..
Other experime�tal condi_tions necessary for good sepaiation are:
(I) There.should be a comparatively large amount of liquid continu­
ously returning through the column.
(2) Thorough mixing of liquid and vapour.
(3) A large . active surface of contact between liquid and vapour.
1 ' : '·: , ',', I J' i
Fractionating Columns
Gene.rally, it is necessary to conduct distillatio� �everal times by
appropriate means in orqer to sipa,rate a mixtur\!, ,of �i�ciqle liq�id�.
This can l:>e avoided by employing fractionating column for a reasonably
complete separation. In fractional .distillation,' special type ·of still-heads
are required so that conden�ation and· revaporisation are affected 1 con­
tinuously. These are known as fractionating columns. · · ·
·A fractionating column is esse�tiallv a Ion; vertical tub� in which the
vapour passes upward and gets partially. condc�sed:· The condensate flows
down the column and is returned evcntuall); to the flask. The'columns are
consiructed so as to offer the following adv<:ntages simultaneously.
(I ) It offe�s a large cooling .surface for the. vapour �o c·;�d�nse'.- :
. . . .
(2) An obstruction to the ascending ·vapour·.allows easy 'condensa-
. ' ;
·. · liquid,
which is a high boiling component. r
320 Pl 11\RMACEUTIC/\L ENGINEERING Ch· I I DISTILL/\ TION 321
J

Fractionating columns can be divided into two groups.

' . Plate columns : Many forms of plates arc used in the ·fracti_onating
/ .

P�ckcd columns : In this type, sonie forrn of packing is used in the columns . These can be divided into two types, which are commonly
. . .

may used in pharmacy.

colum� to affect the necessary liquid/vapour contact. The packing-
''-:,. ,·,; }:.; . . ,.::· .-

rings,
consist 6f single turn helices (spirals), of wire or glass, glass (a) Bubble cap plates
·,
The height of packin g is
cylindrical glass beads, stainless steel rings etc. (b) Turbo grid plates
ating column s
equivalent to one theoretical plate. Some types of fraction Bubble cap column is used . iri lar;c distill��ion p!ants, and is
are shown in Figure 11-14. · , _described below. ,,. ·· '

-�

Weir

' I
j /'

Pear Reid .and

shape disc type Liquid,-·

.
Bubble cap column · down comer
.Figure � 1-14. Diffacnt types of rractionating columns.

Construction· : Packed column consists of a tower containing a

packing that becom.es wetted with a film of liqt.id, which is brought into
Figure, 11-15; Widmer column. Figure 11-16. Construction.of bubble I
coht�ct w_ith the vapour in the intervening spaces.
•cap column for' fractional di�tillation., .....

The :;ame type of fractionating columns can be obtained in various
lengths.·
- . (a) A long fractionating coluinn is ��cessary when the boiling
points of the constituents are lying fairly close together.
(b) A short fractionating �olun:m is necessary when. the boi 1 ing
· points of the constit_ucnts differ considerably.
App°J1catio11s : Packing must. _be uniform so as to obtain proper
channels·: If packing is irregular, -n:iass transfer becomes less effect.ivc.
Packed coJumns are mainly used in laboratories. · Example is Widmer
columri. (Figu_re 11-15).,
'. �onstruction : Th� column consisi°s of a' ·nl!mber �f plates. mciunt�d
one above the other (Figure 1;1-16). The plates have a weir leadin'g°'tci;a
qowncomer. Caps �re present on each plate, which allow the �apour'to
_ · · · · · •
escape by bubbling through the liquid.
Working : Ascending vapour from the �till p,as ses through the bubble­
caps on plate A' and the rising vapour will be richer in the more v.olatile
component. This vapour passes through the liquid .'?� � p_lat; ' 13 and
_
�art�. ally c_ondenscd. The heat of condensation partially ·,,aporizes t�e
l1qu1d. The prnccss of conderrsation and vaporisation will be repe�ted at
plate C and so on all the way up the column. Each bupbJe:.cap, plate has
the same effect as a separate.still. ·::,. -· , ,. ··,. f,·
I
 I
322
....,..
.,,..,�
l'l l1\RMACl:lJTIC1\I. 1:NGINITRIN<i l"h-11 DISTILLATION

AJvontagcs : The bubble cap plate is effective over a wide range of The third c,imponent is willidr
awn at the baSl.' M th..: frac
vapour�liquid proportions and velocities. There is an excellent contact' column. . tio nating
' . .
as the vapour bubbles 1hrough the liquid.·
.....

Ex:imple is. separation of tolu ,.,:

· ene from p:1raflin hvdroc
Disudl"<111tages: (I) A layer of liquid on each plate results in consid­ �pprox1m ately same' molecular \Wi arb ons o. f
!.! hts . The sc . at . . . ,
iso-octane (example for hydrocarb� ) ffi St /° n ol_ �olucne �pd
erable hold-up of liquid over the entire column. n is di c · n the. presenc !
phenol, the relative volatilit)· 'qf . , e 'o,f·
(2) The need to force the ,·apour out of the caps through the liquid . . ,·,.
· ' -O c·ta ne
·.. mcreases ti re r,� re,_ s ep
t1on or toluene .is relatively· eas•
J
ar�7;
led to a large pressure drop through the column. ,.. In · another ex· · .im p 1'
e, ?
,ur ura l 1 add
for the separati oIi of butad"icn . . . , ed
....
fi
· . .
s
(3) The column docs not drain evei, after completion of distillation. . c from · its mix· ture con t'a
butene. 111111g I1utane and.
(4) The structure is complicated making construction and mainte­
nance c:-;pensive. . Appli�.1tions : The liquor from
. fermentation !)reces s . ts a common
source ot etln, noI and contpm
s approximately S lo 1 O�i
AZ.EOTROPIC AND EXTRACTIVE DISTILLATION. aIcoh�I _can bl' prt•p;1rcd by .lZL , ·Absolute
. 'Olropic dis tillation. P111rol .
and d1s1Illcnes. use these types �um rcfi,ne ries
,\z�otropic solutions (or co11sta11Lboiling solutions) cannot be com­ of distillation.
pletely s epar ate d by fractional distillation, because either the vapour or
the liquid in the s till has a mixture of components. The principle of DISTILLATION UNDER
. REDUCED PRESSURE
azcotropic distillation and extractive distillation lies in the addition of a . .
D1st1�/atio11 lllldl!r reduced pre
ssure .na. ) be. stated as a . . .
new substance to the mixture '-U as to inc.reas e the relative volatili\y of ·process 111 which the liquid . I
d1st1llat1on
is d is·t"Jt I ed at a temperatu
re lo\\'e ( than its
one of the two key components and thus making separation relatively b 01Ttng po.int bY the application
of vacuum.
eas:.· ;\;eotropic ternary mi:-tures with minimun, boiling point (or .
. Vac'.1u11: pumps. suction pum
· ma\i111u111 ,ap�ur pressure) arc pharmaceutically important. ps� etc. are .used·-to..1ed ..•uc1.:·,
on the l1qu1d s urface. Distilla' lht: • . s sur
.. , .pre ' .:_ e
.l::en1r11pic dis1il!a1io11 is a distillation method in which azcotropic . . tio1 1 un . d.er red uced · pressur'<: .ts ,as t .
pnncrple of simple dis!illatio .. · , .. . . e d pn the ·
· . 11 \\1.111 some. mo d1ficat1ons : . . ·,, .·
mixture i:� h1;pken by the addition of a third substanc e . which forms a
Principle . : Liquid . ·,· �
nc\\ :11.e(1tp1pe With One Of the COlllpOne1its. boils when v'apour p1:�s sur . · e ·is ,e. ·qual to the. atmos-
pheric pressure. i.e..pressure . ·1 r. e. ·
on ts sur,ac ·
r!1,:
. n:l.,ti\·c \'Olatility of the liquid mixture can be changed by adding . red uced by applying vac If the ext . -,)
".' 111 �I pressure, . is '
uum, 'the boi . lino� pomt . '.
a thi !,1 substance. for example benz . e ne is added to the :iz · .,pir Therefo o.f liquid decreases .
· re' !he liqu,·d bo1l" s at a Iower ·.ter ·
111ixt11re l'r water and ethyl ak1.1hol.13enzene breaks the mixture wall'r- illlJs trated usin!.! .an example , ter. ,.;: n erature._· This principle is
c.' clhyl alcl1l10l and forms a new azeotrope betw e en -benze ne and ethyl of \,a at.er b?tls at 10o oc at an
atmospheric p1:es� sure ;f IOI·-' �, kJ.)a (7 6 O . ...
mm Ho)
:ilcohol. The \'Olatility of the water (more polar liquid) is ennancccl. On . pressure of water .b ·apprc».:i111
:- ·1t1.t
' ·
,.,;
, �9 kP . 7 . At 4ooc• the vapour
0
..,.., _a ( � mm Hg) He
·-'-'
dic;tillatil,11. water distills at (i5.85 °C leaving alcohol and bei1zc',K' t,c­ ex·t··
t.:1 na I pres· s ure is reduced 9 33 kP ncc, t_1e.I
to . . a· (7 0 mm. . Hg) \\ here water bolls
! • � •

:,iml. l'lil· h,ii!ill\} pt1inl or this bi11:11y mi:xturc i� 68.:::'' l' ;ind hcll/\"l\c• • at 40"C.Tlic nc.:t . ,·
. • .ult rs
, t�:;
g1:l:i di:ai!k:: k;n :11!:'. i'tm: ;1icohlll hehirn.l. lt L·an be dislilkd oil :!t an inc·reas e in· · tiie r,ate o f . .
vapour. . mass. trans(er into
7X.::··c. I he bc11: .c11c c:111 be rcl:ydcd. Thus.
1 usint! fractional distilbti1111
111�lhod. ab�oluh.· akohol cari. bt: prepared. The important factor in evapor
�tion i�:
W,hen glycerin is added tu the above mixture. the vapour pressure or
wati;r is lowered .. Practicaiiy pure ·ethanol can be ob'tained from till' Mas s of vapour formed er. vapour pressure .of �vaporating liquid
fractionating tower. externa l pressure
. . \ .
cco rd1 11g to
In extru1.·1ii·e.dis1il/01io11. the third subst ance . added to ihe azeotropk �
.:' this fonnul:1. water is
allowed to evaporat
9..).., kPa (70 mm Hg) pressure . e at 40 oC and.
111ixture is ;.elatively nonvolatik liquid compared to th� -:omponents 10 the 1 n ss of vapour orm
ed in, unit' time
b1: "eparated. is approximatelv• 11 times i· e 7' 60/7 0 : .,or water.
f
· · ·
.. r
 /
324 1'1 IA RMA( Tl 'Tl<.'/\!. FN(,JNITRIN(i C'h-11 DISTil.l.J\TION
·�: 325
Applic:itions : Distillation under reduced pressure 1s csse;1tial. and The capi llar)'. tube is dipped in the boiling
,, _ liquid, so th a t. a st�eam of air
finds� number of applications. bubbles is drawn out. Water bath or oil
bath is used for heating.
°

Pr;venti11g degradation of active co11stitue11ts : .During extraction, . The Claisen flask is connected to
a receiver through· a condenser.
conccnfra tiori or processing at higher t emperatures, ·the. active constitu­ Vacuum pu mp .1 s attached through an
adapter to the receiver. · A small
ents m ay undergo decomposition (inactivation). /\ few examples arc vacuum gauge (m anometer) should be .
inserted between the p�mp and
given below. Hence extraction a nd concentr ation should be done at a the rece I vcr. ··
lower temperature (::::55° C) under red uced pressure.
Categ01J 1 Reaction Exainp!es
- Thermome"ter
En7.ymcs Inactivation mull extract. pancrcatin· ·
Vitamin's ChiJ;.ition thiamin..:. ascorbic acid
C.i lyc\1sidcs Hydrolysis anthr:1qt1inoncs
,\ lkaloids Raccmization hyocyaminc to atropine
Tannins Precipitation phlohatanins to phlobaphcn..:s
pump
Changing physical form : In the preparation of Cascara sagroda
tablet s, granular extract is suitable. Drying at the atmospheric pressure
yi e lds a ciense, compact residue. which is not desirable. · In the initial
stag,:, the liq uid extract is concentrated unde r atmosphcri� pressure or
undl'r partially ·r�duced press ure. until the residue has the consistency of
treat le. The pr�ssure is then q�1ickly reduced, where upon the t1yacly Receiver·
semi-solid s\\·ells up due to sudden evolution or water vapour . This Figure 11-17. Assembly ofappar
a!us for.distillation
produces a light porous n�ass. which can readily be passed through a under reduced pressure (on labo
ratory scale).
sieve to form a granular powder. · Procedure : The liquid to be
. dist_illed is filled one-half to two-thi
voJum : of �he flas . mall pieces rd
Disad�·antages : In vacuun1 distilbtion. persistent foaming occurs. _ _ � � of porcelain are added to the liqu
This ,may be overcome by adding capryl alc9hol to the liquid or by for facilitating d1sti!la 1on and revent id
� � bumping. The capiHary tube and
inset:ting a line air capillar>' tube iwthe second neck of the Claisen flask. therm9meter arc kept m place m the
. . . . . flask .(Figure l ] -17). The require
The stream of air is drawn in and breaks the rising foam. The above acuum i s pp 1ed. The con · d
. � � ! tents are heated gradualiy. The tem
perature
rnetl\od is not suitable for the prepa1;ation of semisolid or solid extracts. rises and liquid gets vaporised rapi
dly due. to vacuum. · The vapour
pa� ses thro�gh the conde ser. · Jhe
� c_ondensatt is collected
Di�lillation Under Reduced Pressure ce, ver. Tl_1c tempera ture 1s note. d d in the re­
_ _ (?wn, which would be' less than the
Assembling of apparatus : It consists of a double-neck distillation boiling point of the liqu id,
nask known a s C!aisen flask (Figure I 1-17)'. Thick walled glas s appara- When a_ large volume of a liqu id
. tus 'with interchangeable standard glass joints ·are used for vacuum . is to be distilled under reduced
ressure, 1t 1s more; conven
� ient to distil coinparatively small volu
distillation. In one of the necks of the Claisen nask; a.thermometer is ; t1111e. mes at a
fitted. Ths second neck prevents splashing of the viole1�tly agitated
_ Large Scale 0rparatus Using Vac
liquid. Bumping occurs readily during vacuum distillatio1i.. Plac111g a uum Stills for Distillation Unde'
fine capillary tube in the second neck of th e flask can prevent bumping. Reduced Pressure · r
.
C? n _str�ction : The general cons tr
uction of a l�rge scale
for d1st1flat1on under reduced pressu 'equipm�nt
re is shown in. Figure 11- �8.
The
 I Cll-11
1'11.\R:\l-\('Fl!TIC·\I. FN(ilNl'ERINCi
: vaculim jacket�d still is general I� mad.e or stainless steel. copper or any
other material. ;,·hich can withstand a high vacuum. :\11 observation
windo\\' in the hood is. helpful to sec the progr�ss of .the distillation and
:?lso'thc lcn·l.ofthc liquid contents. The still is fitted with a drainpipe at
' the hottom and an air vent. The still is connected to a condenser. A
thcrn1omctcr .is i.nco;-p orated in the still. Vacuum pump through vacuum
gauge is connected as shown in Figure 11-1 S.
Therm·ometer
T-:.in vacuum receiver
Fil,!urc I t:-18 .- ,\��,·mb!� t'f app:mllus for dislillatil,n
I
uai.t.:r r,·dm:.:d pr,·��ur,· ll'\1111du�tri:1I scak).
,··: .-· \\'orkinl,!: lh: still is tilkd wi1h 1he liquid to be distilled thro(1gh an
; attachment ,,r a pipe with. a 1:1p. The dthcr end of the pipe is connected
. to a resen tlir or liquid. so thal ii can be lilied at a controlled llow fate.
: Vacuum is crc:He,I by n11.:ans or a ,·acuum t,ump. Using the steam. the
'· - liquid is. i:!r:,dually h,..-:.ited. The tempcratm-c •rises and the liquid gets
. • .!:
·: v�po_i·isel rapid I� due tt) vacuuin. . The vapour passes through . the
. condenser and the condensate is collected into a receiver.
Norn1all)·, ti}\'() n:cei, crs arc titl�J \\'ith suitable arrangement of cocks.
so that thcv can be used alternati,·dv. th..:: distillate being colkctcd from
, one. \\liik. th..• ,,titer is connected !I� the still under vacuum. Thcrl..'tore
. i distillatitin net:J not b� stl1pp�J.
Distill:iti,,n is �wpped while the conll!nts of the tlask 'are surticicntly
Ouid to run ,,ff through th\! dr:iin pipt: at the bottom. \\';hen spongy
po\\'derY mi1ss is' dt::-ired. the still can be provided ,, ifh a stirring
, arran!!e;nt:nt. "hich also hastens vaporization. /\ccording to the �rcquirc­
.' ment;. th�·�apacity may· be a few litn!s to thousands of litres.
·.:r
DISTILLATION 327
STEAM DISTILLATION :
Stecim distillation is a method o( distillation carried with the aid of
steam and is used for the sep<!,ration of hig�-boiling substances from ·
non-volatile impurities.
High-boiling liquids cannot be puriti�d by simple distillation, since
the constituents in the mixture tend to decompose at higher tempera­
tures. In such cases, steam distillation is employed. Steam distillation is
us�d for the sepa;·ation of immiscible liquids.
For substances. which arc insoluble in wat�r and not decomposed by
heat, steam ·distillation provides an alternative to distillation under
reduced pressure .. Steam distillation is the most common e:,arnplc of
differential distillation.
Principle : A mixture of immiscible liquids begins to boil wh'en the
sum of their vapour pressures is equal to the atm9spheric pressure. In
case of a mixture of wa'ter and turpentine, mixtµre boils below the
boiling point of pure water, though the turpentine boils at a m�1rh higher·
temperature than that of water.
For example, the boiling point of turpentine is ab?ut I 60° C. But
when it is mixed with water and heated, the mixture boils at about
95.6° C. At this temperature, the vapour pressure of water is 86.245 kPa
(64 7 mm Hg) and that of turpentine is 15.06 kPa ( 113 mm Hg). The
. sum of the vapour pressures is IO I .31 kPa (760 ;rnn Hg) which is normal
atmospheric pressure. Thus, high boiling substances may be distilled at
a temperature much below its boiling pqint, wlien water (steam) is used.
For voJqtile substances. which are ,;iscible 'with \\;atcr; steam distil·l1l\..
ti<:>n invoJvcs the same principle as fractional-distillation.
. .g .
· Applications : (I) .Steam."'distillati.o n is used fol"' the separation o-f
immiscible liquids. Example ·i� toluene and water.
(2) This n�ethod is used for extra�ting 1�osi of th'e volatile oils such·
as clove, anise and eucalyptus.
(3) It is useful 'in purificatYoh of liquid with high boiling point, for
. - . .
exampl�·'essential oil of almond. .
(4) Camphor is distilled by this method.·
.
(5) Aromatic waters are prepared. by this method.
Ad\'aniages: Volatile oi1s can be separated at a lo,ver temperature in
:steam distillation, without any decomposition and .loss of arom·a.. J(a
substance has low volatility, it can be satisfactorily distilled. provided its·
I
 I ' 329
328 PHARMACEUTICAL ENGINEERING Ch- I I ' DISTILLATION

so that a
molecular weight is considerably higher. than water. steam generator and the nask are heated siinult�neously,
. e. · The mixture
uniform flow of steam passes through the boiling mixtm
' .

Disadvantages : . Steam distillation is not suitable when immiscible into t.he ·

· liquid and water react with each other gets heated. The steam carries the volatile oi I and passes
cible
condenser, which is cooled by cold �vater. The cond�nsed' immis
Apparatus Used for Laboratory Scale fiquid is collected into the receiver;
has been·
. �ss�mbly of apparatus : The asse �bly of apparatu� for ste.am
. Distilbtion is continued until all the non-aqueous liquid separate
liqi:,id form two .
d1st11lat1on on laboratory scal e is shown in Figure 11-19. It consists of a distilled. In the receiver, water ana organic ,
a separ ting flask .....
. , which can be easily separated using
'! avers a

water, distillation
For volatile substances, which are miscible with.
Safety tube :
. . Delivery tube onal distillation.
-8ent tu be� with steam would involve !he sai,,e principie of fracti
..,·1l)'

y· J . , . y . : ,·,,·

Equipment Used on lndu�trial Scale,

Construction : Steani distillation unit is diagr�mmatical l y sho°\\7n in
Figure 11-20, It consists of� jacketed still with a Pffforated p l ate whic�
_
forms a false bottom. · M,itiholes are provided at"the top and side for ·
: can charging and dis�harging. A Floreptine receive1· )s placed between the
still ai1<l condenser. The condenser is cooled by circulating col d water.

Flask containing Distillate

�· · non-aqueous liquid
figure 11-19. Assembly of apparatus for
steam distillation (on laboratory scale).
. metallic 'steam can' fitted with a cork having two holes. Through one
of the holes, a long tube is pas·sed so as to reach almost the bottom of
"'-' the steam generator. This tube acts as a .safety tube, so that in case .the
I

I
pressure inside the steam generator becomes too much, water will. be
forced out of it and the pressure will be relieved. Moreover, when steam
starts corning out from the safety tube, it indicates that the steam can is
alr�ost empty. Through another hol e, a bent tube is passed. The other Steam · _.u____.....ll.__;__�-1.-.--,---"--,- I
end of the bent tube is connected to the flask containing non-aqueous Florentine
liquid (for example, crude containing volatile oil) through a rubber bung.
receive·r
/
This tube should reach almost the bottom of the flask. Figure J 1-20. Ass1.:'mbly of apparatus for I
steam distillation (on industrial scale).
.Through the other hole of the rubber bung, a· delivery tube is insertet'.
which connects the flask and the condenser. The conde11ser is connected Working, : The material from which the volatile ·oil· h�s to �e
·to a receiver flask- using an ·adaptor. Provisions are' made to heat the e:>:tractcd is placed in the still above the perforated pl ate. Steam is
steam can and flask. · admitted to the jacket of the still. The water and material pres�nt in the
Procedure : The ·non-aqueous li'quid is pl aced.in the fl�k. A small stil l are ·he ated to boiling. Simultaneously steam is also injected below
. quantity of water is added ·to it. Steam can is fil l ed with water. The the materials t.hrough a steam pipe from the jacket . The steam carries
the volatile oil :rn<l gets condensed in the .:ondenser. which is cooled by
 330 Pl 1/\Rl\lACEUTlCAI. ENGINEERING
OISTlLLATION
Ch-I I
..
cold waJer. The condensate is collected into the Florentine receiver. the refining of fixP.d �ps :
(2) More frequently used in . .,
Mos t volatile oils are lighter than water and well separated from the ara ted ' from fish live r oil. _'{1tamm E is concen-.
(3) Vitamin A is sep getable
distillate as an upper layer and removed from the upper spout.. The , �sh ii ver oils a11d other : ve
trated by this method from
water can run off from the spout·on th� left and returns to the still.
oils. .
· . Some volatile oils arc heavier than water in 'which case the separation f
.. 1 ed at 1 oooc. Steroi
. (4). Free fatty -act"ds ar. e d 1s . II
. ds ca�-
be obtained
triglycerides can b e ob tam
· ed
is reversed. Oil is collected from the lower spout. between. 1 oooc and 2obe\�• while · as non- ,,
and gums w.1\\ rem· am
Varia�ts : (I) For volatile substances, which arc miscib.le with ·water, from 200;,C onwards. Proteins ted by.
ove mixtu�e can �e �e �ara
dis�ill�tion method combines the principles of the steam and fractional volatile residues·. Thus, the ab
distillations. moleculardistill atio:n: , . ;i :
;j a ,,;;lecule is· dc!i�� � a the _ a��r.a �:
Theory: Th�··;1 ea11 fi:�� .pal{
s
(2) If the S!Jecific gravity of the oil is near 1.0, then separation does
11ng. tn
lecule can move withou t. coq
not take place:. i',� such cases, it may be necessary to collect the whole of distance through which a mo .
the distillate. Further it is extracted with an (volatile) organic solvent. · collision with another.
ed mathematically
as:
The solvent should be distilled off to get t_he volatile oil. The mean path (,l) c�n be express
(II)

\ ·c· MOLECULARDISTILLATION 1,.=lJ�

/1/J
Molecular distillation is defined as a distillation process in "'which
, each molecule in the vapour phase travels mean free path and gets where p = vapour pressu!e, �Pa
•
p ;; de11sity. kg/m
.,
condensed individually without intermolecul�u collisions on application
of vacuu1n. 11 = viscosity, Pa·s
). = mean path len�tli. m
·Molecular distillation is based on the principle of the simple distilla­
halate is
avy molecules) of b uty l ph�
tion with some modifications. This is also called evaporative ,distillation For example, mean path_ (he
or short path distillation. ; of oliv e oil is 20 mm when
measured at a p1essure of
abo ut 30 mm and
Principle·: The substances to be distilled. have very low vapour 0.1 pascal. . of. d1st
· 1"\\a-
pressures: Examples are viscous liquids, oils, greases, waxy materials The cha racteris tics of the substance influence the mi:thod
):
and high molecular \veight substances. These boil at very high tempera­ t ion. According to equation (11 n
and density posses long mea
\ tures. Iii order to decrease the boiling point of :he liquids. high vacuum (a) Liquids having low viscosity
, must be applied. path. Distillation is simple.
sures po,ss7ss low mean free
\ The vapour press_�re �b. ov� the liquid is much lower than that of the (b) Substances having high pres
saturated vapour in cqud1 b �1um. At very low pressure, the distance • path.
y (17),
bc!�wee-n the evaporating s urface and the condenser is approximately eased by decreasing the viscosit
The mean free path can be incr ss_ u re. '.hus,
cqt l to the mean free path of the vapour molecule�. Molecules leaving h temperature and _ lo_w �re
which can be obtained at hig p tble .
the �urface of the liquid are more likely hit the condenser sur(ace than to ecome VO iatile and d1stt\\ahOn •
I� OSS
• nonvolatile substances may b
col Ii e with other molccu.lcs. · Little or .no re-condensation takes place at· ipment based on , the requiremen .
t of
the surface of the liquid. It is necessary to design the equ
ows.
the molecular dist iHation. Some of them are as foll . 'o. '. ce.
. . . the con den sm surfa
. Ap�lications _: Molecular distill ation is used for the purification and t be close to
(I) The evaporatmg surface mus �1th
. .::,
the con-
e . in con tac
separation of chemicals of low vapour pr essure. This ensures the molecules to com
t

(I.)� �urification of che m.ic.als such' as tricrcsyl phosphate, .dibutyl

, phthalate and dimethyl phthalate.

I
 332 °
Pi !ARMACEUTJCAL ENGINE Ch- I I DISTILLATION 333
P ERING
denser as soon as they leave the
. evaporating surface. For this walls of the vessel are provided with suitable, means of heating Uacket).
reason, this process is also known as short pat · ..
. h distillarron Wipers are provided adjacent to the vessel wall. Wipers are connect,ed
(2) The molecular collisions �hould be min · to a rotating head through a rotor.. The condensers are arranged very
. . . imized because they .
· t1on
change ti1e d irec of the path of close to the wall (evaporating surface) as.�hown in Figure 11-21. Vacuum
· rmo Iecular · · · moi ecu les· In other words .
mte distances should be fairly high · It'ca pump is connected to a large diameter pipe at the centre of the vessel.
under very h ig . n be.ach.1eved,
h vacuum, usually of the order Provisions are made for collecting the distillate and the undistilled liquid
pascals. · of O · I to I .0
� ..,. residue at the bottom.
(3) The Ii.q uid surface area must be Wo.rking : The vessel is heated by suitable means. 'vacuum is
. . as lar. ge as possible so I h JI t IlC
vapou1 . is evo I vcd from
t.
Tl1us hJS.
process is· also
. · the surfa ce only, but not by boiling.
called evaporation distil!ation.
applied at.the centre of the vessel and wipers are allowed to rotate. The
feed is entered through the 'inl,et of the ,vessel'. As the liquid flows down
Based on the method of formation the walls, it is spread 'to fo;m a film by PTFE' (polytetrafluoroethylene)
· of the liquid fil 1 m, apparatus may
be divided into two types. . . wipers, which are moving ·at a rate of 3 mehe' per second. The velocity
of the film i's 1.5, metres per second. Since· the. surface is already heated,
Falling Film Molecular Still or -Wiped the liquid film evaporates directly: The vapour (molecules) travels it£
. Film Molec�lar s1·11
prrn . le : I� this method vaporisatio
. c1p
I
. n occ urs mean free path and strikes the condenser.· The condensate is collected
fl owmg qown a heated surfa , from a film of liquid
ce und·er high vacuum · The vapo into a vessel. The residue (undistilled or mean free path not travelled) is
ur collected from the bottom of the vessel and re-circulated· through the
feed port for further distillation. Capacity is about l 000 litre per hour,
Q JFeed

Centrifugal Molecular Still

Principle : In this method, liquid feed is int,roduced into a vessel,
which is rotated at very hi�h speed (centrifugal action).
. On account of
Wiper heating. vaporisation occurs from a film of li q ui d on the sides of the ·
v.essel. The vapour (molecules) travels a short distance and gets con­
Condenser densed on the adjacent condenser. Each molecule is· condensed
individually. The distillate is subse quently collected.
Construction.: The construction of a centrifugal molecular still is
shown in Figure 11-22. It consists of a bucket-shaped vessel having a
diameter of about I to 1.5 metre. It is rotated at high speed using a
motor. Radiant heaters are provided externally
,.. to heat the fluid· in the
i conn
. .
c bucket. Condensers are arranged very close· to the evaporating surface.
Produt Vacuum pump Vacuum pump is connected to the entire. vessel at the top. ProvWons
I ection
are m;ide for introducing the feed into the centre of the bucket, for
Figure 11-21. Wiped film molecular still. receiving the product and residue for re-circulation.; ..J
'1
• • •

(molecules) travels a sh�rt distance and strik . Workin.g: Vacuum is applied. at the centre of the vessel. The bucket
. .1e IS
Each mo1ecu
. . es the condenser near
. by ·
• condensed indi vidually. The dis�i shaped vesse I is allowed to rotate at' high speed. The feed is·. introduced
collected. .
. • llate ·is. su.bsequent1y• from the centre of the vessel. Due to centrifugal action of the rotating
Con stru_ction : The. construction of a wiped film buc.ket, liquid moves outwar�, 0ver the surface of the .vessel and forms a
. . molecular still is film.. Since,,·,he radiant heat;rs heat the surface, the liquid evaporates
sho,wn m F1&ure 11-21. The vessel has a diameter of one
metre. The directly from the film. The vapour (molecules) travels its 'me,an free path
 334
1'111\H,\1,\CUITJC'/\L
,rnd . sln. kc!:i lhl.!. t'Ontkn
, l:NGJNE
.
UUNc;
scr. Tl 1e con den .
... I . 1·1,ic resi.due is sate JS coll ectl:·d into
335
.V"-.S:.l .
T
Ch- I I DIS ,ILLATIOW
. . . ·· . coll(:·ct,"·'d ti·J om t I ic bot another
,<:.JJ1. u I,lt<..'d thr·ou�h to m O t' I
llt:
, .
\·c . requirements of the pharmaceutical industry. It is economical from the
" the f··J
.:� poi 1 ior. r fiurthcr distillati sscl and 1s re-
. . on. standpoint of �onsumption of fuel and water..
. .
The feed water is heated in an evaporator for boiling. The vapour
produced in the tubes is separated from entrained distilland in a separa-.
---.. tor. The vapour is then conveyed to a compressor, which compresses' it
Vacuum and raises its temperature to about I I 8 °C. It then flows to the.'steam
chest wl-iere it is condensed on the outer surface of .the tu�e. During
, pump
connection
condensation, heat is released which is allowed for _heating of the fresh
Co11de11\e1 feed in the tubes to the boiling point. The vapour is condensed and
.dra_ined off as disti!late.

Glossary of S)·mbols
P = Toial vapoui' pressure of th.; mixture. kPa.
H�ater p = Partial vapour pressure of a liquid, kPa.
p0 = Vapour pressure cxertt:d by pure solvent, kPa.
v = Volatility of the compohent, kPa.
·f Feed"' Product J J Residue
X = Mole fraction of component in liquid state.
Y = Mole fraction of component in gaseous stlile.
Fiau
"' rc II -22 · Ccntniug
·r al molecula a = Relative volatility.
r still. p = Density, kg/m3 .
I>i.sadrnntagrs : Con
struction and ope1at1o
. · n TJ = Wiscosity. Pa·s.
compan:d to falling film arc more complic ated
mole cula r s till. J
.
I .
QUESTI.ON BA!'lK
DESTRUC TIVE f>IS Each question carries 2 marks
TJLLATION
.
.
De:;tn1t.·111·,,
I S de�o mpositio n
. .
. distillat
' . pro duc
iun
ts of
a'i'
is a distill, _JOIJ meth
the constituen ts of th
:od 111 which the distiJJate
. .
.1. D�scribe Raoult's law. What is its significance?·
2. Wh;it arc constant boiling m;i{\.jrcs? How are they separated?
in t Ii.c.. ab�enct' of air. . . . . . e organic matter b urot
3. What is meanl by constant boiling mixtures? Give two examples.
-c•i

..
. This pr�cc.ss i; also .
.
.

.
:'

. :known a� d, . . 4. 'Name the materials commonly used in packing of fractionaiing'columns.

.
J .�o :110 :)· yraytil'.C, but on� of the r:O 1't�!�:r1a11.. It IS �ot usefoJ in
a r 1
. 5. List the requisite characteristi;s that a packing material should possess.
fo1 ob1aq11n • s
. P rtant. mdust11al proce
. , �. many val . . uable · prod ucts
fro
sses
. . 6. Di ffcrentiatc between plate towers and p::icked towers.
�natkr. _It _mni]v�:� the he . m wood' coa'I _and an1m
. n1c
ating ·of dr.)_ . 01ga . . �I
111_ the ab.s�·nct• OP 'air'' un mau . er 111 a su1table vessel 7.' Describe the 1:11nstri.1ction of any one fractionating column.
. til 'a ll· . 1
' vo1·at1 e sub
d IS!J·11 alt'· is !ht• tk.,l. ·oni' p' . ts.
. stan ' ces are dn· ven off. The 8. Distinguish be:\\ cen drying and distillation. Explain differential distillation.
os"1J ·io
coal rarbonisation indust
. n pro. d'uc Wood d'istl. lfat1on . .
industry and 9. Distinguish bctwe�·n ·stripping section· and ·rectifying section' of a
. rv- pro v1"de m any
useful materials. rectifying coJumn.
IO.'Name the charJ.ctcristics or a packing material for use in fractionating columns.
COMPRESSION DIS
;I·,

TILLATION 11. Name different types of rectifying columns.

e"omprcssion distilfaiion .
method was deve I oped .
. to mee, t the nee 12. Define distillation. Mentiqn two applications of it as pl!r IP.
Navy and Arni)' for fresh . . . ds of
,v·a< tc'I",· wIllC h' I S obta m
ed . friom sea-wate .
' '
product obtained is quite p� r . o en -fr r The 13. Di ffcrentiate bet\\ cen dilTere�tial distillation' and rectitication.
t e and P) , ro.:,
ee. 1 herefore, it meet
Q

. .
s the 14. Ddine ·ideal platt:" and " (elative volatility·.
! 5. Define · flash distillation'. List applications.
336 Pl li\Rl\11\CEUTIC/d. 1:N(ilNEERING

tach question carries 5 marks

1. r:xplain with n:k\ant procedure the separation or an azeolropic mixture.
2. Whal is .meant by steam distillation? What arc its special advaniagcs?
3. Describe the principles and applications of' steam distillation.
4. What arc constant boilii;ig mixtures? Draw typical boiling diagrams for
constant boiling mixlurcs.
5. Describe the construction of bubble cap column. Whal arc its advantages?
6. Describe a bubble cap rectifying column. What arc the specific dra\\'hacks
of huhhle cap columns.
7. Describe one fractionating column or your choice. List its advantages and
disadvantages.
8. l)cscrih� the conslrucl1on and working, or a distilla\ion apparatus for the
prepjrat ion of distilied \\ atcr.

Each question carries 10 marks.

I. Explain the principle and procedure of molecular distillation. What arc its
applications?
2. Distinguish between plate columns and packed tq\\'crs. Describe the types
of p;:icking for rectifying columns. IIO\\ is absolute alcohol made'?

0
 .,
J
.

12 'b

Ey.�porafion
'./ . ...,..

Factors Influencing Evaporation

Classification of Evaporators ,/ .

,Equiprnept
Theory
Multiple Effect Evaporator

Evaporation is a process of vaporising large quantities of volatile liquid

to get a concentrated product.
Equipment used for the evaporation are known as evaporators. Heat
is supplied to the �vaporator, which transmits it to the evaporating liquid
so as to provjde latent heat of vapo.risation. · Steam is normally used as a
source of h�at. Evaporation is· a surface phe�omenon, .i.e., mass ·transfer
takes place from the surface. Thus no boiling occurs. In practice,
surface evaporation is slow.· Therefore, the practical definition of evapo­
ration is the removal of solvent from the solution by boiling the liquor
in a suitable ve�sel and withdrawing the vapour, leaving a concentrated
liquid residue in the vessel.
Either s.oh..itions or suspensions cari be subjected to· evaporation. The
only condition is that the liquid must be volatile, while the solute must
be nonvolatile. Since heat is supplied, the constituents should be
thermostable. In most of the operations, the liquid is water with a low
solid content. The liquid to be evaporated may be less viscous than
water or it may be so vis'cous that it will hardly. flow. At the end of the
process, the concentrate' will be so viscous that fµrther evaporation will ·
. be drastically reduced.
Evaporation some times overlap with other heat processes, though
some distinctions can be drawn. These are given in Table 12-1.
Although the purpose of evaporation. is" to �btain a concentrated
product, the solvent vapour is sometimes valuable, so recovery is essen­
tial. This prevents the environmental pollution, fire. hazards and at the
same time makes the process econorrdcal.
337
 Pllft,.RMACEUTICAL ENGINEERING Ch-12 EV i\l'Oll.,\TI( JN 339

TABLE 12-1 h · = pressure due to the vap(?Ur of the liquid, actually present in
Distinguishing Features of Evaporation with other Heat Processes the air, kPa
S.No:t:: Evaporation Other heat prodess K = constant, mis
In general mass transfer also depends on the te�nperature.
The residue is a concentrated Drying: the residue is solid.
liquid. Temperature
2 Evaporating liquid is only one, Distillatlon: Evaporating liquid is The hight.:r the temperature,. the greater the value of b and hence
. component in most of the cases. a combination of two or more greater wi,11 be the evaporation. . .
components. . .
At a given temperature, some molccul�s p9ssess higher kinetic en-.
3 No attempt is made to separate · Distillation: It is compulsory to t.:rgy than average, while orhcrs have lower than _average ki11ctic �:n.c_r�i­
the mixture of vapour, even if any. separate each compon::nt. Fast moving· molecules escape from the_ surface of tl.1e ,liq�1id into _vapour,·
4 The purpose of evaporation is to Crysta/liza.tion: The purpose of while slow mo\'i1;g oi1es remain behind. When temperature of the liquid
get a concentrated liquid only, concentrating the solution is to is raised. more molecules acquire sufticient kinetic energy and escape
but not to get crystals as it get crystals. from the surface to vapour state. This is the situation below the boiling
happens in some situation s. poi1n of the liquid.
Below boiling point, vapour is fonne.d from the surface only.. At
Applications boi I ing ·point, vapour is formed throughout the body of the liquid i-lS well
Manufacture of bulk drugs : Evaporation process is used in phar­ as from surface. The vapour pressure of a liquid is lowered when a
macy practice, pharmaceutical industries, chemical industries etc. substance is dissolved in 'it and consequently the b'oilin�� point of the
Manufacture of biological products : Evaporation is used in the liquid increases.
· manufacture of bi.ological products such as insulin, biochemicaJ products Normally, glycosidcs and alkaloids decompose at high tt.:mperature'.
(exa�ple, is penicillin) and plant products. Preparation of blood prod­ . I !Qnnones, enzymes and .antibio_tics arc even more heat-scnsitiye. These
ucts such as blood· plasma and serum involves evaporation. Enzymes, products require special techniques to prevent decomposition during
. hormones and antibiotics are prepared. c\'aporation.· For cxa1)1ple. malt extract is prepared by evaporation under
reduced pressure to avoid loss of en�ymes. Antibiotics are concentrated
Miscellaneous :_ Water containing minerals is subjected to evaporation
by fn:czc-drying.
to get demineralised water after condensation. The water so obtained is
used_ fqr human consumption and for spec.ial. processes: This is some Vapour Pressure
sort of evaporation though 'the process is gen�rally cal led distillation. Rate of evaporation is directly propqrt1onafto the \'apour pressure of
' i ,' . .. . (. . ' . ' .' . the liquid. The lower the p value 'in equation· (l). the greater �we·
· , ' FACTORS INFLUE.NCING ,EYAPORATION · evaporation. Lowei· the external pressure, the lower the boiling point of
th..: liquid and hence .grc':lter will· be the rate of (}Vaporation; · This
· The·rate of evaporation depends on several factors. The relationship
may be expressed mathematically as: conclitio11 is 6ch.icvcd by appl$·ing vacuum. �
KS The nature of liqliid is also import-ant for rate of. eyaporation. Liq­
M = - (b - b ') (1) uids with low boiling points evaporate quickly because of high vapour
· . .· · . ·
.. p pressures at' lo,vcr
.
temperatures.
1; II\\(',
where · M = mass of vapour formed per unit tim'e (Rate), ml/s If the outer ,Ulll'losphere is dry; the value oJ�' will be _low and h�nce
S= surface area c:,f the liquid exposed. m 2 greater the evaporation. If the vapour of the I iquid is rc1110ved as soon
p= atmospheric pressure, kPa as it is formed (under i·c:duc�d pressure "or va:cuu1n), the -�pace above the
b -= ·ma�imum vapour pressure at the tem.perature of air, kPa liquid docs .not become saturated with the vapour� Hence, 'evaporation
·proceeds faster.
 I Ch-12 EVAPORATION 341
340 PI-IARMACJ2UTICAL ENGINEERING
CLASSIFICATION OF EVAPORATORS
Surface Arca
From equation (I), it is clear that the greater the surface area of the I. Evaporators with heating medium in jacket · .
liquid, the' greater will .be the evaporation. For this reason, evaporation · Example: Steam jacketed �ettle (evaporating pan) 'J
i

is conducted in evaporators with larger heating surface area.

II. V apour heated evaporators with tub1:1lar heating ·surfaces
·· ,)

· Moisture Content of the Feed (A) Evaporators with tubes placed horiiontally
Some drug constituents undergo hydrolysis readily in presence 'Of Examples: Horizontal tube evaporator·
moisture at high temperatures. To prevent decomposition, the material (8) Evaporators with tubes placed' vertically
is exposed to lower temperature initially, then exposed to higher tem­
perature for final concentration. For example, dry extract of belladonna · 1. Evaporators with short tubes
(a) Single effect evaporators
is prepared in this manner.
Examples: Short tube vertical evaporator (Standard vertical
Type of Product . Required tube evaporator)
Type of proluct required some times decides the apparatus for Short tube vertical evaporator with propeller
Basket type evapo.rator ..,.
'
evaporation. Open pan produces liquid or dry concentrate. Film evapo­
.

rator yields liquid concentrate. Spray dryer produces dry products with
good sol�bility. Vacuum evaporator gives porous product suitable for
conversion to granules, for example, preparation of granular extract of
casc 1ra for tablet making.
Tir'ne
. of Evaporation
If the time· of exposure is longer, greater will be the evaporation,
provided the constituents are thermostable. Exposure of a drug to a ·
· relatively high temperature for a short period of time may be less
destructive of active principles than a lower temperature with long
exposure period. For this reason, film evaporators are used.
' Film and Deposits
When vegetable extracts are concentrated in steam pan, a film may
�n
be formed; the surface and/or precipitated matter may deposit on the
heating surface. Film reduces the evaporating surface and precipitated
matter hinders the transfer of heat. To avoid these problems, efficient
stirring is necessary.
Economic Factors
Economies of labour, fueJ. floor space and materials are of primary
considerations. The recovery of solvents and the utilizatioh of waste
heat are also important as they involve c?nsiderable reducti?n of costs.
For evaporation, heat is necessary · to provide the (�tent heat of
vaporisation. Hence, rate of evaporation is controlled by rate. of heat
transfer.· There.fore,' evaporator is designed to give maximum heat
transfer to the liquid.
(b) Multiple effect evaporator
Example: Triple effect evaporator .
11. Ev;porators with long t�bes J
(a) Evaporators with natural circulation
Examples: Climbing film evaporator (Rising· film evapora-
000
·
Falling film evaporator
(b) Evap()_�ators �ith for�Ia circulation
Example: Forced circulation evaporator
EQU!PMENT
STEAM JACKETED KETTLE OR EVAPORATING PAN
. . ' .
_ Principle : Steam is supplied to. a jacketed kettle (evaporating pan)
in which aqueous extract is placed. Steam gives out heat to the kettle.
The heat is transferred to the, aqueous extract by conduction and convec-.
·tion. The temperature raises and the escaping 'tendency of the solvent.
molecules into vapour increa�es. Stirring further enh::i.nces the vaporisa­
tion of solvent molecules.
Construction : The construction of a steam jacketed kettle is shown
in Figure 12� 1. It is a hemispherical structure consisting of an inner P.an
called kettle. It is enveloped w.ith an outer pan called jacket. The tw9
pans are joined to enclose a s·pace through which steam is passed..
For smaller quantities, kettle is made up of a single sheet' of metal.·
For larger capacities, several sheets are welded. Thoug � several metals

342 1'11/\RM/\CEUTIC/\L ENGINEERING
are used as a material of construction, for practical purposes· the follow­
ing arc used. Copper is an excellent material for the kettle, because of
· of the pari along with its contents becomes too great.to tilt.. Hen�e, the0
its good conductivity. If acidic materials are evaporated, some quantity
of copper :-voul� dissolve. For such preparations, tinned copper is used .
Iron is' tised for the 'construction of the jacket, because it. has mini mum
conductivity. To prevent rusting of the jacket, the iron is either tinned
or enamelled on inner surface.
A�/i�Jet for the steam and an ou!let (vent) for noncondcnsed gases
are _p·rov,ded near the top of the jacket. Condensate leaves the jacket
through the outlet provided at the bottom. The kettle is provided with
one. outlet for product discharge at its bottom.
.Solvent. vapour
\ \ \\ )JJJ
o Steam + Vent
Condensate +
Concentrated
suspension
. product
. Figure 12-LStcam jacketed kcttk.
Working : Aque��s extract to be eva��rated is �laced in the kettle.
Steam is supplied through the inlet. Stearn gives out its heat
to the
c:ont��ts arid the ·condens�te leaves through the outlet. The
_ conten ts
mu�t be. stirred .manually for smaller volumes and rnechanically
for
larg�r volumes. Mechankal stirrer. is not s�own .in Figure 12-1.
. The
rate Qf evaporation is fast in the. initial stages and decreases gradually as
the. liquid gets concentrated.
.
·�
Any room where evaporation is carried by this apparatus must have
good,v�ntilation to remove the vapo1:1r. Otherwlc:e ..the room is quickly
filled with a dense fog of condensed vapour and water fai'ls from the roof
and runs down the walls. Fans titted over the pan not only' 'remove the
vapour and· prevent condensation in the room, but also accei�rate the r te
4
of evaporation by· quickly removin
· g saturated air from the surface of the
liquid.
Ch-1 :! EV /\PORATION 343;_
The kettle may be fixed or made to tilt. A kettle of capacity 1,1pto
about 90 litres may be made to tilt. But above..:this capacity, the weight:i
.
bottom outlet is used io collect the concentrated product. �--."
II
1• I�
Uses : Evaporating pan is suitable for concentr.iting aqueous and .. :.,
#
thc:rmostable liquors; for exam.pie, liquorice extract .. �
• ,:; ·
Advantages : (I) Evaporating p,i'n ·is constructed bo_th for small 'scale
and large scale operations. . ::·;
(2) It is· simp!c in constr�r;:Jion and easy to operate, clean and;! ·
maintair'i:'
(3) Its cost or installation and maintenance is low.
(4) Wide variety of materials can be used for construction such as
copper, stainless steel an"d alumini4m.
(5) Stirring of the contents a�c;I removal of the product is easy.
Disadvantages : (I ) In evaporating pans, heat economy is less.
Hence. cost per unit material production is more.
(2) It is not suitable for heat sensitive materials due to long time of
exposure.
(3) The heating area decreases as the P.roduct gets more concen­
trated.
(4) As. it is. open type, vapo�r passes into ;he atmosphere, which can
lead to saturation of tpe atmosphere. slowing evaporation as well
as causing discomfort.
(5) Boiling ppint of water cannot be reduced, since reduced pressure
can not be created in open type evaporator.
HORIZONTAL TUBE EVAPORATOR
Principle : In horizontal tube evaporator, steam is passed through the.,
horizontal tubes, ·which arc imlTiersed in a pool of liquid to be evape;e;·
rated. Heat transfer takes place through the tubes and the liquid. outsid� r;
the tubes gets heated. The solvent evaporates and escapes from the top:
of the evaporator. The concentrated liquid is collected from the bottom..
Construction : The construction of a horizontal tube evaporator .is;·
shown in Figure 1.2-2. It consists of a large cylindrical body. with·:
. conical or dome-shaped top and bottom. It is made up of cast .iron or
plate steel. An average size of the body ranges from 1.8 to 2.4 metres
diameter and from 2.4 to 3.6 metres height.
. '.•
 /
344 PHARMACEUTICAL ENGINEERING
. The lower part of the body consists of a steam compartment with an
inlet for steam at one end and a vent for noncondensed gases on the
other end . A condensate outlet is provided at the bottom of the steam
compartment. In the steam compartment, 6-8 stainless steel horizontal
tubes are placed. The tubes are cut long enough so that they .project
about 25.0 millimetres. beyond the tube sheet on both ends. The width
or'steam compartment is usually half the diameter of the body.
At one convenient point, an inlet for feed is provided (Figure 12-2).
0
One outlet for vapour is placed at the top of the dome. Another outlet
for thick liquid is placed at the centre of the conical bottom of the body.
Solvent vapour
- Steam
,.
Vent._
Ch-12 EVAPORATION 345
' ·. .
Advantage : The cost per square metre of heating surface is usually
· ·
less in horizontal tube evaporator.
VERTICAL TUBE EVAPORA TOR
(Short Tube Evaporator) ; ,.
. Principle ; In standar d verticai tu'�e e� apor;tor, liquid 'i. s passed
through' the vertical tubes and tl;ie steam is· supplied from outside the
tubes. Heat transfer takes place through the tubes and the liquid i.nsid�
the tubes gets heated. The solvent evapor�tes and the· v'apour. escapi�
from the top. The concentrated .liquid is collected from the bottom. _
.
Constr�ction : The construction of a �tan�ard v.ertical tube.ev�pora­
tor is shown in Figure 12-3. It consists of a large cylindrical body m�de
up of cast iron with dome shaped top and bottom (Figure 12-3). · In side
the body, caland ria is fitted at the bottom. Calandria consists of a
number of vertical tubes, whose diameter ranges from ·0.05. to
0.075 metres and length of 1-2 metres. About I 00 such tubes are fitted
in a body measuring 2.5 metres or more diameter. Inlets are ��ovided
f�r steam and fee d . Outlets are provided for vapour, concentrated
product. non-con d ensed gases and condensate.
Vapour outlet

•
Concentrated
Condensate

product
· Feed inlet -,. . \
Figure 12-2. Construction of a hori �ontal tube e�aporator. : t
.

m . �m 1
Working : The feed is introduced into the evaporator until the steam -stdm
·., .._,:!

comp�rtment is satisfactorily imll)ersed. · Steam is introduced into the Calandria ... inlet · · 1 ·
' . ·' . ·. �-.�
steam ,compartment. The horizontal tubes receive heat from the 'steam l: • { ' 1

. and conduct it to the liquid due tu temperature gradient. · Steam conden­

sate p�ses through the corresponding outlet. The feed absorbs heat and
. Steam . - .
condensate \\.\.'. JJJ , J �t ..

solveQ\ gets evapor.ated. The" vapour then escapes through the outlet .
I ; ' ,. : �· ' •
' .
· placed at the top. This process is continued until a thick liquid is
. .. ' . � . ; ' .'.
>' �

formed, which can be collected from the bottom outlet. .•'. \•

. .
}

t'•

. Us�s : Horizontal tube evaporator is the best suited for n:on-viscous Concentrated
liquid 01,1tlet
so.lutions that do not deposit scales or crystals on evap�ration, for
example cascara extract. Figure 12-3. Construct.i�; of a short tube evapo�;�/ . ·'
. .
/

346 I
l'I IARMACEUTICAL ENGINEERING
· Workin� : Steam is introduced outside the tubes·. The condensate is
p;ssed th�ough the corresponding outlet and . non-condensed gases escape
through the vent. The feed is introduced in such a way as to maintain
the liquid level slightly above the top of ,the tubes. The liquid inside tl}c
tubes is heated by the steam and begins to boil. As the liquid boils, it
spouts up through the tubes and returns through the central down-take.
It sets yp a circulation of hot liquid, which enhances the rate of heat
transfer. The vapour escapes through the top outlet. Steam is supplied
until 'required concentration of the product is obtained.. Finally, the
product can be withdrawn from t�e bottom 9utlet
Uses :. Vertical {ube evaporator is used in the manufacture of cascara
extract, sugar; �alt, caustic soda. · · · · ·
Ad,·antages : (I) In vertical tube evaporator, tubes increase the
heating surface nearly 1-0 to 15 times when compared with steam
jacketed kettle.
(�(Vigorous circ.ulation enhance$ the rnte 0°f heat transfer.
(3) It can be conne�ted t� a c;ndenser 'and receiver, which. further
increases rate o.f evaporation .. Such attachment is also suitable
for volatile solvents.
(4) A number of units .can be joined to obtain more efficient effect
(multiple effect e�'aporators are d_iscu�sed later).
Disadvantages : The liquid i.s maintained above the level of the
c;la�dria. Hence, the upper layers of the liquid need a long time for
getting heated. This problem can be minimised· by removing concen­
trated liquid slowly at the bottom.
The evaporator is complicated, hence,_ installation cost increases.
Cleaning and. maintenance· is difficult when compared with stea·m
jacketed kettle.
During operati9n, ihe pressure inside the evaporator increases. In
0
0•
�large . evaporators: where the liquid depth may be of the . er of
�or �
_
2.0 metres. the pressure increases to 25.0 kilopascals, leading to eleva-
tion of the boiling point by 5 or 6 C. This reduces the effective
°
temperature gradient and may ·affect heat sensitive materials.
Variants : Short tube vertical evaporator with propeller : In short
tube .vertical evaporator. circul,;1tion ·depends completely on boiling.
Steam is supplied into the calandria to induce boiling. Whe� stea�­
supply is stopped, automatically boiling stops. As a result the particles (1t
any) settle.oown. These particles ·act as nuclei which grow as crystals.
J
Ch-12 EVAPORATION , 347
Therefore, this evaporator is sometimes used as a crystr:illizing �v�pora­
tor. If such crystall.ization is uncJ�jrable, the problem can be avoided by
installing· ::i propeller in the central portion. close to the bottom. By
increasing the revolutions per minute of the prppeller, the capacity of the
evaporator can be doubled.
Uses : Since mild steel or casi iron is us.ed, the evaporator suits well
for clear liquids and crystallizing solutions. Non corrosive liquids and
mild scaling ·solutions can also be handled.
Adl'Ontages : Heat transfer coefficients are high due to high tempera-
ture gradient values. It requires low head-room. Cleaning and
maintenance is easy. It is relatively inexpensive.
Disadvantages : · Heat transfer. coefficients are low due to low tem­
perature gradient. It requires �igh floor space and is more in weight.
Relatively 'more liq_uid is retained. Rate of heat transter' further de­
creases due to high viscosity liq.uids: Since body is large, mild steel or
cast iron are used for its cor:isfruction to make it less expensive.
Basket IJ'J>e evrporator : The basket type of evaporator ha·s a conical
bottom and some times a flat bottom. · In this type, boiling is quite
violent. Hence, the spouting of the liquid leads to entrainment. This
problem can .be avoided' by placing a deflector over the tubes. In this
case, the down-take is annular instead of being central. The advantage
of this type is that entire heating element is a single unit. The complete
unit can be removed for repairs. In addition, the deflec:tcir prevents
entrainment losses completely.
CLIMBING FILM EVAPORATOR (Rising Film Evaporator)·
Principle : In climbing film evaporator, tubes are heated externally.'
by steam. The preheated feed enters from the bottom· and ·flows up ·
through the heated . tubes·.• The liquid ·gets . heated� rapidly :due to ,en� ..
hanced _overal] coefficient o( the preheated ·feed.')The liquid nea·r .. the·:
wall becomes vapour ·and forms sma. ll· bubbles·. These tend to, fuse to.
larger bubbles, which travel up in the tubes along with' e�trapped shig.·;'
The liquid films are blown up from the top of the tubes, and strikes
entrainment separator (deflector) kept' abov�. This .\hrow� ,th�. liquid
concentrate down into the lower part from wh�re it is. withd��n. · . �
. .' . . . '. . . \ )
Construction . : The construction of a climbing•,fii� :��aporator is
shown iry Figure. 12-4. In this evapora�or," the hea.t:ing · unit, consists�f
steam jacketed tubes. Here, the tubes (long and· narrow/are held·
between two plates. An entr:iinment separntor is pla&d at'the fop to tlic .
348 PHARMACEUTICAL ENGINEERING
� Ch-12 EVAPORATION 349
vapour head. The evaporator carries steam inlet, vent outlet and conden- 1•;. :.r ,,.. r·\,
sate outlet. The feed inlet is from the bottom of the stea� compartment. Uses : Using climbing film evaporator, thermolabile substances such
�
. .:..• as insulin; liver extracts and vitamins can be concentrated. Clear liquids,
Deflector Vapour head Vapour foaming liquids and corrosive solutions in large quantities can be oper­
ated. Deposit of scales can be r_emoved quickly by increasing the· feed
rate or reducing the steam rate so that. the pr6duct is unsaturated for a
,.---...... short time. .,.;:,
.

t t t
Cyclone
separator
Pipe foi
Condensate i recirculation
t (6) It requires low hold up and small floor space.-
Feed
Concentrated product
figure 12-4. Construction of a climbing film evaporator.
Working : The preheated liquid feed (to be evaporat d)_ is introduced
� _
from the bottom of the unit. The height of the liquid column is
maintained low, i.e. , 0.6 or 1.2 metres above the botto1:1 tube shee\
Steam enters into the spaces outside the tubes through the inlet. H� at 1s
transferred to the liquor through the walls of the tubes. The liquid _ . (5) If teed rate is high, th'! liqu�r may' be co�centrated insuffi­
becomes vapour and forms smaller bubbles, which tend to fuse to larger
bubbles·. These are of the width of the t1,1bes, thereby the bubbles trap a
part of the liquid (slug) on its way up in the tubes. �� m?re vap�ur .1_ s
_ ' ' .. ,_.:. . . . '
Advantages : (I) In a climbing film evaporator, large area for heat
transfer is provided employing long and nardw tubes.
(2) Since liquid flows at a high velocity, the resistance for heat
transfer at the boundary layers is reduced. As. a result. the heat
transfer is enhanced.
(3) The time of contact bd�'li'::en the'liquor and the heating surface is
· very she>rt. The liquid is in the heater for one second, while its .•
residence time. is 20 seconds in the evaporator. Hence it is
suitable for heat sensitive materials.
' .
(4) Unlike short tube evaporator, the.tubes are not submerged. So
there is no elevation of boiling point 'due to hydrostatic head.
(5) It is suitable for foam-forming liquids, because foam can ·be
broken by an entrainment separator.
Disadvantages: (I) Climbing film evaporator is expensive, construc-
•
tion is quite complicated.
(2) It is difficult to clean _and maintain.
(3) Large head space is required ..
(4) It is. not advisable for very viscous. liquids, salting liquids and
scaling liquids.
. dently... If feed ·rate is low, film'·cannot be maintained. 'Dry
: · patches may
. fonn. on . the tube walls.· ·. ··. . • .. ·L. · ·
.- ,.,
;

FALLING FILM EVAPORATOR

. formed, the slug of liquid is blown up in the tubes fa�1htatmg t�e liquid
• ' '� I ' '

to spread as a film over the walls. · This film, of hqu1d .
continu.cs to
vaporise rapidly. ·Finally, the mixture of liquid conce.ntrate and vapour
eject at a. high velocity from the top of the tubes.
The entrainment separator not only prevents entrainrrien:, but also
acts as a foam bleaker. The vapour leaves from the top, while concen­
trate is collected from the bottom.
Principle : In a falling film evaporator; feed enters from the· top and
flows 'down the walls of the tubes. The liquid gets heated rapidly due to
heat transfer from steam.. The liquid boils and becomes vapour; which
'forms small bubbles. The)_' tend to fuse.to form layers of bubbles, �vhich
travel down the tubes. Concentration takes place during .this do\vnward
journey.. Vapour and liquid are separated at_ the·_ bottom. · · \ ·
. . '·
r
 l'l li\H.Mi\Cl:UTICi\L ENGINEER!NCi
350 '1
Ch-12 EV i\PORi\TIOS 351
film evaporator �s
Construction : The construction of a falling coffee. It is also useful for concentrating the heat sensitive mot rial
fil evaporato�, but is
shown 'in Figure 12-5. It resembles clim bing such as fruit juices.
m
ts of steam J�ckctcd
invert�d. In this e vaporator, the heating unit consis
m comp artme �t. The Adva,ntagcs : (I) Falling film evaporator is suitable for high viscous
tub�s. The feed inlet is from the top. of the stea
nsate outl�t remain s� mc . liquids, because the flo� of vapour fil m is assisted by gravity.
other provisions arc steam inlet, vent and conde
m and 1s connected to
The outlet for the product is provided <!t the botto (2) The liquid hold -up is less and hold-up tim � ,is :very Sll)all.
a cy clone separator. (3) The liquid is not o'verhcatcd during passage and heat transfer
coefficients are high even at low boiling temperature:
Liqui_d (4) Highly acidic and corrosive feeds ·can be conce·ntrate d using
inlet - Vent impervious graphite tubes and rubber lined vapour heads.

Steam--+ Disadva�tagcs : Easy distribution of feed to the i11di-�·idual tubes

Q

inlet may be accomplished using a perforated plate above the tubes or using
spray nozzles. Hence. it is not suitable for suspensions, as the solids
clog the perforated plate. It is not s�itable for salting or scaling liquids.
_ The feed d istribution in the tubes-is 'poor.· For,·continuous .supply. the
liqui d may be recirculated or the ratio.bf feed to evaporation is kept
Condensate high . �
liquid +- -+ _Vapour
FORCED CIRCULATION EVAPORATOR :J
Cyclone Principle : In forced cir�ulation �vaporator, liquid is circulated
separator through the tubes at high pre_ssures by fueans of a pump. Hence, boiling
docs nqt takes place because boiling point is·elevated. · Forced circula­
.
t ion of the liquid al .so creates Sdilw'? fqrm of agitati��·:. When t\1.e)i'quid
leaves the tubes--::ind enters the vap?ur head, pressure falls ,sugd�. n)y.
This lea d s to the flashing of super heated liquor: . Thu_s evaporation is
Liquid effected .
conce·ntrate
' Constn,1ction : The construction of a for.ced circul ation evaporator is
. figure 12-5. Falling film C\'aporator. shown in Figure 12-6. The steam jacketed tubes are ·held. b.etween" two
compa�1:1ent. . r:ce.d tube sheets. The tube measures 0.1 metres insi d e diamete'r'and ·2.5 metres
Working ': Steam is supplied into the steam
re of the boiling !1qu1d IS long. The part of the tupes projec.ts into the vr.pour head (flash chamber).
enters from the top of the tubes. The temperatu
s down the walls of the which consists of a deflector. The vapour· head is connected to a return
·sam e as that of the vapour head. The feed flow pipe. which runs d ownwards and e nters into the inlet of a pum p.
liqui d boils and becom es
tubes.- The liquid gets heated rapidly. The
t nd to fus� t� fo�m layer�
vapour, which forms s maller bubbles. These � Working : Stea m is introduce d into calendria.: Pump sends the
Concentration takes _place
of bubbles, which travel down the tubes. ·liquid· to· the tubes with a positiv� velocity. , As' the' liquid moves up
liquid are sepa'rated 111 the
during this _downward jo,urney. Vapour and through the tubes, it gets heated . and begins t9 boil. As a result, the

cyclone separator. vapour and' liquid mixture rushes out of the tubes at a high velocity.
rate volatile and non­ This mixture strikes the d e0ec.tor, which throws the liquid .qownw ard.
Uses .: Falling fil m evaporator is used to sepa . This results in an effective separation of liquid and vapour. i;he vapour
rials , when th feed is of low visc osity. It 1s used for the
;olatile �ate e
enters the cyclone separator and leaves the equipment. The concentrated
gelatin, extracts of te a and
concentration .o.f yeast extract, manufacture of I
 NG
PIIARMACEUTICAL ENGINEERI
352
Ch-12 EVAPORATION
Fi n ally the concen-
p for ('.iurt11cr cvapor at"I on
liquid returns to the pum
1

collected. THEORY :J '

trated product is
'
, I
In an evaporator, heat is transferred to the evaporating liquid s o as to
prqvide la tent heat of vap orisation. Generally, steam 'is used as a sourc�
of beat. Several heat exchangers have been,discussed, in Chapter 'Heat
Cyclone Flow'." N ormally, tube and �IJ�II hea_t excha ngers are.used for heat
separator transfer. .,.. · - .... ·. . ··
Deflector
The amount of hcat,.which must be transf�rred through the walls of a
calandria. varii.:s wi th the n ature of the liquid to be . evaporated.
,, ... . The,. , ·-
Steam - ,liquids used in pharmacy practic� arc water and hydroalcoholic solutions'
with low solid content. In case of bulk drugs, organic solvents_ ar� also
used.
.�. ,' ._.

- Return pipe Evaporator Capacity

Gases � The total amount of heat required can be obtain ed by considering a
simple diagram o f an evaporator as shown in Figur� 12�7.
� Product
Vapour.
y. _Y, hy
- Feed

Pump
evaporator..
Figure 12-6 . .Forced circulation
rced
under red u ced pressure , fo
·.

If evaporat ion is cond u cted

1
Uses s ubstances. Thi s Steam
. rcu I at.1 on ev°aporator is suitab·le for thermolabile 5, hs
:-·_;,-,
c1 . iver ex tracts . It is
centratio� of insu I"in and I"
method is used for the con , als arc, to be sus-
g operations where cryst
well suited for cryst allizin
pended at all times.
___.,..._ Conden�ate
the h� at transfer S, he
ed circulation evaporator·,
Advantages : ( l ) I n for� vement . '
::: rapid liquid mo
coefficie nt is high due to " '°. Product ' '
to forced circu-
ling are n ot possible due
(2) Salting, scaling and fou ' L, XL, hl
lation . Figure 12-7. Evaporat�r system with its·parameter.s.' . . .. '
because
. table 'or1· the�molabile substan ces
(3) This evaporator is su1
, ," •• : f; r ..

Feed and steam are admitted into th� evaporator. By consumingl

· of rapid evaporation . pin g
ons because pum
(4) It is suitable . c 1or h"igh vi"scous preparati heat, the feed un dergoes evaporation to ' form vapour, which will be
allo wed to escape. -The concentrated product will be collected at its
· mechan ism is used.
hold- u p � f b<_>ttom. Simultan eo usly steam looses its heat· e�ergy. a�d und�rgoes.
ci rculation evaporator, the
D. .1sad,·anta<bTCS : In fo rced . power (pump) 1 s condensation, the condensate of whi.ch will be removed.·. · ,>:�
ipm nt ts expensive, because ···J
•

liqu id is hig h. Th e equ � _ - Let F kg be the feed per hour ·to the .evaporator,. who'se solid
the liquid.
required for circulating content is XF (weight fraction).�nd enthalpy is hp J/kg.·, . ;;;
..,;:;,

,r
 Ch-12 EVAPORATION
EERING
Pl l�RMACF.\JTICAI. ENGIN
354 condensate · may get cooled. All these factors in.f1u7nce' 'evaporator .
m an evaporato:,_
Let L kg . ' be the p roducl collected per hour fro py is
· calculation with respect t o mass balance.
. ·s x. I. (weight fraction) and enthal
whose solute compos1. t ,on i Improving Heat Transfer Coefficients
· .
h 1 J/kg. . . orato:· Evaporator is considered as a· heat· exchanger: Like· a�y heat ex­
. he vap ur lib era ted per hour from an evap
.
Let l' kg . be . cnt hal rY.,,'s changer, heat is transferred from stea111,. to the product. The· general
· (wci�ht fraction) and
o

whose solute con�pos1·(on is,

t

re wat er as there equation for heat transfer can be e_xpressed by equation (6) ·;.:,i:
. rs, • tI 1e \:apo ur is pu
Ii I' Jikg. 1 n most evapoI rato .
1 ,

re y is zc: o. Q = UA.11·
is no entrainment and therefo
}'
(6
where Q = rate of heat transfer, W ·
Material Bal� ncin� tcrialentering and U = overall heat transfer coefficien.t, W/rn2 K
The material ba ance can . be obtained from total ,�a for the
can bc rep n·sc . d by an equat ion
:. ntc A = heatin!! surface area. m2 '.
total material leaving. It Llt = tempc;ature diff�rence, K ·
u... 1

evaporat.ion process . '.. �.

.•'l I

. . · ted (kg .. )
ed (ko ) + vapour libera , Equation (6) can be used to determine the Q.
'

t c ol\ ect
I

Feed (kg) =- prod uc

• ,

, ::,
;

( 1)
I,

p;,L V + Heating ·surface (A in equation 6) musr be large.. For'this ·purpose 1

terms Of more number of t.ubes are moiuN,cd in parallel to form a unit known as-,
. (1) can .al,
n ' -. be wr itte n for materi;-.I b:i lane in·g in ca/anJria. Thc"' overall heat transfer coefficient, U, can be regarded as:'°
Equati •
the solute as.. . ·
o

mass;,;. weight fraction tor

o
follov,s.
FXJ," � fa1, + Vy
(2)
- Fluid film coefficient on steam side - always 'relatively higher.
- Thermal resistance of the metal wall- -- ·neglected because it is
I::ncro v Balancing be th e steam supplied small.
p lied for eva p or ation. Let S k!:
St.,.e.
" m is sup . nsate
th an en tha lpy of h 'kg. L l c.. kg be the co nde Fluid film coeffi.cient on the ljquid �id.c -: low, �ajor_ ,determinant
per hour wi J ce car. 1 �
· · g an ' ent . halpy of s he, · J/kg. c The h�at b:·i\an · · · · in heaqransf�r.
removed havm . vinl!- It. can be
..
ain ed fro m al hea t entering and total he·,1t lea The overall c oefficient ( U) is approximately nearer to the. lowest
obt : .
).
tot

represented by equation (3 '(3)

surface coefficient of the film... Any factor that improyes t�e coefficien(
. g( )
vin
. Heat entering (J) = heat lea J on the boiling side increases the overall coefficient almost proportion�:
ally. Some of the fact ors affecting these·coeffici�nts are: ' -�.-�
i t ten as:.
Equation (3) can also be \vr
. heat in thick liquor (product) -I Steam side - film coefficients' Boiling 'liquid sid�swface · ,1i;
(4)
Heal in feed + = heat in vapour + heat in c ondensate can be "increased 'coefficient can be increased ..' · · -�-,
heat in steam + heat lost by radiation., Tcrnpcraturc drop should increasing" the"vclocit); b)' pumpi�g
· ·' " ation bc,largc the liquid ,. , : ·
by rad iat i n is les s and can be negIcctcd The equ .
Lo�s of he at as.. High temperature at which decreasing the viscosity by feeding · : '.;
terms of mas� x enthalpy
o

(4) can also be written in (5 )

• condensation takes place hotEquid · · . ·.,r
F h + s1i; = Lh 1 • + Vhr + She Amount of non-condensed gas cleaning of. the heating surface .·:1:
. . ... ... ·
saturation tem· in steam should be minimum . : �·;
,.-
. . . tI1e difference between the
is .
'

dif fer en . ce
{

eratur e a
Te mp
and
' ' the b
..
oiling pom . t 0•·r the ·liquid · Gene·rally,
perature of t I 1e ste
· am ·evaporatio n Pumping liquids at high velocities (forced circulation) through. the·
"Ooc .IS sunicient for rapid:
te1npcr ature. differ. ence of 20 _lo ; ' e the t em pe rat ure less than tubes has beneficial effect. Such high velocities tend 'io' -decrease the
. may l1av
· of solution. . B ut 111 practice • the ,eed superhea ted and tI1e thickness of the viscous film and the buffer layer:, :,::.
ng poin t of the liqui d. The steam may be
boili
356 1'11,\RMACl:lil'ICAI. ENGINEERING
357
Ch·l2 EVAPORATION
Overall coefficients may be scrio u�ly lowered because of.­ l'Va o 1:aro s p to. the level o the
� � � � upper tube sheets. The, following
- corrosion o f the surfaces. opc1 at1ons a1- (; attempted to achrcve the
- , deposition of solid material from the l'Vaporating liquid. ?fleets as specified below.
I: The vent valves Vr, V2 and v are
. :_. The presence o f nonco ndens'.1blc ga5cs in the heating stean� (air). 3 kept open and all oilier
valves· nn: c loscd (not shown in Figure
12-8).
Efforts should be made to prevennhe ,1bove effocts. Forced circula­ 2. Now a high vacuum is created in the liqu
. tion is an important measure. i.e.. increase the velocity of liquid flo\y to r:ators. ·
.,. �f
id chambers evapo-
incn:as«: the capacity of the evaporator. 3. !he ste m valve S1 and condensate
� valve c ar� opened. Stea·�
is supplied. Steam first replaces cold air 1
in the steam space of
MULTIPLE EFFECT EVAPORATOR 1 Sl evaporator. When all the cold
'air is removed, the valve 'y
1s cl osed. , , . ' I
.
Vertical tube evaporator discussed earlier ic; a single effect evaporator
(Figure 12-J ). ;,uch evaporators a re connected in several w:1ys so as to . 4. The sup�ly of steam is continued until
th� desired ·pressure p0 is
achieve l:1rge scale evaporation as \\.'ell as gre.JtCr economy. Although created m the steam space of I st evaporat
or · . At th'1s pre
·
multiple effect evaporators are not used in the pharmaceutical industry. the temperature of the steam is r . ' · · · · ·· ·· ssu
' re,
the principks arc of interest and should be l!nderstood. This is illuss 0
:.',·
tratcd using an cxnmple of triple effect evaporator with a parallel feed
mechanism.
. ' ·· ·1

·
·c Advantages : (I) It is suitable for brge s<.:Jk :111<l for continuous
� ...,
operation.
(2) It is higbly econornic:il when com pa.rd with single effect.
(3) About 5 cvapor:1tors C:111 be attach.:d. '
Steam
Construction : Thi! construction of 'a multip1.:: effect �·v.:1rL'r:1tor is S1 '
sho,vn · in Figure 12-8 using J evapornlors. i.e.. trij1le effect evarorator.
The other aspects of coi1struction o f vertical tuhc evaporator i·ernain
same -as mentioned earlier. A perusal to f-igure I 2-8 indicates that the

>
vapour from first 'evaporat or serves as a heating medium for the .211<l i;prg..i uct
Condensate
,I

evaporator. Similarly, vapour from 2nJ evaporator serves as a heating F1 gurc 12-S. Triple effect evaporator
medium for the 3 rd evaporator. Last evaporator is connectc<l to J _
w1.thparallel feed arrangements.... ,
vacuum pump. 5. Stearn gives its temperature �o the liqu
id feed in the JSt eva"ora­
Working : Parallel feed arrangement is used in this example. tor" and gets condenscd. Coi1densate··
_ is 'rcniove.d througt th.e
valve C1• · · • · · ·.,···....,' · · ·
Parallel feed : In this method, a hot saturated solution o f the feed i>s
directly fed to each of the three effects (evaporation) in parallel without 6. Due t� �eat tr�nsfer, the, liqLtid tempera
tu�e increa�es and reaches
transferring the materi;I from-one effect to the other, The parallel feed tlic bodm� p�mt. During this precess, vap
. our ,�·ill be generated
from the l1qu1d feed.
arrangement is commonly used in the coril.entration o f s.alt so lutions, . . . ·. . · .' . · . � .-
where the solute crystallizes on concentration without · increasing the 1:· So formed vapour displaces air in the
:

upper; part ,of ·I st. e,'a�ora­

viscosity. tor. Moreover, the vapour also displace
s the air in the steam
' I

space: of the 2 nd evaporator. ·

' Operations : In the beginning, the equipment is at room· tempe!'aturc . . .
and atm�sp��ric press�re. The Ii9�i<l feed is introduced to all the three 8. After complete displace1nent of air
by vapour in, the steam
co°:partment of 2 nd evaporator, the valv
. e v2 is closed.
 Ch-12 E\'APORATION 359
35& p'11t\ RM:\(TUTIC Al. ENCilNl'ERING
. condensed to give heat of condensatipn. This heat will then· be trans­
9. The. vapour of 1st evaporator transmits its heat to the liquid of'
ferred completely to the liquid. The heat transferred nO\V serves as latent
2nd evaporator and gds conJcns-ed. Condensate is removed
·>.'
. . heat of vaporisation. i.e., liquid undergoes vaporisation· by receiving
through the valve C2· 1.h ese steps continue; 1n tI1e .,� r<l evapora• t or
heat. Loss of heal by any means is negligible: . · :;
also.
As the liquid in the l '1 evapurator gains temperature, the. difkrence The economy or an evaporator may be exp-�essec! as:., .. · ·
in temperatures between the liquid and steam decreases. hence, the rate . total 'mass of vapour produced
of condensation d,::creases. As a result, the pressure in the vapour sp.ace Economy of an evaporator = --· ----------
...
•
total mass of steam supplied . ·····-�
· or° t st evaporator gradually increases to PI by increasing temperature to
ti. which is the boiling point o_f the liquid in I st evaporator. and decrens­ In single effect evaporator, steam produces vapour..onl y° �nce. Hence
ing the temperature difference (to - t 1 ).
1 ' • :· ".-<\ ,

Ec.onomy of a single N units of vapour. prodticed,

/\ similar change takes place· in the 2mL evaporator and the liquid ---· ------- = I
effect evaporator
. reaches th1.: boiling poi 1,1t. Simil.irly. the process will be repeated in 3 rJ N units of steam supplied·
evaporator. Finally three �vaporators (or effects as they are called) cornl: In multiple effect evaporator, one unit- of steam produces ,vapour
to a steady state with the liquid boiling in all the three bodies. many times. depending on the num?er of evapqrat?rs conne�ted. Hence,
As boiling proceeds. liquid levt:I in � :;t evaporator comes down. Feed Economy of multiple N units of vapour produced :
is introduced through the feed valve to maintain the liquid level con­ ---------'--- = N
effect evaporator ! unit of ste�m. supplied
stant. Similarly ;vaporation of liquid takes place in 2 nJ and ·3 rd ' . '
,•
evaporators. To maintain liquid !'evels constant, feed valves F2 and F� Therefore, economy of multiple effect evaporator is N times the
are u�ed tor 2nd and 3rd evaporators. rcspectiv..::ly. This process is 1
\!COnomy of the single effect evaporator. However, such a great economy
c·ontinucd until. the liquid in all the evapor::itors ri.:::ichcs the dc5ircd is approximately true as it depends on ·many factors �(ich:.as temperature.
viscosity. of the feed, temperature range in· the evaporator; ratio 'of \Veioht of feed
� ..
Now the prGduci \'al\'cs arc opened to collect the thick liquid. Thus to the product and pressure difference.
in this evaporato�, there is ;:i continuous supply of feed. continuous
Glossary of Symbols
supply of stea�1 Jn<l continuous withdrawal of liquid from ::ill the three
b = Maximum vapour prc_ssurc at th�,te.mperature of ::iir, kPa. . .
evaporators. · Hence. evaporator works continuously with all the k111" b' = Pressure due to the vapour of t�cJiquid actually present in. the air,
peratures and pressures in balance. kPa. . . . . '. . . .
,- The evaporator can also be fed· by forward feed n1ethod, .backward C = Amount of condensate removed, kg. ' ·· ; ·
f�ed method and mixed feed. method. In the forward feed method, the F Amount of feed, kg.
,=

mother liquor is introduced into l st then transferred to 2 nd and �thc'n to he = Enthalpy of the condensate, J/k.g.
3rd. In the backward feed method, the mother liquor is introduced into hf = Enthalpy of the feed, J/kg.
hL ,= Enthalpy of the product concentrate, J/kg.
the 3rd evaporator, then tr�nsferred to 2nd arid then transferred to I st. In
hs = Enthalpy of the steam, J/kg.
mixed feed method. the mother liquor is introduced into 2nd evaporator hv = Enthalpy of the vappur, J/kg. j
then transferred to 3rd evaporator and then transferred to i st evaporator. K = Constant. mis.
' L =. Mass of product coHeeted fro� evaporator, kg.
Economy of Multiple Effect Evaporator . M = Mass of vapour formed pe-r unit time, m3 /s.
The economy of an evaporator is the quantity of �·apour produced per p = Atmospheric prcssurqihkPa.
unit steam admitted. It is calculated by cons·idcring the following \V-..
Q = Ratc-.of"hcat transfer,
assumptions. S = Amount of steam iotroduced, kg.
S = Surface area of the liquid exposed, m2 .
Feed is ;dmitted at its boiling point. Therefore, it does not require t.t = Temperature difference. °K.
any more heat to raise its temperature. Hence, the supplied steam gets
360 Pl·IARM,\C.TUTIC:AL ENGINEERING

XF = Solid content in the feed (weight fraction).

XL= Solute composition in the product (weight fraction).
U= Overall he.it transfer coeflicient, \\' /r.1 2 : K.
V" Amount of vapour l.iberated. kg.
y = Solute composition in vapour. (weight fraction)

QUESTION BANK
Each question carries 2 m_arks
I. Explain the term Evaporator capacity.
2. Define evaporation in terms of capacity and economy as applied to
evaporation practice.
3. Explain the construction of calandria. Give its uses.

Each question carries.5 marks

I. Elaborate the concept of multiple effect evaporation. What speci fi<.:
advantages does it offer?
2. Describe the construction and working or film evaporator of an�· one typl'.
3. Explain the c'onstruction and \\orking of a forced circulation ·cv:iporalor.

Each question carrirs to mnrks

I. Ho,,..
do film cvappra�or funcli;n'? .Elaborate the answ<:r with a neat sk.etch
of one sut.:h '!vaporator. List the n1erits. and demerits of film evaporator
0

system.
2. Classify C\'aporators. Describe construction and working of a film
c,·aporator.
3. fa plain the terms 'multiple effect evaporation· ant.I \·vuporator capacity'.
Hcl\� many effects generally go into a multiple eff.cct evaporator?
4. What do you understand by 'multiph.: effect evaporator"? Describe one
such evaporator. How do you feed such evaporator'?
 13
Crystal I ization

Characte;istics of Crystals.
Pharmaceutical Solids - Terminology
Theory of Crystallization
Equipment
Caking of Crystals

.. .
Ci)'stalli:ation is· the spontaneous arrange.111.ent ·_of the particles into a
repetith"! prdcrly array, i.e .• regular geometric pa'tterns. '.
In matter. particles ar\! ·pl"l!scnt randomly due to thermal agitation.
In gases the disorderliness is highest and in liquids it is modl!rat·e. The
liquids can solidify into C'rystalline forms. whenever· :mr.1ctio11 forces
between particles �re sfrong enot1gh 'to overcome· the disorderliness.
Cl)•stalliza·tion can take place directly from vapour of a st1bstancc. Exam­
ples are solid camphor from camphor vapour, solid iodine from iodine
.v�p(iur. St1ch a process is known as sublimation. Crystals: arc com­
monly obtained f rom liquid state. Example. is-salt from :brine. This
chapter of crystallintion deals with the later type; i.e., from. solution .to
solid state.
Crystallization differs from prc�ipitatiqn' in that �he. p;�duct·is depos­
ited from a supersaturated solution. Precipitation occurs. }\'.hen solutions
of materials react chemically to form . a. prodtict:.. �vhich. js sparingly '
soluble in the liquid and th�rcfore deposits out. · · · · ·
Drugs nre most commonly used in the solid state (pow.dcr fo.rms) in
the following dosage forms. · · ·.. · · ,···· · : '· '
1. Bulk powders for internal use, examples are fine powders and··
gr�nulcs.
, Bulk powders for external use, examples arc s11uffa: dusting
powders and tooth powders. .. . \ '

3. Simple and compound- powders for'intcrnal use... ,1 •. '

4. Powders in the form of compressed {ablets and tablet trit't1rates.
5. �owdcrs enclosed in cachets 'and �apsules. ·
361
362 Pllt\RMt\CEUTICAL ENGINEERING
In many occasions, drugs are supplied in the solid state even in the
injection dosage forms from the point of chemical stability.
Applications
'fh�· use of drugs in the solid state has several advantages.
Purification of drugs : Crystallization is used as a purification
process. It is used" for removing impurities from pharmaceutical prod-
Ltcts, i.e., recrystallization technique.
Better processing characteristics : Crystallization technique is used
to change the micromeritics of drugs such as compressibility and·
wcttability.
�Ease of handling : Crystallization facilitates various' operations such
as transportation and storage. � ."
Better chemical stability : C ry stallization increases the stability of
drugs. For example, amorphous penicillin G is less stable than crystal­
line salt. Amitryptyline is more stable in crystalline fonn than in
arn.orphous form. '·
Improved physical stability·: Crystalline forms play an important
role. in pi'pduct properties such as suspension stability and hardness of a
tablet. · Using dehydrating materials such as · dehydrated alcohol and
glyc�rol, the stability ?f hygroscopic substances can be enhanced.
Improved- bioavailability : Some drugs are more effective in their
crystalline form. For example, penicillin G docs not dissolve immedi­
ately in the gastri<;: fluids. Therefore, its degradation decreases. Hence,
bioavailability of penicillin G enhances.
Sustained release : Drug substances with different sizes of crystals'
-can be used in the production of sustained release dosage fonns. For
example, protamine zinc insulin in crystalline form slowly and continu­
ously releases insulin from the site of injection for prolonged periods.
Miscellaneous : Certain crystals are used in the production of semi­
conductor devices, laser beams and artificial gems.
CHARACTERISTICS OF CRYSTALS
Crystal Lattice
A crystal can be defined as a solid particle, which is formed by the
solidification (crystalli;z:ation) process (under suitable environment) in
which structural units a:-e arranged by a fixed· geometric _pattern or
lattice':
Ch-13 CR YST/, LLIZATION 363
Crystal lattice is de tined as an orderly internal arra�gement of parti-
cles in three-dimensional space.
. The geometric form in which struct�ral units arc arrang�� in a crystal
is determined by means of X-ray diffraction pattern. TIJ.e .!hree dimen­
sional arrangement of particles in a crystal is also known as space
la/lice.·
The units that constitute the crystal structure are .ions, atoms or
�'f- '.
n1olecules.
- Ions with opposite charges are b<;mded together b; :�·lectro�atic
• attractions as in the crystals of sodium chloride..
Atoms are bonded together by covalent bo:fd as in diamond, and.
graphite.
-· In most organic compounds,· molecLdes are' held together by van
d1,;r Waals' forces and hydrogen bonding. Examples are naphtha­
lene an� p-hydroxy ��Foic acid.
The smali';�t geometric portion. which repeats to build up the whol.e
crystal. is called a unit ccli.
A crystal is bounded ,by pl,ane surfaces called faces.
0
In t hc crystal, the angle between · the two perpendiculars to the
intersecting faces is termed as the axial (IIJgle.
,lxial length can be def!ned as the distance between the centres of
two atoms.
If a crystal is fractured, each fragment oLthe crystal also pos­
sesses plane surfaces \.Vith characterisf·ic · axial
,. · angles of the
original cryst:.il.
·· .Certain properties of. c1ystals such, as refracti�e index depend
upon the direction in the _crystal along which 'the determinations
arc made.
Crystal Systems or Forms
A finite n�mber of symmetrical arrangements are possible for a
crystal lattice and these may be termed as crystal forms or crystal
.l')'.l'f<!JIIS.
Depending upon the axial length and axial angle, crystal f<,mns ar�e
designated as et!bic. hexagonal. tetragonal, orthorhombic, mo'noclinic
and 'triclinic. They are shown in Figure 13-1. A chemical· substance
may exist in more than one form, i.e., polymorphism. .,.,,, ·
364 J> IIAIU,fACEUTJCAL ENGINEER-iNG Ch-13 CRYST!\Ll.lZA TIO� 365

of faces' is sallle in all specimens. It is the characteristic of', p, rticular

substance irrespective of the relative sizes of the faces.
A.P.- The shape and size of the crystals formed are markedly dependent on
f-
b b .f-b the conditions under which crystallization is carried out. For example,
. . griseoful\'in crystallized from acetone has a different form from the sume
drug crystallized from benzene or chloroform.
CUBIC TETRAGONAL liEXAGCNAL
a :a p =- y = 90° a -= p :a y :a 90'' u = II = 90° . y = l 20° Depending ori the arrangement of fi.1ccs. crystal habits arc described
. a-b·c·
Eg. Sodium chloride Urea, Potassium
a-bi'c
Ice
.
in different ways. These art: show·n in Figure 13-2.
'

· Potassium chloride dihydrogenphosphate Thymol

• Pl.Mt TA6:Ji.AR
e.g.: Naphthalene e.g.: Tolbutamide,
Cyclizine

RHOMROHEDRAL
u := � :a y t 90''
b ORTHORHOMCIC
:= 0 = y =. 90°
0.

a;bi'c
Eg: Barii;m sulphate
Sulphacetamide
B [:)\!MIT

e.g.: Sodium chloride

·CCl.l.iM;'lAR
·e.g.: Fluorocortisone acetate
c Triamcinolone Jcetonide

a b ·a
Pb TRICLIN!C
_/ _ / BLADED
MONOCL!NiC e.g:: Resorcinol
u "' i1 90 °' y 'f- 90 .
:=
a 'I- P 'I- ·1 = 90�
a,. bi' c a i' bi' c
.e.g.: Sucrose e.g.: Phenolphthalein AC!CULAR
Ephedrine hydrochloride Copper sulphate J
e.g. Nalidixic acid
Figu� 13-J. Different type:; of crystal svstems
• · Figure 13-2. Different types _or crystal habits. with examples.
with characteristics and ex.impl.:s. .
Columnar : Ro<l like particles having a width and thickness exceed­
Crystal lfabit ing that of nl!�dl'e type par\!rLes. The term prismatic may also-be used.
Crystal is a, �olyhcdral solid �vith numbt;r of planar surfaces. A Blade : I'.ong, thin and flat particles, which can also be referred .t o,,as
_
substa �ce crystallizes 111 such a way that the angle between a given pair being lath shaped. ,
366 PHARMACEUTICAL ENGINEERING.
367
C'h· 1:1 CftYST/\1.1.17.ATION
guishable in each form, polymorphs
Plate : Flat particles o f similar length and width. Th�y arc als� though the drug is chemically indistin
to a number of properties such as
de noted as being lamellar or micaceous. differ significant!)' with respect
dissolution rate.
Tabul�r : r-lat particles of similar le. ngth and width., but posscssmg
_
. density, melting point. solubility and
orphs slowly convert i nto
gr�ater thickne ss and flakes. Metastable polymorphs : These po lym
ion is so slow as to be ne gligi ­
Equarit : Particles o f similar lcligth, width and thickness. _ , .. .., stable pol) :norphs. 1 r the r ate of convers
product. metastable pol ymorph.s
ble d11ring the expected life of. a drug
sicochemical propcrtks.
Acicular: Needle like prisms. arc prcf�rrcd !)ccause 0f thei r unique phy
melting points. hi gh�r solu­
The rncta�table polyrnorphs have lower re,
ir stable polymorphs. Therefo
PHARMACEUTICAL SOLIDS-TERMINOLOGY bility and hi gher dissolution than the s. For exam p le ,
of dosage for.m
Pharmace utical powders an: available either i� amorphous i•orm or 111 . these arc preferred in the production ch vary in
talline forms, whi
crysta 11'me fiorm. Further cry stalline solids s uch as polymorphs , h y d rates riboflavin can exist in three different crys Hie
per litre to 1.2 g per litre.
and solyates are used in the manufacture of dos·age fio. rms. water solubility at '25°C from 60 mg
morph ordinarily results in in-
· increased solubility of metastable poly
Crystalline Soliqs creased dissolution and absorptio n.
loyed when met asta b l e
Crystalline solids have definite shapes and an orderi)' arrangement o f
. Stable polymorphs : Th e se arc emp
rapid decomposition.
·
un1ts. Thcse are incomp r essib le. These sho w dcfm =•·t e melt'mg po mt. polymorphs arc not suitable: on account 0f
Example s arc sod'ium c11 1 onde,
· ure a, benzylpenicillin anJ aspirin�
Crystall in e forms have lo w solubility and dissolutio n. This fact has Crystal Hydrates
ociafe with water. · The
bee n t�ken as a1� advant�ge t� produce sustained r elease products. Ex­ Some drugs h:ivc greater tendency .to a�s
_ hydrcac. Examples are caffeine
ample is protam111 e zmc msul 111 susp e nsion for injection. resulting substance is refe r red to as Jr11.�
monohydrate etc. The ,\1,1{))'­
hydrate. thcophyllinc hydrate, ampicillin
gives better b io availability than
Amorphous SoHds drous form dissolves mo re n:adily ;rnd
forms arc Jh e preferred ones.-, ,
Amo rphous solids do not have spcci fie shapc·(Greek: amorphe meant hydwus form . Therefore , ,anhydrous
neutral molecules. S odium .
.
without form). The stru�tural u�its are arranged randomly in the solid. Water can combine with positive_ ions and
official in IP and BP. S ome
Thes� do not have defin1te me ltmg points. Examples are glass' pitch, carbonate dccahydratc, Na2C 0 3. I OH20 is
ates. Fo r example, soditfm
plastics and novobiocin. , · substances· form a number o f crystal hydr
Na2C03.8H20 , Na2 C0 3.6H20 ,
Amorpl�ous form �f a c ompound is alway s more soluble than the carb�natc is avail.able as Na2(;;Q:,. I Ol-120,
, arnpicillin monohy drate
-
correspo ndmg crystall ine form. Therefore ' it may exh1'b1't better thcra- Na2C03.SH 2 Q.,and Na2C 0 3.H2,0 . Similarly
. . .
pcut1c act1v1ty than the crystalline form. .' For exampIe, amorphous and amricillin trihydrate are available.
' . . . . . .
novob�oc�n (ant1b1ot1c) has s1gmficant biological activity than crysta II'me Crystal Solva tes
·
novob 1o qn. ociate with solvents to
Certain drugs bvc greater tendency to ass
e solvates are also known as
It i,s-' not alway s possible �o de te r�i� e the solids as cry stalline o r p roduce cryst.alline forms of solrntes. Thes
with n-pentanol or ethyl
amo rphous by casual observatio n. For example, beeswax and paraffin pse11dn111r11phs. Examples arc fluo rocortisone
ntanol dissolve much 111'.)re
although appear to be amo rphous assume cry stalline arrangcmel'ts ' whc11 acetate. Succinylsulphathiazole with n-pe
lphathiazole. Therefore , for
heated and allowed to cool slowly. rapidly than non-solvated form of succinylsu
s are preferred.
Polymorphs better bio:ivailability, solvate forms of drug

�ertain dr�gs can exist in more than one crystalline form. S�ch .a lsomorphs
crysta,lline form, the
phenomenon ts known as polymorphism • About 63o/c.0 of barb'1turates When two or more substances ·possess the same
in the saturated solutio n o f
..

67o/co of s tero1'ds and 40 0Yo o f sulphonamides exhibit polymorphism. Al� crystals of one such substan'cc can be g rown
• 0
368 l'l'IJ\RMACEUTICAL ENGINEEl;I!'-:G Ch-13 CRYSTt\LLIZATION

the other. This phenomenon is known as isomorphism. Such substances · 1_'. i"
(3)' Formation of a new solute as a result of chemical reaction. . 'I !l
are said to be isomorphs (having the same shape). For example, chrome
···.. �
(4) Addition
. of a substance,' which is more soluble in solvent. . thatl.
alum K2S04.Cr2(S04)3.24H20 is isomorphic with potash alum the solid to be crystallised._ ·
K2S04.Al2(S04}J.24H20. The chromium in chrom.c alum has the same . ,,
valency as alumii1ium in potash alum. In the ;.ibsencc of seed crystals, significant supersaturation is neces-·.-.
sary to initiate the crystallization througl��formation of nuclei. The ·rate.
of separation. particle sizc, uniformity and distribution depen_d on two 1
successive largely indepe1.1dcnt processes, namely, n,ucleation and gro\yth:-·
THEORY OF CRYSTALLIZATION
Mechanism of Crystallization of nuclc.i. · w

The mechanism of the crystallization of substances from the solution

(B) Nucleation = Nuclcario.11 refers to the �irth of vc?' sm�II bodi7�::;
is explained using figure 13-3. . _ _
of;\ new phas� withm a homogenous supersaturated liquid phase.
. t,ot\ of soi,.,_ Particles (ions, Nucleation is a consequensc of rapid local fluctuations at the molecu­

-----. · [±]
. t� atoms or molecules) lar level ,vhrn molecules or ions or atoms are in random motion in any
. Loose aggregates

LJ.
small volume.
.. .. .. ... ...
Addition of
Cooling of solution ..,· · :·
� _ ; .. :. /:· crystal or
',• ·. · Initially sevcra·I molecules or ions or atoms associate to form clusters .
J
. ·;. ·• ·: • ·bre1kin9 of
-.. . clu5ters

11
Solution � Supersaturated
wuk crystal These are loose aggregates, which usually disappear quickly.
(Saturated or . . solution However, ·when enough particles associate to form an embry o, there
Add1twes
unsaturatEd) is a beginning of the lattice arrangement and the fon:natiori of a new
� ·'l � solid phase. In most of the cases, embryos have short li, es and dissolve
1

Embryo {Lattice as soon· as they form. An embryo may grow to such a size that. it is in
arrangement)

·�·l
I thermodynamic l.'quilibrium with the solution.
Diffusion 1nd
·,· deposition of The initially formed crystals arc of molecular size, \yhich arc termed
particl�s on as nuciei.
nucei
Nuclei On certain occasions, the nuclei grow in dimensions .that are limited ,
°by . the amount of material available arid thus fonn crystals.
Crystal growth Nucleation
Several methods are available for nucleation. These arc:
Figure 13-3. Mechanism of crystallization 'of
' ..

(I) Soft or weak crystals on impact with moving parts in a crystallize(:

solutes from a solution and the steps involved.
can break into fragments which act as nuclei.
The formatiog of crystals from solution involves three steps. ·.. :.
(2) Small crystals which are· formed in the· previou_s process are
(A) Supersaturation added to act as nuc,lei. ·;,,
EB) Nucleus formation
(3) In a supersaturated solution or' under poor mixing, needle Jj,ke
(C) Crystal growth
structures are observed on the ends· of crystals. These structures .
.,(A) Supersaturation : When the solubility of. a -:ompour.d in a grow faster than the sides of the crystals ang come out to give,:..
� ·
soh;.ent exceeds the saturation solubility, the solution becomes SLipcrsatu­ crystals of poor qual\ly. ' ,,:.:
rate�d and the compound may precipitate or crystallize. Supcrsaturntioon
(C) Crystal growth : Crystal· gl'owth is a .diffusion procesf and .·
can be achieved through:
�;°urface phenomenon. from solution, solute. molecules or ions reach the
(1) Evaporation of solvent from the solution. faces of a crystal �y diffusion.dJ_n reaching th� sur�ace, the molec.ule� or· ..
(2) C_o_oling of the solution, if the solute has a positive heat ofsolution.
_
1
ions must be acr;.cpted by the crystal and orgamzed mto the space lattice.·.
.
p
370 PHARMACEUTICAL ENGINEERING
This phenomenon continues at the surface at a finite rate. Neither the
diffusion nor the interfacial step will proceed unless the solution is
supersaturated.
Mier's Supersat�ration Theory
Mier's theory of supersaturation postulates a definite relationship
between concj!ntration and temperature at which crystals will spontane­
ously form in an initially unseeded solution.
Accord°ing to it, the supersolubility curve represents the limit at
which, nucleus· formation begins spontaneously and consequently the
point where crystallization can start in the absence of any solid particle.
t
Normal solubility
curvf
curve
'A----(.
c
0
:c;
G an area rather than a line.
...."'
·1:
D C B (2) If the solution is kept for long�r periods, nu�leation starts well
· 8
Temperature --•
Figure 13-4. Mier's supersaturation theory,
CPDE represent the path of cooling .
·c' . .
A plot of temperature vs. concentration of solute is shown in figure
13-4 . The curve AD represents the.nor�al solubility. Any point on the
curve represents the solute in equilibrium with the solvent. This is the
maximum limit for the solubility of a subst�nce. The curve FG repre­
sents the supersolubility, which is roughly parallel to the 'normal solubility
curve. It represents the limit at which nucleus formation begins sponta­
neously. The region enclosed between these two curves AB and FG is
referred' to as metastable state, indicating that the syst�m is unstable and
undergoes changes.
. The liquid may often be cooled a few degrees below its freezing
. point without crystallization t.tking place. · Crystallization starts if this '
limit is exceeded. Consider a point C with a ddinite composition and
temperature. On cooling this solution, crystallizatiori'is expected to start
from point P, however, it does not happen.
According to Mier's theory, crystallization do not s.tart 'at P but it ,
takes place sqmewhere in the neighbourhood of the point D. when
certain conditions are specified.
Ch-13 CRYST,\Ll.lZATION 371-':
· ·'.
Mier· states that under ideal conditions of crystallization· nucleu;:.
formation starts at FG and crystal growth begins.
Then concentration of sµbstance roughly follows the curve DE.
.
Conditions for obeying Mier's theory:
.
(I) The solute arid the solvent must be pure.
(2) The solution must be free from solid solute particles.
(3) The solution must be free from foreign solid matter.
(4) The solution must be protected from entry of any particle.
(5) Soft or weak crystals must not form during the process.
(6) There should not be any fluctuations in maintaining the tempera-
· ;·
ture.
Limitations:
(I) According to Micr's theory, crystallization st� at supersolubility
curve. But general te�dency is that crystallization takes place in
. below the supersolubility curve.
. "''
( 3) If the sol_�tion is available-in large volume, nucleation starts well
(,
below the supersolubility curve. This is because formation of "'
nuclei depends 0n accidental collisions of molecules of solute.
These collisions are more in large volumes than in· small volumes.
(4) Mier's theory is applicaole when pure solute and pure solvent
are used. In practice, it is i.mpossible to get them in pure stat<::,
(5) For crystallization, the soluti<�>n must be stored for longer peri­
ods. Puring storage, millions · of dust particles can enter.
Nucleation can be initiated not only by solute molecules, but.. _.,
. also by dust particle.s.
,Solubility Curves
Solubili� curves are useful in.predicting the experimental conditions
desired for crystallizing a substance.. Since supersaturation is achieved
by reducing the temperature, t�e influence of temperature on the solubil-
, ..
ity. of a substance is important. .
A substance di;isolves and goes into solution, if the solution is not
satu'.�te�. ': the �elution is supersaturated, crystallization takes place.
Equ1hbnum 1s attamed when the solution is saturated. The' graph drawn
by taking temperature on x-axis and solubility on y-axis gives the·
372 / l'I IARl\1/\Cr:lJTICAI. ENGINEERJN(j l"h-13 CR YSTAl.1.IZA TION

solubility curve, which represents stable equilibrium conditions .. The (4) Curve 4 represents sodium carbonate. This curve is unusual.
metastable c.ondition of the_ substance is, also represented in dotted line. Herc solubility of sodium carbonate increases with temperatt1rc,
The solubility patterns of some substances arc shown in Figures 13-S(a) if it is in hydrated form. Once the compound turns
· . into mono-.
and (b). hydratc form, its solubility dccr'cases.
-.P
.

EQUIPMEN:J'
..., •, J
In commercial practice, it·is highly desirable to-have the product not
.
�o
VI N
::, :x: only of uniform size, but also of a particular size distribution. It is neces­
.--��
' �IQ'
'.;iary to control the formation of nuclei, since the - n�mbcr of nuclei controls
the size of c�ystals. Once ti1e nus lei are fon��d, :they start growing.
� a.·
C O
"'0 . 1.., fl� . � ,· . :
Dcpcrn.ling on the conditions of crystallization, it is possible to ·•
VI ....

"' "'
t �
- Stable
a.. Q.
control or 1)1odify the nature, of the crystals obtained.
--- Metastable ' '
(I) If the solution is cooled slowly, just above saturation
- point, crys-
tals of larger size arc form�d since the number of nuclei is less.
Temper,ature
(2) !(the solution is chilled rapidly; a crop of small crystals is
(a) formed, since rapid cooling increases the· degree of supersatura­
tion resulting in a large number of nuclei.
(3) When polymorphs exist, careful temperature control ,and seeding
with the desired crystal form are necessary.
(4) The habit or shape of a given form is often '.highly dependent on:
· (a) impurities in solution,
(b) pll,
(c} rate of stirring,
(d) rate of cooling,
T!!mperature ( d) solvents.
(b)
Very rapid rqte of crystallization can result in the entrapment of
Figure 13-5. Typical solubility curves of certain substances. impurities in the crystals.
The following conclusions can be dra;n regarding the .effect of Crystallization equipment is classified according to the method em­
temperature on the solubility. '".' ., .. ployed for producing the, supersaturated solution. Some large-scale
(I) -Curve 1 represents potassium nitrate. Thi� is the most common crystallization equipment are discussed below.
type in which the solubility of a substance increases'"with tern�
perature. Agitated llatch Crystallizer
Principle : In agitated batch crystallizer, saturated solution 'is made
(2 ) Curve 2 represents sodium. chloride. The solubility increases
with increase in temperature, but to a marginal ext�nt. supersaturated by reducing the temperature. The crystals' are formed
from the supersaturated solution. Agitation of the solutfon facilitatc;s t�e
(3) Curve 3 represents sodium thiosulphate. Here sol�bility in­ production of uniform size crystals.
creases rapidly with temperature. But inflections are observed in
the curve to represent different hydrates. · · Construction : The construction of an agitated batch crystallizer is
. .. .
shown in Figure 13-6. It consists of a cylindrical contai11er with a

I

PHARMACEUTICAL ENGINEERING
own
conical bottom. A propeller is fixed centrally, which _rotates on its
axis with the help· of a motor. Pipes made up of good material for
. conducting heat arc run from right bottom to left top of the crystall izer.
Q.,,,..·
Water .­
Agitator shaft
outlet
Water
inlet
Figure 13-6. Construction of agitated batch crystallizer.
Working ;· Solution to be subjected for crystallization, is placed in
the crystallizer.· Cold water is passed througn the pipes continuously.
Due to cooling. the solution becomes supersaturated and crystals are
formed. The propeller is allowed to rotate, which serves two purposes.
Firstly, it increases the rate of heat transfer thereby helps in.maintaining
the temperature of the solution almost uniform. Secondly, It keeps fine
crystals in suspension, which facilitates them to grow uniformly. Other­
wise, large crystals or aggregates may form. The crystals_ are collected.
from the bottom by a suitable mechanism__for the separation of mother
.
.
liquor.
ii Advantages : In agitated crystalliz�r, crystals fom1ed arc .more uni­
form and also more fine compared to older crystallizer such as ''iank
crystal Iizer.
Disadvantages : It is a b!\tch_ or disconti�uous equipment. Solubility
is least at the surface of the cooling coils. Hence crysta! growth is most
rapid at this point and the coils rapidly build up with a ma�s of crystals
that decreases the rate of heat transfer.
·., 1:t_;
Ch-13 CRYSTALLIZATION 375 _.,
Swenson Walker Crystallizer
· Princip,lc : C rystallization is induced by passing the cold water in a·
direction opposite to the flow of hot concentrated solution. This results
in supersaturation and subsequently crystals are deposited. Agitation
prevents the accumulation of crystals on the cooling surface. The
crystals are simultaneously separated from ' the mother liquor and there-
.
fore it can be used as a contrnuous process.
Construction : The construction of a Swenson Walker crystallizer is
· shown i i1 Figure l 3-7. It is a linear: type and consists of a long open
trough about 0.6 metres wide and 3· metres long with a �emi.;cylindrical
bottom (sid'e �iew of Figi'.1re 13-7). The. trough is welded ;ith a water
jacket externally. Long pitc� spira·l scrapper is fixed as close to the
bottom of the trough as possible (top view of Figure 13-7). Spiral
scrapper rotates on its own-axis with the help of a motor. For higher
capacity, maximum of four such units are joined together. · For still
.
higher capacities, several such sets are placed one above the other. In
this arrangem7nt. the solution flows from cne set to its below set.
Open trough
/ A�itator Open trough J�cket
8-·
--- Connection between
Jacket TDi> view "J'!:,'lo sets
view
Figure 13-7._ The construction of Swenson W�lker crystallizer.
.
Working : The hot concentr�tcd solution to be �rystallized is fod at
left side of the trough. Cf>oling water enters ;through (other end) right
side in the jacket. Due to cooling of the hot solution,' supersaturation is
achieved and crystals begin to form. _ If necessary, 'the size of crystfils
can be controlled by injecting an extra amount of cooling water into the
selected sections. Spirai scrapper rotates on its ownlaxis at a speed of
7 revolutions per minute. It helps in agitating the 'mixture and convey�.
ing of the crystals. It also prevents the accumulation of crystals oh the
cooling surfaces by lifting them. This resul�s in a suspension,· which
allows the crystals. to grow ind,'.\{dually. Thus aggregation ts prevented.
 .i 7 (, l'llt\RMACEUTICJ\L ENGINEERING (.'Ii· I J C:RYSTi\LLIZJ\TION 377
. .
Draining table is itttached to one end of the crystallizer. Motilcr The crystallizing chamber consists of a bed of crystals suspended in .
. liquor and crystals together over flows into the draining table. While nn upward flowing stream of liquid. Supersaturated liquid flows through
crystals are rctai11cd, the 1nothcr liquor is sent back to crystallizer. · The· the bed of crystals, which arc maintained_ in a fluidized st:ite. A unifo nn
· temperature is thereby attained. There is a continuous gradation of
wet crystals a:e conveyed _lo a centrifuge.
crystals in the chamber. Coarse crystals settle at the bottom. \�·i�ile fine
· · i\ screw conveyor can also be used in place of the draining table.
cryst�ls 1:emain abov: coarser ones. · Very fine crystals overflow through
Screw cot1veyor wi.t h a slight inclination lifts the crystals from solution _
the liquid and enter into the re-circulating system. which then combine
and deliv'ers to a centrifuge. Mother liquor · overflows at a convenient
with fresh feed. f-rom time to time, coarse crystals are taken out throuoh
point ..' "'
the opening at the bottom o_f the chamber. · · ·
Advantages : (I) Large saving in floor space, material and labour
costs can be achieved in Swenson Walker crystallizer.
(2) lt is a continuous process.
(3) Crystals of uniform size and free from in�lusions or aggrcg�tions
, . can be obtained. ._ Vapour
head
Disadvantage : The scrapper may break, the crystals to a little extent,
while agitating t'1e' suspension.

• Krystal Cryst:.1llizrr
Principll' : In Krystal crystallizer,. concentration or liquid and crys­
Heater or
tallization are obtained in different chamb�rs. namely vapour head and
crystalling charnber. The concentration of liquid (supersaturation) is
ind'ficed by evaporation of hot solvent with the help of a vacuum P,_Un�p. j
In the crystallization chamber, the supersaturated solution and ·crystals C�;stal
are' maintained in a fluidised state for uniform crystal growth. As the growth
crystals of desired size settle down by gravity, the fine crystals and chamber
Circulating
supersaturated soiution is recirculated for further crystallization. Crys­ pump � Product
tals of desired size arc collected from the crystal growth chamber. discharge

Construction : The construction of a Krystal crystallizer is shown in
f '. Figure 13-8. It consists· of a vapour head 'and crystallizing chamber.
Vapour head consists of a l�ng tube, which extends almost to the bottom
of crystallizing chamber. Other end of vapour head is connected to con­
denser and vacuum pump. A pump is provided which allows the. feed to
enter vapour head. On its wa:y to vapour head, a hc:!ter is provided.
Working : Solution is puinped, which passes through the heater.
.The hot solution enters the vapbur head. Because of reduced pressure,
the hot solutio_n undergoes flashing,· which results in the· formation of '
solvent vapo_ur and supersaturated solution. Vapour is re;inoved by
suction pump. Supersaturated solution passes through long cube belo\v.
The operation is controlled i'n such a way that crystals do not form in the
vapour head but should form in the crystallizing chamber.
Figure 13-8. Krystnl cr/stallizer.
Uses : Krystal crystallizer is u:;ed for crystallisation of sodium chlo­
ride and magnesium sulphat,e.
Advantages : (I) Krystal crystallizer is preferred when large quanti�
ties of crystals of controlled sizes are required. .
(2) This crystallizer is available in very brge sizes with a body up
to 4.5 metres diameter and 6.0 metres height.
·.
�acuum .Crystallizer
Principle : In vacuum crystallizer. supersaturation is obtained by
acli:ibatic evaporative cooling. When warm saturated solutioh is intro­
duced into the crystallizer, due to high vacuum the solution undergoe�

' .
378 ' PHARMACEUTICAL ENGINEERING
Ch-13 CRYSTALLIZATION 379
flashing. A part of the s olv ent gets evaporated, th�reby cau sing cooling
1

�ausc s supersaturation and cryst�llization. · The evaporation of the sol­

of the solution. From the re sulting s upcrsatu,rat1on, crystals a r� pro-
vent en hances the yiel d. Flashing of the solution in the crystall izer leads
duced.· . . 10 ebullition, which keeps the crys tals in suspension, until they b�come
Construction : The constru c tion o f a vacuum cryst allize'. · is show � in large enough to fall into the discharge pipe. The propellers mix the
. a cyli dri al body with a conical
F 1gure 1 .)"-9 . Vacuum crystallizer i s n c
contents thoroughly and prevent the content s reaching the discharge pipe
witho1,1t flashing. With the help of puh1p, the product is collected and
subjec ted to filtratiqn or centrifugation to <:>btain c'.rystals. The filtrate
· returns to the feed.
Uses : ,Vacuum crystal lizer· is suitable for• therm olabile substan ces,
due to low temperature conditions.
Ad\'antagcs : (I) Vacuum crystallizer is very simple without any
m oving parts.
(2) Corrosive materials c an be u sed, as inner surface can be made
acid resistant.
(3) It can be constructed as large size as desired.
(4) It c an be operated either batch wise or conti n uously.

CAKING OF CRYSTALS
Caking can be defined as th e process of formation of clumps or cakes
when cryst�ls are improperly stored.
· After crystal l ization, the cry s tals are :equired to be stored in bulk'
either for further use or for transportation or for the formulation of
dosage forms. The crystals m ust retain good flow properties during
s torage. For exam ple, they can pass freely from hopper to d ie in case of

Figure 13-9. Construction of vac�um crystallizer. tablet punching. During storage, crystals may tend to form a cake. This
prob l em is ·serious in ca s e of smalJ packages than in bulk packages. I n
n p ump
bottom. A condenser is attached to the cry�tallizer with a vacu u � s ome cas es, the pressure of a thumb can easily break the lumps , but
� d1schar�e
1· � between The bottom of the c rystallizer is attached to considerable pressure is requir ed to break the cake in some · other cases.
l nte�na l ly the body of the crystallizer
ca n be lined with aci d '

Critical humidity is the humid ity above which crvsta l s abso:b mois-·
,!'

���:·tant · materiai such as kad or r ubber. Two prop ellers ar � p l .::ced ture and below. which they .do not ;bso�b moisture. • .,,,;,
the disch arge
above discharge pipe to prevent short circuit of the feed (to
When' a cry stal i s placed in contact of air, whose �umidity is below
p\pe).
. 'he the critical humidity, the crystal remains dry. On thcf other hand, if th<!
Working High vac uum is created usi�� a va�uum pump : air contains more moisture than cr.iti�al humidity� the crystal ab sorbs
o th so lut'. on ,
vacuum so created must correspond to a boilin g point � : moi s ture.
is fed i nto
bUt I OW er than the feed• temperature. Hot saturated solution . · Th\! crysta ls get a s aturated film on the surface by ads.orbing mbis­
at a c nveni ent p •
o mt. Soluti• ' un d e� gocs flashing
crvs'ta
the -� llizer o on
., ture. So formed s�turated· solutiG:, concentrates at the points of contact
1s allowe.d ad1-
which results in evaporation of soI vent. Th'is process . by capil.lary fort"c s . When water evaporates or when the temperature
resultant cool mg
abatically so _that the crystallizer body .is cooled. The decreases, crystalli1..ation of solute take s place to form a solid bridge.
' •
I
 380 l'l lt\RMACEUTICAL ENCilNEl:IUNG Ch-Iii CllYSTAI.LIZATION
381
Factors Affectin� Caking QUESTION BANK
Size of the crystals : Crystals of larg�r size contain more void Each question carries 2 marks
• spaces. On the other hand. crystals of smaller size contain less void I. Dclint" crystal lattice and cryst:il habit.
space and possess more points of contact. The more the points of · 2. Enumerate the charactcri�lics of' crystals.
contact, the higher will be the rate of caking. I-knee. smaller sized
3. Ddin.e crystal and critical humidity.
particles tend to cake more than the larger particles.
4. Enumeratc different types of crystals.
ghape of the cr)'stals : Spherical particles possess the least po�si.�le
5. N.:ime a suitable crystallizer for the following.
points of contact. The points of contact increase as the crystal shape (:1) to get large sizcd'crysta!s.
deviates from spherical shape. Hence, distorted crystals tend to cake (h) to cryst:illizc large quantity of suhstam:c.
more than the spherical crystals.
E:acl1 qurstion carries 5 marks
Humidity : The higher the hL1midity of atmosphere to which Cl)stals I. Dcscrihe the working of agitated batch crystallizer.
arc exposed, more will be the rate of caking.
2.
Time of exposure : The higher the time of exposure, the more will
be the caking. provided the exposed atmosphere has humidity more than
critical humidity.
Impurities in crystals: The crystals can be coated with the impurities
Jerivcd from mother liquor. This may increase ar decrcasl: critical
humidity. Once the critical humidity changes. the property of caking also
changes. For example calciLtm chloride and magnesium chloride arc the What ire the conditions to be taken during cryst
allization io obtain large
impurities for sodium chloride crystals to ;ilter it's critical humiJity. sized crystals? ·. " '
Melting point of crystals : Melting point of ccnain crystals is near 9. Describe how n ucleation and Cl)'Stal gr<?Wth take
. place .during cry�tullization.
room tempcrature. crystals may melt. Then soliJilication by fusion of I�·. What arc the pharmaccutical application's of cryst
alli i:ition?
the melt kads to caking. Eacit question carrie.s IO marks i; •·t� ,•
Temperature fluctuations : When temperature is increased. melting I. Discuss th� Mi�r"s super-saturation theory of
· crystalliz�tion. What arc the
of the crystals takes place. Subsequent decrease in temperature leads to limitations of the Mier:S theory?
,
solidification. Therefore, temperature fluctuations cause variations· in 2. Explain the principle, construction, working and
advantages of vacuum .
the solubility, which may lead to caking. crystall.12cr. . . · ··
3. Giving ·neat dia�ra�. describe the constru�tion
Prevention of Caking . and work'ing of Krystal
crystall1zc r. Write its adva.ntages and applications. · ·
(I) -Crystals must be more spherical in shape, with the least �oints of 4. Draw a neat labelled diagram of Swenson Walk
er Cl)'st
contact. . •
construction, working, advantages and disadvantages. allizer. Discuss the
I
(2) ,C ry stals must be larger in size with more voids and must be of a
narrow size distribution.
(3) Crystals must have highest possible critical humidity.
(4) Crystals must be coated with powdery inert material to prevent
absorption of moisture.. For example, table salt is coated with
magnesia or tricalcium phosphate. Similarly, flake calcium
· chloride is coated with anhydrous calcium chloride.
 Ch-14 J?�YING
I/;:..,-
383
/
ifrtications
�--P r'epa�i;n of bulk drugs:. l�-�:J'!_.CE_ar�tio�_of bulk.drugs, drying
is the final stage of proces sing..,...A few examp��s
. are:
d ried alumin ium hydroxide'
14
Q
• .,

- spray dried lactose

powd ered ·e�tracts
Drying step is essenti;�certain operation s suih as crystalli�ti6n ..,
Drying and filtration. "-.....
·
... �
........ ,

. · Preservation 'of drug products :�'Drying 1s necessary m o rder tci

Theory of Drying
Classification of Drying Equipment
Equipment
nts. of water or other
/Drying is defined as the removal. of. small amou
eat
· liquid from a material by t he apphcat1on of h �
ids me �han i cally by
The liquid medium may be remov ed from t he. sol.
n. It ·� chea� r to '
a filter press or centrifuge or ther mally by vaporisatio .
a le
remo·te liquid by mechanical l y t han thermally. Th e refo �e, 1t is adv1s ?
ctmg to the dryin g
to reduce the liquid as much as possible be fo re subj
e
avoid det erioration. A few examples are:\'
t,rt?
Crude_ drugs Q.S animal and vegetable origin - chemical decomposition ,,
Blood products, s ki n , tis sue - microbial gro\Yth.
Synthetic and semisynthetic drug s - chemical decompo sition
Effervescent tablet s - chemical decomposition
(aspirin ,. penicillin s )
Improved characteristics : Drying produces material s of spherical
shape, uniform size, free flowing and enhanced solubility. Sotne �pe­
cific areas.of importance arc:··
(1) Granule s are_dr�:d to improve thS, f1ltjdit:t__and compression

r,rocess·:, '.. . . . . · characteri sti'cs. Th�eare essential for the :Production of tablets
and evap oratio n rc d inguishabl by the re lat1'v'.�. ��nt1t1 �s �a-nc!-- :capsures..
D!)'in.g a ij �
procfucr65t� med 1s
of..liquid re��J ,from the. �d-� ev�porat1on, the (2) Yisco�.... ;J.!"'JL 5-ti£�L_ll!.�@1�.. are not free flowing. Drying
y., ln drying, ��
eithec r o ncenttated solution or su spension or wet slurr mod ifies these characteristics. Exampl es are male f;m extract,
so l id i s the product malt extract and oleoresi n.
1

-,,::=-- �
. The liquid.to be poriscd may remain : Improved handling: �'2Yfil o m....9istu.��-m�kes.J!!s_m.��.!:i¥,:IJJ�ht
crystals,
on t he surface of t he solid, as in dry i ng of salt _i�ajghLanq reduc�s t�C? bulk. Thus cost of transportation will .be less
solverit removal from a sheet
of and storage will"be efficient. If moisture is present, sizi: reductio n of
entirciy inside t he sol'id, � in . ·
drugs is difficult. Drying reduces the _moisture content.
P9lymer,
of so l vent removal
__'partly outside and partly inside, as in case THEORY OF DRYING
· · · from pharmaceutical powders.
unsat�rated . �ith t�e In a wet solid mass, �wat er may be present as bound water and
Drying is possible when the enviro�ment is .
n ent 1 s a n import ant
m unbound wat er.
water vapour. · Hence, humidity in the ' enviro
� sev:ral methods- are Bound water o i sture) is the minimum water (rt'/<?isture) held by the
det erminant for drying of \he solid s ;, Thou.
ng• tech 1� ue· (nonther�al ma ena that.exerts an equilibrium vapour pressure less than the pure
available, thermal methods and freeze dryi � .
theoretical • · ·
-
) - ar inc �ded re. " T his chapter deal s wit h the wath at the same temperatl!re .
method e l he
g. .· Unbound water moisture) is the amount df water (mois ture) he,ld by
p ri�c i ples and equipme nt emp l oyed for dryin
·the. ma ena t at exerts an equilibrium vapour pressure equal ·to that of
pure water at the.same temperature:- �- ------..�
1

382
 '' G:h-14 DRYJNG 385
384 l'I IAH.MACElJ IIC,\L ENGINITIU NG
Equilibrium moisture content in a wet mass is shown below.
Unbormd water exists largely in the voids of the solid. Thus, ill a
non·�-)'groscopic ma� all the liquid .is unbound \\'atcr. In a " ..,, Vapour pressure of wet mass -
hygroscopic matcr'ial, ihc unbound moisture is the liquid in excess of the Vapour pressure of atmosphere
--
equilibrium moisture content, corresponding to satur,it_i�rn humidity. Sub­
,- .

�--At equilibrium Amount of

stances containing bound water are often called hygroscopic suhstonc·es. water;. EMC
The distinction between bound and unbound water depends on the
material itself. These arc described below.
. Wet mass
The characteristics of air .. such
..,::,,

Hygroscopic as temperature_ 1nct humidity are

vVapour pressure maintained constant. Depending on these conditions, the solid5 may
materials
Contains of wet ·soli is absorb or lose moisture. · ··
;!!:_ er in: Bound Condition les an the
-fine capillaries water · �hen air (of constant temperat�re and humidity) is continuously
vapour' pressure · · passed ove the �olid cgn� ining moisture more th�n EMC, then
,-ce-ll and fibre walls
- ysical interaction of pure water � ?
solid los�o water continuously till EMC is reached. This phe-

I
. 3-°menon is kno �n as desorptiony-- .· ·

J
. .
.(pf When air (of constant _temperature and humidity) is COl\tinuously
,./
Vapour pressure
Non-hygr�sc.opic passed over the solid COQtaining moisture less ·than EMC, then
. Contains Condition of wet solids is
matenals Unbound sol\d adsorbs water continuously till EMC is reached. This
equal to vapour
Water in void water phen_omenon is known as sorprion.
;)>
pressure of pure
spaces, The behaviour of desorption and sorption is shown 'bel�w. ·Fro\11 the
water
above .observations it is clear that, material can be dried up\to EMC 'but
Heat must be transferred to the matcr.ial to be dried in or,der to sup ply not below it.
the latent heat required for vaporisation of the m0isturc. Water diffu.scs Moisture in the solid> EMC of solid
through the material to the surface and subsequently. evaporates into the Moisture
.,i'

air stream. Thus drying involves _both hea. t trpn sfcr and mass trarisfcr
operations simultaneously.
' .
Theory can be discussed in two heads namely equilibrium relation-
ships and rate relationships.
.
'" . Wet
mass
//Equilibrium Rcla�ionships �-
'J "s- At a gi�e� temperature'and hu�idity of air . .....
.·. .

(Air e.f....constarit tGmperaturn and lu@idit�· passed over the �ct

. ' .:.:

.
sol�. After a long exposure, equilibrium is reached . Or att111__ :11ng McasurenJcnt of EMC : The EMC of a material can be determined
equilibrium, fu9'her �xposure will not alter mo istu:e co�tent in the solid. as follows. The solid samples are placed in a series of �losed chakbers
_ .
Ac:: this stage0,·apour pressure of the wet solids 1s equal to that of th� such' as d���1!.�· Each chamber consists of· solution (de�iccant),
surrounding �tmosphcre. · Hence there is no driving forc-e foJ �1ass which maintains a fixed relative humidity in the enclosed air spaces. In
tr� er. other words, the solid samples are exposed to several humidity condi­
V F.c 'librium moisture content (EMC) : It is the amount of water tions. The exposure is continued until the material .attains, a co·n.siant
w�ight (equilibrium conditions). The difference in ,the final and initial
present in the solid whic_�_exci;ts , ,. pressure equal to the -.:ipour
. weights gives the moisture content.
pr�ssure �f t�e atmosphere surrounding it.:...
/ Ch-14 DRYING . 387

4"'rrcc mois content FMC : Free moisture content (FMC) is the

am� unt of wat,:_W.hat is free�asv} to 'evapotii.i£jrom the solid surfac�
·, G
P·l·!J\RMACEUTICAL ENGINEERIN
(%) . .
w� by _taking relative humidity
386

Equilibrium· moisture curve is dra

.
Under the conditions of satur:ition humidity (I 00% RH), the EMCis
t on y-axis (F'1gu,e 14-1 ).
on x-c1.Xis and moisture conten the minimum moisture content. Under these conditions the water must
be bound water which is minimum at that temperature. Th; rei11aining is
.,./ Bentonite unbound for which the FMC for a �1!.iven �condition can be written as:
�� mo� total water con�ent - equilibrium
·, '

'- · "
/

moisture content (EMC)·

.The distinction between free and. equilibrium moisture depends on
the dry ing conditions .

. �clati����!P� __ . .
Rate relat1onsh1ps can be studied by cons1denng a simple model,
Relative �umidity-;per cent which .m1m1c the conditions of a dryer. In this model. wet slab of
20 40 60 80 100

material of sufficiently high moisture content to be dried is placed in a

ctting material.
Figure 14-1. EMC .cUl'Ves-for tab\ _ tray whose bottom and sides are insula!ed. The air is blown over the
s the selection ef the
. n1.r EMC ·. The EMCcurv e .permitf he product. Drying
Appl1.cat. 10n
solid unJer constant drying conditions (air velocity, temperature, humicdr
e xperirnental conditi
qns to be used for drying o of the
ity and pressure arc maintained constant). The superficial water diffuses
r,e content. reac\ es the I � ve I through the surrounding stationary air film and is cai ied a\�·ay rapid!�
, be stopped whe
shoull · istu
n the .mo
d ed . J ·
ns. Over drying can be avo1 by the moving air stream. .� _ · . ·
··,
EMC under the exposed condit1o . _ ·
C val l\es var y dep end ing on a number of Periodically the slab is weighed: _The difference ,in th'e weights· of
C : EM
/( Factors:Jfe.cting' EM two su,;,·essive periods gives the loss of moisture content, i:e'., amo unt ·
factors. <l°ricd .. The moisture present i!l the solid can be expressed on a wet
:Vature of material: weight or dry weight basis. The?i"':the following calculations are made:
zero.
have an, EMC of practical)y
( 1) Nonporous insoluble Solids mass of· water in sample (kg )
·:a-• .

· · Example is talc. % Loss on drying (LOD) = · x' I 00

. · · ues ::ire
anic su b stances, the EMC val total mass of wet sample '(kg)
(2) For fibrous or collotdal org
highOand variable. '. mass of water in sample (kg)
' C values are mu ch higher and vanable. % Moisture
·· content (MC) = x I 00
1 , the EM
··

(3) For porou.s so rds . ess to , :. _mass of the dry sample (kg)
cap1•11 anes that have no acc .
The water may be held in fine vap our pre ssun:
id may r educe the ·' iri\a�p{e
�f�a;��
the surface . The dissolved sol
. :'.' · _;�: .:�!iiht' - (kgj' . ·,'. �
· · ·:
y bound.
rate = .
and water may be molecularl
Drving
. time (h) x weight of the dry solid (kg)
· Drying rate is plotted against the midpoints of the time period.
t l'Avatllre of air: . . . o.� . ,.
. , • EMCof a\1 ma_tena ls 1s zer
· 0 humiditv
f' i( \) 'F, or· 'air of zer . Similarly midpoints of the moisture cont ent values can be plotted.
. . decreases.
f increases, the EMCof solid
(2) As the temperature o :m . . . From the data obtained by th� above experiment, a graph is plotted
nt for a g1\i'en tem per a t u re and hum1d1ty of by taking FMC on x-axis and drying rate on y-axis. ·The curve., so
EMCof solids is a consta . I 0001c
ilibrium cur ves (Fi gur e 14-1) are_ continued u: p .to . o . obt�ined (Figure 14-2) is called drying rate curve. It repre7ents different
air · If the · equ
tent so o b ·
tain ed (EM C wit h saturatc,d a1r ) 1s the char:·-gcs during dr) ing as explained below.
RH the moisture con as h'ig,J 1
.
ts ture at whi ch the mat eria l can exert a vapour pressure
'
Ieast mo
water at the same temperature.
as that exerted by liquid
(
 Ch-14 or.YING 389
NEERING
0

p 1-!ARMACEUTICAL ENGI Hot air Evaporation

I

388
Constant
rate
• \ ) Rate of evaporation
Critical - rate of diffusion
period

Diffusion
�, A I t Second critical.
g I Constant (3) The time corresponding to CD represents the first falling' rate ·
/ point/
N . I rate I D ·•• period (or unsaturated surface drying). During this ·period, ·the·
:J:
C'
� period I surface water is no longer replaced at a ,rate fast ·enough to
::..< .: I First Equilibrium moisture
·t� :� I I falling maintain a continuous film on the surface .. Dry spots begin to

''
content /
I rate appear and the rate of drying begins to fall of(.. T;he point D i:. '
referred to as the second critical point. At this point, the film of
en
I
-� period
c:

I · .
I surface water is completely evaporated.
I
Dry spots Evaporation

"'' "'' �:' ·�1--r,-� .l�:�i.:

Second falling
Moisture content rate period

Figure 14-2. FMC curve. R<!te of evaporation

> rate of diffusion
:.,.... '-""=:,�· ..,.;
· z djustment'
· · za
resents the ,mt
rate period
··:r.a.·
::· .:�.::�:··.
.• - ... ·..
r .. -
. ., •,.!.,.i·&'.·7� ·
".,� ·.·�Jk'°.T
-,,,. f[., ....................
.. ,.,.,, ...
he time correspon�ing t� AB rep
solids absorb. heaat and.
_ the
.
per10d. . During this pcnod, the . s to Diffusion
. tune, the moisture begin
temperature increases. At the same ·
(4) The time �orresponding' to DE r�presents 'the.sfc;nd falling rare"
some
drying sol"d A�cr
. ";vaporate and. thus tends t?. cool the _ .
I li�g.' rat es be- period. During this period, the. rate of dryipg falls even n:.ore ·
ting and coo
time ' the tem· perature stabilises (hea· ....vet b u lb rapidly than the first faUing rate. During this period,.. the rate of
1s eq ua I to the .
come equal). This temper ature t B · .drying is dependent on the rate of diffusio� of vapour of mois�·
referred by the pot ri .
temperature ·,of the drying air and is ture to the .surface of tNet�olid. Point E is referred. to as the�
· '· .
Evaporation equilibrihlh moisture content.

! Hot afr

-ffl
At equilibrium, \ • •
Initial rate of heating
adjustment • ' . • i-''
• rate of working Second falling �· ·�¥:--; -..- ...-r-:. - - Rate of drving
,period
rate period � .. ,:;· I -Id��;;:::, &";;,;,; > "J" CX:
,..- � ."';').::.:r;.C..-':::1.:"� rate of diffusion ·
;�••. �-:,..:.!.-;:..:-...

____
Temperature Temperature �..., ...,,,,.
,T:···
� ·�� .• ..• ·-�r.,
..... !lfc.r.:•·
....• , •...--s'".v.·:�.:-:
� ,.- ·., of water vapour
decreases
increases ............. ,
t r e
,;../

tim e cor resp ond ing to BC
(2) Th e .
period. The temperature remains
constant. The moisture evaporatin
bv the wat er dif fusing from the iriterior of the solid._: • mo1sture
.,
diffusion is equal fo the rate O
content at the end of constant rate
represen�s the constdan _ a� (5,) Beyond E, the drying rate is equal to zero. Therefore, tempera­
ry1ng is
constant and rate of" ture and moisture content remain constant. Beyond, E, continued
- re placed
g f�om the sur�. ac� . drying is was�e of time and energy: ·;
!:'h e r �te of
Thc.<;tirves may have different shapes for different levels of, moisture.
f evapor. at"I on • The
� If the drying is carried above 'the level of CMC, only constant rate
(point C) is�
�. ·- ,. .

,�isture con
 Ch-14 DRYING
391
390 1'11,\ RM/\Cl:l/TIC,\ I. l'N( ilNl·TIUN< i
Con:;truction The construction "of a tray d ryer is shown in Figure .
pcno
· d oc� urs. If the drying is started for the material whose. initial 14-3. It con sists of a rectangufa r chamber whos e walls are insulated.·/
7/
. , .
moisture, content is less than CMC, then, falling r� te per iod occ ur� �- Trays are plac.ed inside the heating cham,ber. The n u mber of trays may .
vary with the s ize of the dryer. Dryers of laboratory size may contain a ·
CLASSIFICATION OF EQUIPMENT minimum of.three trays, wher� as d ryers of industry size·may contain·
The classification based on the metl�od of sol ids hand I ing is more more than 20 trays. Each tray is rectangular or sqµare and about' l .2 to.
. 2.4 metres square in area. Trays arc usually loaded from 10.0 ·to I 00.0
su itable when special attention is given to the nature of mate�·1al to fie
dried. Dryers arc classified as given in Table 14-1. millimetres deep. The distance br.tween the bottom of upper tray and
( upper) surface of the s u bstance loaded in the s ubseq uent tray ,nust be
TADLE 14-1
sifi ion of Dryers-Mechanism, 40.0 millimetres.
cs, Advantages and Disadvantages Alternately the trays can be placed in trucks on wheels, which can be.·
rolled into and out of chamber. Two such trucks can be arra11ged ·inside
Type of dn·er Examples Advantages Disadvantages dryer. Dryer is titted with a fan for circulating a.ir over the. t�y.s.
and mechanism /
\'� ro'
Electrically heated elements are provided inside· (father than 'outside) to.
Static Bed Dryer heat the air (steam also can be us ed as it is cheaper).. In the corner .of �he·...
. l'-1'�{'<
Systems in which t.lJ.crcj;s �y drycrv"Attrition is not Only a fraction chamber. direction vanes (not shown in Figure 14-3) arc p_laced to direct
no relative moven1!,;Jlt and freeze observed .o -air in the expected path.
aofong the �(lli<l particles dryer �
.,particles ,�
, ,
bcing dried. ahhough there directly c�:po:;.cd
____,,________ -
, may be bulk motion of thc
entire drv ing mass.
Moving Bed Dryer Heater
systems in which tile �m The cntire mater- �ition is
drying particlcs· arc ·'dryer .. ial is continuous- possible
�rtially separated so that ly exposed to

-
they flow ovcr each O(her heat source Air
, ,:_ ·

/'Fluidised Bed Dryer - outlet

Systems in which the solid "rluidiscd Solid-gas contact vt{trition or
particles arc partial!� bed dry c� ,s excellent. particles takes
suspended in an up_ ward uniform drying place -
moving heated g.as system
�... : . . . . 0 r.�., ' ... ·� ·-,. 1·,···
Pneumatic Dryer '
Figure 14:3, Tray dryer.
Systems in which dry inl! �pray. �licicnt ;inc)
12articles are cntraincd dryer rapid drying Working Wet soli� is loaded into trays. · Trays·· are pla�ed iri the

·7
'.
and conveyed at a high chamber. Fresh air is introduced through inlet, which passes through_,the .
velocity cas stream ...
<>1 .b..�and �eated up. 1:he hot air is c�rcul�d by means of fans at
2 to 5 metre per second. T urb ulent flow 'lowers the partial vapour
EQUIPMENT . pressu re in· the atmosphere and also reduces the thickness of the.\air
.
�AYDRYER boundary layer. The water is pi� up by air. 'As water-:evaporates
. Principle : Jn tray dryer, hot a:r is contin u o u sly circ ulated. For�ed from the surface, ih_c water aiffuses Imm the· interior af'th,e salid_by
.
,convect ,on hc::iting
, takes place to remove moisture from the solids
. ':.apilbry action. These events occur in a single pass of air. The time of
placed in trays. Simultaneou sly. the moist air ,s removed par t",::i llv• .
 ' f'I (

392 393
1'111\RMI\CEUTIC/\L ENGINEERING

contact is short and the amount of water picked up in a single pass is

small. · Therefore the discharged air to the tune of 80 to · 90% is
circulated back through fans. Only IO to 20% of fresh air is introducec.l. · Principle : In drum dryer. a heated hDllow metal drum rotates on its
_Moist air is discharged through outlet. Thus constant temperature and longitudinal axis. which is partiallv dipp<;d in the solution to be dried.,,,
.

n '\,
. unfform airfiow over the material can �e maintained for achieving- The solution is carried as a film on the surface of the dry�r and dri�dto
· . ·
uriifomiarying. . • form a layer. A suitable knifc scr.aps the dried mate!9l, while the drum
. is rotatj_ug_-
In case of'wet granules (as in tablets and capsules) drying is �o;;tin- ·
ued until the desired moisture content is obtai.ncd. /\t the end of drying,
------ - ,,.... - - ·.·,.., Y Dried film
Liquid �
trays (trucks) are pulled out of the chamber and taken to a tray dumping film ........... /,
station. --....,,./, . �
I
•discs : Stic2�.'.1�:.:i.':!s..tt-.P..1.<:stic substances,. gra111;il.r \
P �nuss or crystal­ · Spreader I . ·• ;
�e-materials, precipitates�,!nd pa�t.es can be dried in a tray dryer. Crude

r�·
rdried. -- .
:- .
. arugs, cTie'mi'cafs; PO\�ders, tablet granules or parts, of equipment arc
r
� '{< Doctor
knife
.
�dva�taocs : In tray dryer, h!l_ndling_or matcrsJ.s (loading and
u oading) c �� _b _': .d<?.��_wi�h_?ut_ l_?s::�/
. . Figure 14-4. Drum dry er. ,
Tr.ay....d.zy�r is Qpcr.ate_q batch-wi�c. Batch drying is used exten­
sively in the manufacture of pharmaceuticals for the following �uction : The construction of a drum d�yer is' shown in Figure
reaso 14-4. It consists of a horizontally mounted hollow steel drum. of 0.6 to
3 .0 metres diameter and 0.6 to 4.0 metres length, whose external . surface
,. f

a) ach batch of material can be handled as a separate entitv.

�h; ;tch sizes in 'it�e pharmaceutical industry arc relativ�ly is smoothly polished. Below the drum. feed .pan is placed in such a way
small (250 kg or less per batch) compared with the chemical that the drum dips partially into the feed. On one side of the ·drum a
industry ( I 000 kg or more per hour). spreader is placed and on the other side a doc.t?r's knife is placed to
scrap the dried material'. A storage pin (or a qmvcyor) is placed
(c) The.same ·.equip,nent i.s readily adjusted for use in drying a
connecting the knife to collect the material.
�i.9e
. v.ariety of materials.
(<!}, V�able _pr£s!.uc_ t. ��S�� be handled efficient!)'. · : w¢"king : Steam is passed inside the drum. Heat transfer coefficient
_ o�drum metal is high: Drying capacity is directly p,roportional to the
/ isadvantages : Tray dryer �q_uir!!.LJilQrc la..boullQ-. (.oad�and .uri.!oaci.
?.D surface area of the drum. Heat is transferred by 'tonduction to 'the · ·

.� ·
Hence, cost increases. The process is time consuming. �
· Vari;rnts : Tray dryer may be operated under vacuum, often with
indirect' heating. This is done in special vacuum· tray dryers for drying
vitamins and other heat-sensitive products.
, '
<\ •
� '
Tunnel dryer : In this type. trucks ar,e loaded with wet material at one
end of the tunnel. The tunnel comprised of a number of units. each of
which is electr9-statically controlled. The solids get dried and· the
· �·
product is discharged at the other end of the tunnel.
material. S imultancously drum is rotated at a rate of 1-10 revolutions
per min'ute. The liquid material present in the feed pa� a thin··
layer to the external surface of the drum· during its. rotation. The
material is completely dried du'ring. its journey in slightlyless' than one
rotation (i.e.. from one .side to anoth�r 'srdc_. of the drum): The dried
material is scrapped by the.doctor's kriifc. which then falls into a storage
bin. TJ1e time of contact of the material. with hot metal is 6 tt"15
seconc.ls only. Therefore. processing conditions sue!) as til,l\ thickncss,--
ste.arn temperature arc closcl.}1 controlled.
'f

""
 394 1'1 IARMACEUTICAL ENGINEERING
. . . s. -· _
/Uses : Drun:�- d " d
d �-�.£-�_�.:>_� 1g .../1ut1. ons, s_Iv.
umes, suspet/
�St_?��-
etc. The pro ducts clned arc milk products, starch products, Ferrous salts,
DRYIN<,
?e - n the
Ch-14

susp ensions of zinc oxide, susp�nsion of kaolin, yeast, piginents, ritalt ·• more). An inlet for hot air. is pl�cc_d in t�e ro�J of tbe cham \ � � �
\�11 1� l 1g urc 14
extracts, antibiotics, glandular extracts, insectici des, DDT, calcium and inlet carrying spray- disk atomizer 1s s�t 111 the roof (sho_
m diameter ..;10d
ba rium ca rqonates. 5). The spray disk atomizer is about 300. millimetres_
� 000 to •<;O •000 revolutions p::r minute. Bottom of
rotates at a specd of -',
�gcs : (1) In drum dryer, drying time is less, only a
/ f�w the drvcr is connected to a C)1clon e scrarator.
-
seconas. · Therefore, heat sensitive materials can be dried.
(2) Drum dryer occupies less space, as it is compact when compared.
,,.,-, to sprqy dryer.
(3) As a thin film of liquid is formed on -thdarge heating surfa<:e,
rates of heat transfer an d mass transfer are high..
�) · The prod uct obtained is complet e ly dried and is 111 the final
form.
·DI,advantages'.;..(!) Ma;ntenance cost of a d,um d,ycc ;, h;ghec than
/
rli :���.:�:�'"'°'' ace csscn,;aJ to contrnl feed cate, film th;ck­
/' ness, speed of rotation an.d temperature.
(3) it is not suitable for solutions of salts with less sol�bility. ·
Variants: A vacuum drum dryer encloses both drum and feed line
iri' Figure 14-5. Spray dryer.
a vacuum chamber to facilitate drying of heat sensitive materials.·
It is
es.
suitable for drying of drugs susceptible to o>.idation and to V/orking : Drying of the 1�1pterial in spra:r dryer involves 3 stag
. . I

recover
solvents. ( i) Atomization of the liquid.
In a large scale, instead of one drum, two drums are set in
parallel, (2) Drying of the liquid droplets.
rotating in opposite directions with a common feed inlet. The feed can be (3) Recov ery of th e dried product.
introduced on to the DRUM either by spraying it on the top .or d is
by Atomi=aiion ,of the liquid to form liquid �roplets : �he fc�
introducing from the b suitable
introduced through the atomizer either by gravity or by ,usmg
ies of the final produc t �cpen_d
SPR'AY DRYER pump to form ftnc droplets. The propc� , . of ato1� 1zer ts
on the droplet tonn. hence . the selcct1o · o the _typ
Principle ; In spray dryer, the. fluid to be dried is atomized into fine important. Atomizer of any type : pneumat f atomizer. pressure nozzle
1.:

droplets, �hich are thrown radially into a moving stream of hot gas, and spinning disc atomizer'may be used. · ' ·· •
The temperature of the droplets is immediately increased and fine drop­ that the d_ r oplcts sl1oul, d be
Th� rate of feed is adjuste d in such a way
lets get dried instantaneously in the form of spherical particles. This of th drym� chamb er. At
coinpleti:ly dried before reachin g the walls
process completes in a few seconds before the droplets reach the wall or be over hc�ted .
the same time. the product should not
e

the dryer. _ .
D,:rin.� .of the liquid drople ts : ·Fine dr� plcts ar� drie. <l in th1t �r) _il)g
C�:mstruction: The construction of a spray dry er is shown in Figure
14-5. It consists of a large 'cylindrical drying chamber with a short -chamber by supplyi1.1g hot air through the 111Icy , . . ,
conical bottom, made up of stainless steel (diameter of the· drying . The surface of the liqui d drop is dried immcdiat_cly �o form a· �ough
chamber 'ranges between 2.5 to 9.0 metres and height is 25.0 metres or shell. further, the liquid inside must escape by d 1ffus11�g throu�h the
shell at a ,particular rate. At the same time. heat transfer from outsi de to
 396 Pl IARMACEUTICAL ENGINEERING

Ch-14 DRYING
397
inside takes place at arnte greater than liquid dif usion rate. As a result,
f

heat inside mounts up which allows the liquid to evaporate at a faster
rate. This tendency of a liquid leads to rise in the internal pressure,
which causes the droplets to swell. The shell's thickness decreases
where as permeability for vapour increases. If the shell is neither elastic
nor permeable, it ruptures and the internal pressure escapes.
The temperature of air is adjusted in such a way that the droplets
should be completely dried before reaching the walls of the drying
chamber. At the same time, the product should not be over heated.
Recovery of lhe dried producl : Ccntrifugal force of atomizer drives
the dr9plcts to follow helical path Particles arc dried during their journey
and finally fall at the conic l bottom.
All these processes are completed in a few seconds. Pa11icle size of
the final product ranges from 2 to 500 mm. Particle size depends· on
solid content in the feed, liquid viscosity, feed rate and disc speed.
. Spray dryers of maximum size have got evaporating capacity up to
/ , nd diameter of 9.0 metres) and expensive..
2000 kg p�r hour.
(3) By using suitable atomizer, the product ofuniform and cont:olla­
ble size can be obtained. Free flowing product of u111form
spheres is formed which is very convenient for tabletting process.
(4) Fine droplets forme� provide large surface area for heat and
mass transfer. Producfshows excellent solubility. ' · ··
C5'5 Either the solution or suspension or thin paste can be dried. in
one step to get the fin�! product ready for package.
�it is suitable for the drying of sterile products.
¢Gonstituted product appears more or less similar to the fresh
material.
_ dispe'.sed phase
(8) Globules of an emulsion can be dried with the _
inside and layer ofthe continuous phase outside. On reconstitu-
tion, the e��l;i�ill be formed.
i�ad ntagcs �Spray dryer is ve� b�y (height of 25:0 metres
;;;:
Such a huge equipment is not always easY. to �rate.
•' / I
I

c Spray dryers are used compulsorily, if:

/�� 7-:°' .cl[' The thermal efficiency is low, as much heat is lost 111 the
� �e roduct is a better form th�n that obtained by any oiher ' discharged gases.
ryer.
Variants : (I) Spra:t dryer can be constructed in such a way as to suit.
The quantity of the material to be dried is large.
sterile products.
(3) The product is thermolabile, hygrosc9pic,or undergoes chen:iical
(2) It can be operated under closed conditions to recover solvents.
decomposition.
(3) It can be operated under oxygen free environment.
A· fev, products that are dried using spray dryer are: (4) It can be constructed in such a way _that the flow of liquid and
acacia " chloramphenicol gelatin plasma gas may be co-current, count�r curre'nt or a .co';1bination of both
adrenaline hcxaminc ·
succinate serum in the same unit. . · ' · ' , ,· ·: =""
bacitracin citric acid hormones soaps congeali ng: '
barium sulphate coffee extract lactose sodium phos- (5), The same eqipment can be used for spray .
. sulation co ting) of s li-<1 an. d q�id particle ;.
blood detergents methyl cellulose phate J 6) It useful for enca� r � _ H �
_ �
borax dextran milk starch .
b9ric acid extracts pancreatin sulphur" . �UIDIISED BED DRYER (FBD) . . :
cnlcium sulphnte ferr s sulphate penicillin vaccines � . Principle : In fluidised bed dryer, hot air (gas) is passed at high
pepsin vitamins
' (;

fru t juices · pressure througl) a perforateiil,·w�ottom 0f the contair.er �ontaining gran­

yeast
dv· ntagcs : 1.Spray drying is a continuous. process and drying is
/_ very rapid. Drying completes within 3 to 30 seconds.
Labour costs are low as it combines the function of an evapora-
tor, a crystllizer. a dryer, a size reduction unit and a classifier.
ules :o be dri�d. The granules are lifted from the bott?m and s4spende9
in the stream of air. · This condition is called fluidized slat_e. 'fhe hot
gas is surroundirlg ev'e ry granule to completely dry th�m. Thus, \nateri­
;ls or granules are uniformly pried.
.
Co�struction : Two types of bed dryers are available, vertical fluid
. \

bed dryer and horizontal fluid bed dryer.

 398 PHARMACEUTICAL ENGINEERING

The construction of a vertical fluidised bed d ryer is shown in Figure h·l•I UH.YING 399
. .
J 4-6. The dryer is made up of stainless steel or plastic.· A detachable jl11idisccl stole. The gas surro�nds every gra�ulc to completely'dry t�em:
bo,;I is placed at the bottom of the dryer, which is used for charging agd The air leaves the dryer by passing through the bag filter. The entramed
discharging. The bowl has a .perforated bottom with a wire mesh particles remain adhered to tht"foside surface of the bags. Periodically
support for placing materials to be dried. A fa !1 is mounted in the upper .
the bags arc Shaken tO remOVe the entrained particles.. . ,
p

part for circulating hot air. Fresh air inlet, pr�fiiter and heat exchanger ' f I .
Intense mixing between granules and hot gas proviqes uni' orm con­
0

are connected serially to heat the air to the re'\uired temperatures. The
temperature of hot air and exit air are monitored. Bag filters are placed
above the drying bowl for the recovery of fines.
ditions of temperature, composition and particle size distribution.· Drying .
· is achieved at constant rate and falling rate period _is very· short. · Any '
.
attempt to. increase the air velocit)I may result in eritrainr1_ent. : .. , •.

i t
Inlet Outlet The residence time for drying is about 40 minutes:· The material is
Fan left for some time in the d ryer for �eaching ambient temperature. The '
bowl is taken out for discharging. The end product is free flowing.
_/Uses : Fluidised bed dryer is popularly used for: diying of )ranules in
_ _
/the production of tablets. Flu1d1scd bed dryer can be used for three
Recirculation . operations such as mixing, granulation and d rying. It is .modified for ..
control I ,-, . · ,,-, ..,.....,
coatm
. o f.. granu es.
ilvantag.cs �Fluidi��d bed ·dryer requires less time to complete '
Air
heaters drying, i.e., 20 to 4.0 minutes compared to 24 hours of tray dryer.
Handling time is also short. It is 15 times faster than the tray
Detachable dry er.
bowl
Wl't is available in different sizes with the drying capacity ranging
.+".f--+- Fluidised from. 5 to 200 kg per hour.
solids
(3) The drying containers are mobile, making handling simple and
reducing labour costs.
W'fhe thermal efficiency is 2 to. 6 times than tray d ryer.
Figure 14-6. Fluidised bed dryer. �t is also used for mixing the ingredient� · 8:nd its' · mixing effi-
Working : The wet granules to be dri_ed are placed in the detachable
ciency is also high.
bowl. The bowl is pushed into the dryer. Fresh air is allowed to pass (6) Hot spots are not observed in the dryer, be�ause of its excellent
through a prefilter, which subsequently gets heated by passing through a mixing and drying capacities.
heat exchanger. The hot air flows through the bottom of the bowl. . (7) Higher drying tempuaturcs can be used that are not .�· ossiblc in .
Simultan·eously fan is allowed to rotate. The air velocity is gradually tray dryer.and. truck dryer. . ·
increased. . ,.',:
(8) It facilitates the drying of thermolabile substances, since. the
When the 't'elocity of the air is greater tha'n settling velocity of contact time for drying is short.. .'. ·.
granuJes; the granules remain partially suspended· in · the gas stream. (9) It can be used either as .batch type. or continuous ,fype.
After some time, a point of pressure is reached at which frictional drag .
( I 0) It has a high output from a smaJl fl
. oo�, space.
on the pa11icles 'is 0equal to the force of gravity. The granules rise in the
container because of high velocity !!as (1.5 to 7.5 metres per minute) and ( 11) The free movement of individu'al particles eliminates the ris �of
• later fall pack .in a random boiling motion. This condition is said to be soluble material migrating as may occur in static beds .
v
'
 400 !'I IA RMACEliTICAL ENGINI.TRING
• Ch,14 DRYl!'-G 401
/J>isadvantagcs : Many org':�nic powders develop �lectrostatic charges
�µring drying. To avoid this, efficient electrical earthing of the dryer is \Vorking : The material to be dried is spread on trays. Th\� trtys are
e?sential. The turbulence of the fluidised state of granules may cause placed on thr.: shMvcs. Prcssurr.: is Jccn.:ased up to 30 to 60 kilopascals
attrition of some material� resulting in the production of fines. But by mr.:ans of a vacuum pump. Door is closed firmly. Steam or hot air is
using a suitable binding agent this problen1 can be solved. Fine particles supplied into the hollow space of jacket and shelves.,, Hqt transfer by
may becorne entrained and must be collected by bag filters. conduction takes place. At. this vacuum, evaporat\on, of water'
from the material takes place at 25-30° C, '.ion account of lowering
Variants: Plug flow dryer: It is a rect�ngular fluid bed dryer having
.different compartments for fluidisation. The material is made to 111ove of boiling point. Water vapour passes-into the condenser where condcn-.
· �--"
'from inlet through different compartments to outlet. Different drying sation takes place.
conditions can be maintained in the compartments. Often the last At tl{e _end of the drying, vacuum line is disconnected.. The material
. • .'
. .. ."·'· . .. .)' .. .
is collectcd from the trays. ·
,; •; .

compartment is fluidised with cold gas to c�ol the solids before di�­ r·
charge:
rscs : Vacuum dryer can be used 'for drying of the following:
(� Heat sensitive materials. which undergo decomposition.
·VACUUM DRYE�
Principle : In vacuum dryer, material is dried by the application of
Gtf'
Dusty and hygroscopit 1\':1atcrials.
1

•vacuum. When vacuum is created, the pressure is lowered so that water
boi Is at a lower temperature. Hence, water evaporates faster. The heat
transfer becomes effi�ient, i.e., rate of drying enhances su,bstantially.
Connection to
--.. vacuum pump
receiver
. Figure 14-7. Vacuum dryer.
Construction : The construction . of a vacul!m dryer is shown in
Figure 14-7. It is made of a cast iron'1heavy-jacketed vessel. It is so
strong that it can withstand. high vacuum within the oven and steam ·
pressure in the jacket. The enclosed space (approximately 1.5 metre .
cube) is divided into a number of portions by means of 20 hollow
shelves, which arc part of the jacket. These shelves provide larger
surface area (about 45 to 50 metre square) for conduction of heat. Over
the shelves, metal trays are placed for keeping the material. The oven
door can be locked tightly to give an air tight seal. The . oven 1s
connected to a vacuum pump by·placing condenser in between.
\)'JDrugs �;ontaining toxic solvents. These can be separated into··
closcd containers.
(4) Feed containing valuable solvents. These are recovered by
condensation. •
f.(l' Dr_ugs which arc required. as porous end products.
¢}; Friable dry extracts.
Advantages : .{.,(y Vacuum dry er provides large surface area for heat
/ transfer.
�Handling of the material, trays and equip�nent is easy.
Q/'11 i.s easy for switching over to the next materi�ls.
� Hot water of desired 'temperatures can be supplied.
(5) Electrically heated hollow ·shelves can be used.
Disadvantages : (!) lh vacuum dryer, he�ransfcr coefficients are
/ low. ; . ·
(2) It has a limite�ctpacity and used for batch process.
(3) It is more expensive than tray dryer. Labour and running costs
are· also high. .r
(4) Sometimes, there, is a danger;.( over heating as the material is in
contact with steam heated surface for longer period.
FREEZE DRYER
Freeze drying is also known as lyophili::ation, i.e.. system IS made
solvent loving for removing the same.
402 PHARMACEUTICAL ENGINEERING
�nciple : In freeze drying, water is removed from the frozen state
by sublimation, i.e., direct change of water from solid into vapour
without conversion to a liquid phase. Solid-liquid-vapour equil'ibri�m
phase diagram of water is useful to decide the experimental conditions.
Th,� drying is achieved by subjecting the material to temperature anT
pressures below the .trig_te poillt,(in practice, below eutectic tempernture
is essential). Under these conditions, any heat transferred is used" as
latent heat and ice sublimes directly into vapour state. The water vapour
is removed from the system by condensation i"i1 a cold trap m·aintaincd at
a temperature lower than the frozen mattrial. //
Construction : The construction of a freeze dryer is shown in F,igurc
14-8. It consists of:
(I) Drying chamber in which trays are loaded.
(2) Heat supply in the form of radiation source, heating coils.
(3) Vapour condensing or adsorption system.
(4) Vacuum pump or steam ejector or both.
Heat transfer
To vacuum
Frozei. fluid manifold
Isolation
valv�
- Refrigerant
Heated
shelves Condenser
Chamber
' Figure 14-8. Schematic diagram of freeze Jryer.
The :chamber for vacuum drying is generally designed for batch
operation. It consjsts of shelves for keeping the material. The dist.1ncc
between subliming surface and condenser must be less ,than the mean
path of molecules. This increases the rate of drying. Th� condenser
consists of a relatively large surface cooled by solid cad,on dioxjdc
slurred with acetone or ethanol. The temperature of the condenser must
be much.lower than the evaporated surface of frozen substance. In order
to maintain this condition. the condenser surfac.e is deaned repeatedly.
Ch-14 DRYING Jr\ / o 403
Working : The working of freeze dryer consists of the following
steps.
( 1) Preparation and pretreatment
�2) Prefr'!ezing for solidifying water
,..B) Primary drying (sublimation of ice under vacuum)
�ccondary drying (removal of'iesidual
· vacuum) , ·''
moisture
·
_
· · ·
under high•
· ..
(5). Packing
Preparation and pretreatment : The. volume o( solut.ion · introduced
"into the container is limited by its' capacitf':' Satisfactory freeze drying
beyond a .certain limit of depth· of liqi:iid is. not: possiole.7 Therefore ·; .
pretreatment is essential. The solution is pre-concentrated under normal ·.
vacuum tray drying. This reduces the actual drying by 8 to IO times. . ·
The final product becomes more porous. Liquid or. solid desiccants are
also used for this purpose.
Prefree:ing to solidify water: Vials,,ari1pou:\�s or bottles in which the
aqueous solut1on 1s packed a� frozen in cold _ shelves (about -50°,i;).
During this stage, cabinet is maintained at. low temperature and atmos- .
pheric p;essure. The normal,, cooling rat�. is about J to 3 Kel�in p�� .,
minute so that large ice crysta-ls with relatively larg� holes are formed on·
sublimation of ice . This is also resp�nsible for giving a porous product.
· £·i111arydryi11g (sublimation of ice under 'vacuum) : In this step, th�
material to be dried is spreas , 1:}S much large surface as possible for
subli1m,tion._ H,c· temperature a11d pressure .should be below, the triple
point of water. i.e., 0.0098 ° C and 0.533 kilopasc�ls, ' (4.58 mmHg)
·· for
the sublimation, when �vater alone is present.
When a solution of solid is dried, the depression of fretzing point of
water occurs. Hence, it is essential that the temperature be brought
below the eutectic point. The pressure _.and temper;:1ture at 'which the
frozen solid vaporises without conversion to a liquid [� referred to� the
eutectic point. Depending on the drug substance:dissolved in water· the
eutectic point is determined. The usual range is from -10 ° C to 3.0�C.
The condition of 1 to 8 K belo:v, eutectic point is �ufficient.. . .
Vacuum is applied to the tune of about 3 mmHg (0.4 kilopascals) on
:,)
the frozen sample. The temperature
, :
is linearly increased to about
, '
30 °' C
I '
i:n a span of 2 hours.
Heat (about 2900_ kilojou.les per kg) is supplied which transfer� as
latent heat and ice sublimes directly into vapour state. The heat'coritrols
the movements of ice layer inwards. It has to be controlleci in such a
 ..
• 1

40 5
404 1'111\RMACEUJlrl\L ENGINEERING Ch-l·l ·lJl,YI�</'

manner so as to get highest possible water vapour at ice surface without (7) Material can be dried in its final container such as single dose
melting t�c material. As. soon as vapour molecules �re forme'd, these are and multiple dose vials.
rernovecj: The overall driving force is -the temperature difference (also �terility can be m:iinta,ined.
vapour pressure difference) between evaporating
. :
surface and condenser.
. (lJ) The linal product can be stored ut ambient temperature, if well
As the drying proceeds, t. hickness of .the frozen layer decreases and seakJ by providing inert atmosphere.
the thickness of partially dried solids increases. Primary drying stag_e Disad,antagcs : (V"('Thc product is ;ronc to oxidation_, due to high
. remove:, easily removable moisture. During 'this stage, about _ 98% to / porosity and large surface area. Therefore� the product should
99% water is removed. Still traces of moisture
__.-.... . is., present in the sample.
. . be packed in vacuum or us111g inert gas or 111 a container
· Secondary drying (Removal of residual moisture under high vacuum) impervious to gases.

-
.
During this stage, traces of moisture is removed. The temperature of · f1) Equipment and runni.ng costs arc high.
.
the solid is raised to as high as(50t� 60°.l:., but vacuum is lowered below v1' It is diflicult to adopt the .method for solutions containing non­
that is used in pfimary drying (50 _mm_lig)_ . Th� rate of drying is very aqueous solvents.
low and it takes about 10 to 20 hours.
("1" The period of drying is hish (rarely less than IO hours). Time
Packing : After vacuum is rep·l�ccd by inert gas, the bottles and vials ca1in0Tt1e shortened.
are closed.
scs : Freeze dryer is most commonly used in the· pro .ductio.n of QUtSTION BANK
A
do;age forms, such as inje�tions, solutions and sus'pensions. It is� U\ed Each qucsticin carries 2 marks
for drying of a number of products. I. l)i:;ti11guish bet\\'el'll t.lryi11g andevaporation.
(I) Blood plasma and its fractionated pro9ucts. · , (ii,c suit:1blc dryers.
(2) Bacterial and vira;I cultures. ( i} (jr;111ular free !lowing solids
I ii) Wet bricks before sending to kilns
(3) Human tissue (arteries and corneal tissue). (iii) Sticky pastes.
(4) Antibiotics and plant extracts. (i,) hHid products like llorlicks.
(5) Steroids, vitamins and enzymes. _,. Dcli11e critiGd moisture content :ind equilibrium moistur� content.
Sev�·ral o.ther products such as f�od items (prawns, mushrooms, meat ·4. [)-:fine huu11ll moisture and free moisture content.
and poultry prod1,1cts), coffee and tea concentrates and citrus fruit juices 5. Mrntio11 th,� fo..:tnrs afTceting constant drying rate.
are dried. Ci. CLissil y dryci-s giving suitable examples.
°

/Advantages : The entire operation is carried out well below the
Areezing point. This offers several advantages.
�Thermolabile mate�ials (heat sensitive materials) can be dried.
(2) The product retains its bulk volume. It is porous 'arid uniform".
1"he reconstitution of the material is easy.
Q/' Denaturation does not o.ccur.
� Migration of salts and ether solut<;s does not take plafe.
d Loss of volatile material is less.
(6) Moisture level can be kept as low as possible without dccompo
sition.
7. List the critical eondit_ions for drying or various substances.
8. Dcline drying. Give its importance in the formulation of dosage forms.
C). E:-;pl:iin how :igitator dryers arc useful to d ry:,rasty and sludgy mat�;.ials.
I 0. l lnw do yuu obt:iin the rate or drying curve for a given llrying oper:ition?
Gi,·e its applications.
Each qi;cstion carries S marks
.
I. Recommend a suitable dryer for drying the following substances ,rnd
substantialc your ans\l'i.;r with at least two n:asons.
( !\) Li,·er c:-;tracts
!H) C,ranular solids
( C) l':1sl)'. m:1tcrials ,; "-.:

- -�
406 l'I IARMACTliTICAL ENQINEERING

(D) Granules of heat sensitive drugs

(E) Viwmin 13 comrle:-. granules
(F) Colloidal soluiion
2. Describe the drying rate curve for a nonporous granular solid.
3. Describe the principle \\'ith the help or :1 labeled diagram of nuidised bed
dryer.
4. List the ph :irmaccutical applicatio�s of freeze dry ing process . Give salient
features of the process.
•
I
5. Describe the construction and working,of a nuidizcd bed dryer.
6 .. Explain the principle of spray drying with suitable labeled diagrnm.
7. Describe the drying rate curve. Explair: its applications.
8. Explain the principle and working of drum dryer.
9. Compare spray drying with drying in a vacuum shell dryer.
10. Explain the factors to be considert:d in the selection of a suitable dr):er.
I !., !·\plain th<.: operation and applications of fluidised h..:d· dryer.
12. Describe the function of drum dryer and its uses.
13. Describe the"ratc of drying curve for a crude fibrous drug.
14. Explain the principle of freeze drying. What a;c its applications in
ph�rmacy?
15. Compare the operations of spray dryer and tray dryer.
16. Describe the concept of spray dryer. What are its advantages? Compare
"'
the spray drying with other methods of drying.
·C
Each question carries JO marks
l. Explain the construction, operational details of freeze dryer. Describe its
applications in pharmacy.
2. Describe the concept of spray drying. Describe the speci fie advantages of
spray dried product over drum dried·
material..· /\!so list the pharmaceutical
applications.
3. )!ow do you classify dryers? Describe in detail the constant rate and
f�lling rate periods. /\dd a note on critical mo\sturc content.
4. for drying of milk, we can use either drum dryers or spray dryers. Which
dryer will y�u prefer and why? Discuss drum dryers in detail.
5. Discuss the· construction, w'brking. advantages and disadvantages of spray,
dryer.
(>. Explain the theory behind drying and rate of drying with suitable graphs .
I
 15

Hun1idification and Dehumidification

Humidity Charts and its Utility

Humidification
Dehumidification
Refrigeration
Air Conditioning

f/11midificutiu11 is a unit operation, which involves the transfer of liquid

water into water vapour. l
Though the definition describes the transfer of liquid into vapour, the
reverse process is also possi�le. The process in which the moisture
(humidity) is decreased (transfer of vapouryto liquid state) in the air is
known as dehumidification.
These transfer processes depend on temperature and humidity tltat are
already present in the air. Therefore, it is an equilibrium process. In
humidification, the dry air 'is p::issed ova a liquid/so that liquid evapo­
0

rates into the gas stream. ln case of d rying of \\'Ct solids, the reduction
of the moisture content of the solids is the main 'aim. The humidifica­
tiorJ of the air stream also occurs, which is a secondary effect. In
dchumidific:itio.n, liquid vap1;)\:f from the air is removed by condensation
as in the disli'llation process. Air conditioning and drying
.
also involve
.o
humidification and dehumidification operations.
In the normal e��ironmental conditio�s. the air has a certain humid­
ity. Different seasons, day and night timings also exhibit variations in
the hui11idity and temperature. Such variations influence the characteris:
tics of raw materials, finished products ad processing conditions ..
The behaviour of solids in the presence of moisture (when these are
present in tht.: ambient conditions) is of ,.co.rsiderable importance in
pharmacy. Based on their reactions, substance arc classified as:
(a) Hygroscopic substances have the natur�l dency of absorbing
moisture or water. Examples are vegetable ugs such as digi-
,
407

408 l'I·l/\RM/\CEUTIC t\L ENGINEERING
talis leaves and chemicals such as sodium sulphate. Liquids
such as 'glycerin, absolute alcohol and concentrated sulphuric
acid are also hygroscopic.
(b) Deliquescent substances have the natural tendency to absorb
)Yater and liquefy. Examples arc calciurp chloride, potassium
I carbonate etc,
(/) E.f]lorescent f11bstances have the natural tendency to loose water.
Examples arc borax, caffeine, quinidine sulphate etc.
Applications
· Preservation of pharmaceuticals : The effect of humidity on the
materials is as follows.
'(I) The substances absorb moisture and undergo chemical degrada­
tion .such as hydrolysis and oxidation, when they are exposed to
excessive humidity.
(2) Physical stability of drugs and dosage forms can be affected.
(.'h-15 lllJI\IIDIFIC/\TI�· 1'1 /\ND DEIIUMIDifICATION 409
C�111pressio11 of tablets : In the granulation section, air conditionir'.P
if necessary the conditions are 45% RH and 22°C. In th;
is optional.
tablctting section. the conditions arc less than 20 °,'o RH and 22°c.
Manufocture of soft gelatin capsules: The temperature is usually in
the range or ?.0 ° C to 22 ° C and the humidity is c9ntrollcd to a maximum
or 40% RI f :11 the processing areas and bet�veel 20 and 30% RH in the
drying areas.
The comiJosition and prorerties of mixture of air and water vapour arc
es�cntial to maintain the desired environmental conditi}ins. The thermal
properties of such a mixture are also important. The discussion in this
chapter is devoted to air-water syste;m: however, the· principles can be
a13plied to liquid gases also.
Definitions
The b·asic definitions of different terms involved arc discussed
.
111
order to appreciate the ti1cory, practice. handling of equipment etc.
'

·For example, gelatin capsules absorb moisture and become ·soft , Humidity (H) : It is also known as humidity ratio. It is mathemati­
and sticky. Suppositories and creams become liquids. cally exrressed under any given set 'of conditions as:

(3) Low humidity has adverse effects. For exam�le, hard gelatin mass of vapour present in the air (ko)
f-l11miclit1- 1 H = ---· ______________________________________________________________________________________________________________
. :::- - (I)
capsules loose water and become dry and brittle.
•
·if
mass of d ry air (kg)
Therefore. controlled humidity should be maintained. .. ..,,
Normally, the amount of vapoL!r is measured in terms of pressure. but
Evaluation of dosage forms : Environmental test chambers are not in 'm:-;ght terms. · Let the partial pressure of \�ater vapour in the
.
designed to carry out stability and shelf life· testing of drugs. The test . samp!e .or' air in que�tion be p.,, kilopascals. Then humidity in equation
chambers offer reproducible temp�rature and humidity conditions. Cli­ (I) may be expressed as:
matic conditioning is also required for herbal research, pesticide research partial''vapour pressure pA
and zoology. of water in air
Humidity, H = ----c------- - --­ (2)
Processing conditions in unit operations :. In case of normal drying partial vapour pressure
of dry'a1r
and freeze drying, experimental conditions are chosen based on humidity
consideration. Since molecular weights of water and air are 18 and 29, respectively,
then humidity at the tempcraiure and pressure can also be written as:
Maintenance of animals and equipment : According to the Drugs
and Cosmetics Act and Rules, in many cases the anirn.1! house should be lvl.4p;1
H=----­
l8pa
air-conditioned. Sophisticated electronic (analytical) equipment are placed (3)
Mn(l - p_.J 29 (1 - p,i)
. and the work is carried in air-conditioned rooms.
where J\.(1 = molecular weight of gas or vapour (w�ter)
Fabrication of environmental condi_tioners : The principles have Mn ""' molecular weight of air
been applied for the construction of equipment such as dehumidifiers. air
conditioners and refrigerators._ Some manufacturing areas wl1ere humid­ Humidity at saturatcdgas (air) (//_.) : At a giveri te' mperature and
ity is controlled are given below. pressure, i r the gas in vapo:.ir (air) is in equilibrium with the_ Jiqu_id gas,
 410 l'l lARMACEUTJCAL ENG_JNEL:RJNG

then that gas is said to be saturated. If Hs is the saturated humidity and Ch-15 IIUMIDIFICATION AND DEllllMIDll'ICATION 411
PA is the vapour pressure of the liquid, then,
' . pew point : It is the temperature to which a mixture of afr�water
I
'

.M.,1P,1 vapour must be cooled (at constant humidity) to become saturated (i.e.•
Hs =---------------------------------- (4) to be in equilibriumwith liquid at,f;c dew point).
MJJ(I - P11)
Percent humidity (H,.i ) Percentage of hL1midity may be expressed. Dry bulb temperature : It is the temperature of moist air when it is
at certain temperature and pressure. as: measured at rest by any iristrument. which is not affected by the·mois­
tu�e content of air or by radiation.
actual humidity (1-1)
Percent humidity (H,i) = ---------------------------------------------------
_ _ _ x_ JOO (5) Wet bulb temperature-Theory : \Vet b°L!lb temperature is the dy­
saturation 1-iumidity (1--ls)
n�mic equilibrium temperature attained by a water surface when exposed.
At humidities other than O and I 00 percent, the percent humidity 1s to air urder adiabatic conditions.
less than relative humidity. Consider a case in which the air is unsaturated at a given temperature
Relative humidity (HR) : -Relative humidity is expressed as a per­ and humidity. Such a stream of air is passed over a wet surface under
centage. !t is defined mathematically at a temperature as: adiabatic conditions. i.e., no heat is received frorQ ot giver\ to ihe
• -
surr�undings during the operation.
actual partial pressure of water
vapour in the air-water mixture (p) The initial iemperature of the.wet surface is approximately that of the
Relative humidity, Hu = --------------------------------------------------------------------------- >: J 00 (6) air. A partial pressure difference. (driving force) is set up between air
c' partial pressure of water
vapour at saturation (ps) and wetted surface. The \Vater tends to evaporate from the surface and
Humid volume (V) : It is the volume occupied by a unit mass of dry
ti ·�
inl:reases the· humidity of the �ir. As a result, the temperature of the
gas aiid its associated vapour surface decreases and sensible heat will be transferred from the air to
wetll:d surface. Ullima�ely a steady state will _be reached at which the
_ Humid heat : It is the heat required to raise unit mass of dry gas and loss of heat due to the heat of evaporation is e:-:actly balanced by the
its associated vapour through one unit difference in temperature at h�at passing from the air into the water as sc:nsih!c heal.,_ Under these
constant pressure. conditions, the tempei-ature of water remains constant. This temperature
0

is called wet bulb temperature.

Mathematically it is expressed as:
If tho initial temperature of the wetted surface is less than wet bulb
s =Ca + f!Cw (7) temperature. it will rise to the wet bulb temperature. Since heat transfer
where s _= humid heat, kJ/kg·K and mass transfer are observed in the above process,. their coefficients
arc important and are effected by many factors. The wet_ bulb tempera-
0

Ca = specific heat capacity of gases kJ/kg·K

C11 • = specific heat capacity of vapour, kJ/kg·K ture depends upon the temperature and humidity of air.· . _
H= humidity
-
For air-water system HUMIDITY CHARTS AND ITS UTILITY
Humid heat = 1.00 + 1.9 H kJ/kg-K Humidity Charts
For- engineering calculations. the properties of mixture of air and
Saturated volume : It is humid volume of saturated vapour. water vapour are necessary. Humidity charts or psychomelric charts arc
Enthalpy : Enthalpy of air-water vapour is the heat content of I kg helpful for this purpose. Three types of plots are shown in Figure 15-1.
of dry air and its associated moisture (water vapour) expressed as _ Humidity vs. temperature : In this chart. h,umidity (expressed a� kg
kilojoules.per kg of dr); ai1·- of water per kg of dry air) is plotted on y-axis and temperature (in °C) is
plotted on x-axis at atmospheric pressure.· The plots a�e curved and ea�h
represents a definite humidity value. The following informat'ion may be
412 l'I IARMACl:U.TICAL ENGINEEJUNG
obtained from '·'·
the . chart. Ch-1:i JIUMIOIFICATION AND DEl!UMIDif·'ICAT
ION ' 413
. (a) An� ppi'nt 0;1 the chart represents the temperature and humid Humid heat vs. Humidity : This line is plotted by takin
ity g humidity
of the sample of air. on the right-hand edge (y-axis) and humid heat (kilo
joules per kg·Kelvin)
(b) The curved line marked 100% gives the humidity of saturated along the top of the chart (x-axis). These lines
arc useful for designing
air at various temperatures. . the air conditioners.
Specific ·volume vs. temperature : The line
for specific vol·ume of
dry air (and fo.r the saturated volume) is plotted
with temperature on x
axis and metre cube per kg qry' air along the left
edge of chart on y axis.
The humid v9lume of a sample of air at
a given temperature and
humidity can be found by linear interpolation
to the humidity-tempera­
ture curve.
Adiabatic �ooling lines : The groups of lines
, which are right side of
the saturation curve, are the adiabatic cooling
curves. These curves
serve two very useful purposes. Firstly, they
can be used to determine
humidity. from the knowledge of wet-bulb
and d ry-bulb temperatures.
Secondly. these curves show the changes
in humidity during drying
under adiabatic conditions.
lJse of Humidity Chart
Humidity chart is a source of.data on a defi
nite air-wat�r mixture. A
�ortion of the chart is shown in Figure
15-2. Assume that a given
stream of unsaturated air is having a temperatu
re, IJ· It can be repre­
sented by point A. By moving vertically dow
nwards, the axis gives the
temperature, t 1. which is d ry-bulb temperat
ure. Point A is used to
illustrate the usefulness of chart. The follo
wing type s of data can be
obtained from the chart .

Humidity (Kg/k5)

.
1· Figure 15-1.. Humidity chart, air-water at I .atmosphere.
(c) 'To the left of the saturation curve ( I 00% RH), mixtures of air'
· and water vapour can not exist.
(d) Curved lines below the saturated air curve (I 00% RH) represent
various percents of humidity, narndy 60%, 40% etc.
Temperature; •c
Figure 15-2. Use· of humidity char
t.
 Pl IAIUv1i\CElJTICi\l. ENGINEEIUNG.

.)1) llumidity: from point A moving horizontally t<;,wards humidity

. axis gives an intercept point 13 on axis, which is the hti'midity of
Ch-15 11 \JMIDIFICi\TION AND DEIIUMIDlr:ICi\TION 415
the sample. In adiabatic humidification, the air is in con'tact with the liquid at
(2) Dew point : From point A moving horizontally towards left to constant temperature. The J1Umidity at the interface (Hi) must be greater
. the l 00% line gives an intersection point C. Moving vertically than humidity (H,.) of the gas, so that the air gets .humidified.·. Since
. from C downwards to temperature axis gives an intercept point water is vaporised, the latent heat is transferred from the liquid to gas.·
D, which is the dew. point temperature, t2. .The gas temperature (ty) must be higher than the interface temperature
(/;) in order that sensible heat may flow to the interface. (Heating or
(3) Adiabatic-saturation tcnipcraturc : From point A moving along cooling without the addition or subtraction of moisture content is called
the adiabatic cooling line towards the I 00% jine gives an inter­
sensible heating or cooling).
·seetion point E. _Moving vertically froi'n point E downwards to
temperature axis gives an intercept point F. which is the adi­
abatic;-saiuration temperature /3.
(4) Humidity at adiabatic-saturation : fr0m p<;iint E moving hori­
zontally towards humidity· axis gives an intersection point G,
which is the humidity at adiabatic saturation line.
In a similar manner, humid volume and hu1riid heat can be obtained,
by considering the corresponding lines, humid volume and humid heat
lines, respectively, as shown in Figure 15-1.

HUMIDIFICAITON
Humidification is the· process of increasing the moisture in the air.
Applications
In pharinaceutical industry, if special conditions are not prescribed,
the humidity required for various operations is from 20 to 30% RH and
°
the temperature is within the range of 20 -27 C. Hence, dry weather
°
humidification is necessary.
By sp'�aying water into the air path, at <l' temperature higher than the
dew po'int temperature and lower than 'the dry bulb temperature, cooling
and ·humidification are achieved to the desired conditions. For this
purpose, absorption refrigeration system is employed.
Mechanism of Humidification
The interaction of gas and liquid and the co1;1ditions of humidification
an: shown in Figure 15-3. The x-axis indicates the perpe11dicular
distance to the interface. The ordinate · represents temperature and
humidity.
Broken arrows represent the. diffusion of vapour through the gas
phase. Continuous arrows represent the flow of heat (both latent and
sensible) thro'ugh the gas and liquid phases.
Figure 15-3. Conditions in adiabatic humidifier.
Hi and I; represent equilibrium conditions of interface (saturation
- conditions). Latent heat flows from liquid to gas and sensible heat flo�vs
from gas to liquid· get balanced, Therefore, there is no te_mperature
gradient in the liquid,
DEHUMIDIFICATION
Dc:h11111idificutio11 means decreasing of humidity (removal of mois­
ture) from, the air.
Dehumidification is accomplished by bringing the moist air in con­
tact with a cold surface (liqoid or solid). Many large air conditioner
plants incorporate automati·c control of the humidity and temperature of
the issuing air. Temperature control is effected with the aid of thermo­
couple or resistance thermometer. Humidity is controlled using a
thermocouple recording of the difference between"the wet �d d ry-bulb
·
temperat:1rcs. r
 Ch-15 HUMIDIFICATION AND DEIIU:\11DIFIC:\TION 417
..J I 6 Pl 1/\RMACEUTICAL ENGINEEIUN(i ' t"
Unbroken arrows represent the flow of heat · (both latent and sensible)·
Applications through the gas and liquid phase). �
. Dehumidifiers. arc used in special heat transfer devices to liquefy va­ In this •case. humidity of air, i-ly, is greater than the humidity at
pour b) removing their latent heat. Such systems ar-::.called condensers.
1
interface. Iii and, thcrt!fore, water vapour diffuses to thciintcrface. Since,
. In pharmaceutical industry, many operations arc carried at a stated vapour is condensed to water, latent heat is transferred to the water. So .
humidity to get optimum results. · In many parts of India (e.g., Bengal, the temperature of the surface tends to rise and that of the air decreases.
Kerala etc.) the air is very humid and it becomes difficult to carry on' It ,vould be expected that the air would .cool �t constant humidity, until
operation with hygroscopic substances even in air-conditioned room. the dew· point is rca�hcd (Figure0t,�-4).
Hence, dehumidifiers are installed for certain operations. Since ti and )i; represent saturated air, Iv . must be greater than !j.
Mechanism of Dehumidification Hence the bulk of the ai, would be saturated ,with water vapour. at that
. temperature. The sensible heat is transferred into the water.
Th e principle of dehumidification is illustrated in the Figure I 5-4. If
the temperature of the surface is lower than the dew point of the gas, COLO AIR
condensation takes place and the temperature of the gas falls. SURFACE
Humidity, H
The conditions at a particular point in a dehumidifier arc shown in
Figure 15-5. The x-axis indicates the perpendicular distance to the Temperature, T
interface. The ordinate represents temperature and humidity. (Broken
arrows represent the diffusion of vapour through the gas phase.
Moisture
high temp.
Temp . falls
LateQt heat
Transfer of Water vapour
· ·:_·._:_.· . condensed
latent heat Sensible heat
> . moisture
� .... .. :,, _._,.. ,.
•.r1• ... )� -:, .• , ':
condensation

Distance
Cold surface Temp. rises (until
(below dew point) dew point reaches) Figure 15-5. Condition of dehumidifier.
The air in· co_ntact with the surface is cooled below its dew point.
Cooling ( due to Subsequently, air from a distant place condenses, which requires 'time to
condensation)
cool. Therefore, effective mixing enhances the dehumidification. Nor- ·
mally, the temperature and humidity are reduced simultan�ously
throughout the process. After dehumidification, the gas can be reheated
>

mp
to its original dry-bulb temperature.

Air of Rehe,t,:: � W�te< Approaches to Dehumidification

Different approaches to dehumidification are described in Fig. ! 5-6.
>
desired
temperature
(a) Moist air is broug_ht in contact with a spray of cold wat�r, whose
Cold surface further temp:!raturc is lower than the dew point of the enteri!lg, air.
temperature rises (Figure I 5-6a)
. Figure 15-4. Principle of dehumidification process. (b) Humidity c,an be reduced by compressing· the air (Figure 15-6c) .
. TC'mperature and humidity arc reduced simultaneously. During compression, the �artial pressure of the vapour i1ncreases.
 1'11/\RM/\CFl JTICAI. l:NGINEF.!UNC i
Ch-15 HL!MIDIFICATION AND DEIIUMIDlflCATION 419
takes
As soon as it reaches the saturation value. condensation is necessary. rt is done intermittently o; continuously. Silica gel
place. The water gels liquefied and drained off. has to be regenerated as soon. as or even before it adsorbs 40%
of its weight of water.

- REFRIGERATION
Mechanical refrigeration is a__prQ,ess ol_lowering the temperat!:!f�_Qf
a substance less than that of ittsurroundings.
-->The.simplest f��� of refrigerati�ii observed in daily life is the use of
ice.. Ice absorbs heat from the su rroundings and melt. During this
(a) Spraying of water on .moist air. I
process the surrounding area becomes .cool du e to the loss of heat. The
capacity of refrigeration is expressed in tonne.
A tonne of refrigeration is defined as the rate of heat re moval from
Adsorbent the surrou ndings equivaient to the heat requ ired for melting I tonne of
silica gel ice in one day.
If the latent heat of fusion of ice is taken as 336 kilojou les per kg.
one tor.ne is equivalent to heat removal at a rate of 14,000 kilojoules per
____.. Dehumidified air
._____ hour.

(b) Adsorption of moist air. Application

Refrigeration is used extensively in air condition'.ng plants in the
areas for comfort and processing areas. It is used in several other areas
___________
Compres\ion
as given below.
>
(I) Removal of heat froll! ch_emi�al reactions
Gas
Low pressure
--------� --
(2) }r�servation o{ti;;mol;bil�--;ubst�nc-;s: For example, -insuliD,
ACTH, p1tu1tary hormones an vace1nes are stored in refrigera-
-� �
tor. It is extremely important to store all blood produ cts such as
---,--

whole human blooq at as low a . temperature as possible above

"y freezing point.
Liquid (3) Liquefy processing gas.
(4) Separation of vapour by distillation.
(c) Compression of moist air.
. tion. (5) Purification of products.
' hc�· for. achieving ddnimidifica
(6�ferential freeze-out of one component from a liqu id mixtu re.
F.1gure 1,;
.-6. Approac
ugh a.
. . . a sol id adsorbent smfoce or thro
, (c) Moist air is pa sscd. O\�Cf cati on occ urs
15 -6b) · Dehumidifi
, ., liqu id adsorb.ent spray ( r·igure
�e�nh
vapou r r:e ssu�c . ·, The ads orb ents
du e to the lowering of wat er - Refrigeranl is a liquid which readily absorbs heat when evaporatsd at
.

bcnts a� ,
i. :

mina. fhe ltqu 1� ac;i so1

u sed arc silica. gel or activate d alu or organic�
a low tempe rature'1ifcf'pressure and gives out heat ori_fo-;iensing at a
. n o ,an ic. salt s (bri ne , lithium chloride ) higher temperature and pressure. Refrigerants may be primary or
sol u tio ns o .
f ation of adsorbents
. • u.s ··....·thv• lcne l!� ly:col. Reactiv
comp9und . s s1u cl:�, secondary.
 �:o PHARMACEUTICAL ENGINEERING
Ch-15 Hll!\1llllFICJ\IIClN AND DElllJMID!FIC/1TION
421
�ry refrigerants are those liqui.ds that change from a liquid t o a
The basic construction of refrigeration
gas after absorbing heal . . . . . ---- cycles i? shown. in Figure
.· . 15-7. The cycle operates at two prc�surc
s, high and low; to enable the
�bei"of refr1g�rahts�are av.tiiable, �hich p�rm,i� the. selectio n prnccss to produce a continuous cooling
_ effect. The sequence of event:;
for a specific application. Examples of primary. refrigerants and their in the n.:frigcrntion cycle is e;-.;plaincd by
taking basic components in
chemical c onstitu tion are given below. · order.
Numerical .Ch�micalname (a) Receiver or condenser : The !)quid
refrigernnt is 'kept in a
container namely condenser. The refri
gerant is u11dcr pressure
·. :..:.., .
designation
and the vapour and liquid phases are
Rll Trichlorofluoromc1hane (Cl3Fc;)., in equilibrium.·
. (b) Exponsio11 \'Clll'e: It is a device. whi
' RI2 (frco11, 12): Dich'forodifl�q�o,�ttha�e (Cl2J:2C). ch controls. tlte rate of !lo\�
- of refr igerant into the evaporat_or, convcrt
in!_i the refrigerant from
."- . '.\ .

Ch.lorotrifluoromethane (CIFjC
.

R.13 high pressure to low pressure 'TheYrefr

: igerant enters a low-
I : ,, • .• ·

Dichlorofluorometihttnc (Cl2FCH) ·
· . . . .
•

R21 pn.:ssurc zone.

. R22.. ChlorodUlu.oromethane (CIF2CH) ··
- 22)
(Freon
.. ·
Rl.}3 Dichlorotetnifluoroetharie
· ·.

Ethylene
Propylene.
. Ammonia·

'da�y refrigerants are those_ H�uids, which act only as heat .<.
cart -xamples are brine, air an water. ,
· The choic�Lof ,a suitable refrigerant. depends upo many factors,
�
altho�gh a fe�y are mentioned below. · · ·'
(I) The latent heat of vaporisation should be large SO that tne
desired cooling effect :is produced. · ·
(2), At.normal temperature and pressur�, re�rig�rant must b�. in va­
,po�r ph�e andJHl�ompr'ession and coohng at shouldbe ltquefied Expansion valve
··':Li!' _ ;
il .
e� y, .. ,.. ·: i ..,.:._; ·'
i
· .. :.. ·' ···-. . .• .·.. · Figure 15-7. Basic construction of refrigeration cycle.
. (3) Th� pressure required to liquefy the:vapour' �t �e}·�frig��ant i�,
(c) Ev<1pwaror: Subsequently, a mixture of vapour and liquid enters
the condenser section must be SO as to mamt�m It usually a
the cvapoiator, which consists of coils. Herc the refrigerant
rooin temperature.
evaporates by absorbi_ng he.at from the space. The molecules ,
(4) The vapour pressure of refrigerant llquid. in·1he evaporat or sec­ m·ovc apart by breaking intenno!ccular forces. The energy (h�at)
tion must be maintai_ned at about -15 °C greater than.1the rct1uired for this process is 'taken from the surrounding cnviron­
atmospheric pressure. men. t. i.e .. space, '!Vl1ich is to be cooled. In this step. liquid
(5) The specific volume of the refrigerant vapour should not be vap9rises completely: though some liqtiid still remains.
large. (d) LiquiJ t,'ap : A liquid trap is used to remove liquid. which ·is
Principle
· · ' : ·
.· then relurned to receiver {condenser).·
(1!) Co111pri:.1.rnr : The saturated vapour is allowed to pass through
The refr:geration eye!� ;s _also known vapour compression cycle.
. . ""·�
-·· the compr.:.ssor .. During compression. heal of co111pression is
This is illustl'ated using single-stage vapour
�·cou1prcss1on. ·
added to vapour and tlie prcssu;c raises. The compression ,s
 Ch-15 I IUMll)IFIC/\TION /\ND DElllJMlfllFIC-1\TIOl--l
422 I
1'11,\IUvl/\tHJTJC,\L FNGINITRISG
The refrigerant effect is detineJ as the amount of he:it removed from
adiabatic and on the discharge side it produces a supersaturated the surroundings pi.:r unit mass ·flow of ref'rigerant. J
gas. 'The valve should be opened very slowly. /\ part of the
li�ui<l vaporises. to give a stream of high v:locity. (ii) \Vork is being done on the -refrigerant vapour to compress it.
I !�at or compression is expressed as:
( I) /'rmclc11ser : The supersaturated v:ipour flows t0 the· condenser
. '. where. the gas is liquelicd. · These condensers can be :iir-coolcd l'.i.:ul ofco111p {'i.�1'io11 \ hc1 - Ilg (21)
.
0
·

or ,vater-coolc<l.
when: /,[.:. cnth�i-rpy of the discharge. k.l'kg
h�
Thus. one cycle is completed as shown in figure 15-7. and the
process cont inucs.
= enthalpy of inlet compressor'. U/kg

. The work of compression is determined by multiplying the heat of

.
Theory co111pressio1·1 by the mass or flow.' · ·
;1\11 ideal refrigeration cycle is a reversal of CarnOt cyck as per the Combining cqu:::itions (20) and {21 ). COP can be \Vrittcn a·s:
second law of thcrmodynamics. Similar to Carnot cycle. refrigeration rcfrioer-ati:10 effect
· also depends OIJ the working temperatures, i.e., temperatures al whit.:11 (' ()/' -- ______ ::.___':____________
.
(22)
heat is a<ldc<l and rejected. Hence, the l!fticiency or et)t:lfo:ic11t or work input for CQt�1pression
.
. .
per!<.)nllancc (COP) may be expressed as: Two parameters an: important for the pcrf;rman,ce of a refrigerator.
r
heat absorbcd f om The rate. at \.\'hidi refrigeration is obtaincd depends' on the wci!.!ht and
low temperatun.: source · volume of a refrigerant circulated per tonne, though several othcr� factor.5
COPg "" ( 18)
net \vork input arc also involved.
The mass flo\\' rate of the refrigerant -:irculatcd per lonn� of c;ip:1city
T1,iRh c. '�·

( l ()) is detcrmincd by:

1i1igh - Ttrm !{ate of rcmov:il
where T O
absolute temperature. K. of heat (kJ/h)
Rc/i·1�1:,i.:run1 111a:1s //011' rate. (l-.gih) (23)
· J'hl: COP of the refrigeration cyclc ts defined :.is the ratio nf th:: Refrigerant effect
rc:frigeration effect to the work input. (k.likg)
COP will be less than that of the ideal cycle. I -!000 kJ/h
J\s mentioned in the working of a rd'rigcmto.r,, the n:fril!�ration
process can be understood from the pressure-enthalpy (heat content) Qiuw
chans. During this process. the n:frigcrant uridcrgoes a change in The theoretical volume of vapour to he handled per tonne may be
enthalpy. Essentially the refrigeration process consists of ev:iporation expressed as:
and C?mpression. 1heon.:Nca/ rnllllm.: of h1pn1II' (111\h) �· m:iss flo,N r:ite x v.
. g (24).
(i.) t\s the liquid evaporates, it takes heat from the environment (thL�
�vhi;re Vg spcciti� volume of the SUL'tion vapour entering th!.! compres-
00

interior of refrigerator or substance placl!d in it) so that environment get�

•

sor.. m J/1,;g.
coolt:d. The net refn/,erant ef[ec:I (RE) accomplished in the evaporator
· may b l' written as: · · · In order lo achievc low te:npcraturc dfcct. it is nccess:::iry to have a
high compression ratio. A single stage refrigeration cycle c:innot yield
Net n.'.frigeratini effect, Q1ow = hg - h t (20) low tcrnpcratun: effect. To avoid high comprcssion ratio. it is ncc�ss:::iry
�·here /,?. = enthalpy of gas (vapour) lcavinf! the e·vaporator;. kJ/kg to have sevcra! stagl!s of comprl�ssi_on. lt is necessary for low tempera­
ture applications.
hr '= enthalpy of liquid leaving the condenser, kJ/kg
r
424 PliA RMACEUTICA I.: ENGINEERING
·A-refrigeration system that consists of more than.one stage of com­
pression is defined as multistage refrigeratiqn system.
Temperatur&s from -IOI.I to ..:.n °c can be obtained by using refrig­
eration system containing multistage systems.
AIR CONDITIONING
Air co11ditioni11g is the process of treating air so ;is to control its
t�mpcrature, humidity, cleanliness and distribution simultaneously lo
meet the requirements of the conditioned space. " .,
In the production. area, a desired environment, Le., humidity and
temperature, is maintained. Therefore, air conditioning facilities are
essential. Today many offices and pharmaceutical plants arc equipped
v.;ith air conditioners.
Applications
Promoting the human comfort : Human body feels comfort when
the heat produced by metabolism of human body is balanced by the sum
of the heat dissjpated to the surroundings and the heat stored in human
. body. Air purity is of utmost importance. For example, increase in
carbon dioxide adds discomfort. The efficiency <ilcd health of workers
s�ould be maintained at safe tolerance limits.
Maintenance of proper conditions for the manufacture, process­
ing and preserving of material and equipment : The following areas
arc identified.
Compression of tablets : In the granulation section, th� air condition­
ing is optional, if necessary the cond_itions are 45% RH and 22 °C. In the
tabletting section, the conditions are less than 20% RH and 22 ° C. In the
production of efforvescent products, dry snups, controlling humidity is a
vital factor. The relative humidity should not exceed 1 0 to 15%. antl
temperature is at 22° C.
Alam!fact11re of soft gelatin capsules : The temperature i::; usually in
the range of 20 ° C to 22°C and the humidity is controlled to a maximum
of 40% in the operating areas and between 20 and 30% in the drying
areas. '
;
Manufacture of sterile products : in case of parenterals and ophth:il­
mic' products, the environmental conditions are much more ;;tringent in
filling and sealing rooms. Therefore. ,the standards of clcari air quality
arc of greater importance. In the production of all biological pro�ucts
(Schedule C. & Ci) air conditioning is essentia!.
Ch-15 I IUMIDIFICATIO� AND DEHUMIDIFICATION 425
Environmental test chambers : These are designed to carry out
stability and shelf life testing of drugs. They offer reproducible tempera­
ture and humidity conditions. Climatic conditioning is also required for
· herbal research, pesticide research an9 zoology.
Maintenance of animals and equipment : According to the Drugs
and Cosmetics Act and Rules, the animal houses should be air-condi­
tioned. Sophisticated electronic (analytical) equipment are stored and
the wo1.l is carried out in aii· conditioned rooms..
Appro,1chcs for Achieving Air Conditioning
Normally thc air is allowed to reach complete saturation by providing
appropriatc conditions. Then humidity· is fixed. In· commercial cquip-
111c11t. the conditions arc somewhat indeterminate and the exit humidity
is not quite saturated. Therefore the exit humidity is fixed by varying
water tcmrcrature according to the characteristics of the speci fie piece of
equipment :11 !1and. This can be achieved by re-heating to the aesircd
' ,
tl'mpcr�turc.
Consider the following example. When air is. entering the equip­
ment. let the initial dry bulb temperature of the air be t1 and humidity be
,!i 1 It i� rl'prc:;cntcd by point A. Let the desired dry-bulb temperature
be r: and humidity be li2 at the exit point air (point B). The exit air
attains the de$ired conditions in any one of the following methods.
(A) The sequence of steps is shown in Figure 15-8. The air is first
allo\\'cd to �ttain the desired humidity by treating with water using
humidity chart. It is rcprescntc� by point C (wet bulb temperature. l3).
.
...- 1000/o Humidity
Desired curve
humidity
__
_..
___,..B j
·--
Temperature, 0
(
Figure· 15-8. C:::'.11gcs in ,,ir tcmpcrattirc anil humidity for air C\mditioning
proc.:ss ( Approach A). using I 00% humidity line of the psycho1m:tric chart,
426 l'l lAl{M/\Cl:UTlCAL ENCilNl:L:R.IN,,
Ch-15 lltl1'11DIFIC/\TION /\ND DElll::-.l!DIFICATION 427
Then It 1s heated to attain thc dcsircd temperature of t2 at the same
humidity. This"path of air is represented by ACl3 in Figure 15-8. . Air cleaning is usually provided using !illers. whi9h can be· �leaned for_
reuse or disrosablc. Coolirig is achieved using eithc.r water or by direct
(13) The scqucncc of skps is shown in Figure 15-9. In the second cxpa11sio11 in refrigerated coils or air washas. Steam or hot water c_oils
approach, air is preheated to a temperature, t.1. Subsequently, the air is ;uc. used for heating. 1-lumidi tication systems may be provided by
cooled along the adiabatic cooling lin<.:, until it reaches the dcsir<.:d surface type water nozzles. steam huri1idifiers or spraye? coils.-
,
humidity. It is then reheated so as to reach the dc�ired temperature of 12.
Equipmcnt : Air conditioning :involves spccialis�d applications of
This corrcsponJs to path ADCB in Figure 15-9.
basic thermodynamics. hydrodyna1�1ics and nuid flow principles.·
Principle : In this type of air conditioner, approach (B) is used. The
air. is heated to a higher temperature, followed by cooling along an
adiabatic cooling line to reach tile d<.:sired hun).i<lity. It is then reheated
�
"' -� - to the desired te;nperaturc at constant hlimidity. Thus the path ADCl3 is
�
.
?:
O'l
:.<:
-0
O'l
Desired
Adiabatic.
folkmed.
:.<:
humidity
Construction : Thc constr�ction of the equipmentjs shown in Figure
15-10. '_
A
D Spr;iy
Finned
H1 finned heating
nozzles·

..
I I heating

-
I I coil
t I: tz It� co:L�
0 .\
Temperature, (

Figure 15-9. c'h:mgc:; in air tcmpcraturc and humidity for air condi­ Fresh �
tioning proc..:ss (ApproJch 8), ba:;cd on adiabatic cooling lin�. air inlet --...

· Types of Equipment
MoJcrp air eunditiuning equipment generally fall into two classes.
. 'l. Self contained air conditioner (unitary or packaged)
, Central air·conJitioner (or field erected).
Water Md Damper Fan
l. Self contained air conditioners' : These systems include win­ reservoir eliminator
. \

. dow mounted or \Vall brad:d conditioners.

�lost of these units art: air cooled, though \Valer-cooled typ<.:s have
also be�n made. Room air enters the casing at the front pani.:I. It is
mixl!d with p::irt of the outdoor air. This mixture is forced over the
cooling coils by a centrifugal fan, which is driven electrically. Somc of
the moisture in .the air is condensed and disposed off by means of a
single ring of the propcllr.:r type of condenser. The units arc hermetically
scaled. Reciprocating compressors using nontoxic rcl'rigerant a11d driven
by capacitor motors are used.
2. Central air conditioning system : l'he'.:>c systi.:,ns may si.:rve one
or �cvcral areas with conditioned air bcihg supplied through duct network.
Figure I 5-J 0. T) riql. central-stationed air
- unit and
C\ln<litionin!? control svstcms.
·,
\\'orking·: The principle employed in this equipment is approach R .
Outdoor air and room air is·drawn into the equipment using a fon. ,\ir
quality is 11_1ai11tained by allowing the air Jo pass through the filters in
ord..:r to remove ,•rnspcndcd particle�. r\ir is.then ·allowed to pass through
finneJ coils and heated (as imlicat.:d Crom point/\ to D in, Figure 15-9).
The hot air is then passeJ through wat-:r sprays and is adiabMically
cooleJ and humidified (line DC in Figure 15-9). The pump draws water
rrom !he re'iervoir below anJ spr::iys 011 the air stream. T,he ·pump also
 . Ch-l.$ -UUMIDIFICATIONANQ DEHUMIDIFICATION
42.8 PJIARMACHITICAL ENGINEERING
429
Jelivc:rs water to give a curtain of water to eliminate most o� the Hen�e, air conditioning is provided under assumed conditions keep­
entrained sprays. The air then enters the eliminator bafnes where the .
.-mg variables fixed. Allowances .. have to be made
· for,changes
·· in the
last t:ntrained \Vater is removed. In the pump discharge, .there may be a assumed conditions.
heat.:r N � provision for steam injection to adjust the water temperature.
Glossary<,fSymbols
A second .set 01· coils performs the final rc-he11ting (line CB in f:igure Ca = Sp�ci fie heat capacity of gases. kJ/kg.
15-9). The final temperature may be regulated by con.trolling the steam Cw = Specific heat capacity ofvap<;>ur, . ·•· kJ/kg.
..
in the second set of coils or by controlling a bypass damper as shown in COP "". Coefticien.t of performance.
Figure 15-9. A fan draw:, the air through the ar;paratus and discharges it H = Humidity, kg/kg.
to the point of u�c: From this point, the air is sent to the required areas HA = Per cent humidity.
through ducts. HR = Relative humidity.
H5 = Humidity at satumted gas (Air).1
Temperature is regulated by thermostatie:illy controlled heating or
J h "" Hour ; --
cooli:1g units or by a combination of hcating-1:ooling units. nd = Enthalpy of discharge leaving ·comp"ressor, kJ/kg.
Circulation take» place naturally within area. but it .is necessary to hg = Enthalpy of gas leaving evaporator. id/kg.
usec'mech:inical means to re-circulate air (to replenish air period:cally hr = Enthalpy of liquid leaving the condenser, kJ/kg,
with fresh aii) or by ventilation, which circubtcs fresh air only once._, in MA = Molecular weight of ga.c; or vapour.
an hour or so. Ms = Molec.ular weight of air.
PA = Vapour pressure of liquid, kPa.
VJri;,nt: Equirmei1t bas..:d on the proccss·corrcsponding to th..: path Ps = Vapour pressure of the air, 'kPa.
P.Cl3.c,f tigurc 15-S is tilso .available. It is similar to that shovvn in PA == Partial pressure of. water in air, kPa.
. Q "" Heat absorbed from low temperature source (net refrigerating effect),
Fi·!.tl\l?. J 5.:9. In.stead of using heating coils a,; shown in Figure 15-10,
:-;t;,:.11 is ·injecicd directly into the water. The mechanism of pumping. kJ/kg.
�!!lJ Sj}rJy!ng is similar and maintains the desired temperature (as shown T = Absolute temperature, K.
V = Humid volume, ml /kg.
by CS i.n Figure 15-8)'. The. rest of the apparatus is 'exactly similar to
vg = Specific volume, ml/kg.
t:iat shown in Figure 15� I 0.
s = Humid heat, kJ/kg·K.
w = Weight of moisture, kg.
Air Conditioning--Calculation of Load
W "' Heat of compression (net WQrk input), kJ/kg.
The cooling or heating equipment is. provided to remove or to add
heat at the rate at which it is produced or removed. To estimate the
QUESTION BANK
capacity of the air conditioning equipment. the following procedure is
used. Each qoestfon carries 2 marks
Slcp J. The tempaature conditions (outdoor and indoor temperature) I. What are humidity charts? W�ite their uses in pharmacy.
arc designed for \Vinter and summer outdoor temperatures. 1. Draw a humidity chart and give its significance.
Stq>. 2.. Sp:ie<: cooling load is calculated. 3. Define the terms, humidity and dew point.
(a) .Direction and magnitude of wind velocity. 4. Wr�te the utility of humidity charts.·
(b) Outside hun,idity -and temperature. 5. Oifferentiate between humidity and relative humidity,
(c) The nature of co11struction matcri:ils. 6 .. What are the applications of dehumidification/humidification?
(d) Oricntatio11 of openings. windows and doors. 7. Explain the principle of dehumidification
(e) Period of occupancy and the number of persons in the room
8. Explain the principle of humidification. ·
and thl'ir acfr.-ities.
9. Differentiate dry bulb temperature and wet bulb temperat1Jrcs.
1.0. What are the applications of air conditioning?
430 PHARMACEUTICAL ENGINEERING

Each question carries 5 marks

I. Describe the imponant features of humidity charts.
2. Describe the working of a refrigerator.
3. What do the term dehumidification means? Write a note on the applications
of dehumidification.
4. With a neat diagram explain principle and working of an ai� conditioner.
 16
Corrosion

Theories of Corrosion
Factors Influencing Co
· rrosion
Types of Corrosion
Prevention and Control of Corrosion

.Mc.tals spontaneously undergo gradual destruction when exposed to the

atmosphere.. In chemical terminology. such destructio� is kno'wn as
corrosion.
Corrosion is defined as the reaction of a metallic material wi'th its
environment. which causes a measurable change to the m,:teria!" and can
result in a functional failure of the metallic compo;1cnt or � of a ·Jomplete,
.
.: . .
system.
. ..: . .
Exposure of the surface to air. wafer, a"i1d .. caustic chemicals arc,:
responsible for corrosion. Since metals. �re "g6od ,' c�ndlictors; they'.
undcr,!O, electrochemical changes on their surfaces. · The compound ,fhat
is fonm:d during corrosion is referred· to as corrosion 'product ,and the
metal surface is said to be c<jl'roded.. 1 he corrosionr/1n•dia nre gcncraJly , .
liquids (mostly aqueous solutions). ht)t also solid�·and ga_se�:·· : .·' · .
· The surface changes due to corrosion arc carried through the equipment!,
ai1d destroy the perf�rmance ·and fabricatio11 in du� .��ui·
. '
sc:
·..
Some times,
• � (f,.;> . ·, : • • . . • •.
the leached ml!tal may contaminate the product: ·:·The material of con'-·
struction must be resistant to corrosion and erosion\, Hence. adcquate_ 0

atte11tio11 should be paid v.11ile selecting the materials for constr�1c.tion of.
CC] ll i J) lllC 11 t.
Corrosion can be either dry' o·r wet type.
Dry corrosion : It involves the direct attack of dry gases (air and
oxygen) on the metals through chemical reactions. As a result- an oxide
layer is formed over the surface. This type of corrosion is' not comn.10n.
• t ,·.

Wet corrosion : It involves the direct attack of aqueous 'media·

(strong or dilute. acidic or alkaline) on metal tl,irougl1 elec,t�ochemical

431
 433
432 1'111\RMACEUTICAI. l:NCilNEERIN(i
Ch· I c, CC>RIWSION
diITcrcnt m�ta!s; the corro.sion is
reactions. The moisture and oxygen arc also responsible. This type of When galvanic cells arc formed on
reactions, arc illustrated 1_1smg. the
corrosion is quite common. known as �a/\'(lllic corrosion\ These
. such 'ns hydrochloric ac1�.,
Applications melals ·in ti i c presence of clctrolytc sollition
. Knowledge.of corrosion is helpful in certain areas to prevent problems.
Corrosion Reactions on Single Metal
dering the corrosicm
D�s and punches : In the compression of tablets, dies anl punches Electrochemical reactions arc illustrated by consi
i.c and cathodic areas_ arc
sho�ld be free from rust and corrosion. Chromium plated dies and on a piece of iron in hydrochloric acid.� Anod . _
1mpcrfe��1ons (lo:al�sed
punches arc used, so that the problems such as pits and abrasion can be formed on the surface of iron, owing to surface
s) or d�e lo variations
avoided. stresses. grain orientation. inclusions in the mefol .
ons may occur (Figure 16-1 ).
Milling equipment : In these equipment. a perfect fit between the in the environment. N umcrous tiny reacti .
moving parts should be maintained for effective size reduction. Though
' ·, .•.• '1

Anode (oxidation)
corrosion docs not effect .the performance of the mill or product. surface corroded·
imperfections do not facilitate proper cle,aning of the· equipment. Hence, Electrolyte
.. ,
,,l i

(HCl)
I.he �ssociate<l prnblems persist.
Chemical processing reactors· : Diverse nature of solutions which
come in c'ontact with the reactor surface often lead to corrosion on Cathode
account of corrosive 1ncdia and environmental conditions.
Fermente.rs : Glass. glass-lined and stainless· steel (S.S.) mat�rials
are used for tht: construction of the ferm�ntors. During Jermt:ntation. the
·-:-• Iron. piece , ,
release of trace metals from the equipment may have delett:rious effects
on the ,enzyme. system and metabolic pathways of the organisms. The
possibl�. corrosi0'5l aspects 'in formentors are pits and crevices, which
make it difficult to clean 'and remove the contarnination. Most of the
Figure 16-1. Ekctrochcmical. mc�hanism. of corro­
• operations arc conducted ·at normal· tcinperatures and the pH of the arc 11lustra1eu.
sion. Different areas on the iron piece·� . .... .. '
media would be around neutral. Maintenance of hygiene, need for
.

,vith the release of

sterility and prevention of contamination are important considerations in Reaction at anode : Oxidation. takes place
detac hed from the solid
the construction Of fermentl!rS. electrons. Positively charged iron atorns· get
' ·c.�
surfa ce and enter into soluti'on (electrolyt e) as positi ions. ve
Storage containers : Prolonged storage of reactive chemicals �le�ds . - .� ... \

(indic ated by rough surface)

to corrosion of the containers. At anode: Fe � Fe +-+ + 2c··
This chapter highlights the general aspects of corrosion sue� as (oxidation)
und the external
corrosiv� environments,, principles, types of corrosion and mt:asurcs to · The released free cJcctro1is (ncgati_v c c�a_ rge) pass m ', !

c1rcu1t.
• • \ .: .�:�: I \; ! .,/

prevent corrosion.
• • ''

s occurs whh the

Reaction at cathode : Reduction ·of constituent
:the cathode an� re�t
THEORIES OF CORROSI.ON takin'g up ofel�ctrons. The free el�ctrons reach. .
hy�rogcn . ions Jn .,.e
The .metal surface undergoes an electrochemical reaction with the with some positively clf:1rgcd species _such· as
J
. . .
ter itself d1ssoc1atcs to
moisture and oxygen in the atmosphere. This theory is known as electrolyte solution. In the abse1�ec of acid, w�
•
e/eclrochf!mic:a/ theor y of corrosion. The mechanism involves the forma­ generate H ions.·
+ .

tion of a galvanic cell {anodic and cathodi.c areas). by different metals + (indicated by formation of
At .cathode: 21-1 + 2c- -"7 H2i
(for example. Fe and Cu) or in different areas on the same piece of metal tit: bubbles at the surface)
(l{cducti'<''1)
(for example. iron).
 l'I IAR\li\CTU'rl(.'AI. ENGINFERIN(i 435
&J
'e Ch·lh CORROSION
· The amount of metal ,(iron) which, is dissolved i,; the electro
. lyte is · The corrosion current !lows at the expens;e of the anode metal, which
propo1t1�nal to the , umber of lectrons 110,ving, which in """ as t I1e cat hode meta 1·.1s protecte d.
tum Iy, w 11crc
°
� � is Jcpcnd ­ !,!<.:ts co�rodcd C9.{lllnuous
.
ent upon the polcntral and resistance. of the metal.
In so.me cases, evolution of the hydrogen ·gash slow.· The'accumula� ·•
The OYerall reaction: Fe + 71120 -) Fe(Ol l)i +· 112t tion of a layer of hydrogen on the cathode surface slows ·down :the·
Rl.'J brown rust .corrosion. This is called cathodic.: polarisation. It forms ·an insulating
.
. �I'·!£I.1 cvo.ut1on of HJ accompa111cs rap rd corrosion such as hyd
. cmbnt I • . . ro gen
layer that ·slows down or stops the elcctroc.hcmical reaction. ··, · · .
tlement. Depletion of hydrogen also enhances corrosion. In -Corrosion involving Oxygen ·; ·.: .. , .. ; :····
moderate concentrations of 1-12, corrosion slows down. }.''

The oxygen dissolved in an electrolyte can react with accumulated

Corrosion Rl•actions Hctwcen Metal�. hydrogen to form water. Depiction of hydrogen. la�'er al. lows corrosion
.
<i:tlva1�ic corrosion results fro111 thl' th1w of currcnl ti·1, 1n to pr�ceed. · .' ,...
. :1 ni.1rc
a�l1v1: 111ctal (a11 odc) to a lcs.s activc 111c1;d (catl t11d..:j. For c:xarnp At cathode: 02 + 2H2 � 2H20 Corrosion proceeds.due to
. k. ii ii c
�.tssoh·l·:; a11d hmns an anode, whill.' .; 1 ,ppl.'r (Cu) Ii.inns lh l· ,:;nlwJc. depiction of hydrogen
I h�-.l' two 111ctals f11r111 two electrotk·s and th...:ir presence i i
: ;111 cl l' L'trn­ The above reaction takes lJlace in acid .media. When the corrosion
lyta: .,oh1tio11 Ii.inns a gah·anit: ,·di (Fig me J 6-2 ).
media is alkaline or neutral, oxygen is absorbed. The ·presence :of
moisture (or water) promotes· corrosion. The eflective concentration of
oxygen in v.:ater adjacent to cathode depends upon the degree. of acra- ·
tion, tcmperature,;mcl presence uf dissolved salts. · . :,.

FACTORS INFLUENCING CORROSION , .

A number of processing factors affect thc,rate of corrosion.:

Solutio,n pH
Anode Cathode Th.: pH affocts the rate of corrosion of metals by one or'the three
, ' (Zn) (Cu) general patterns.
oxidation reduction ( I l rv1ctals such as i'ron dissolv� rapidly. i'n'. a�id.i� s9ll;tio·,;·. In
the middle pH range (4 to 10), the concentration of H" ions i,s
low. Hence, the corrosion rate is controlled · . by the rate
. of
Electrolyte (HCl) .
transport of oxidizer (o�ygc11).
Figure 16-2. Gal.vanic ml!chanism o f (2) Certain amphotcric metals dissolve rapidly in either acidic or
· corrosion
Reactions between different kinds o(m basic solutions. Examples arc aluminium and zinc. Corrosion
etat's.
proceeds. · · ···.·
'spo�ta.neous reaction can occur when two electrodes
are connected
through an extenJal wire. Rea<itions at anode and cathod (3) Noble metals arc not affe.ctcd by pH. Examples arc golJ and
e arc: . . <.
platinurn.
At ano.de:_ Zn � zn++ + 2 e- (ind:cated by roug h surface)
(oxidatiun), . . The 1-1+ ions have a tendency to t�ke up :�lcctroris to' forrri Hi gas.
Therefore, 1-1 + ions capture electrons and promote anodic corrbsion. �
At cathode: 2H+ + 2e- � H (indicated by format1on of
' '
2t
(Reduction) bubbles at the surface) Oxidising Agents .,
Oxidising agents may accelerate the corrosion of�ne class of matc'ri-

.....
 436 . Pi IJ\RMAlTlHiCJ\L ENCilNEERINCi
als. whereas retard another class.
(Jxidizing agents such as oxygen (02) react with hydrogen to form
water. Once hydrogen is removed. corrosion is accelerated. For
example, copper in sodium chloride solution follows this mechanism.
Oxidising agents retard corrosion due to formation of surface oxide ·
films, which makes the surface·more resistant to chemical attack. There­
fore, adsorbed oxygen layer is essential. Thus a balance between the
power of oxidising compounds to preserve the protective film and their
tendency to destroy the protective film determine the corrosion of the
metal. For example, an oxide film is rapidly formed on stainless steel.
This film cannot be dissolved or destroyed easily even in severe op�rat­
ing conditions. However, sulphuric- acid and hydrochloric acid can
easily destroy this oxide film.
Tcmpcr;aturc
The rate of corrosion tends to increase with rising temperature. It has
a secondary effect. The influence bf .temperature on corrosion may
follow several of these mechanisms.
(I) Increase in temperature reduces the solubility of oxygen or air.
The released .oxygen. enhances the corrosion.
·
\2) Increase. in temperature induces phase changes, which enhances
· the rate of corrosion. At high temperatures, organic chemicals ·
are saturated with water. As the temperature decreases.' water
gets condensed.
(3) Oxygen is needed for maintaining iron oxide film, which pre­
vents corrosion: In the absence of oxygen (due to increase in
temperature). the corrosion of stainless steel increases.
(4) Copper-based alloys do not depend on the oxide. film for corro-
5ion.
Velocity_-
When the corrosive medium moves at a high velocity along the
metallic surface, the rate of c�rrosion frequently increases. High veloc­
ity has, the fol\owing effects.
(I). Corrosion products an; formed rapidly, hecause ·chemicals (in­
ch1dii1g oxidising substances) are brought to t'he corroding surface
· at a higher· rate.
I'
Ch-I& CORROSION 437
(2) The accumulation of insoluble film on. the metallic surface is
prevented. Therefore, corrosion resist.\_11ce of these films
',:,... ·
decreases.
(3) The corrosion products (or film) arc ·e?,si,ly stif1c�(:�1�d carried
away, thereby exposing the -nc\". .surfaces for corrosion'.. "·
I
; •
"' •
• 1
-dZ3
Thus corrosion proceeds unhindered. This factor is responsible for
thl.! corrosion of a number o�: equipment parts; sucg ·'as> condenser;�
evaporator pipes (in the vicir�ity of bends in the: pipes), propellers,'
agitators and centrifugal pumps. Corrosion occurs fr�qucntly in .small
Jiameter tubes/pipes through which cor�osivc liq.uid may be ci�culate.d at
high speeds as shown in the above examples.· ·:.,. ·,: ,:·
Surface f<iims .,...
Once;: corrosion is started, its further progr�ss is often controll_ed by,
the nature of surface films. A variety of surface,. films. hayc been
observed.
,.
' • '. • I I\ �J .! ; ,
Thin oxide films arc formed on the surface of stainless steel (rusting).
These films tend to retain or absorb moisture, which delays the tinie of
drying. Hence. the surface exposure to atmosphere or corrosive vapour
increases the extent of corrosion. :rhc rust. films formed on low alloy
steels an: more protective than those formed. on unalloyed steel.
..
Insoluble salts such as carbonalcs and sulpliates may be precipitated
from hot solutions on the metal sur'races.. These·. protect the metal
surfaces.
If the firin is porous (example is zinc oxide), corrosion continues.
Nonporous films (example is .chromium. oxide film on iron) prevent
further corrosion.
Oil and grease films ll"!aY occur on the surfaces either intentionally or
naturally. These hims protect the surface from direct contact with
corrosive substances. Examples are metals submerged in se\.vage or
l.!lJUipment usecj for processing• oily substances.
Other Factors
1
The c<,>ncentration of corrosive chemicals, in .the cnvironment influ­
ences the rate of corrosion. In equipment such as distillation columns,
reactors and evaporators. the concentration, can change co11tinuously,
making prediction of corrosion rate difficult. In addition, corrosion rates
arc seldom linear over a wide range. Concentration is important .during
rlant shut-down. The presence of moisture that collects duri�g �ooling
438 < ·11.1 (, U >RROSION 439·
l'l li\RMi\(TlJTICi\L ENG"INEERIN<,
Ekctrochcmical corrosion : This type of corrosion occurs at dis­
TYPES OF CORROSION
cn·tc points of metallil· surl:H:cs when ekctricity,rlows from cathodic
Pure metals and their alloys tend to enter into chemical unio�1 ��ith area 1·0 ,111\)Jic area. Metallic surface gets divided into _anodic portion or
the components of a corrosive medium to form stable compounds. Corro- catllmfa: portion.
sion can be broadly classified as follows.
I. Fluid corrosion, General
· 2. Fluid corrosion, Localised
Fluid Corrosion : Localised ..
Fiuid corrosion is the most frequently observc<l on_ different 101.:;;ti���··
· 3. Fll!id corrosion. Structural. in a rnall'ri,il. It occurs in numerous \\-il)'S. It is Cufth.;r dassificd ·a..�
4. Fluiq corrosion, Biological givrn in Figure l6-.3.
Fluid Corrosion : General Specific site corrosion : Mechanically weak spots or dead spots in a·
When cofrosion is generally confined to a metal surface, it is known n:actir:,!� v�ssd cause �pccific sil� corrosion.
.
as general corrosion. This type occurs in a uniform fashion over the ln:er-granular corrosion : Selective. corrosion that occurs in the grain
entire exposed surface area at a wide range of temperatures. General boundaries in a metal/alloy is called as i111ergra1111/ar corrosion.' Micro-.
corrosion is. of two types. . .
scopic examination can rcveai"dearly the intcrgrnnular corrosion.. When;
Physicochcmical corrosion : l"hc effects of this type arc swelling., se\'crc, this attack causes a loss of s.tr· cngth ·and ductility out of propor­
crazing. cracking. softening etc. Examples arc plastics and nonmetalli1.: tion to the amount of mefrll actually destroyed by corrosio'n. Crysts-llinc
material. grain s.1ructurc as such is i1ot.attacked appreciably. One example is: ·,·
d
Fluid Corrosion, Localised Austcnitic Nit'ric hot condition Grain boundary
+
Specific site corrosion
stainkss steel acid , pn:cipitation
1.
· 1� lntergranular corrosion
t Pitting corrosion
Crevice corrosion
Stainless steel is stabilized hy incorporation of_niobium<titanium or
rnrbon (less than 0.03%,). O 1c\i!:
•· ··

l'iiting i.:orrosio11 : This type uf corrosion results in dcvclop1111:11l of

2. Stress lndu�ed corrosion
pits and cavities. Tl'lcy range from dcep·cavities of.small 'diameter to
shallo\\' dl."prcssions. E:-.ampl� b:
� Stress corrosion cracking
· L Corrosion fatigue . Alloy of aluminium Aqucuus chlorides
L Freiling corr�sion or stainless steel + solution
-------.··\Cavities · .,,.

3. Llquld flow relate� corrosion Pitting of a metal occurs when there is a break in the protective oxide
Erosion. layer and i111pcrlcctions. ,>rj the underlying metal. . Inhibitors· arc some­
t
Impingement attack

.t
times helpful in preventing pitting corrosion. : ... '

Cavitation erosion Ctevice corroiion : In this type, corrosion occurs in· �rcviccs because
solutions arc retained at sue!� places. which takes longer time to dry out.
4. Chemlc:1 reaction related corrosion When this occurs� the intci1sity of attack is usually more severe than
Galvanic corrosion surrounding areas of the same surface. Crevices are fonncd because of
, Oxyge� concentrati?n cells · the metal contact with anotl1cr piece of the same or other metal or\,·ith a
Hydrogen embrittlement nonmetallic material. Corrosion in the crevices is due to a number of
Figur� 16-3. Classification of localised nuid corrosion
"'"�'"'� ,-.� oiv<'n h<'IO\V:
.
440 l'I li\RMi\CElJTICAI. E!\GINEEIUNG
Deficiency of oxygen.
l\�idity changes.
- Buildup of ions.
Depiction of inhibitor.
Str:css induced corrosion : RcsiJual internal stress in' Ihc metal or
externa't applied stress acc<.:leratcs the corrosion. Re.:;idual internal. stress
· - Molten zinc 011 stainless steel.
is ·produced by:
Di:formation <luring fabrication.
Unequal rah: of cooling from high temperatures.
lnt�rnal stress rearrangements involving volume changes.
Stress induced by rivets. bolts and shrink fits.
Eliminating high stress areas prevents this type of corrosion. The.
external stress can be kept at minimum by i:rnploying suitabk experi­
'mental conditions.
·::: Stress corrosion cnk·king : At the surface. if the tensile <;tress is
i:qual to or mon: than the yield �tress. the surfal'e tkvclops cracks� lhis
is 1-.nown as stre.;·s c01iusio11 cracking. Examples arc:
- Colc.1-l'urmi:d brass develops crack in the environment of ammonia.
1:inbritth:ment cracking of steel is observed in caustic soluti�1n.
C11n·o.,io11 Ji1:ig11!!: Corrosion fa_tigui.: is the ability of a metal surL1n:
to withstaml rl·p..:atcd cycles of corrosion.· The metal surface is stn:sscd
and simultaneously attacked by tJ1..: corrosive media. ·Pits (rnnccntraiion
poi.nts) indic:1ting corrosion arc fonn..:d initially, which furth�r ckvelop
into cracks .. !\� this pn)ccss continues. the surface loose� it� fatigue
r..:sistanl'c :rnd ultimah: failure of L:quip111ent.
The protective surface oxide 1ifm reduces corrosion. Under cycli� or
repeated '-tress conditions, n1pture of protcctivc oxide films takes placc ·
at a higher rate than at which new protective films can be. formed.
Therefore, the rate of corrosion is enhanced.
· Fretting c01'r<1sion : Fretting corrosion occurs ,vhcn metals sliqc over
ea,;h other anJ cause mechanical damage to one or both. During relative ·
movemi:nt of metals. two processes may occur. (i) frictii.inal heat is
gencrat'cd, which oxidizi:s the mftal to form oxide films (ii).removal or
the pro\ectivc films resulting in exposure or fresh surface to corrosion
attack.
This cari be avoided by using harder materials. minimising friction
by lubrication or by proper designing of the: equipment. so th:ll no
relative n10vcm..:nt of parts takes place:.
Ch-16 CORROSION 441
Flow related eorros_ion � Ciquid metals can cause corrosion.·. Usu­
ally thi: driving force is the tendency of the liquid to dissolve solids or
penetrating the metal along the grain boundaries at- places of -wetting.·
Corrosion rate is enhanced at high �emperatures. A few examples arc:
-- Mercury attack on aluminium alloys.
hnpinge111c:11t corrosion : This is also referred to as erosion�c'o,:r�.�ion ·
or rdoci1y uccdermecl corrosion. It is accelerated by remov_al of
corrosivi: products (such as oxide films), which would othenvisc tend to
stifle the corrosion reaction.
Erosion , Erosion is the destruction of a metal by abr;sion ·,·a�d
attrition caused· by the now of liquid/gas (with or without suspended
St)lids). The additional factors that can influence erosion includ�·: ., .•
_=Alloy contents of the steel (for example, chromium,
' . ., '·
c9pper, ,i1angancsc etc.).
=Pipe system design and component geometry.
=Water anc.1 steam composition (especially pH and oxygen
content).
The USC ot' harder metals and changes in velcfoitv .or environment are
� ' ' '· · . ' · .
used to. pn:vcnt erosion.
-:53
Ca\·itatjon erosion : Formation of transient .voids or vacuum bubbles•
in a liquid stream passing over a surface is kn9wn a:jcavitatio11. Th<:
bubbles may collapse 011 the mt:tal surface thercl;iy causing severe impact
or e,plosivc effect. Therefore, con.siderable Jamagc, and corrosion is
obs�rved. Th� protective films·also get destrc{yed d�·�·.fo i111pdct . ,
_
Cavitation erosion is observr;Rt,,_around propellers, rudders in pumps
etc. Rcd1;sign, u�..J of a more resis'tant metal and protective �eatings ar�
.
· required . to avoid this type of corrosion.
.
Chemical rt•action related corrosion : Corrosion involves chemical·
react inns sul'h ::is oxidation ai1d reduct.ion at anode_ and cathode., respec-
·· '
tively. ,
.
Gafra111,· corrosioil Galvanic · corrosion is associated with the flo.w
or cLirrei1t. to a less.:active metal (copper cathode:) from a -more-a�tive
metal (zinc anode) i'n the same environment. Coupling of two 1netals,
which are ,;,·idely separated i·n the elcctrochenikal ·series.· gene�ally l?ro­
duces an accelerated attack qn the more active metfll. zinc. i.e .. anodic
corrosion. Therefore,· a combination of metals which are as close as
possihlc in the electrochemical series ·should be chosen.
442, J l'I IAR��ACEU'l lC'i\l. ENGl,NITRl�G
In galvanic c.JrrC$ion. the ,effect of area is \'Cl)' important. For
example, steel rivets on copper (Cu) plat�s will corrode much more
rapidly than a steel plate with copper rivets. Corrosion at the :mode may
be I 00 to 1000 times' higher. if the two areas arc same.
Protective oxide films h:n<l to reduce galvanic corrosi0n. Insulating
materials can be placed between two metal faces to prevent <.:0rrosion.
For example. plates when bolted together, specially designed pla:;tic
washers can he used.
Oxygc:11 concc11/ralio11 ,·ell : This type of corrosion is due to the
presence' of oxygen ckc:trol) tic:. cell, i�e.. a difference in the amount of
oxygen in solution at. one point exists when compared to another.
Corrosion is accelerated where oxygen .concentration is least, for exam­
ple. under gaskets. st11ffing boxes etc., because formation of an ox_idc
tilm is not possible. This also occurs. under solid substances that may be
deposited o.n a metal surface as ready access. to oxygen is shielded.
'
{h-1<, CORROSION 443
corrosive products and other insoluble constituents of cast iron. When
ihe layer of graphite and corrosive products is impervious, corrosii>n will
cease or slow down. If the layer is porous, the corrosion wil! progress
by galvanic behaviour between graphite and iron.
Wli'L'll carbon steel is heated for. prolonged percods at temperatures
. higher than 455 °C. · carbon may get segregated, :which is then trans-.
formed into graphite. Hence, q1e stnictural strength of.steel is, affected.
Employing 'killed steel or low alloyed _st'ee,l s of'd�romium and molybde­
num or chromium and nickel can prevent this type of corrosion.
Dezincification : This type of corrosion is seen in brass that contains
more than 15'% zjnc. J n brass, the principal product of corrosion is
metallil' copper, which may redeposit o� the plant. · Another _mechanism
involws the formation of zinc corrosion\products ,leaving the t.op�r

Redesign/change in mechanic:al conditions must be, used to overcome

. residue. ..
Corrosion may occur as plug filling pits (plug type) or as continuous
this· situation. jayers surrounding the unaffected core of brass (general type). It can be
I �\'tlrogen �·111hri11/e111e111 I lydrogen can penetrate carbon steel ;md reduced hy the addition of small amount of arsenic, an!imony or phos-
reacts with carb'on tn form methane. The removal of carbon results in phorus to the alloy. '
Jern:ascd strength. Corrosion is rossihle 'at elevated temperatures as
Fluid Corrosion : Biological
significant hydrogen partial pressure is generated. This causes a loss of
ductility. (hydrogen embrittlemcnt) and failure by cracking or bliste1ing The metabolic action of microorganisms can cit.her' dir�ctl)·" r indi> o
of the steel. Resistance. to ihis typc of attack is improved by alloying � cctly cause deterioration of a metal. Such a process is called biological·
� chromium/molYbdcnuni.
with . . corrosi(/11. Microorganisms associated with corrosion are either aerobic
,,r anannbic. The causes for biolL)gical corrosion arc:
Hydrogen damage can also result from hydrogen gcnernh!d by . '
( i.J Producing corro�ive environmeht or,altering em:ironmentc1l com-
electrochemical corrosion reaction. The atomic hydrogen formed on the
position.
metal surface diffuses into the met.ii and forms molecular hydrogen at I < • '\,

micro-voids. The result is failure by c1nbrittlcmcnt, cracking and blister­ (�) Creating electrolytc-con(·cntration cells on the metal surface.
ing. This phenomen�1n is observed in solution of specific weak acids (3) !\ it<.:ring resistance to surface films. 1.
such as hydrogen sulphide anJ hydrocyanic acid. ( ,1) l 11 fluencing the r,1tc of anodic/qthodic reaction.
.
Fluid Corrosion : Structural Rl·ducing bacti:ria
Sulphates Hydrogen Calcium
In structural lluid corro5.ion type. the structural (mechanical) strength
Anaeropic
· s�lphitc f . sulphite
is reduced on account of corrosion. This may occur when one compo­
nent of the all�y is removed or released into the solution. The corrosion
products may remain in the plant. Two examples are presented here.
On iron

.......
Graphit,c corrosilin : Gr:iphitl! is an .illotropy of carbon. Graphite in soil
corrosion occurs in gray c:ist ·iron. The metallic iron is converted into
corrosive products leaving a residue of intact graphite mixed with iro11 Iron sulphide . ·
(corrosion product)
444 l'll/\R:-.1,\CEUTICAI. LN< ;1;,.;1TRIN(i Ch-I(, C<lllROSION, 445
The role of biological corrosion Ill.I)' be cxp!airn:d using ,111acrl)bic methods such as electroplating, cladding. organic coatings should be
sulphatc·rcducing bacteria in slightly acidic o.r alkaline soils. considered. The thickn�ss of the I inings is i1�portant ( I 00 mils).· Effec­
As these bacteria thrive under these conditions. they will continue lo . tive linings can .be ohtriir.cd by, bonding directly to substrate metal or
promote this reacdon �in�il failure of the pipe occurs. building. multiple layers or lami nation.
Organic .coatings are used as ·linings in equipment such as tanks.
PREVENTION A.ND CONTROL OF CORROSION piping. pumping lines and shipping .containers. Some examples of the
linings arc:
Selection of Proper Material
- Ceramic - Carbon brick - Plastic
Corrosion should not be permitted in fi ne mesh wire-screens. ori fices
and other items in which dimensions arc critical anJ changes arc not
-· Elastic - Glass-coated
.
··· ,Organic

permitted. A thin non-reinforced paint-like coating of less than 0.75 ·mm thick­
ness should not be used· in seryices for which full protection is required
In many cases, non-metalli c materials will be useful and attract i ve from corrosion. Some examples· of l inings and uses are:
from the point of view of economics and performance. These -.hou·ld be
consid\!rcd if their strength. tempcr;:iturc and design -;pecilic:11i,111s arc Tin coated steel (tin platcJ - food containers
satisfactory. Lead (P?) coating (Teme plate) - roofings
Permio;sible corrosion rates are important factors and d i tTcr with Aluminium (Al) coated steel - high temp conditions
equipment. Appreciable corrosion can be permitted for tanks and lines. Zinc (Zn) coated steel - many atmospheric conditi�ns
if antic.ipate<l a_ nd allowed for thickness in its design.
The corrosion characterist ics of chemicals and limitation� nf con­ The cladding (i.e., mechanical bonding) of steel with an_ alloy is
struction· materials must be considered from the li tcratu,·e before sckcting another approach to this problem. For instance, special glasses can be
equipmcn�. In addition, process i ng c onditions to which the 111a11.:rial is bonded .to steel so that the liner is of 1.5 mm thick which is impervious:
exposed should also be cons ic,kn.:d. For this purpos.;, relevant lit�raturc Equip1t1cnt and pipings are lined m this manner and routinely used in.
should b<.: consulted. severely corrosive acid services.

Proper Design of Equipment Altering Environment

In the design of equipment. a number of fi,ttings c;uch as baffles.
stiffeners. dra in nozzles, location of valv<.:s and pumps �11ould be . consid ­
ered.' Corrosion can be minimised, if the equi1.ment des ign fac.:ilitatcs: ·
- E.lirnination of crevices·
Complete drainage ·of liquids
Ease of cleaning
Corrosion can be combated or reduced by employing the following
. enyironmcntal conditio ns.
( 1) Removing air from boiler feed water prevents the influence of
· water on steel.
(2) Reducing aeration prevents the fonnation of passive oxide film
in stainless steel all.oys by acidic media.

Ease of inspection and maintenance (3) Pumping of inert gas into s�lutions' prevents the contact of air or.
A dircct contact between two metals should be avoided. if they an: oxygen as in case of nickel based alloys.
separated widely in the elec trochemical series. Otherwis.e . they ,hould (4) · Reducing the temperature.
be �1subted. Equipment should be suppo11cd in such a way tll,1t it will · (5) ';liminating the moisture.
not r<.:st in pools of liquid or on damp insulating mate rial. " .,. ((1) l{('ducin g the vclocit)'. or turbulence.
Coatings and Linings (7) Shorteni ng the time. of exposure.
Nonmetallic coatings ,1nd lini ngs can be applied on steel and other . Addit;on of acid media should· be done as a' last SiCP, so that
materials of c9nstruction 111 order to comhat corrosion. Approp riate maximum diluti on can be obtained .
446 Pl IARMACEUTICAI. l:N(il�U:RING

Inhibitors Ch-16 CORROSION 447

The corrosio� inhibitors arc added to the environment lo Jccn:ase
corrosion or metals. These form ptotedive films·.
Adsorption type; for example. adsorbed on the metal.
�cavcngcr type, for cxamplc, n:movc corro-.ion agents.
Vapour phase type, for example, sublime and condense on metal
. c: surface.
Examples of inhibitors arc given below.
. Sacrificial anode inethod ·: In· this me.thod, anodes arc kept in
clcl'.trical contact with the meta� ft�l be protected (cathode). The anodes
arc sacrificed, sin,r;.c'it goes into sofution (Figure 16-4). For example. for
the protection of iron and steel tanks. the metals such as. zinc, alu­
minium. magnesium and thei� allpys arc used as ,'sacriti�ial ,'.�nodes.
These are used in limited pH range when high, solution r�te is ,accept­
abk, since .these arc amphoteric.

/nhibiturs Material protect((d in the 111c:dia Anode metal· is selected from the electrochemical series amongst the
inetals present below the tank metal. . The anode should not be poison­
Chromat\!s, phosphates, silicates - iron and steel in aqueous solution. ous and not detrimental to the product.
Organic sulphides, amines -- iron and steel in acidic medium.
Impressed emf Method : This is also known as appliecf. current
Copper sulphate - stainless steel in hot diluted :,ysrem; i.e .. external voltage is impressed between rank and electrodes.
solution of sulpt1uric acid , The negative termina't' of power supply is connected to the material to be
protected. Therefore, the nat�ral galvanic effect is avoid��-and the
Inhibitors are generally used in quantities less .than 0.1 % by weight. anode· is maintained positive (Figure 16-5).
In some cases, the amount of inhibitor used is critical.
Cathode +
Ca.thodic Protection (no corrosion}
The cathodic protection is based on the galvanic action between the
+--

metc;1l(s) of the. plant. (cathode) and anode suspended in the solution. The
metal to be protected is made a cathode, i.e., electrons are supplied, there • Earth
by dissolution of metal is suppressed·. T.his can be achieved by two
methods.
: +-- Metal i:ontainer
(I) Sacriticial anode method·
Electrolytic to be pr�tected
(7) Impressed emf method solution
Anode
Sacrificial
anodes
Figure 16-5. lmprcssccJ currcnt cathode protccti?n. 1' •

-ve cathode _ Since anode. is not 'consumed, any conducting material, metal or non-·
(no corrosion) corrodable alloys can be used. For example, in case of sulphuric acid
�nJ ·deionfsed water. graphit� and high silicon steel are compressed. The
Metal container
to be protected .
anodes can be buried in the ground or suspended in the aqueous solution
of electrolyte. . · . .. ,.·
Advantages : (I) This method is used tor largc· tanks to store mild
corrosive liquors. In tht!se cases, mild steel i:; used with' negligi-
blc corrosion. · . ,
.,
\
Electrolytic solution (2) Cathodic protection method is si.mple and the most effective.
(.3) It is inexpensive. It enables the.use of cheaper material for pla.nt
Figure 16-4. Simple sacrificial an,1,h:s. construction. \
448 l'l l1\R1'1ACUJTIC'/II. ENUl:-;ITRIN(i Ch-16 CORROSION 449

Disadvantage : Corrosion cannot be reduced to zero. Each question carries 5 marks

I. What is corrosion? Mention the factors that influence rate of corrosion.
Anodic 'Protection 2. Explain measures you suggest to check the problems of corrosion..
In the method, a predetermined potential is applied to the metal 3. Write electrochemical theory of corrosion.
specimen and the corresponding current changes arc observed. During 4. Describe the biological corrosion and suggest the preventive me;::surl!s.
the ,initial stage. the current increases indicating the dissolution (corro­
sion) of the metal. When the current reaches a critical point, passivisation 5. Describe the mechanism of corrosion of iron.
occurs, i.e., the oxide layer sets in a suitable oxidising environment. The 6. Define corrosion. Give its causes. ·classify corrosion.
potential at critical point is called passivali11g pote111ial. Abov� this
Each question carries 10 marks
passivating potential, the current flow decreases to a very small value
I. · What is corrosion? Name the various types of corrosion. How can
called passivating current.
corrosion be prevented?
..The passivaling currenl is defined as the minimum protective current 2. Discuss various types of corro.sion and suggest the methods to tackle the
density required to maintain passivisation. same in pharmaceutical industries.
At this staie, an increase in potential will not corrode the metal since
the latter is in a highly passive. state. For example, in case of stainless
steel, titaniuf11 becomes easily passive and cannot offer cathodic protec­
tion. In such cases, the corrosion rate may be slowed down by the �1se
of anodic current.
. Advantage: Anodic protection requires a small current. The anodic
.::protection method is utilised in the transportation of conc�ntratcd sul-
phuric acid. � ..,

Disadvantages: (I) Corrosion cannot pc reduced to zero.

(2) This method cannot be applied for·metals. which do not passivate.
A proper mate.rial should be selected for a specific process ba�cd on
the literature and by personal experience. The factors influencing rnrro­
sion will not only help in selecting the right kind of material, but also
suggest the processing conditions. It is equally essential to identify the
type of corrosion, if it occurs. Since the theories of corrosion arc
known. it is possible to adopt appropriate preventive measures.

QUESTION BANK
Each question carries 2 marks
I. Explain the terms· pilling co1Tos?on· and ·gahunic wrrosion'.
2. Give the applirntions or prokctive linings :ind co;itings "ith rc�pl·ct to
corrosion control with suitahle cxampks.
3. What is the role l�f plastic \\ a\h,:r�= in tlw corrosion of ml't.ils?
4. How oxide tilms ar.: f1)rn1<·i1" \\'li;11 ;:r� its ;id, ;mtagcs?
5. l lighlight the rok of o:,.:ygcn in th-: rnrrnsion of metals'
(
 Ch-17 �1/\TUU i\LS OF CONS rn.tTI 10'.': 451,
4. Resistance to thl.'nnal shock i.e., operati11g.,tc111pcratur.c ,·.
5. Ease of fabrication
'6. Cost
· 17 7. Mai nten:ince
Selccting satisfactory materials forthc construction of pbnt cncoun­
_tcrs pr,1blems involving chemical. phys:ca+ a.nd economic factors.··
Materials of Construction
FACTORS-,INFLlJENCl:\(; SELECTION OF l\:lATERIALS
Chemical Factors
.Factors Influencing the Selection of Materials n,�· container or equipm�·nt should protect th\.- integrity \Ir the con-:
Chissification of Materials for Plant Construction
Ferrous Metals . tent:,. ,\l the sa111e time. the nmtents should not altq the .pwpi.:rtics of
Nor,-Ferrous· Metals the mateiial \\ith \\hich the vc:..sel is mad�. When' these arc in c.ontact . ..
Non metals-Inorganic \\it ii c:1c h Ol her. the effects 111:11
. . h:
. undcrstOild i11 t\\'O
. \\'a\',·
- .. .
Nr;nmetals-Organic
(a) Thc contl.'nts 111ay n:act arid thus gct co11taminakd with .the.
material of the plant.
A numbl·r or equipm�nt arc us<..:d i;1 thl.'. manufacture or pharmaceutiv�,k.
(�) The drugs and chcrnicab may destroy the 1 :1aicrial of".the plant.
bulk Jrul!-,. antibiotics. biuiogical pruducts etc. In addition. sc, e r.ii
acccssori� <- such. as c:untaim:rs for pniccssing and packing of tini,h1.·d Cootaminatio,r of the product : The impurities in. chemical sub­
products. ar1.· css1.·ntial. t\ witk ,:iriety or materials can be utilised 101 the s'tancc:; ur bulk drugs may be fr\lm different sources. The soh-cnt action
.
construction of equipment. Tl1e \ucccss or failure of a new cht..:1111cal !Tia) cause. coi-rosion, so that tli1... \raees of metal ions used in construction
plant or in the impro,·emcnt of an cxi:,.ting facility depends on: tend to pass i'11to solution and contamin:ite the product. Sub!.-t::rnccs such
as gl,1s�. silica, !..:ad. cast iron. :,l\:t..:l. tinned iron and a varictv of allovs
0

. / 1. Dc�ign of equipme11t
I Selection of matt..:rial arc used in the construction of a chi.:mical plant and 1110�1 of the.m ·
3. Technique or fabrication proJucc contamit}ation.
i11
The 1.ksi!.!n (construction) and ,,·c,rking of equipment emp oyed Even though impurities arc present in traces, these ma\· <;ause the
l
rs. ' i hc
u�it operati;ns have been discussed vividly in various chapte product to decompose. for example, heavy metals inactivat� penicillin.
g the
knowledge on the properties of mar..:riab. is t:,ssenti:il for. 'selectin The appearance of the pr?duct may also be effected by ch;rnges. in
. right .kind of materials. colour. Glass vcsseLs may, give up traces of alkal.i to the .�olvcnt, though
vkd:,! 1.' un this is unlikely. if the vessels are of hard glass .. Sometimes, roduct . .
' The purpose of this chapter is to prnvlde a ,,·orkin:," kno\. c0nta111111ation may be innocuous and non-toxic.
1ct11.111. 1 l1h
some or the major types of materials available for n111,1n
Ii :i\,.l·· lntlucnce of chemicals on'the material of the pl:rnt: lhe solutions·
will detenninli' whether a process is e:q)cnsi\c or t:Plll\'k\.
cal J.: t:1il� ,·,1
decitks th<..: p1'oti( anJ utility of th� rnd product. The tcdrni . that come into contact w'ith thc equipment arc generally corrosive in
th,: fabrit: ation an: not within t\ic ;;cup<..: of this chaptt: r. bl.'c1u s1.· 11 n,·,�,h. n:iturc. In· addition, equipmcnt are exposed to .extremes of pH,
tempera�·
sp1•cial expt:rtise. which ·may not be relevant.
.. tur<..:s and pressures. As a rc:,,ult, the material gets corroded. losing its
. strength and durability. Therefore; the life of the equipment is reduced.
'

ion of a ·m:iter ial tor the constr uction of eq �iprnen t depcnJs

Tht: sl!kct • • 1 • !,

0n the following properties. The knowledge of m::iterials of �\ant cons. trnction ass.ists great!� i.�.
I. Chemical' resistance providing a plant that will be;resist:int. to . atta..ck of. acids,. alkalis.. oxidiz-·
. . .•

2. Structural stn:ngth ing agents, tannins etc. New alloys having special phys\ca\ apd chemic�!.
3. Resistance to physical shock i.e .. operating pre ssu
re

450

452 PHARMACEUTICAL ENGINEERING
properties have, been developed to meet the problems of chemical
reactions,
Physical Factors
Strength : The material should have sufficient strength so that it can
withstand the stresses or rigours to which the material is subjected in the '
production. Iron and stainless steel can satisfy these properties. For
example, in the compression of tablets, the dies and punches should have_
sufficient mechanical strength to transmit the applied pressure, otherwise
tablets are poorly formed. Glass satisfies the property ofstrength, but is
.
breakable.
Generally tablets. capsules and vials are preserved in blister packing.
The packing materials should withstand the rigors of handling, shipment
and transportation: Plastic materials are used, because these offer suffi-
cient mechanical strength.
J\erosol containers must withstand pressure as high as 960 kPa to
1.20 MPa at 55 °C. Tin plate containers can satisfy this condition. while
plastic c�ntainers canno"t be used due t9 its poor m"echanical strength.
l\1a�s : Many times, the equipment should be transported or m_oved
fro� one place to another. This is possible when the material is light in
weight, when oti1er factors are satisfacto,ry. · Similarly, plastic material_ is
em.ployed for the manufacture of containers for use of pharmaceuticals
and cosmetics on account of its light weight. As a result the cost of
transportation reduces.
' 1 . . •
,vca·r properties : These properties become important. when there is
a possibility of friction between the moving parts. For example, during
milling and grinding, the grinding surfaces wear off and these materials
will be incorporated into powder as impurities. Such type of mills
should be avoided, when drugs of high purity are required. The risk of.
contamination is more due to wear of ceramic or iron equipment (sieves
etc.) ..
1::: During tabletting operations, the upper and lower punches rotate
continuously. In this process, the wearing of these punches is high.. .,
" FOR PLANT CONSTRUCTION :J
Thermal conductivity : ln chemical industries, several equipment
such as evaporators,· dryers, stills and heat exchangers are used. The
. material employed for their fabrication should have good th.ermal con­
dtiGtivity. However, the resistant films greatly retard the process of heat
transfer. For example, iron, glass or graphite tubes are used in the
fabrication o( heat exchangers, so that effective heat t:ans fer is possible.
Ch-17 MATERIALS OF CONSTRUCTION 453
. Thermal expansion : If the material has high co'!fficient of expan­
sion, the design of plants may be greatly complicated. This increases.
stresses and the risk of fracture when temperature changes. The materiaJ.
should be able to maintain siz_e and. shape of equipment· at working
temperatures.
Ease of fabrication : During fabrication, the materials undergo
var:ous processes such as casting, welding, forgin& and machinisation
.etc. For example, glass and plastics can be easily moulded into contain­
ers of different shapes and sizes. Glass can be used as a lining material
for reaction vessels· used in the chemical industry. Iron and steel
undergo various rigours of processing· during fabrication.
Cleansing : Smooth and polished surfaces allow the process of
cleansing easy. Materials that can be obtained �vith such a finishing are ·
ideal. when �crup�lous cleanliness is necessary. For example, stainless
steel and glass arc suitable for this purpose.
Sterilisation : In the production of parentcrals, ophthalmic products,
antibiotics and biologicals, sterilisation is an essential step, \,:hich is
obtained by autoclaving. The material should be capable of withstand­
ing the 1kccssary treatment, usually steam and pressure .. In most ,;:ases,
cleansing is a preliminary step to the sterilisation of apparatus ar.d plant.
For exaniple, equipment anµ vessels are made of stainless steel. because
they can be.sterilised.
Transparcnc}· : Transparency may be a useful property because it
permits the visual observation of the changes during a process.· For this
reason, borosilicate glass has been increasingly used in the construction
of reactors, fermentors etc.
Economic factors : Initial costs and maintenance of the plant must
be economical. Here the main concern is not simply to obtain the least
cost material. Low wearing qualities and lower maintenance may·well
mean that a higher initial cost ts more e�onomital in the long run.
CLASSIFICATION OF MATERIA,LS
Materials of pharmaceutic�! pla1:1t construction ·can be classified as
shown in Figure 17° I.
Different' materials and their properties are discussed so that !ight
kind of materials can be selecte-u· :;or the desired purpose and, function.
1

454 !'I IAR\1ACTlJTIC /\I. ENGINl:l:RINCi
FERROUS METALS
Iron met:il is one of the widely used materials for the construction of
plants. because· of its mechanical strength. abundant availability and
·lower cost. Some varieties of iron arc discu5sed.
CAST IRON
C�s't iron consists of iron with a proportion of carbon (beyond 1.5%).
Th�' propcrtie:s of iron depend on the amount .of carbon present in it.
Cast iron is abundantly available. inexpensive a1�d therefore widely used.
A number of types :O_f cast iron are available (Table 17-1 ).
Materials of construction
I
('li-17 Mt\TI-:IU/\1.S OF CONSTRUCTION
(2) Casi ii·on is attacked by dilute sulphuric acid, dilul 1 nhrl d
and dilute as well as concentrated hydrochloric -acid.
(3) Since cast iron has low thermal c.:onductivity, it cannot be u d
for he:it transfer in stills.
Uses : It is com111only used for the coristruction of:
(I) Supports for plant
(2) Jackets of steam pans
(3) Linings with enamel. plastic or suitable protective 1natcrial
M.odilications of cast iron : Cast iron is not considered corrosion.·
1:c�i�t:1111. The characteristics of cast iron can be altered by alloying with ..
uthcr clements such as silicon, nickel :md chromium. (sec Tab!� 17-1)
Co 111 mc rcia I Types : Duriron and Durichlor.

,- _______ ___
Metals No'i1-metals
TABLE 17-1
[_, __, Different Types of Cast Iron Alloys
Non-Ferrous
r----+--·_· ---,
. Ferrous·'
Tip<'.1 of Co111positio11 Disc..1Jva111agcs
CU.\ I iro11
Cast Stc·�I Stainless
iron cart.Jon steel (iru1 C,l'.,t , CMbon I .011· cosl. ,:asy to cast 13riIlk. rnor
1rPn si licPn into.intricJte sh.ires and resi:,'itam:c to in:r,11.:t
Aluminium Lead
. li11i1�gs. h,r grinding anJ shock
halb. Jjl'S.· il]lf)t.:lkrS.

Inorganic Organic \-la!..:,dilc i<hitc: c;1st irnn Corr.nsion n:sistunt . Ty re11 less i.:Js: lv
. glass i r, 11·1 carbvn·-:2.5% Tyr..:1} \1S) to machine machine
----i n::
Rubber Plastics I ligh Silictii\- Ri.:sistanl t,, corrosion, Not casil) m:khined
'.;ili((lll 1.3-1 <,''l,, o.\idising c111 ironment. and welded
Fi�u re 17-1. Classificati'ln, l'f materials .c;1,t ir1111 c:1st iron ri.:ducin� cn, iron merit.
us..:d for the construction oi· rbnt. lls..:d i� sulrhuric acid
s..:1Yic..:s.
A'dvantagt·s: (I) C::ist iron is cheap. Therefore. it is used in pl::ice or
. e,p�·nsi\'l: pbnt material with cc,atings or linings of en::irnel or Nicf;c·I s1,p..:ri,1r tlni°ghness, (hidisin;; agcn:s
rc'Sl\ta:11 imr,1cl rc:si�tJnt. eJs:, to such us nitric acid
pb�tic.'
L.1··a in1n 11i.:IJ .rnd- machinj!. an.: highly detrimental.
t2) 1t i,; n.:sist:111t to concentrated �1dphuric 2c;id. nitric :1cid ,rnd C.:orrn�i11n rcsistJnt and . There is little ;mack
dilute alkalis. ... he.it rc:sistant. froin 1:i.:utral or
(3) Since cast .iron has low thenrnl conductivity. it .is used for the :,lkalin..: solution
con,trnction nf outer surface of jackets of steam par\<;.
CAH.130:\ STEEL OR MILO STEEL
Disad\'antagcs: (I) Cast- iron is \'Cry hard and brittle. 'therefore. it Carbon' st�cl .is an iron allo�, ·which contain� only a smal-1,percentage
is dirticult to machine. This di,;arlvantagc can be overcome by or carbon.. AdY:rntagcs of ca�bon steel arc:
the 'addition of' different material<; to i111provc its performance.
456 · PIIARMI\CEUTlCAL ENGINEERING Ch-17 MATERIALS 01' CONC:TRUCTIO'J 457
( 1) Carbon steel is cheapest. Therefore. it is preferred. STAINLESS STEEL
· (2) It is easily weldable and is frequently used in fahrication. Stainless steel is an alloy of imn. Usually, it contains chro1nium and
Disadvantages of carbon steel are: nickel, which make the steel corrosion resistant. StolnleSs steel is
'{I) Carbon steel has limited resistance to corrosion. This property stabilised by the addition of titanium, niobium or tantalum. Minor
can be improved by preparing alloys. · amounts of other elements such as copp�r, rr{�lybdenum and selenium
arc added. Stainless steel also .has the
. ·advantage of ease in fabrication.
(2) lt reacts with caustic soda, brine and sea-water. Alloying it can . -s:>

reduce this reactivity. The abundant use of stainless steel is due to the properties such as:
heat resistance
Uses : Carbon steel is used for the construction of bars, pipes and - corrosion resistance
.
plates.. lt is used to fabricate large storage tanks for water. sulphuric
case of fabrication
acid. organic solvents etc. It is used for supporting st�ucturcs such as · cleaning and sterilisation
gi'indcrs and bases for plant vessels.
- tcnsi le strength
Variants of carbon steel : The properties of carbon steel tan, be
altered by alloying it with other· metals.· Some of the· metals and their Depending on the composition. stainless steel alloys arc available in.•
properties are: three groups . viz., ma11ensitic. fcrritic and austenitic. These arc given in
'
Nickel (Ni) - improves toughness, corrosion resistance and .low tcm­ Table 17-3.
peratu re properties. TABLE 17-3
·chromium (Cr) - increases hardness. more abrasive resistance and · Different Types of Stainless Steel
resistance to oxidation. Co111posit ion A clrnntagcs . . Disad­ Uses
.
Si'licon (Si).- increases hardness, more abrasive resistance and resist­ vantages
ance to oxidation.
'\lar:tcnsitic (c.g: Type �10)
Molybdenum (Mb) -- provides strength at elevated temperatures
Chr0 . 111iu.n: 12-20'�0 .l'vlildly corrosion Ductilit;, Sinks. hc nch tops.
The .ypes of alloys of carbon steel arc given iii- T:iblc 17-2. Carho11 : 0.:2- 0.4%, resistant. 1s poor storage tanks.
Nickk upto 2.0% atmospheric and buckets. mixing
TAl,3LE 17-2 clements etc.
organic exposures
Different Types and Alloys of Carbon Steel
Fcrritic (et-form) (c.g: Type �JO)
Variety of Composition Advantages Cl)ro111ium : 15-30% Belter corrosion not good Tower linings.
carbon steel Carbon :' 0. 1 °/o resistant: easy to against bafnes. separator.
Low alloy !Low concentration - High mechanical-strength Nickel : nil machine: resistant reducing tower.; heat
steel of iron. carhon, - (\1rrosions resistant to to oxidation and· agents. . exchangcr. tubings.
manganese, nickel. environments. tc1riperaturc. hydrochloric condensers.
,chromium and - Walls or rlant can he thin. (urto 800° C) acid furnacc parts.
molyhdcnum pumps shafts.
valve parts.
Alloying. nickel ". - Increased hardness
with nickel - High corrosion resistance Austcnitic (y-form)
- Improved low' temperature Chromium : 13-20% Highly corrosion Not easy Fermcntors. storage
properties. Nickel : 6-22 % resistant: readily to machine . vessds. evaporators.
- Ahra.sion rcsista�t Carbon : cleaned; steriliz­ . extrnetion vessels.
Alloying with nickel
- Corrosion resistant ()_ 1 °/o < 0.25% ahlc: easy to weld; sm�II apparatus ,
silicon. chromium
chron1ium - Resistant to oxidation 11on-m;1g11ctic ( l'tmncls. huckt:!s etc.)
) ..
Pl IAllMACElfflC/\1. ENCiINEERlNCi
458
NON-FERROUS METALS
ALUMINIUM
A number of aluminium items are used 1n regular day to day life.
Aluminium is cheap, light in \Veight and offers adequate mechanical
strength. In addition, aluminium equipment can be easily fabricated.
Further, aluminium can be strengthened by cold working. Their mainte- ·
nance and cleaning is also easy. Hence, its utility is mostly recommended.
However, the use of aluminium 111 the construction of p-lant and equip-
1
mt.'1t is Limited.
Advantages : (I) l-ligh resistance to atmospheric conditions. indus­
tri:11 fumes. v;:ipour and fresh or salt :vaters. Aluminium can be
used with concentrated nitric ;:icid (above 82�10) and acetic acid.
(2) Thermal conductivity of aluminium is 60% that of pure copper.
Disadvantages : (I) The mechanical strength decreases greatly above
150°C.
(2) ·Aluminium cannot be used \Vith strong �austic soluti0n.
(3) Many mineral acids attack aluminium.
(-l) Oxide and hydro-oxide films arc formed rapidly, when its surL1cc
is exposed. Normally this tilm is thickcn�d- by chemical a11d
electrolytic means. These provid� so called anodised finishes.
Uses : A !-Upcr grndt.: is preferred for food and phannact.:utical use. It
1s used in many hc!at transfer applications. These arc used ns meat
storage containers.
Aluminium alloys and modifications : A number of .aluminium
· alloys arc available with improved qualities -and !Pcchanical propc11ics.
Afuminiurn_alloys arc usc_d in .the constructi.on of equipment 'producing
medicinal sl!bstanccs. ',sin�e aluminium docs' not affect the salts.
Aluminium is non-toxic to microorganisms. It has considcr:1blc use
in bio�'nthetic processes such as the production of citric acid gluconic
acid and streptomycin by deep culture methods. It is most (1scful for the
construction 9f containers namely drnms. barrels. rail t:rnkers etc.
LEAD
Lead has the lowest cost and is used as collapsible tube material
particularly for non-food products such as adhesi\ cs. inks. paints· and
lubricants. Lead tubes with _internal linings :ire sometimes used for
fluoride tooth-paste. I.cad chamber process is used in the m;:inufacture
of sulphuric acid.
45q�
Ch-17 :'\1/\TFIUAI. '- OF C:0:S.:STRl!CTIO:-J
Disadv:inta;�cs: (I) Lead has low melting roint ancrhcnce pl)Ssesses
poor structural qualities..
. .
(2) li has high coefficient of expansion. Therefore, temperature
strain results in permanent deformation.
In pharmaceutical practice, lead ·has little use. because of the risk of
contamination even in traces produces toxicity and of cumulative nature.
It is used for the construction of cold water pipes, waste pipes and
dilt1iion tanks for laboratories.·
Lead alloys and modifications.: Lead alloys with superior pcrform­
ann: ou.il.itics ha\'e hecn establi.<;hed. For example. :icid k:id :ind copper
k:1d ;1rl· used in chl·micil industric�. Some 111ct:1ls :1r.: :1dckd 10 kad l0r
:1lt.:ri11g J)ro11crtics_.
Silver :111d c0ppcr ··· improves corrosion resistance.
. . . mcc.
improves crccp and ,·:it1gue n:s1st::
Antimony. tin. arsenic·· hardens. still melting point is low.
l.ead-lincd steel structures arc used for the construction of pipes.
\ a Ives. vessels designed for operations at high temperatures. lluctuating
krnpl·raturcs or \·acuum.
NO;\i!\l[TALS-INORGANIC
(; LASS
!\ lllll.llbcr or !.!1:iss anicks arc used in Jail\' !if�. (ibs-; has the .
:1tl\-antages 01· sup;rior protecti\ c qu;:ilitics. attral:ti\'enes:; and low co'st.
IL is chc111ically inert to a large c\tcnt and available ;n a· v:iricty of sizes.
sh;1pt:s and colours. Glass c0nuincrs pr:ictic;:illy offer excellent barrier.
:it1 :1inst every clement except light. UV rays ::::id sunligiH arc harmful to
ct:rt:1 in ingrcdients and bring about chc:11ica 1 Jcteriorat inn. Protective
act ion against I ight can he achieved by ambcr-·col0urcd gb,s. Piotect ion
:1�ai11st IR rays can he obt:tined b) using green glass. Tl1t� disaJY:rnt:igcs
:ire its fr:1gility a11J \\eight.
.,.
lilass is 1.:onsidcred as :1 supl·r-coolccl liquid. though i1 i-; seen in solid
state. ll1c constitut:nts arc 1m·scnt in amorphous state. (ilass is "tom­
posed nr tilt.: lollo\\ ing constituents.
Sand
, ..,,·
- si Iica pure (si I icon dioxide, Si02) - qase material
'·
So�la <1sh - sodium cmbonatc (Na 2_C03) - improves the propertie,s
. l .irnc stnnc - ct1lcium carbonate (CaCO :,) - imrro\'C'- 'the propcrties
C11lkt - hroh.cn glass ,;":;· - fusion a·gcnt
 160 PHARMACEUTICAL ENGINEEB.IN G
,, Ch-17 MATERIALS OF CONSTRUCTION 461
Silicon dioxide is having a tetrahedron structure. The glass that is
(a) Oxides leach into the solution. raises the pH. hydrolyse or
prepared by silicon dioxide alone is the most' resistant. but relatively
catalyse ,chemical reactions.
brittle. It can be melted and moulded at high tt:mperatures. Therefore,
cations such as sodium, potassium, calcium, magnesium, aluminium, (b) Some times, glass flakes arc formed in the solution.
.
boron, iron etc., arc added. These cations (available as oxides) modify However, boron oxide enters into the structural configuration of glass
the physicochemical properties of glass, so that it is suitable for the and docs not leach out and hence is used in parenteral packiri gs.
manufacture of glass with desired characteristics: However, this glass
has low chemical resistance. Some varieties of glasses are given in TABLE 17-5
'.fable 17-4. Types of Glass used in Pharmaceutical Industry IP
TA13L.E 17-4 Types General Properties Uses
Some Varieties of Glasses description
Type of g/u,ss Composition Advantages or uses Highly resistant Resistant to alkali Cont ainers for buffered
Borosilicate leaching, less brittle. and unb'uffen:d, aqucot1s
Soft gbss Sodium silicate W!aking glass bulbs aml window glasses (Alkali and earth low thermal e:-.pansion solutior:s and. injectables
(soda glass) Calcium silicate cations arc re- easy to clean and
I lard glass Potassium silicate Glass apparatus, which resists the placed by boron) sterilise.
(potash glass) Calcium silicate action of acids II Trc:itcd soda-lime Surface alkali is ncutra· Containers for bufkred,
Flint glass Potassium silicate Optical instrument because of.it5 glass . !iscd by sulphur dioxide aqueous rnlution with
(Potash lead Lead silicate·' rcfi:activc indc:-. vapours. Glass surface pH bclO\'". 7.0, dry
.(
glass) is resistant to wafer. '}'" powders. olcogenous
.kna g!Jss Zinc silic.ite Laborutory glass\\'ar.:, because of its solutions.
""""
Barium horosilicate resistance to acids and alkali Ill Soda-lirnc glass It releases compara.tivcly Dr)' powders, olcogcnous
Pyre:-; glass Silicon dioxide Lahora10ry glass\\'are and reactor vessels, more alkali. It o ITers solLIJions.
..,
'13oron oxide because of its resistance to heat mo�erate hydrolytic
Sodium oxi.de resistance.
I Small amounts of IV Gencral purpose Not for parentcrals, used
potassium calcium soda limc glass as containers for tablets,
magnesium tj 11(� oral solutions, suspcn-
. Quartz glass Pure silica Silica crucibl.cs, distilled water stills sions, ointments and
(for high purity), because of its IO\\. liquids for ex\ernal use.
coeflicicnt of expansion. It withstands
temperature sh0Gk uptq I 000° C.
GLASSED STEEL
Glass containers used for pharmaceutical purposes arc given in Table Glassed steel is an inorganic product of fusion, Which·is cooled to a
17-5. These types are classified' into four groups. These have varied rigid co.ndition without.crystallising. It requires spec ial considerations in
degree of chemicml resistance. The reasons for the low chemical resist­ its design and use. These surfaces are applied to heavy vessels: Nor­
ance arc a$ follows. Most of the alkali oxides such as Na20, K20, MgO mally, several coatings arc fused in a furnace. Glassed steel combines
• the corrosion resistance of glass with the working strength of steel.
and CaO enter the spaces within the structures and reduce the strength of
inter-atomic forces between silicon and oxygen. The oxides decrease the Advantagrs of glassed steel are:
melting point of glass and are comparatively free to migrate. This (I) lt has excellent resistance to all acids except hydrofluoric acid
behaviour creates a number of problcrns in their use. These arc:_
� :111d hot concentrated sulphuric acid.,
0 . "'
 1'1 IARMACUJTICJ\L LNGINU:RINU Ch-17 MATERIALS OF CONSTRUCTtON

(.:) It. ,· .. u1 li.:. attacked by ho.t.alkalille solution. P.articu!arly suitable p!1><.:<.::,S is called l'llll'lllliSlllio11. Soft rubber with 25 :/0 ur mon'.' ulpl1ur,
t� 1 piping when transparency is desirable ..
1 is kno,vn as hord ruhher. l l ard rubber ·has the advantages of h rdn
and str�noth. So it is used for making gloves, barids, t'ubes 'and stopp
(, I i't i, hri tt k and �ets. damaged by thermal sJ10ck. Hence it is .::>
• . . •· : • : ,,,

p11>h:\.'kJ using glass lined with epoxy polyester fibre glass. Synthetic Rubber : Synthetic rubber has taken greater importa CC
(·l) A· nit-:k,1tcd crystallised ceramic m�tal composite form of glass over natural rubber due to .its superiority in properties such as reslstaracc
h:1, �_up�rior mechanical properties compared with conventional to oxidation. solvents. oils and ·other chemicals. Some synthetic: rub bcr
� h,,,,·d skcl. materials with their properties are reported in�able 17-6.·
(" l i ,L1,, linings arc resistant to: T,\BLE 17-(, ·.
(;i l A II rnnccntrations of hydrodlloric acids upto l 2CJ'0 C.
(I•> I >il11te conccntr:itions of sulphuric acid up to the hoiling, ---------------------.'-
Smt/;.:tic l'1u11crt ic s .''
--�----��·,
Some Varieties of Rubber.
>
I 111 i 111.
I,. I \I! concentr:11i1·11h of nitric acid upto boiling point. rnhher ·- ------------'--'-----
(,:,1 .\,id resistant �lass with improved alkali resist;mce (up to . I. Nc\\rrcnc • Diles nnt bu1:n rcaJi ly lnsul.iting material in electric'
r,11 12). ([)tll) i.:hlun•- like 11atur,d r�Jlibfr.· cablcs:· conve) or belts in coa I
prcne) .,.: 'Stabk al high ' mines. making hoses in the
l Sl·, : ( , ,;,., lined ste1:l is used for handling of stronf.! :icids. alk.ilis
1
tcmpcratur.: .. transportation of oils. fZ. ubber
,,nd �:il111: ,,·!,ai(1ns. ,· For s.mall-scalc rna1�11facture and pilot plant work. st;ppcrs, cap-liner�. aropper
gla��1.·d �t,·,·I , �·ssels :m:. used. assemblies, for
eye_ JropS etc.
2 :-.:iirik • Rcsist:1nl W ui I' anJ
NO:'\;\lETALS-ORGANIC ruhhcr ""h ,·nh.
I{ l' B BF.H .,. l\11l� I rubber • RcsislJnl tu t:s,·d for dosurcs or freeze JrieJ
111i11cT:1l ai.:ids & :rlblis rmd11ct C(1ntaincrs b�c:iUSC of its
R.11bb,·1 1, ust•d a:, such tlr as linin!.!� rnakrials l�)r the c,1:1struc:;on (If lo" ·" atcr , apnur rcrm�abili l>.
I . i.:011ccntr.itcJ .iciJs
pla11h., lL,1:1 11:.tm:11 and synthetic rubbers are useJ. ( c.,i.:epl 11 itrii.: a11J
;\',1tural Rubhl·r: Rubber is a naturally occurring pol ) mer. \\hich ,� s11lph11ric acid l
obtain1:d a.,, b1e, from rubber trees. 'lt is a common c,arnple of an -1. Sil:-:on , IZL·sist:mt tn
elastomer. Ela.1tu1111:r is a substatYcc t!1J.t can be stretched readily and ruhh(·r ([)\lly- high & Im\' tcmrerat(1rcs.
wlwn r�·k:1,;d. rapidly reg:iins its origin::il fo:111. attad; to aliphatic
' ' soln:111s. oils anJ greases
Soft Rubber : Th(.' naturally occurring. polymer is known as soft

____________�-
5. l\1lyisorrenc • Stable at high temperature..
rubb�'I.' .. It is a pol) 111er uf 11101101111:!ric isoprcnc (C5H 1, ). f hus, rubber is
a 1wl:- i�11pr�·11c "ith a i'1m11ula (C5l l :,i ) 11 . Soll rubber ha� the advantagcs --�-··-. ________
. .
1r.111slui.:cnt. lk,ih,ik.
_:__..:.;_

or t, ...i,:.:2 1.:,i;,1,1J1t tn dilute mineral aciJs. dilute alkalis and salts. The
d1s.1J\ anl:lt.!C is that soli rubber can be attacked by oxidising media, oib
·anJ {nganit solvents. Soft rubber is used as lining matcri:ils for plants.
a:, 1t 1.:a11 btlJH.I ca:,ily to the steel.
Addition 01' carbon black to the soft rubber gives hardened rubber. It
is used for making. tyres. tubes and conveyor belts.
·i::
Hard Rubber : When soft' rubber is mixed with sulphur. \\\1f'l'>leci
and set into a gi\'en shape .. it retains its form. The sulphur combines
\\'ith the polymeric chains of rubber and cross-links between them. Tlti�
S: 111hctil· · 1 ubbL·r is thermoplastic. but \\hen 111(:-;ed with sulph11r.
":1r111cd a11d Sc'! i11to a gi,·c11 shape. it re.t a ins· its form. V11lcmii::otio11 of
rubber is p1Jssibk. It i'., used for making glo\es. bands and tubes. caps
for vials.
Rubber 1s a soft material. but can be hardened by· adding carbon
black.· H:1rck11ed rubber is used for making tubes. tyr�s and coi1veyor
belts.
, ..
 464 PHARMACEUTICAL ENGINEERING
Ch-_17 MATERIIII.S OF CONSTRUCTION
iii,<:: 465
PLASTICS I. J?.igid materials
Plastic materials have hccn in common i.1se in_ various ways in our. 2. Flexible materials
daily life. These are light in weight so that transportation is easy ancl 3. Metallic'surfaces
cheap. These are available in a variety of shapes implying thaJ it can be 4. Plastic cements
easily fabricated. Plastic containers are used for storing a number of 5. Special case plastics
substances· such as inorganic salts and weak mineral acid. In machin��.
plastic materials are preferred wherever moving parts are present indicat­ I. Rigid ma.tcrials : These are phenolic resin� with various· inert
.
ing that it offers less friction. These have better resistance to fillers. These arc used in the fabrication of a number of items. For
environmental factors. In a similar manner, plastic materials _also used in example, Keebush is a rigid material (phenolic plasti�) and is used for
the construction of plants. gears, bearing etc. It is light in weight. Some of .its applications are:
Plastics are syntheti� resins containing long chains of atoms linked to - Gears. - Bearing -: Vessel,s
•· form gi��t or macromokcules (polymers). They "have high molecular ··· Pipes - Fitti.ngs -· Valves
weight ( l o 3 to 10 7). -- Pumps � ,Ducts - Filter presses
Plastics have several advantages. These are: Disadvantages : These arc resistant to corrosion except o;,<: idising
(I) Low thermal and electrical ;esistance. substances and strong alkalis.
(2) Excellent resistance to weak mineral acids.
(3) Unaffected by inorganic salts. 2. F_lcxible materials : These are thermoplastic materials. These
. (4) Resistance to slight changes in pH.' materials can be rigid or flexible depending upon the amount of plasti­
cizer added. These are used in the fabrication of:
Pia.sties have disadvantages also. These are:
- Tanks - Pipes - Ducts·
(I) Low mechanical strength
- Funnels - Buckets
(2) 1-!ig'h expansion rates
Basically, t\vo types of plastics .are u;ed in pharmaceutical industry. 3. I\Ietallic surfaces � Plastics of polyethelene or polyvinyl chlo-
. .
ride types arc used along with plasticizers for the coating of rr1ctallic
Thermosetting plastics : Ther111ose1ti11g plastics can be formed un-· surfaces. These are used to protect the metal from corrosion. These
der heat and pressure. But these cannot be softened or remoulded, C"Ce linings arc applied on:
h%rdened. Some thermosetting plastics are made of pl�enolic. and urea
·- Tanks - Yesseis
resins.
- Stirrers - Fans
Thermoplastic plastics : Thermoplastic plastics are formed by the
application of heat and pressure and can ·b.e softened and remoulded. -t Plastic cements : These arc used for spaces between acid
This is a specific advantage. Scrap and rejected ai1 icles can be worked resistant tiles and bricks
again to get new materials. a so
�· Special cases : Plastics ar� used as guards for mciving p 11 f
Soine_ thermoplastic mat_erials and their uses arc given below: 111ach111cry. Nylon and PVC fibres are woven into filter cloths .:ind are
Polyethylene - cables, buckets. pipes used for aseptic screening.
Polypropylene - milk cartons, ropes
Polyvinyl chl_oride - gloves. water proof garments
Teflon - gaskets, coatings
Based on the utility of plastics in plant construci1on. these can be
categorised u.s:
.466 PHARMACEUTICAL ENGINEERING

QUESTION .BANK
Each'question carries 2 marks
I. Write the usefulness of glass lined equi,pment in the pharmaceutical plant.

Each question carries 5 marks

I. Explain the importance of stainless steel in pharmaceutical industry.
2. Write a note on the utility of glass and stain.less steel in .pharmaceutical
, industry.
3. Describe steel as a material of plant construction.
4. Name five 9111portant classes of plastics. Mention their applications 111
nhnrmaccutical industrv.
:,. uescnbe the steel alloys used in pharmacy practice.·
6. What are the properties of glass? What arc its applications as material of'
construction?
7. Describe various types of iron as materials 01 construction.
 18
..
Phannaceutical Industry-·Establishment:
,·

Pharmaceutical Industry
Plant Location
'Plant Laycut
Utilities and Services ··
Industrial Pollution and' Contrql
Industrial Hazards and Safety . ·

The development. of a compl!ih-:: plant design requires cons;deration of

many factors. · ·'The role of costs and profits is very important.· The ·•
0

application of engin�ering principles in. the design of individual

equipmerit is equally important. Iri ad�ition, ma:ny factors such as plant
. location, layout, operations and control, utility and safety should be
considcrad.

PHARMACEUTICAL INDUSTRY
The pharrm.ceutical industry differs from most other industries in that
there exist a considerable degree of specialisation in· it. Since products
arc so varied, no firm engages in all aspects of pharmaceutical manufac­
ture .. The products· can be classifie� arbitrarily on the following lines.· ·
Crude and processed botanical drugs: India grows a 'large number
of vegetable dru�s and supplies th<:;m to manufacturing houses in India
and nbroarl. '!'here is a steady. demand for drugs consumed by Ayurvedic
and Unani Practitioners of medi.cine.
Fine chc.micaJs and pharmaceuticals : In India, a large number of
pharmaceutical manufacturing houses purchase fine chemicals and in�
dustrial chemicals from firms, which specialise in their manufacture, ro'r
converting them into tablets, ointments, capsules, injec�ions . and
. other
pharmaceutical preparations.
Proprietary drugs : With the decline of dispensed medicine�, the.
prc-pacb:d products such as tablets, capsules and parenteral products,
 Ch- I b l'I IARMACEUTIC A I. INBUSTR Y--EST ABLlSI IMENT
468 Pl 1/\RM/\CEUTIC/\I. !:NCi!'°JEERiNG
Normally: primary factors exercise greater influence th.an .secondary
arc now prescribed and consu:ned in large quantities by hospitals and
nursing homes. Hence. a number of firms engage in preparing prop ri ­
a'
factors. However, it will be di fticult to make clca�--cut 'decision .
between these types of factors. Sometimes, the second�ry"fa�tors m�:?
etary �drugs. Some manufacturers have built a name f�r � h e have greater i·nfluence on location. · · · ',·,,
.
pharmaceutical industry and for themselves. by their resea rch act1v1t1es.
Thus efforts are continued to develop better formulations of old drugs Fundamental or Primary Factors
a�d discovery of new drugs. However, such manufacturers a re limLted in ·I . Raw materials
India. ,,,
2. Market
3. Energy ava i lab�lity
Definitions of Manufacturers
4 .. Transportation facility
Manufacturers arc engaged in the mechanical or chemical transfor­ 5. · Labour supply
m�tion of inorganic and organic substances into new products. . ....
T he above definition also includes assembling of components or prod- · I. Raw Materials: The availability of raw materials and wst of its'.,'.
transportation will be major determinants. Pharmaceutical industry uses'
ucts. Pharmaceutical manufacturing has been d\vided into three kinds. the following types of raw materials.
l . Biological products (a) Crude drugs
2. Medicines and botanicals (b) Inorganic chemicals
3. Pha�maceutical preparations (c) O rganic c hemicals
The biol�gical products industry includes ;'estai:Jlisl1ments engaged It would be economical to locate the pla'n t nc1arer to the source of raw .
_ _
primarily in the production of bacterial and viral vaccmes. toxms and · materials particularly wh<!n they a're consumed in large volumes. 'F�--\
analogo'us. products (such as allergenic extracts). serum, plasma and example, raw materials for perfume industry ·are aromatic plants." These :
other blood derivatives for human and veterinary use.'' cannot be'. transported because importa�t acti�e princ�le� may' be· los � ·
_ _
The medicina.l and botanicals industry includes "establishments en­ and materi als get spoiled. Hence, the industries undertaking extract1ori ·
gc:ged primarily in the manufacture of bulk medicines, organic �nd arc located nearer to the place �f cultiva.tion as in Hi;n?,ehal Pradesh _;irld .
. ·. · '·' ' '
inorganic c hemicals. their derivatives and· processing (gracing. gnnJrng hilly areas of UP. . , · ·
and �nilling) of i:>ulk botanical drugs and herbs.'' - If raw maicrials arc not locally available or danger�us chemicals, the
. . .
�'"'.mcrcase enormously .
· T he phani;aceutical preparations industry includes "�sta�lishments re1g I1l c I1argcs an.d -nsk· o f dangers-
{. .. I f raw materi-
engaged primarily in' manufacture, fabricati� n or pro�essing mto phar­ als arc stable. otiicr factors take importance over this facto�.
maceutical preparations for human and veterinary use.
2. Market : M arket exercises a strong i�tluenc� 9n·the establish­
ment of i ndustries. Whcic mark.ct is regional, the industry is located
PLANT LOCATION nearer to the market. The bulk drug industry is located in a place w h ere
. The sel��tion �f a location fo� the c�nstruction of a pharm�ceutical drug formulatio1i industries are'located, since bulk drugs are the feed for
or che�jcal plant is a ·vital decision to be taken..becaus� it J�termine<; the formulations and buyers are found_ncarby. ',:.,
_ _
the bal.ancing of investments and pro tits. 1 here tore. location ot the plant
has ;i strong influence on the success of an _industri�I v�nture.. Care 3. Energy availability : Fuel ai1d pow�r are the energy so�rcci;··
should be exercised ii) choosing the plant size. Pr'. m�nly the plant which exert the same kind of influence as the ra� materials'. ·Now-a-;·:
_ days, electricity and diesel engines have been developed and a·re availabie
'should be locateri where the cost of production and d1s� n?ut1on can be
_ _at many places. In many cases, plants create power.on their ow�· fo�' the
min.imum. But other factors such as room for expansion and general o
living conditions are also importmt. smooth functioning of the indus�ry. 1'heref re, industry·can be l�eated ·
1. Fundamental (Primary) factors remote to the power generation plants. ' ·
2. Qerived (Secondary) factor<;

470 PHARMACEUTICAL ENGINEERING
4. Transportation facility : Transport is the lifeline of modern
industry. Transport facilities are needed for bringing raw materials and
distribution of finished products. An industry tends to be localised at
places, which have a developed means of transport 5UCh as railway, road
and seaport. _These facilities are normally available in metropolitan
cities or mega-cities such as Bombay, Calcutta, Madras, Hyderabad and
Bangalore. Hence, most of the industries arc located in these cities.
If the sale price of the finished product is very high, because· of
technical considerations as compared with freight charges, transportation
may not outweigh other factors. The kind and amount of products anc'l
raw materials determine the most suitable type of transportation facility.
There is. also a need fo� transportation facilities for th!! personnel.
s'. ·
.
Labour supply: Low wages and abundant labour help in locali-
sation of certain industries such as tea. However, pharmaceutical and
chemical plants require skilled labour. who are better paid and often
highly mobile. Therefore, industries can be located a\l.:ay from areas of
labour concentration.
, ·Consideration should be given to prevailing pay rates, restrictions on
number of hours of work pe\ week, competing industries that. can cause
dissatisfaction or high turn over· rates among thi.:: workers, racial prob­
le.ms and variations in. the skill and intelligence �f the workers.
Dcr.ivcd (Scc.ondary) Factors
I. Climate and soil
2. Government concessions
3. Water supply
4. Waste disposal
5. Site characteristics
6. Flood and fire protection
7. Community factors
I. Climate and soil : Climate and soil are very important for
industries bas�d on agriculture:. For example, Ayurvedic drugs arc
mainly plant-based products. The soil and climate arc suitable for
cultivation of medicinal planis in the state of Kerala. These formula�
tions are largely produced in that state.
In pharmaceutical industry, many �p'crations have to be carrit:d oul in
�ir-conditioned rooms, in dust free environment and under humidity
contr�I. A location which is very hot during summer ,•/ould� n(i'l be
suitable as it is subjected to dust storms and drying up of water supplies.
Further an area ,·,here the humidity is very. high would not be suitable
Ch-18 PHARMACEUTICAL INDUSTRY-ESTABLISHMENT 471
· from the point of cost, contaminatio�, difficulties of maintaining labora­
tory animals in proper condition and the efficiency of labour and
supervisory force.
· Industries based on production of antibiotics etc. ·are normal,ly _ 1.<r.:
catcd in a place wherein the microbial contamination' in the environment,,
is low and the ambient tt:mperatures· throughout the year are cool. For ·
example, I.DPL antibiotics plant is located in Rishikesh (in UP) and
Karnataka Antibiotics and Pharmaceuticals Limited (KAPL) is located in·:-
Bangalore, Karnataka . State. , ;,'.. . ,I
If the plant is located in a cold climate, costs may be increased by thf?�·.
necessity of constructing protective shelters around· the process··
equipment. Special cooling towers or _ale equip�ent may �e required, if
· · .. · · 1::
the prevailing temperature is high. . ·.,
. .
. . . �·,
:
2. Govc.rnmcnt concessions : Government subsidies :and. tax con..:.:
cessions have been provided for the industries located in' cert:1in notified_.'.
areas. These areas .have been declared as industrially backwRrd and the'.'
government offers incentives such as low wages; cheap pow·er, tax,:
concessions etc. Previously such areas were not ,,e,coµomicapy feasible,
but now due to government concessions, these areas_ are _developing fast.::
3. W�tcr supply : The processing industries use large quantities o'f.
. water for cooling, washing, steam generation .and also as ·a ·raw material .·
(liquid orals). The plant, therefore, must be located wher_e a d,ependable ...
supply of water is available. A study should . be conducted regarding the.:
_
supply position of underground water and/or surface water a�d the1r. '
_ .
seasonal variations. The quality of the water is also very important ·m
pharmaceutical industry, as purified water is C(?nsu111ed in 1°'.rge qu� . �tities: :·
The temperature, mineral content, silt or sa�d content, bacteriological
- content, cost of supply and purificatio� treatment"must also_.be consid-..
ered while choosing a water supply. A. detailed: estimate of, ,warer
requirements both for the present and future must be.made.
4. Waste disposal : Ip recent years 1 many 1Jegal restri�tiohs. '·
have been placed on the methods for:gisposing
· of w�te materials from
the processing industries. .
.. �· :· . ;·, ,,. ·
(a) When orga�ic or inorganic chemicals are manufac�ured, there
may occur· problems of't1oxious gases being produced and._ dis­
chargeiTn to the atmosphere or into the sea.
(b) If the industry' is engaged in the manufactur� of biological
products from raw materials obtained from slaughter houses
 472 l'Hi\RMACEUTICAL ENGl:--:t:ERING
. or pathogenic organisms, the waste disposal does pose a prob­
lem. bttt" a minor one, bec�use the raw material h:rndled is not in
huge quantities.
The site selected· for a plant should have adequate capacity and
facilitib for correct waste disposal. Attention should also be given to
potential requirements for additio.nal wask treatment facilities.
5. /Site characteristics : The topography ·or 'the land and soil
structure should be considered, since both may have a pronounced effect
on construction costs. The cost of the land. local building costs and
living conditions are important. Futme changes may make it desirable
or necess::iry to expand .t.he plant faciliti£:s.
6. Flood and fire protection : Many industri::il plants are located
along large bodies of water and there arc risks of flooa or hurricane
dama·ge. Before choosing a plant site. the regional history of natural
ev'enis ofthis kind should be ex�mined. In case of major fire. assistance
from .the fir7 departments should be easily available. Fire hazards in the
imme.diate surt'ounding area of th:e. plant site must not be overlooked.
7. Community factors : The character and facilities of a commu­
nity can have quite an effect on the location of the plant Cultural·
facilities of the community arc important for sound growth. Churches,
temples, libraries, schools, civic theatres, concert associations and other
· s�·milar groups, if active and dynamic, do much to m::i.ke a c�mmunity
progressive. If a minimum number of facilities for satisfactOI)' living of
plant personnel do not exist, it often becomes a burden for the plant to
subsidize such facilities.
Special Provisions of Factory Premises-Location
The factory shall be .Located in a sanitary place remote from filthy
surroundings. The factory shall. be situated in a place which:
(a) Shall not be adjacent to an open sewage, drain or public lavato­
ries.
(b) Shall not be adjacent to a factory, which produces disagreeable
or obt. toxious odours or fumes.
(c) Shall not be adjacent to a factory. which einits large quantities
of soot, dust or smoke.
, The factory shall not constitute undue danger to adj�ccnt Ii fc and,
property. State laws and other related laws should be consult�d.
Ch-18 PHARMACEUTICAL INDUSTRY-EST/\l3LISHMENT 473 ..,,,..,,
No location can meet all the requirements ideallyj but the best
compro1nise has to be made by 'considering viui�us points objectively
_
and gathering relevant. information. /\fre, rons1der111g' all the above
poiPts, a projec.t report has to be prepared. It be.comes necessary for the
entrepreneur to acquaint himself 1J'JJJ1 _
all the leg.ii controls, :Vh1ch arc
existing. I\ r�w su,<;;.h' acts are:
lndian Factories Act .
Drugs and Cosmetics Act arid Rules.
PLANT LAYOUT
_ Once the location of plant is decided, the problem of layout has to- be
tackled.
Plant !arout is a coordinated effo1i to achieve the final objective to
. integrate. m;chines, materials and personnel for econc:,mic.:production.
Lavo.ut can be described as location of different :departments and
a'rrant!.ement of machinery in a department. A proper layollt ha's the
adva;tage fron1 the point of work_ers, · labour c9sts, other production
costs. produ.ction controls. supervision and capital investment. Layouts
arc of two types.
(a) Process layout or functional. layout
(b) Product pr straight Iinc layout
Process larnut or functional layout : In this type, all machines of a
particular etas; doing a particular type of work or process are arranged
_ .
together in a separate dep:_1_;:tment. For example, all, cuttmg machines
may be placed in one dep' a-itment, i.e., cutting department., :The advan-
tagcs of this type are: ··,
(aJ More effective supervision can be achieved.'
(b) Division of labour or. specialised.work can be provided.
( c) Less disruption of production is possible; , ·: · .. · ·
(d) Good scope for e�p�nsion.
This type of layout may not be possible. in the pharmac.eutical and
cliemical. industry, because a number of unit operations should be. per- .
formed in. a sequence.
. Product or straight line layout : In this type. all machin,es doing
. various ope�ations are arranged in a line. The advantages of this type �f
layqut arc:
(a) facilitates qui'Ck and smooth processing of. �·ork.
(b) Reduces cost of material handling usi�1g conveyor. ,
474 ;
PHARMACEUTICAL ENGINEERING Ch-18 PHARf-1i\CEUTICAL INDUSTRY-ESTABLISHMENT 475
· (c) Reduces manufact�ring time and speeds up the manufactur- improving the layout during plant construction.. Mode !� are' �lso useful
ing cycle. _
for instr.uction and orientation purposes after the plant ts completed.
(d) .Facilitates proper use of floor space.
(e) Re.duces inventory of work-in progress. 1. Identification
(f) .Reduces inventory of finished goods.
This type of layout is more suitable for th t:: . pharmaceutical and
j Processing area I I Handl;ng area I I Storage area I
I Equipment layout in a unit
chemical industries. Some times, a combination of these two layouts is
also used.

Procedures of Layout ↓
The procedures of plant layout arc shown in Figure 18-1. A proper Processing upits layout
↓
layout in each case includes arrangement of processing areas, storage .
areas and handling areas for efficient coordination. The layout of process-
ing units in a plant, the equipment within these units must be planned. Structural layout
0↓
Then detailed piping, structural. and electrical design should be devel­
oped. This layout can play an important part in determining construction !l
arid manufacturing costs. Ti1Us, these must be planned carefully with Piping layout
;:mention being given to future problems that may arise.
Some factors which guide the layout are:
↓
Electrical layout \
(a) New· site development or additions to a developed site.
/ (b) Type and quantity of products to be produced. 2. Drawi;gs of plant layout
(c) Type of process and pr�duct control. Scale drawing with. elevation for
(d) Space available and space required. equipment and process
(e)
(f)
Operational convenience,and accessibility.
Economic distribution of utilities and services.
↓
(g) Type of b uildings and building code requirements. Analysis of layout
Three dimensional model,
(h) Health and safety considerations. computer graphics
(i)
U)
Waste disposal problems.
Auxiliary equipment. ↓
(k) Possible future expansion. Detailed drawing
Scale drawings indicating complete description with elevation can be
Fioure 18-i. Flow diagram of procedures
used for determining the best location for equipment and facilities.
to� an appropriate design of plant layout.
Elementary layouts are d. e.velope'd iirst. By analysing all the factors that
are involved in the plant layout, detailed recommendations can be pre­ Special Pro\'isions of Pla.nt Layout
sented fin-ally. Drawings and elevations including iso.metric drawings of The rn:mi;es should be suitable for the purpose of drug manufactur­
.:the pipi�g systems can be prepared. im:. It means that all possible measures should be taken to �revent
In the recent years, three-dimensional models arc often ·made for . co;ifusioJl or mixing-up ·o( substances or materials and contam1n�tron.
making proposed plant layouts. These have the advantage of indicating The bu i IJ ing for the factory shall be constructed so as to permit the
_
errors in a plant layout easily. In adclition, models are useful in production under hygienic conditions. They shat! �on'.orm to. the condi­
tions laid down in the Factories Act. 1948 (63 of 1948).
 476 l'l !ARMACEL!TICAL ENGINEERING
I. The part of,the building used for manufacture shall not be used
as slee�ing place.
2. No sleeping place adjoining the b�ilding shall communicate
therewith except through open air and through an intervening
open space.
3. The walls of the. room 111 which manufacturing operations arc
carried out shall
(a) have a height of six feet from the floor.
(b) be smooth and waterproof.
(c) be capable of maintaining cleanliness.
(d) have no chinks or crevices.
The flooring shall:
(a) be smooth, even and washable
(b) be in such a way as not to permit any retention or accumula­
tion of dust
(c) have no chinks or crevices.
The buildings arc arranged to permit economic production. The
muting of goods should be logical so that successi\'e unit operations can
--�-e done in adjacent.rooms with supe_rfluous transpc:"tation. For example
in the tablet section, there should be separate rooms situated closer for
.
granulation, drying. sieving, mixing, compression and, if any, coating,
.
successivelv.
Adequate facilities should be maintained to provide safety and fire
p�o�ection. Rc�ulation controlling escape route.s in case of fires, pro­
�
v1d111g fire fightmg equipment, fire alarms and measures to· be taken for
prevention of breaking of fires and their spreading should b� complied.
Devices should be installed in every room where process operations
re
� car'.icd on. so that in times of emergency the power supply can be
1mmed1atcly cut off from the transmission machinery.
Building meant for storing and handling should be segregated and
isolakd. 1:hesc satisfy the provi.sions of the act.
UTILITIES AND SERVIGES
Utilities
The basic utilities required for an industrial plant arc power and
water.
The primary sources of energy for the supply of power are heat of
combustion of fuels. Fuel burning plant� are of greater industrial
Ch-18 Pl IARMACEUTIC:/\1. INDUSTRY-ESTABLISHMENT 477
significance than hydro-electric fuels, because the pl1ysjcal location of·
fucl burning plants is not restricted.
In �chemical industries, power is supplied primarily in thP. form of.
electrical energy. Agitators, pumps, hoists, conveyers, compressors and
similar equipment are usually operated by electric motors. Sometimes,
internal combustion engines and hydraulic turbines are employed:
When a new plant is being set up, a decision must be made on either
to USC purchased power Or to SCt up its own· power ·unit Jt may be
possible to obtain steam as a by-product from the self-generation of
. desision.
electricity. This factor may influen·ce the final
v 1
- Power can be transmitted in variou� fon�1s·, such as·- m�chanical ·
energy, heat energy and pressure energy. It is-essential to recognise the�
different methods for 'transmitting power. and the best one to 'suit the
particular proces� should be chosen. For example, steJin is generated ,
from the cheapest fuel expanded thro�gh tu'rbines fo gener�t� th'c neces- .
sary plant power and exhausted, �team is ·used in the process he�t.
· Water for r·ndustrial purposes can be obtained either from' the plant's
own sourc� or from � municipal a1:�ply. If demand for water is brge. it
can be obtained from the plant's own drilled wells, rivers. lakes. darn
streams. Before the company agrees .to go ahead with any new project.
it must ensure itself of a sufficient supply of water for ..all industrial.
sanitarv and safety demands for both present and future.
..
,i
The water used in 111anufacture shall be pt1re and of drinkable quality ..
(rec from pathogenic microorganism·s.
Maintenance Services
Many of the problems involved in maintenance are .due to the' faulty
design··and layout of plant and equipment.
Sufficient space and facilities for maintenance �ork must be pro­
vided in the· plant layout. It is essential to. :_consider · maintenance
regulations w · hile making ct'ecisions on equipment. Too often tre design
engineer is conscious only on installation costs and. fai 1,s to recognize the
maintenance costs. - On several occasions. the maintena�ce cci�ts can
easily nu-IIif y �he advantages· of a cheap initial instillatio�:· For example,
a compact system, of piping, ·valves and equipment may be· cheap and
convenient for the operator's use, but maintenance of the system may be
costly and involves time consuming dismantling operations.
I t\Strumcnts arc used in the chemical industry. tb . measure process
variables such as temperature. pressure and density. 'Automatic· control
478 PHARMACEUTICAL ENGINEERING
J
Ch-18 Pl!ARMACEUTICAL INDUSl�RY-ESTABLISHMENT 479
h:15 bee� ac�c ptcd as the best and the resultant saving
_ s in labour com­
bmed with improved ease and efficiency of opera 2. In dry cooling towers, the temperature of the condensed water
tions· has more than
offset the added expense for instrumentation (Use of high decreases. due to conduction and convection for the transfer of
speed comput­
ers). In general, one centrally. located control heat from the water fo the air.
_ room is used for the
recording and regulation of the process variables.
3. Cooling ponds are generally considered for heat removal when
Storage. suitable land is available at a reasonable price. It is normally
assumed that heat discharged to a cooling ·pond is lost through
I. Adequate storag facilities for raw materials, interm
_ � ediates, recy­ the air water interface.· '
cle materials, reJec.ted materials and fuels are essen
tial · for the 4. Spray ponds provide a viable alternative to cooling ponds when
operation of a processing plant.
land costs arc too high. It is estimated that· a spray pond
2. Bulk stor�ge f liquids is generally handled by
� a closed spheri­ required only about 5 to I 0% the area of a cooling pond due to
0

cal or cylindrical lanks so as to prevent the escap

e of volatile the more air water contact. In addition. drift losse� and corro­
material and minimizing contarninatio�.
sion problems are. less severe than in cooling towers.'
3. Liquids with vapour pressures above atmospheric
_ pressure must
�e stored in vented tanks. Flame arrest mechanisms must be Water Pollution Abatement
mstalltd in all openings. The problems of handling a liquid waste �(fluent is 1nore complex
4. Gases are stored at atmospheric pressure in wet than handling a waste gas effluent. The w,aste liquid may contain
or dry seal gas­
holders. dissolved gases/solids or it may be slurry ' in· either 'concentrated or
5. High pressure gases are stored in spherical or diluted for'lns.. Because of t_his complexity; priority' should be given to
horizontal cyli�­ the possibility of recovering part or all of the waste products for reuse or
drical vessels under pressure.
for sale.
6. �ol id products and raw 'materials are either
.stored ' i n weather Frequently; it is economical to install .recoyery facilities rather than
tight tanks with sloping roofs or in out door bins
and mnu'.lds. waste treatment equipment. If product �ecovery is not capable of solving
the waste disposal. problem, waste treatment..should be done. One of -the
INDUSTRIAL POLLUTION AND CONTRO
L functions. of the design engineer is to decide w�ich treatment process or
Thermal Pollution and Control combination of processes will.. best perform the ne<;esjary task of clean- ., .
Various off-stream cooling S) Stcms are requi·red to ing up the waste water eff1t1ent. This treat���t could. be. physic;!,.
.
1
handle thermal
discharges from processes because: chemical or biological in nature, .depending upon ·the type' of waste
involved and the amount of removal necessa,ry. .,
I. Changcs in temperature cause potent-ial damage
_ to the aquatic
environment. Physical treatment : Larg�{,floating or suspended par.ticles are re­
2. High temperature causes reduction in the assim moved first. Sc1lirnentation and gravity settling methods are employed .•
ilative capacity using circular clarifiers, ,vit.h continuous chai,n·sludge scrapers.. Adsorp­
of organic wa$tes.
tion process is employed using activated carbon for ,the removal of
3. Federal enactments are ·more stringent regarding water
tempera­ · refractory organic substances; toxic substances and colour. Thr.ee differ­
ture standards.
ent mem.brane processes, viz.,· ultrafilfration. reverse osmosis and
�ooling towers are most often considered for this service followed by electro-dialysis arc used as the, final treatment and for in-plant recovery
cooling ponds and spray ponds in that order. · systems.
I . In wet cooling towers, the condensed cold water and �mbien Chemical treatment : Chemical methods are generally used t-0 re­
t air
are intimately mix�d. Cooling results from the evaporation move colloidal matter, c.olour, odour, acids, alkalis,. heavy metals and
of a
portion of water .. oiL Such ::i tre::itmcnt is generally brought about by ,coagulation.
floccul::ition. emulsion breaking. precipitation and �eutralization.
480 PIIARMACEUTICAL ENG!NEERIN(i Ch-.18 · PHARMACEUTICAL INDUSTRY-ESTABLISHMENT
. 481

Biological treatment : If common bacteria arc found in water. many
organic materials will be oxidized to form carbon dioxide, water, sul­
phate and similar inatcrials. This treatment consumes oxygen that 1s
dissolved in. water and may cause a depletion of dissolved oxygen.
Air Pollution Control
' Air pollution control can essentially be classified into two major•
categories.
- Those suitable for removing particulate matter.
- Those associated with removing gaseous pollutants.
Air pollutants are removed by chemical and physical �cans in the
following_ manner.
I. Coarse diameter particulate matter can be removed with low­
energy devices such as settling chambers, cyclones and spray
chambers.
2. Sub-micron particles must be rem�ved with high-energy units such
· as bag filters, electrostatic precipitators and venturi scrubbers.
3. Intermediate pal\icles can be removed with impingement separa­
'tors or low-energy wet �ollect�rs.
4, · Gaseous pollutants can be rc'moved from air streams either by
absorption, adsorptio1�, condensation or incineration.
. ·most 1-iandboob. Hazards ·due to industrial ch�micals can be minimised
INDUSTRIAL HAZARDS AND SAFETY
Toxic and corrosive chemicals, fire, explosioris and plant personnel
Chloroform, benzene, chlorinated hydrocarbons; .low-bqiling ,frac:
tions of petroleum are some of the. common solvcnts. used in'
pharmaceuti�al indust ry . Solvents used· in · the extra�tion of plants;
purification of synthetic drugs and in.chemical analysis· should �e.h.an-�
, · ·' · ·· · .
died with care:
In pharmaceutical industry, most o(the dennatitis can be attributed
to synthetic drt1gs, especially to acridines and phenothiazine compounds.
It has been noticed that fair people are gcl)erally more susceptibl,e to skin
irritation than dark people. The only' pro�ection from skin re�ctions is to
observe cleanliness and to remove the people from �he areas as s9on as
the first sign of skin reactions is noticed. Wherever practicable, applica:.
tion of barrier creams before commencing the. work has be_e_�·· found
useful in protecting individuals.
While grinding vegetable drugs, dust evolved, is. irritati.ng. · For
example, capsicum. and pod-ophyllum .affect the eyes and. irritation is
painful. Therefore, goggles are to .be worn. Some ·indivi_ duals. art: so
sensitive to ipecacuanha.. that they develop symptoms of asthma, when
e�posed even to 111inute traces of its dust.
Tolerance levels for toxic chemicals have been set by Federal Regu­
lations. Flammability and detonability of chemicals arc ava_ilable in
if there is stri�t observance of safety rcgulatio�� and protectiv:e mc�tsures
of good house-keeping principles, besides their full and intelligent'.coop-
eration in the handling of dangerous chemic'als ahd drugs. ·
• . '
l

falling to accidents are the major health and safety hazards enco·untcred
in -the. operations of plants in processing industries. Dust Explosion
. ' . In pharmaceutical industry, a number ofgrindin_i. op�rati;�s .is '
Chemical Hazards
.

employed. If iron or stone pieces get into the disinr'egrator. or· other"·
Tough . ma�y common substances are apparently innocuous, pro­ similar grinding mills, sparks "are emi�ed, which' mjghf bring about
longed 'breathing and/or skin co.ntact prod�ce ir�itation and may briog explosion with some easily combustible m�terials. Therefore,' suitable
about permanent impairment of health or ev�n death, precautions against accumul.:rtion of dust should be taken.' · 11 has b�en
t\.fany che micals can cause severe burns, if these come into contact found tl1at in pharmaceutical ancL�=1cillar/factories,·dust of starch
. '· •'"·
.and
.
• • 1 • .· • . • · · •· '
with living tissue. Living tissue may be destroyed by chemical reactions dextrin besides or6anic substances are extremely hazardous.
I .
' '
•
' •f ,...
i, ' ,, • I • < '' ' ., '

Stich as:, The methods used for controlling

. dust in the. pharmaceutical
. ir\dustry
,, >
(a) Qehydration by strong dehydrating agents. � ... are:
(b) Digestion by strong acids and bases. (a) Filtration
(c) Oxidation by strong oxidizing a.gents. (b) 'Inertial separation
Eyes and mucous memb'ranes of the throat are .particularly suscepti­ (c) Electrostatic precipitation
ble to the effect of corrosive dust. 1�ist and gases. In addition. many
chemicals are very toxic. flammable or detonable: I
 Cli-18 PIIJ\RMACEUTICAL lNDlJSTRY-ESTAI3LISrJMENT 483
482 PHARMACEUTICAL ENGINEERING
Every type of..!nechanical dc1\1'1t:e should be examined periodic�lly by
Fil' tration : In this method, air which contains dust is sucked or a competent person.
blown through a suitable mechanical barrier. whose pore size is suffi-.
ciently small to. retain particles. Materials used for this purpose include Noise Abatement
paper; felt, wool, cotton-wool and nylon. The filters oft.en take the form The design engineer should i1_1clude noise studies .in the d�sign stag·e
0

' ·
df pads or panels fitted to the walls and windows of building: A large of any indcistrial facility.
variety of filter bags are available, which can be attached to a parti�ular To attain. efficient, effective and practical noise control, it is neces-
machine where dust is produced. "sary to understand noise sources in the process, their acoustic properties
Inertial �eparators : Example is a cyclone separator. In this method, and characteristics· and how they interact to create the. overall· noise
air is allowed to circulate in a spiral manner through a cone-shaped situation: Table 18-1 presents typical process design equipment provid­
vessel. Due to centrifugal force, particles of drugs are thrown outwards ing high noise levels and potential solutions to thi� .Pro�lern .
to the walls of the cyclone separator. They slide down to a hopper,
.· �
which ca·n be subsequently withdrawn. Cyclone separators are particu­ TABLE. 18-1
larly suitable for attaching to machines. These- can form an integral part Equipment
,
Noise Sources, Leyels
.. and Poteqtial
.
Control Solutions.
of the design of certain mills arid mixers. Equipment· Sound level ,. , . Possible noise . .
Electrostatic precipitators : It consists of a number of earthed tubes. in dBA at 3 feet·· control treatments
Fine metal wires are stretched between the tubes. Several thousand volts
of direct current is applied on metal wires. The high potential difference Air coolers· 87-94 Aerodynamic. fan blades,
between' the tubes and the wires ionizes the dust particles that are carried deer.case revolutions per minuk,
increase pitch,
by air stream. The dust is deposited on metal plqtes from which it 1s
include tip an'd hub.seals, '·
collected periodically. . decrease pressure. drop
. .·
.

Fire and Explosion Hazards Com prcssors 90-120 Install muffli::r� on_ lntakc _and exhaust,
A single fire or explosion can spread to adjoining units. Careful enclose the machine with casing.
plant layout and judicious choice of constructional materials can reduce vibration isolation and
such events. Hazardous operations should be isolated by. conducting lagging of piping system
them in separate buildings or by the use of brick firewalls. Brick or Electric 90-1.l O Acoustically lined· fan co�crs,
reinforced concre.te' walls can limit the effects of an explosion, particu­ motors enclosures and motor mutes.
larly if the roof is··designed to lift easily under an explosive force. Heaters and 95-110 Acoustic plenums, intjikf! muffiers,
Equipment should be. designed to meet the specifications and codes · furnaces lined and damped duds.
of ;ecogniz�d aut�orities such as Indian Standards A�sociation, Ameri­ Valves <80-108 Avoid sonic vel�cities, li�it· pre�sure
can Petroleum Institute (API) a�d American Society of Testing Materials. . drop and mass flow, replace ,vith:
The-design and construction of pressure vessels and storage tanks shouid special low noise valves; vibration
I . ,
isola�ion and 1.agging.·' ·, ·'· .':
follow API and ASME codes. .: :
· Adequate·vehting is necessary and it is advisable to provide protection Pipes . 9-105 Inline silencers, vibration
. isolation
and laggin1;: . : . ,: ., . ' .
by using both spring-loaded valves and rupture discs. Possible sources of
· fire are reduced by eliminating the unnecessary ignition sources such as
Safety Regulations
flames, sparks, heated materials. matches, smoking, welding, cutting and
static. electricity. Spontaneous combustion and non�explqsion proof · S;ifcty must be a paramount consideration in the design of phctrma­
electrical equipment are the potential ignition sources. The in.stall at ion of ceutical industry. The factor,ies Act, 1948 is very 3omprehcnsive. . It
�ufficient fire alarms, temperature alarms. fire-fighting equipment and includes provisions on cleanl'iness, ventilation, lighting and,heating a�d
sprinkler systems must be specified in design. the prevention of over-crowding.
r
484 PIIARMACEUTICAL ENGINFERING
Ch-18 Pl 1/\RM/\CEIJTICAL INDUSTRY-EST i\BLISHMENT 485
The intention of the Occupational Safety and Health Act (OSHA) of
QUESTION BANK
1970 is "to assure so far as possi.ble every working man and woman in
the nation safe and healthy working conditions and to prcscrv.e our Each question carries 5 marks
human resources." Two of the standards directly related to workers I. What arc possible industrial hazards? How can tly.:y be controlled?
health, ind important in design work are: 2. What met�ods arc employed for preventing the hazards of
· handling and.s::,
(I) toxic hazardous substances. use of poisonous chemicals in industry?
(2) occupational noise exposur�. 3. Explain 'industrial pollution and control. "
The first factor concerns with the normal release of toxic and carci­ 4. What methcds arc employed (or preventing the haza�ds of handling and
nogenic substances carried via vapour, fumes, dust fibres or other media. use of poisonous chemicals in industr;?
Compliance with the act requires the dcsigne�. to make calculations of 5. Write a note on plant location.
concentration
' s an� exposure time of plant personnel .to toxic ch�micals
during normal operation of a process or a plant. Their release could Each question carries . 10 marks � ro,"'-
.
emanate from various types of seals, c.ontrol valve packing or other I. Describe the fac1tirs that should be considered regarding plant loc.ition and
similar sourcei. Normally, the designer can meet the lirnits set for layout.
exposure to toxic substances by specifying special valves, seals, vapour
recovery systems and appropriate ventilation systems.
The Federal Register should be examined closely for the list of
materials declared hazardous, acceptable material expus'ure time and
\?necntration before beginning the detailed design of a ·project..
The occupational noise exposure standmd requires well planned. ti1J1ely
execution of steps. It is best to prepare two noise spcci fications during
plant design itself. One to define the designers own scope of work and
the other to set vendor noise-level requirements for various pieces of
equipment.
Other standards in the safety area most often cited by OSHA are the
}:ational Electric Code and Ma�hinery and Machinery Guarding. which
must be considered in detailed designs.

Personal Safety
Every att.empt should be made to incorporate facilities for health and
safety, protection of personnel in the plant des;gn. This includes (but it
is not limited to) protected walkways, platforms, stairs and work area.
Any ·unavoidable physical hazards must be clearly defined. In such
areas. means for exit must be unmistakable. All machinery must be
guarded with protective devices. In all cases, medical devices and first'
·aid must be readily available for all workers.·
;

APPENDIX-!

FRACTIONS AND MULTIPLICATIONS OF UNITS

(A) Greek Alphabets

A a Alpha N v Nu
[3 p Ucta - l; Xi
r y Gamma 0 0 Omicron
t:,. 0 Delta f1 1t Yi
E c Epsilon p p Rho
z s Zeta ·:r. Cl" Sigma
0 e Theta y u Upsilon
I Iota 1ir< ct> Phi
"" 4>
K K Ka:·pa x x Chi
t\ /\. Lan1bda '11 \jJ Ps�
M µ Mu n (J) Omega

(B) SI Units
Fraction Prefix Abbre- Power Prefix Abbre-
viation viation
IQ-I deci d 1 01 dcca da.
10-2 ccnti c. 102 he eta h
10-3 mil Ii m 103 kilo k
I 0--0 micro µ 106 mega M
10-9 nano n 109 giga G
10-12 pico p 1012 terra T
10-15 femto f
10-l 8 atto a

487
 ....
J

Apdx-11 NOTATIONS AND AB13REVIATIONS" 489

P,'operty /Jnits in fi,/1 names

1J Abbreviations
!\:;
APPENDIX II
for the units
..
. Rate of discharge of liq�id meter cuhe per r:n inute m 3 /min
(A) Some Notations of Units and their Abbreviations in SI Units Rate of drying kilogram per hour· kg/h
Rate of �mry of feed kitogram per �our kg/h
Property Units in full names Abbreviations
for the units Specific energy milli.ioule per kilogr::irn mJ/kg

/\cc.:cleration clue to gravity metre per second square mls2

Speci fie surface
..
metre square per meter cube m2 /m3
Speed of rotation Revolutions per second r/s
Amount of heat joule J
Steam pressure pascal Pa
Capacity of a pump metre cube per hour m 3/h
Stefan Boltzmann constant watt per metre square �elvin4 W!rn 2·K4
Centrifugal force newton N
Surface area metre square m·
Concentration ·Moles Mol
Molarity M Surface energy rn�llijoules per mqtre square mJ/n, 2
N9rmality N Temperat_ure. Degre� Kelvin K
Molality · m . Degree Celsius oc
Density kilogram per metre cube kglm3 Tensile strength mega pascal Mpa
Displacement in pump metre cube per minute m /min
3
Them-.al conductjvity watt per metre squarc·Kclvin W/m2·K
Drop in head metre m Time second ( or minute or hour) s (or min
Energy joule J or h)

Enthalpy per unit mass joules per kilogram J/kg Velocity metre per second .mis
Film coeffic.:ic.:nt or watt per metre square·Kelvin W/m 2 ·K Viscosity pascal.second Pa·s
Surface c.:ocfficient Volun1e metre cube (or litre) m3 (or I)
force newton N \V ork clone watt hour W·h
Fre Juency hertz Hz Young's modulus mcgapascal Mpa
Gravitational force newton N
Heat transfer joule J
Heat transfer coefficient watt per metre squarc·Kelvin W/m2 ·K
(B) Some lmpor!ant con,·ersions in SI Units
Meat transfer rate joule per second J/s
Pascal (Pa) = N/m2 = kg/m·s2
Height or length metre m
,metre Newton (N) = kg/rn
Length m
kilogram Joule (J) = N·m = kg.m2/s2 .
Mass kg
N·m = J
Power watt · W •t1••

Pressure pascal . Pa
N·m/s = J/s �w
pascal J/s = V.' .,;;::,
Pressure drop Pa
mctre \\' = N·m/s
Pressure head m
488
 I
i\pdx·U: INTER-CONVERSION OF UNITS 491

Meas11remenl Unit Conversion facto_r Reciprocal

APPENDIX-Ill
Viscosity 1 lbf·s!:n 2 6.894 x I0 3 Pa·s 1.451 x I o-4
1 lbf-s/ft 2 47.88 Pa·s 2.0886x I o-2
. INTER-CONVERSION OF UN I TS
Volumt! I fl3 2.832x I o-2 in3 35.315
TABLE-I 1 in 3 L693xto-s m3 61.024
FPS to SI Units I US gallon 4.54x I o-3 m3 220.264

Measurement Unit Conversion factor Reciprocal

Area I ft 2
.. 9.290x I o- 2 m2 TABLE-2
. 10.764
I in2 . · · 6.452xJ0-4 ml 1550
. � ... Interconversion of Units (Fundamental
and Derived) with Conversion Factors
Density 1 lb/ftl . 16.0185 kg/ml 6.243x10-2 -
1 lb/inl 27.680 kgJm3 3.613x10-s Unit Conversion factor x unit Reciprocal·
Energy, work I Btu l .055x I oJ j ules .9.478 JxJ0-4
? J fact = 30.48 cm (or ml) 0.03281
and power
1 pound (lb) = 453.6 gram 2.2046x I o- 3
Force I lbf 4.448 N 0.225 ...
I cm· = ! .639'x l o-5 m 2 . 6.1024xlO�
Heat transfer Btu/s·ft2 ° F 20.44 kW/m2 ·K 4.89x 10-2
I dyne � 0.01 mN 1. 0 0
coefficient . ·
I d)·n,:/crn 2 = O.i Pa 10
Length 1 foot 0.3048 meter 3.2808
i -cm H20 (4 ° C) = 9.80:.: 1 o-2 kPa 10.205
I inch 2.54x I o- 2 meter 39.370
l cai = 4.184xJ0-3 kJ 239.00
Mass 1 pound (lb) 0.4536 kg 2.2046
l ('-,�, = I.Ox i o-7 J 10 7
I US ton 9.072x10-4 kg 1I.02x102
•r,

l 0 C-m 2 ·h/kcal = is.604x 10 2 K·rn 2 /k\V l.162xlQ-3

1;.1ass flow rate I Ibis · 0.454 kgls 2.205
l c�l-mis·cm 2 · ° C =.4.1&4xl0 2 W/m·K 2.39x10-3
Power I ft. lbf/s 1.356 W 0.738 � ..,, = 6.895 kPa 0.145
I mmHg
l [bf-ft l.355x!o-J kJ 7.38xJ0 2 2.39x 10-2
· Pressure I lbf/in2 6895_ Pa . l.45x J()-4
1 cal/s·cm 2 ·° C = 41.84 kW/m2 ·K .,.
.
I atm. 1.0 I3x I 0_2 kPa 9.87x10-J
I bar 100 kPa 0.01 TEMPER ATURES
1 inHg 3386 Pa: 2.95x J0-4
·,TABLE-3
Stress 1 lbf/in2 6.8948x I oJ kPa . l.4504x I o-4
Interconversion of Temperature
°
Thermal I Btu·ft/h·ft2 ·° F L730 W/m·K 0.578 and Rclevant Equations
conductivity 1 Btu·_irii'h·ft2, ° F 0.1442 W/m'·K. 6.935
I R (Rankine) = (1118 ) K'(Kelvin)
Thermal . 1 °F·ft2 ·hl8tu 1.761x10 2 K·m2fkw 5.679x 10-J
resistance I lbf/ft2 4.788x 10-2 kPa l K (Kelvin) i.i '"� = 1.8 R (R;mkine)
20.886 -c:•:i
TR (Rankine) =_T° F + 459.67
Vacuum I inHg (60 ° F) 3.377 kPa 0.2961
I inH2 0 (39.2 ° F) T°F (17ahrenheit) = T R - 459.67
0.2491 kPa 4.0 145
T°C (Celcius) = ( ° F- 32)/l .8 ° C
Velocity I ft/s D.305 mis 3.281
I in/s T°F (Fahrenheit) = 32 + l ..8° C
0.0254 mis 39.37
t.T° C = 1.8 t.T° F = t.T K
490
 I
:\pdx-lV IJ[ITSITIO'NS AND MEANINGS 493
Black .body : It is a body that radiates maximum possible amount of
energy at a given temperature.
APPENDIX-IV
Blending : It is mixing of powdc:rs smoothly and inseparably together.
Bound water : Is the min.irnum water held by the material that exerts an
DEFINITIONS AND MEANINGS equilib.rium vapour pressure less than tht! pure water at the same
Actual screen : A screen which does not give perfect separation about the temperature.
cut diameter of the powder. Bulk transport ls the movement of a large portion of a material from
0
Agitation : Refers to the induced motion of a material in a specified way, one location to another location in a given system.
usually in a circulatorr_ pattern. insiric a container. Caland�ia : It is a steam compartm�nt, which consists of a nu.mber of
Air bindin.g: ·1n centrifugal pumps, the entry of air into the pump at the· tubes fitted in a vessel and is included in the evapor4tor.
initial stage practically stops oelivering · the liquid. This phenomenon Caking : Is the process of forma_tion of clumps or cakes when crystals arc
is known as air binding. improperly stored. r
·c'
Amorphous solids : These are the solids which do not have soecific C:1vitation : it is a phenomenon of foni1:ition of vapour bubbles and their
shape. · � " •
sudden collapse in a pump.·
.
Attrition : It involves breaking down of the material by rubbing action Centrifiigal effect : It is ex.pressed as a ratio of y entrifugal force to .
, .
between two surfaces. gravitational force. . .
Axial angle : It is an angle between the two perpendiculars to .1e Centrifugal force·: It is due to inerti': of a r�tating body and it acts �n the
intersecting faces in a crystal. · rotating body in a direction away from the point or axis of rotation or
Axial flow of liquids : The flow of liquid that acts in a direction parallel re.volution.
to t�e impeller shaft. · Centrifugal pump : An hyJra�ltT� machine which converts the mechanical
energy into pn:ssure energy by means of centrifugal force.
00

Axial length : It is the distance between centres of two atoms in a

crystal. Centrifugation : It is a unit operatiot1 employed f<?r separating the
constituents ·present in a dispersion with the aid of centrifugal force.
Azeotropic distillation : ·11 is a distill�tion md16d _in which azeotropic
mixture is broken by the addition of a third substance, which forms a · Clarificanon : It is a process or'separation-of liquids containing solids not
new azeotrope _with one of the components. exceeding 1.0%.
Azeotropic . solution : It is a solution which distils unchanged at a, Coefficient of thermal conductivity : Is defined as the quantity of heat
flowing per second across one square metre area of cross section of a
constant temperature.
slab of the material of one metre thickness, whose faces are_ maintai11ed
· arranged on a shaft.
Belt idlers : These ·are supporting rollers, which are <\t a steady temperature difference of one dcgrc: Kel.vin.
below the belt.
Compression : It is a means by which the material is 1.:rushed between
Bernou-lli's theorem: States that in a steady state, ideal flow qf a incom­ rollers by the application of pressu�e.
pressible fluid, the total. energy per unit mass, which consists of Conduction : It is a process in which heat flow in a body is achieved by
pressu_re energy, kinetic energy and datum energy, at any point of. the the tr.ansfer of the momentum of individual atoms or molecules with­
fluid ' is constant. · ·
out mixing.
Binary liquids : Arc those liquids which arc miscible with one another in Convection : H is a process in which heat flow is achieved by _actual
all proportions. .. mixing of warmer portions with cooler portions of the same material.
Biological corrosion : The metabolic action of microorganisms can either Corrosion : Is a reaction of a metallic material with its environment,
directly or indirectly ,causes deterioration of a metal (corrosion). which causes a measurable change to the material and c'an result in a
, . .
492 function,\! failure of the metallic component or of a compl_ete system.

494 Pl IAR'.vlACEUTICAL ENG!NEER!NCi
Apdx-lY
Critical humidity : Is ·the humidity above which crystals absorb moisture
.Energy bal::rnce : The law of conservation o( energy states that the energy
·c.and below which .. they do not absorb moisture.
Crystal : It is a solid particle, which is fonned by the soliclififatLon
(crystallisation) process (under suitable environment) of a substance in
which structural units are arranged by a fixed geometric pattern or
lattice.
.· Erosion : It is the destruction o� a metal by abrasion and attrition caused
Crystal growth .: It is a diffusion uf solute molecules or ions from
solution to reach the faces of a crystal, which helps in their growth.
Crystal hydrate : It is a solid substance which associates with water.
Crystal· lat tice : It is the orderly internal arrange111ent of piirticlcs in three
···
dimensional space.
Crystallization :· ls a spontaneous arrangement of the particles into a
repetitive orderly array, i.e., regular geometric pat.�erns.
. · ...
Cutting : It is a mean s of tearing the material by a sharp blade.
Dalton's law : It states. that the total pressure cx�rtcd by an ideal gaseous
mixture is equal t.o the su1i1 of the individual partial pressures or the,
component gases, if alone were present and occupied the total vollirne.
Depth filtration : It is .a fiitration proces,;, in which the slurry penetrates
to a point where the diameter. of solid par1iclc� is greater than that of
the tortuous void or channel.
Destructive distiliation : It is a distillatiun method in which the distillate
is a decomposition product of the constituents of the organic matter
burnt in the absence of air. . .
.
Diaphragm : lt is a flexible physical barrier.
. .
Distilla�d : The feed liquid mixture to be distilled.
Distillate (co�dcnsatc): The liquid condensed during distillation.
, Distillation : It is a separation of the components of a liquid mixture by
p�ocesses involving vaporisntion 'and subsequent condensation at
an(?ther place.
Double acting pump : lt is a pump that· Ji:splaccs waler on both halvcs of
· the cycle of the movement' of the pumping eiement (piston or plung.er),
. i.e., during up-stroke and down-stroke. ·
Drop-wise condensation : It is a process in which the condensed liquid
• c�llects as drops thar may range from microscopic size up to drops
that are seen with the naked eye..
Drying : It is .a process of removal of small amounts of water or other
liquid from Qa material by the \!pplication of heat.
Energy : The energy of a body is measure of the capacity or ability of the
body to do work.
·,
j
DEFINITIONS ANO MEANINGS 495
output must be same as the .en.ergy input in any process.
1, "'' �
Equilibrium m9isture content (EMC): ls the amount of water present in"°
the solid,-which exerts a vapour pressure equal to the vapour pressure
of the atmosphere surrounding it
by the. flow of liquids or gases.
Eutectic point : The temperature and pressure at which the· frozen solid .·
vaporis�s without conversion to a_ liquid.
Evaporation : It is a process of vaporising large quantities of volatile
liquid to 'get a conccntr.atecl product. .
Extractive distillation : It is a distillation metho� in which azcotropic
mix.lure is broken by the addition of a third substance which is rela­
tively nonvolatile liquid compared to the components to be separated.
Film type· condensation : A p.rocess in which' the condensed liquid wets
the surface on which it is condensing and forms a continuous film of
condensate.
Filter aid : _It fonns a surface deposit which screens out the solids and
also prevents plugging of the supporting filter medium.
Filter cake: The accumulated solids that are retained on the filter
. meciium..
Filter mc�iu.m : ls a porous medium used to retain the solids..
Filtrate: The clear liquid that has passed through the fiiter·mepium.
Filtration : ls a process of separation of solids from a fluid by passing the
sam'e through a porous medium that retains the solid but allows the
fluid to pass through.
Filtration centrifuge : A centrifuge in which solids pass through the
porous. medium based on the difference in the i:lensities of the solid
and liquid phases on application of centrifugal force.
· Flash distillation (equilibrium distillation): It is a distillation process in
which the entire liquid mixture is suddenly vaporised (flash) by pass­
ing the feed from a high pressure zone to a low pressure zone.
Flaw in .a particle : It is a structural weakness th.at may develop into a
crack under strain.
Flight in conveyor : The conveying mechanism such a_s screw element
used in the scr, v conveyor. i
Fluid dynamics : It .deals with the study of fluids in motion.
Fluid flo,w : It is the study of flow of substances that do not pernrnnently
resist distortion. j
 Apux-lY DITINlTIONS AND Ml:ANINGS ·
497
496 PIIARMACEUTICAL EN(i!NEERIN(i
Fluid statics : It deals with the fluids at rest in equilibrium. Kinetic ener�y : Of a body is the energy p osscsscxl by the body by virtue
of its motion.
rluiclisc<l state : �l is a state in which solids arc suspended in a stream
of Laminar flow (viscous now) : Jt is a fl ow, in \';hich the fluid particles
air.
rnow. in·l.lycrs or lamin;.ir with .one layer sliding over the other.
Forced convection : It is a l1cat transfer process in which mixing o f .
fluid Laminar mixing: Is the mixing of two d issimilar liquids thrnugh laminar
is ob.taincd by a stirrer or agitator or pumping the fluid for recirculation. .
now, i.e .. th� applied shear stretches tke interface between them..
Fourier's law : This law states that the rate of heat flow throucrh
a Latent IH�,�t of •,aporisation : Is defined as the_ � uantit_ y of heat req� ir�d
uniform metal is proporti onal to the area, the temperature drop;;:, and
' to convert a t1nit mass of the liquid at its b o 1lmg point from the hqu1d
inversely proportional to the length of the path of flow
to the vapour stale without a change in temperature. ·
Fractional distillation : ll is a distillat ion process in which. vapor
isation Manometers : These arc the devices used for the measurement of pres­
of liquid mixrure gives rise to a·mixture of constit
uents froni which the sure diff1: rcn.ce at a point of lluid.
desired one is separated in pure form.
Ma tei:ial bala.ncc : The law o f conservatio n of matter states that . material
Fractionating column : It is a special type o f still-head in which c onden­ cannot be dc�troyed or created, it can be changed from one fom1 to
. sation and revaporisation take place simultaneously. another.
. . ., . ·
Fr"e moistur:e content (FMC) : Is· the amount of water that is f ree (easy) Micr's supersaturation' theory : Postulates � definite rc�ationship
to evaporate from the surface. between concentration and temperature at which crystals will sponta-
Galvanic corrosion : Corrosion associated with the flow of current to a neously form in an initially unseeded soluti on.
l�ss-activc metal (cathode) from a more-active metal (anodi;:) · in the Miscible liquids : These liquids arc miscible inall proportions. .
same i;nvirontncnt. .
Mixing : Putting together in one m ass or assemblage with m o r e. or less
Grey �ody : It _is a body ·whose absorpti°vity is constant at alt wavelengths
. tlwrou�h diffusion of the constituent clements among one another.
ofradiation; at a given ti::111per·ature.
Mixing : �s a process that tcnds to result in a randomization of dissimilar
-
Heat exchanger : It is a hcaiin!!. .device' used for transferrino heat
one fluid (hot gas or steam) to another fluid through a metal wall.
. ;;:, from particl·:s within a systcm. .· .
Molecular <liffu�ion : ls the mixing a·t molccldar level in which mokculcs
Heat interchanger : It is a heating device used for
-
transferri_ng heat from dirfusc due t o thermal motion. .
one . liquid to another liquid or from one !!as 'to another oas thro·uah a ..§)

· · � Molecular distillation (short path distillation or evapora_tive distilla­

' etal
. wall.
;;:,
m .
Ideal s creen : A screen which sharply separates the feed mixture in such tio,n: It is a distillation method in which each ll\Plcculc m the vn.pou1;
phnse trav�ls mean free path and gets condensel individually without
a way that th; smallest particle iii the oversize will be just larger than
inh·nno!ccular collisions on appli�ati on of vacuum.
the largest particle in the undersize.
Natural con netion : It is a heat transfer process in which mixing' o f
Ideal solution (perfect solution) : h is a solution in which the attractions !luids is acco1nplishod byf,.M'the natural currents set up, wher, body of
between. unlike molecules a·r e. of the· same order as between like· flu id is heated. , .,,
.,,.,

molecules.
lm;,PaCt : It involves the· 'operation of splitting the material apart; when a
�lump of material strikes against the rotating hammers.
Inertia : It is the intrinsic property of a body by virtue of which it cann ot
0 .
. ..
Nucleation· : . i.t refers to the birth of very small bodies _ of _ a. ne-.�· ph_asc
within a homogenous supersaturated liquid phase, w,h1ch 1s responsible
for crystallisation. ·

Q,·cr-sizc powder : Tl1e 111atc'.r·1 al ·that r em ains on the ·given_ screening

,,

change by itself its state of rest . or uniform r1otion along a straight line.
surface.
Isomorphis m : It is a phenomenon in whi ch tw o or more substances
Partially miscible liquids : These .are t�e liquids, which �re miscible in
· possess the same crystatl inc· fonn and ·crystals of one such substance
one another �t one particular proporti on.
can be gro:vn in the saturated solution of the other..

49S PHARMACEUTICAL ENGINEERING
Permeability : It is the now rate of a liquid of unit viscosity acr�ss a unit
area <;>f cake thickness under a pressure gradient of unity.
Pitch : It is the distance the propeUer would move through · the fluid p�r
. revolution, if .!?lippage docs not occur. · . allowing it to come in contact with the cold su�face.
Polyn1orph : It is a chemical substai1ce, which can exist in more than one
crystalline· form.
Potential energy : It is t.he energy possessed by the body by virtue of its
posi\ion or configurat,ion. o
• •
Power pump : It is a pump in which the moving element (pistorJ or
plunger) is actuated by some form of �nergy other than steam.
Pressure head: It is defined as the height of a column of liquid of know.n
·· density, which is numerically equal to a pressure term.
Pscudomorph : It is a solid fomi, which arise ,because of inclusion of
small amounts of solvent of crystallisation.
Radiar -now of liquid : It is the flow of liquid that acts in a direction
vertical to thc: impeller shaft.
Radiation : It isQa process in which heat flows through sp:ice by means of
electromagnetic waves.
.
Raoult's law : It. states. that the partial v apour pressure of each volatile
constituent is equal to the vapour pressure of the pure constituent
multiplied by its mole fraction in, the solution at a give11 temperature.
Rd'al solution (perfect sohJ(ion) : The solution which does not ob.ey ideal
solution behaviour or which do not obev. Raoult's law . " ...,.
.
Reciprocating pump: It is a pump ·in wl1ich the pumping element moves
in a forward and backward directions in a cylinder.
Reducing valves: These are the valves used in order to maintain uniform
. pressure in one part of the system at a level lower than the pressure in
another part of the system.
Reynolds number : It is a ratio of inertial · force to viscous
. force of a
flov,ing fluid.
·Rotary positive displacement pump : It is a pump in which liquid i,
·. mechanica:lly 'displaced by the" rotation of one or more elements within
a stationary housing.
Scdimcnta.tion centrifuge : A centrifuge that produces sedimentation of
solids based on the difference in the den:;ities of two or more; phases of
the mixture.
Self-priming pump : It is a pump, which can remove air from casino� bv.
suitable mechanism. ·
Ap<lx,IY DEFINl"rlO:>JS AND ME/,NINGS 499
Sieve number : It indicates the number of meshys per )inear length of,
0.0254 m (one inch}
a..
Simple distillation : Is a pr.ocess of converting a �ingle. 'constituent from
liquid (or .mixture) into its vapour, transferring the. vapour t_o another
place and recovering the liquid by condensing the vapo�r, usually by:
.
Single acting pump : It is a pump, which displaces \\'ater on one hal(of
th1.: cycle of the movement of the pumping element (piston or plunger)•
.
i.e., during the down stroke.
Size reduction: Is a process of reducing large solid unit masses (vegeta­
ble or chemical substances) into s_mall urtit masses, coarse particles or
fine particles.
Size separation : It is a unit operation, that involves the separation of a
mixture of various sizes of particles into twoJor more portio9s . by
means of screening surf�ces.
Steady state system : Tl�e system· is said to be ·in steady state, if the
operating conditions do not vary with \imc:
Steam di�tillation : It is a l)l�thod of distillation carried with. the aid of
steam anct.Js" used for th� 'separation of high boiling substances fro.�
nonvolatile impurities.
Stoichiometry : It m'cans carrying out of calculations, based on quantita­
tive relationships.
Sublini"ation : It is a process in \;hich direct change of water from solid
into vapour takes place without conversion into a liquid· phase.
Supersaturated solution : Is one that contains· more of the dissolved
solute than it would normally contain in a saturated solution at a
definite temperature.
Su.rface coefficient : It is the conductive capacity of the stagnant film for
the trans for of heat.
. Surface filtration : It is a screening action .(filtration process) by .which
. pores or holes. of the rnedi�m prevent the passage of solids.
Tangential now of liquid :. It is the flo\� of liquid that acts in a direction
tan o�ent to the circle of rotation around the impeller shaft.
Thermal condl!ctivity : It is the reciprocal of thermal resistance.
Turbulent flow : A flow is said to be turbulent, if the Reynolds number is
more thar. 4000 in' a pipe.
.
Turbulent' !low : It is the flow in which the fluid particles continuously
transfer momentum to adjacent layers.
500 Pl Ii\ RM AlTl JTIC AL ENGINEERIN(i

Turbulent m1xmg is mixing due to turbulent flow, whi.ch results in

random fluctuation of the fluid v�locity at any given roint within the Al'f'ENDIX- V
system.
Unbound }Vatcr : Is the amount of water (moisture) !1eld by the material BIBLIOGRAJ>HY
that cx'e11s an equi�ibrium vapour prc�surc equal to th.:11 of pure waler
at .the same temperature. I. L.,\ Ra\\lins. /Jc:111/ey 's Textbook of l'harnwceutics, gth edition; Oailicrc
Tindall. L,.111Jo11, 1977.
Under-size powder : The material that c;an pass through the screening
surface .
2. · S.J. Carter, CopJler & Gunn's Tutorial Pharmacy,, 6111 edition, The · · Kothari
Buok Depot; Homb:iy, 1972.
Unit cell : It is the smallest geometric portion of the crystal, which repeats
3. J. Pulderman, Introduction lo Plwrmaceutical Production,. Novib, The
to build up the whole crystal. llagqe, 1990.
Unit, orieration : A process frequently consists of a fewer number of ·L \-I.E. i\ulton, l'harmacc11tics, ELBS Churchill Livingstone, 1988.
distinct individual steps. Each step is called unit operation.
5. L. l.achman, I !.A. Lieben'nan and J.L Kanig, The Tlzeory and Practice of
Unit pr�ccss : It is one in which several unit operations arc ·combined in a !11J11strial l'harmucy. 2nd & 3 rd editions, Lea &. �ebi ger, Philadelphia, 1970
se quence to achieve the objectivr;s of a chemical or physical pr9!ess. .
& !985.
Unsteady state : If the operating conditions are varying with time, then (1. A.L. Gennaro, Remington "s Phar111accutical Sciences, gth edition, Mack.
the system is said to be in unstead y state. l'ublishin g Company. Pennsylvania. 1990.
Validation : It is a procedure that demonstrates the ability of consistently 7 . .I .I. \V eils. !'harmaceutical l'reformulutions, Ellis Horwood _Limited,
producing a product \Vith the established specificatioDs under ideal Chi,kt.:ste:-. 1988.
"conditions. 8. Indian /'/wrnwcopocia. 3 rJ edition, The Controller of Publications, Delhi,
Valve : It is a d;vice used to control the rate of flow of fluid in a pipelirl'e. 1985.
Variable area meter : It is a device that mensures the area of flow, so as (). \\'.L. 1 BaJgcr anJ J.T. Banchero, /11trod11ctiu11 lo Chemical Engi,ieering,
lv!c(ir,m-l lill lfook Cl.)mrany, Singapore. !955.,
to produce a constant head differentinl.
10. \V.L lvkCabe, J.C. Sn1ith and r. Harriott, Unit Operations of Clzemi�a/.
Variable head meter : It is a device that measures the variation in tbe
£11gi11eeri11g, 5th edition, :VkGraw-Hill Book Company, Singapore, !993.
pressure across a fixed constric_tion placed in the path of flow consist-
ing of a constant area. · 11. IU !. Perry anJ D. Green, Perry's Chemical Engineer's Handbook, 61h
edition, �kCiraw-llill Book Company, Singapore. 1984.
Vi!:cous flow : A flow is said to be viscous if the .Reynolds number is less
than 2000 in a pipe or the _fluid flows in layers. i 2 . .J.M. Coulson. J.F. Richardson, J.R. Backhurst and J.H. Harker. Chemical
Fnginccriny;, V olumc 2. i st . and 2 nd edition; Asian Book Private Limited,
Volatility : Of any substance in solution may be defined as the. equilib­
riuf!1 partinl pressure of the substance in the vapour state divided by
New Dt.:lhi. l 998.
.
I J. l l.i\. Lieberman and L. Lachman, Pharmaceutical Dosage Forms. Tablets,
the mole fraction of the substance in the solution. - .. V olume 2, Marcel Dckker, Inc., New York, 1981.
·. .,.
Vortex : It is a strong circulatory flow pattern manifest:, near the impeller
l
I ·L K.E. A vis, I I.A. Lieberman and l�. Lachman, Pharmaceutical Dosage
shafr Forms. PareJJtcral Afedications, V �lumc 2, 2nd edition, Marcd Dekker,·
. ...
Youn g's modu:,,, : The ratio of the lon:;.itudinal stress to the longitudinal l1H�., New York, 1993.
strain within eb:.tic limits. 15. C.V .S. Subrahmanyam, Tatbook of Physical Pha,Jizaceutics, 2nd cdj.tion,.
\
Zro'tropic mixture : It is a mixture whoso:: total vapour presstlrc is always V allabh l'rakashan, Delhi; 2000.
intermediate between those of pur.: components. 16. M.L. Schrort: General Pharmacy; 'f>art I, National' £look Centre, Calcutta.
1970..
,; ,,·,j: 501
.•
502 PHARMACEUTICAL ENGINEERING

17. R.M. Mehta, Pharmace11tics-/, 2 nd cJition, Vallabh Prakashan, Delhi, 1998.

18.. n.M. Mithal, Textbook of Forensic Pharmacy, I o ni edition, Vallabh
Prakashan, 1999.
19. O.P. �hanna and M. Lal, A Text book of Material Science and ,\Jetal/11rK)',
Dhanpat Rai & Sons,
20. B.S: Jaiprakash and R. Venugopal, Chemistry for Engine,?ring Students,
Subash Publications,
21. M. Peters, and· K.D. Tirmcrhaus, Plant Design and Economics for Chemi­
cal Engin�ers. J fd edition, McGraw-Hill lnterr.ational Book Company,
1981.
22. G.T. Austin, Shreve 's Chemical Process lnd11stries, 5th edition, McGraw­
Hill Book Compan�, 1986.
23. R.K. Bansal; A Textbook of Fluid Mechanics and Hydraulic Machines, 6th
edition, Laxmi Publications (P) L)d., New Delhi, 1998.
24. O.A. Hougen, K.M. Watson and R.A. Ragatz, Chemical Process Princi­
ples, Part J and Part Jl, CBS Publishers & Distributors, New Delhi, 1995.
25. P.K. Nag, Engineering Thermodynamics, 2nd edition, Tata McGraw-Hill
Publishing Company Limilecl, New Delhi, 1995.
26. Indian Standard: QuMtitic� and U11i:s, flurcau of Indian Standards, New
Delhi, 1995.