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SICA SENIOR SECONDARY SCHOOL

NO. 2

SESSION: 2018 – 19

CHEMISTRY INVESTIGATORY
PROJECT
TOPIC: PREPARATION OF DOUBLE SALTS

SUBMITTED BY- SUBMITTED TO-


XXXX XXX
CLASS: XII ‘A’
ROLL NO:
CERTIFICATE

This is to certify that XXX of Class XII ‘A’ of SICA S.S.


SCHOOL NO.2 has successfully completed the
Chemistry Investigatory Project on the topic Preparation
of Double Salts
under the guidance of Chemistry teacher Mrs. Annie
Thomas in partial fulfillment of curriculum of
Central Board Of Secondary Education (AISSCE)
for the academic session 2018-19.

INTERNAL SIGNATURE EXTERNAL SIGNATURE

SCHOOL SEAL PRINCIPAL SIGNATURE


ACKNOWLEDGEMENTS

I would deeply like to thank our Honourable Principal,


Dr. XXX , Vice Principal , Ms. XX and Chemistry
Teacher , Mrs. XXfor giving me a golden opportunity for
making a successful project on the topic
Preparation of Double Salts.
I am thankful to my esteemed teacher for guiding me and
providing lab facilities to conduct the experiments .This
project helped me to explore my knowledge, and do
research work.
Secondly, I am grateful to my parents for providing me all
the materials required to complete this project within
limited time in an organized manner.
CONTENTS

TITLE PAGE NO.


1. DOUBLE SALTS 01
2. MOHR’S SALT 03
3. POTASH ALUM 06
4. AMMONIUM ALUM 10
5. METHODS OF PREPARATION 12
5.1 EXPERIMENT 1
5.2 EXPERIMENT 2
5.3 EXPERIMENT 3
6. BIBLIOGRAPHY 19
DOUBLE SALTS
Double salts are salts containing more than one cation or anion,
and are obtained by combination of two different salts which
were crystallised in the same regular ionic lattice.
Examples: Aluminium Sulfacetate(Al2SO4(CH3CO2)4) ,
Rochelle’s Salt(
KNaC4H4O6·4H2O) etc.
Each salt in the mixture has its own unique crystal structure.
Properties of Double Salts are –
1. A double salt is combination of two or more different salts.
2. A double salt completely disassociates in ions in water and
gives simple ions. An aqueous solution of a double salt is
composed of cations and anions which were in the initial two
salt compounds.
3. A double salt can be easily analysed by testing the presence of
simple cations and anions present in it.
Points of Difference between Double Salt and Complex Salt
are –
1. Double salts completely dissociate into its ions in water
whereas Complex salts do not completely dissociate into its

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ions in water.

2. Double salts give simple ions when added to water whereas


Complex salts do not give simple ions.

3. Double salts can easily be analyzed by determining the ions


present in the aqueous solution whereas Complex salts cannot be
easily analyzed by determining the ions in the aqueous solution.

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MOHR’S SALT
(AMMONIUM IRON SULPHATE /
(NH4)2SO4Fe(SO4)2.6H2O)

Ammonium iron sulphate, or Mohr's salt, is the inorganic


compound containing two different cations, Fe2+ and NH4+, and
an anion SO42-. It is classified as a double salt of ferrous
sulphate and ammonium sulphate.
The ammonium ions make solutions of Mohr's salt slightly
acidic.
Mohr's salt is named after the German chemist Karl Friedrich
Mohr, who made many important advances in the methodology
of titration in the 19th century.

STRUCTURE:

This compound is a member of a group of double sulphates


called Schonites or Tutton's salts. Tutton's salts form monoclinic
crystals and have formula M2N(SO4)2.6H2O (M = various
monocations). With regards to the bonding, crystals consist
of octahedra [Fe(H2O)6]2+ centers, which are hydrogen bonded to
sulphate and ammonium. Crystals are monoclinic in shape.

PREPARATION:

Mohr's salt is prepared by dissolving an equimolar mixture


of hydrated ferrous sulphate and ammonium sulphate in water

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containing a little sulphuric acid, and then subjecting the
resulting solution to crystallization. Ferrous ammonium
sulphate forms light green crystals.
Detailed steps of preparation of Mohr’s salt will be discussed
later in this project.

PROPERTIES:

CHEMICAL FORMULA (NH4)2SO4Fe(SO4)2.6H2O

MOLAR MASS 284.05 g mol -1 (anhydrous)


392.13 g mol -1 (hexahydrous)

APPEARANCE Blue – green solid

DENSITY 1.86 g/cm3

MELTING POINT 100 to 110οC ; 212 to 230οF ; 373 to


383K

SOLUBILITY IN WATER 269 g/L

INPURITIES PRESENT Mg , Mn , Ni , Pb , Zn

n - FACTOR +1

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USES:
1. This salt is used as an efficient source of ferrous ions( Fe2+ )
due to its long shelf life.

2. It is used in the Fricke's dosemeter to measure high doses of


gamma rays.

3. It is used in titrations as a reducing agent where KMnO4 is


used as an oxidizing agent.

4. A solution of Mohr’s salt is used as a ‘primary standard’


because of its purity and high stability.

5. A solution of Mohr's salt can be sprayed on a lawn to kill


moss without harming the grass.

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POTASH ALUM
(POTTASIUM ALUMINIUM SULPHATE/
KAl(SO4)2.12H2O)

Potassium alum, potash alum, or potassium aluminium


sulphate is a chemical compound: the
double sulphate of potassium and aluminium, with chemical
formula KAl(SO4)2. It is commonly encountered as
the dodecahydrate, KAl(SO4)2·12H2O. The compound is the
most important member of the generic class of compounds
called alums.
It is very soluble in water. The solution of alum is slightly
acidic.
When heated to nearly a red heat, it gives a porous, friable mass,
which is known as "burnt alum". It fuses at 92 °C (198 °F) in its
own water of crystallization.
Potassium alum may be a weak irritant to the skin.

STRUCTURE:

It crystallizes in cubic structure and lattice parameter of 12.18 Å.


Potassium alum crystallizes in regular octahedra with flattened
corners.

PREPARATION:

NATURAL OCCURENCES: 1.Potassium alum dodecahydrate


occurs in nature as a sulphate mineral called alum-(K), typically
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as encrustations on rocks in areas of weathering and oxidation of
sulfide minerals and potassium-bearing minerals.

2. In the past, potassium alum has been obtained from alunite


(KAl(SO4)2.2Al(OH)3), mined from sulphur – containing
volcanic sediments. In order to obtain alum from alunite, it
is calcined and then exposed to the action of air for a
considerable time. During this exposure it is kept continually
moistened with water, so that it ultimately falls to a very fine
powder. This powder is then lixiviated with hot water, the liquor
decanted, and the alum allowed to crystallize.

INDUSTRIAL PREPARATION: Potassium alum is now


produced industrially by adding potassium sulphate to a
concentrated solution of aluminium sulphate. The aluminium
sulphate is usually obtained by treating minerals like
alum schist, bauxite and cryolite with sulphuric acid.If much
iron should be present in the sulphate then it is preferable to
use potassium chloride in place of potassium sulphate.

Methods of preparation of potash alum in laboratory will be


discussed later in this project.

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PROPERTIES:
CHEMICAL FORMULA KAl(SO4)2.12H2O
MOLAR MASS 258.192 g/mol (anhydrous)
474.43 g/mol ( dodecahydrate )
APPEARANCE White crystals
DENSITY 1.75 g/cm3
MELTING POINT 92 to 95οC ; 198 to 203οF ; 365 to 368K
BOILING POINT 200οC ; 392οF ; 473K
SOLUBILITY IN WATER 14 g/100 ml ( 20οC )
36.80 g/ 100 ml ( 50οC )
REFRACTIVE INDEX 1.4564
TASTE Astringent taste

USES:
1. Potassium alum is used in medicine mainly as an astringent
(or styptic) and antiseptic.
2. Potassium alum is used to reduce blooding and to relieve
stings and bites.
3. Potassium and ammonium alum are the active ingredients in
some antiperspirants and deodorants, acting by inhibiting the
growth of the bacteria responsible for body odour. Alum's
antiperspirant and antibacterial properties contribute to its
traditional use as an underarm deodorant.
4. Potassium alum is used as a fire retardant to render cloth,
wood, and paper materials less flammable.
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5. Alum has been used since antiquity as mordant to form a
permanent bond between dye and natural textile fibers
like wool. It is also used for this purpose in paper marbling.
6. Alum solution has the property of dissolving steels while not
affecting aluminium or base metals.
7. Potassium alum was formerly used as a hardener
for photographic emulsions (films and papers), usually as part of
the fixer.
8. Potassium alum is also effective for preventing gum disease
and cleaning teeth.
9.Alum is used as a flocculant to remove unwanted colour and
turbidity from drinking water. When added to raw water reacts
with the bicarbonate alkalinities present in water and forms a
gelatinous precipitate.This floc attracts other fine particles and
suspended material in raw water, and settles down at the bottom
of the container.
10. Alum is also used in many skin problems like acne and
pimples.

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MELTING POINT 93.5οC ; 200.3οF ;

AMMONIUM ALUM
(AMMONIUM ALUMINIUM SULPHATE/
NH4Al(SO4)2.12H2O )
STRUCTURE:
It is a white crystalline double sulphate usually encountered as
the dodecahydrate. It has a hexagonal crystal structure when in
an anhydrous state and a cubic crystal structure when in a
hydrous state. It has an octahedral coordinate geometry.
PREPARATION:
NATURAL OCCURENCES: The dodecahydrate occurs
naturally as the rare mineral tschermigite.
INDUSTRIAL PREPARATION: Ammonium alum is made
from aluminium hydroxide, sulphuric acid and ammonium
sulphate. It forms a solid solution with potassium
alum. Pyrolysis leaves alumina.
PROPERTIES:
CHEMICAL FORMULA NH4Al(SO4)2.12H2O
MOLAR MASS 237.15 g/mol (anhydrous)
453.33 g/mol (dodecahydrous)
APPEARANCE Dull white crystals
DENSITY 2.45 g/cm3 (anhydrous)
1.64 g/cm3 (dodecahydrous)

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BOILING POINT 120οC ; 248οF ;
398K(dodecahydrate)
MELTING POINT 93.5οC ; 200.3οF ; 366.6K
SOLUBILITY IN WATER 15 g/ 100ml at 20οC
(dodecahydrate)
pH 3 to 5 (slightly acidic)

USES:
1. It is used in water purification.

2.This salt is used in tanning, dyeing and in fireproofing textiles.


3. It is used in vegetable glues.
4. It is used in porcelain cements.
5. It is used in deodorants.
6. It is used in the production of grinding powders and as
precursors to synthetic gems.
7. Ammonium alum is a common ingredient in animal repellant
sprays.
TOXICOLOGY OF AMMONIUM ALUM:
Alum was once a common pickling ingredient used to promote
crispness in preserved vegetables, due to the way it reacts with
natural pectin. It has fallen out of use from a suspected link
to Alzheimer's Disease, and is no longer recommended for
pickling.

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MY PROJECT: METHODS OF PREPARATION OF
DOUBLE SALTS –
EXPERIMENT 1: PREPARATION OF MOHR’S SALT
AIM: To prepare a pure sample of Mohr’s salt.
REQUIREMENTS: Beakers, china dish, funnel, glass rod, hot
plate, Ferrous Sulphate crystals, Ammonium Sulphate crystals,
dilute H2SO4, ethyl alchohol.
PROCEDURE: 1. Take a 250ml beaker and add 7.0g ferrous
sulphate crystals and 3.5g of ammonium sulphate crystals to it.
Add about 2-3ml of dilute sulphuric acid to it to prevent
hydrolysis of ferrous sulphate.
2. In another beaker , boil 20ml of water for about 5 minutes.
Add the boiling water in the first beaker. Stir it continuously
until the salts have completely dissolved.
3. Filter the solution to remove undissolved impurities and
transfer the filtrate to a china dish.
4. Heat the solution in the china dish for some time to
concentrate it to crystallization point. Immediately place the
solution in the china dish over a beaker full of cold water , on
cooling , crystals of Mohr’s salt separate out.
5. Decant off the mother liquor quickly. Wash the crystals in
china dish with a small quantity of alcohol to remove some
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sticking of dilute sulphuric acid on salt.
6. Dry the crystals by placing them between filter paper.
REACTION:
FeSO4.7H2O + (NH4)2SO4 FeSO4.(NH4)2SO4.6H2O(aq)
(Ferrous (Ammonium (Mohr’s Salt)
Sulphate) Sulphate)

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EXPERIMENT 2: PREPARATION OF POTASH ALUM
AIM: To prepare a pure sample of potash alum.
REQUIREMENTS: Beakers, china dish, funnel, glass rod,
wire gauze, Bunsen burner, Potassium Sulphate, Aluminium
Sulphate, dilute sulphuric acid.
PROCEDURE: 1. Take a 250ml beaker. Transfer 2.5g of
potassium sulphate crystals to it. Add about 20ml of water. Stir
to dissolve the crystals.
2. Take another 250ml beaker and transfer 10g of aluminium
sulphate crystals to it. Add about 20ml of water and add 1ml of
dilute sulphuric acid to prevent hydrolysis of aluminium
sulphate crystals to it. Heat for about 5 minutes and filter the
solution if milkiness still persists.
3. Mix the two solutions in a china dish and place the china dish
over a wire gauze placed over a burner. Stir the solution with a
glass rod. Concentrate the solution till crystallization point is
reached. Place the dish over a beaker containing cold water.
4.Crystals of potash alum will separate out. Decant off the
mother liquor and wash the crystals with cold water.
5. Dry the crystals by placing them between filter paper.

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REACTION:
K2SO4 + Al2(SO4)3.18H2O + 6H2O
K2SO4.Al2(SO4)3.24H2O
(Potassium Sulphate) + (Aluminium Sulphate)
(Potash Alum)

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EXPERIMENT 3: PREPARATION OF AMMONIUM
ALUM
AIM: To prepare a pure sample of ammonium alum.
REQUIREMENTS: Beakers, china dish, funnel, glass rod,
wire gauze, tripod stand, Ammonium Sulphate crystals,
Aluminium Sulphate crystals, dilute sulphuric acid.
PROCEDURE: 1. Take a 250ml beaker. Transfer 15.8 of
aluminium sulphate crystals to it. Add about 15ml of water. Heat
the solution to dissolve the crystals. Add requisite amount of
water to make it upto 25ml before that make sure it is
completely dissolved.
2. Take another 250ml beaker and transfer 3.3g of aluminium
sulphate crystals to it. Add about 15ml of water and add 1ml of
dilute sulphuric acid to prevent hydrolysis of aluminium
sulphate crystals to it. Stir the solution until it is completely
dissolved. Add requisite amount of water to make it upto 25ml
before that make sure it is completely dissolved.
3. Mix the two solutions in a beaker. Allowing the beaker to
stand at room temperature will produce only few crystals of
ammonium alum.
4. Place the beaker over a wire gauze placed over a burner. Stir
the solution with a glass rod. Concentrate the solution till
crystallization point is reached. Place the dish over a beaker
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containing cold water.
5.Crystals of ammonium alum will separate out. Decant off the
excess water to expedite the drying process and you will big –
sized crystals.
6. Dry the crystals by placing them between filter paper.
REACTION:
(NH4)2SO4 + Al2(SO4)3.18H2O + 6H2O
NH4Al(SO4)2.12H2O
(Ammonium Sulphate) + (Aluminium Sulphate)
(Ammonium Alum)

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BIBLIOGRAPHY
1. Chemistry Class XII Part-1 – NCERT
2. Comprehensive Practical Chemistry – Class XII
3. Wikipedia and other websites

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