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Laboratory Manual 110P

laboratory manual for B.pahram students

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0% found this document useful (0 votes)
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Laboratory Manual 110P

laboratory manual for B.pahram students

Uploaded by

PrashantSingh
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
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ONE BEAT COLLEGE OF

MEDICAL SCIENCES
SANT GARH NAGAR, BHIRA-LAKHIMPUR-KHIRI-262901

Laboratory Manual
D.Pharm I year
Subject: Pharmaceutical
Inorganic Chemistry

Page 1
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SANT GARH NAGAR, BHIRA-LAKHIMPUR-KHIRI-262901

Index

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Experiment No. Title


1. To identify Magnesium Hydroxide.
2. To identify Ferrous Sulphate.
3. To identify Sodium Bicarbonate.
4. To identify Calcium Gluconate.
5. To identify Copper Sulphate.
6. To perform limit test of Chloride and Sulphate.
7. To perform modified limit test of Chloride and Sulphate.
8. To perform limit test of iron.
9. To perform limit test of heavy metal.
10. To perform limit test of lead.
11. To perform limit test of arsenic.
12. To determine the swelling power of Bentonite.
13 To determine the neutralizing capacity of aluminum hydroxide gel.
14 To determine potassium iodate and iodine in iodine solution.
15 To prepare Boric Acid.
16 To prepare Potash Alum
17 To prepare Ferrous Sulphate
Experiment No. 1

Object: To identify Magnesium Hydroxide.

References:

1) “Indian Pharmacopoeia” , Published by the Controller of Publications, Ministry of


Health and Family Welfare, Government of India, New Delhi, Page no.

2) Chatwal G. R , “Pharmaceutical Chemistry Inorganic”, Himalaya Publishing House


5th edition , Vol-I, New Delhi, page no.

Chemicals: Dil. Ammonia solution, ammonium chloride, disodium hydrogen phosphate

Theory:

Procedure:

1. Dissolve 15 mg in 2 ml of water.

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2. Add 1 ml Dil. Ammonia solution. A white ppt. is formed.

3. Redissolve the ppt. in 1 ml of 2M ammonium chloride.

4. Add 1 ml of 0.25M disodium hydrogen phosphate. White ppt. is formed.

Observation Table:

S.no
Observation Inference
.

Result:

Experiment No. 2

Object: To identify Ferrous Sulphate.

References:

1) “Indian Pharmacopoeia” , Published by the Controller of Publications, Ministry of


Health and Family Welfare, Government of India, New Delhi, Page no.

2) Chatwal G. R , “Pharmaceutical Chemistry Inorganic”, Himalaya Publishing House


Volume I, page no.

Chemicals: Ferrous Sulphate, Potassium Ferro cyanide, Barium Chloride, Distilled Water

Theory:

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Procedure:Identification for Iron

1. 1ml of the solution is taken


2. 1ml of Potassium ferro Cyanide (5% W/V) is added
3. White ppt. is obtained, which becomes Blue.

Identification for Sulphate

1. 50 mg of ferrous sulphate is taken.

2. 5ml of water and 1 ml BaCl2 solution (10% W/V) is added.

3. White ppt is obtained

Observation Table:

S.no. Observation Inference

Result:

Experiment No. 3

Object: To identify Sodium Bicarbonate.

References:

3) “Indian Pharmacopoeia” , Published by the Controller of Publications, Ministry of


Health and Family Welfare, Government of India, New Delhi, Page no.

4) Chatwal G. R , “Pharmaceutical Chemistry Inorganic”, Himalaya Publishing House


5th edition , Vol-I, New Delhi, page no.

Chemicals: Sodium Bicarbonate, Phenolphthalein, Magnesium Sulphate, Distilled Water

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Theory:

Procedure :

Identification for Sodium

1. Take 5ml of 5%w/v of solution of substance in water.

2. Add 0.1 ml of phenolphthalein solution. Pale pink color is produced.

3. Heat the solution, gas is evolved. Solution becomes red in color.

Identification for Bicarbonate

1. Solution of the substance is taken and magnesium sulphate is added to it. No


precipitate is produced.
2. The solution is the boiled. White precipitate is produced.

Observation Table:

S.no. Observation Inference

Result:

Experiment No. 4

Object: To identify Calcium Gluconate.

References:

5) “Indian Pharmacopoeia” , Published by the Controller of Publications, Ministry of


Health and Family Welfare, Government of India, New Delhi, Page no.

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6) Chatwal G. R , “Pharmaceutical Chemistry Inorganic”, Himalaya Publishing House


5th edition , Vol-I, New Delhi, page no.

Chemicals: Calcium Gluconate, Ferric chloride, Acetic acid, Potassium Ferro cyanide,

Ammonium Chloride, Hydrochloric Acid, Distilled Water

Theory:

Procedure

Test 1

1. 5 gm of CaCO3 in 80 ml of 2M acetic acid after effervesence ceases.

2. Boil for 2 min. cool the solution and dil. to 100ml with 2M acetic acid.

3. Filter the solution. Take 0.2 ml of filterate.

4. Add 0.5 ml of 5%W/V potassium feero cyanide solution. Add 50mg of ammonium

chloride. White crystalline ppt. produced.

Test 2

1. 1ml of 3%w/v solution is taken.

2. To it add 0.05ml ferric chloride solution. Yellow color is produced.

Observation Table:

S.no. Inference Observation

Result

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Experiment No. 5

Object: To identify Copper Sulphate.

References:

7) “Indian Pharmacopoeia” , Published by the Controller of Publications, Ministry of


Health and Family Welfare, Government of India, New Delhi, Page no.

8) Chatwal G. R , “Pharmaceutical Chemistry Inorganic”, Himalaya Publishing House


5th edition , Vol-I, New Delhi, page no.

Chemicals: Copper Sulphate, BaCl2, Distilled Water

Theory:

Procedure

1. 50 mg of copper sulphate is taken.

2. 5ml of water and 1 ml BaCl2 solution (10% W/V) is added.

3. White ppt is obtained

Observation Table:

S.no
Observation Inference
.

Result:

Experiment No. 6

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Object: To perform limit test of Chloride and Sulphate.

References:

1) “Indian Pharmacopoeia” , Published by the Controller of Publications, Ministry of


Health and Family Welfare, Government of India, New Delhi, Page no.

2) Chatwal G. R , “Pharmaceutical Chemistry Inorganic”, Himalaya Publishing House


5th edition , Vol-I, New Delhi, page no.

Chemicals: Dil. Nitric Acid, Silver Nitrate, Dil. Hydrochloric Acid, Potassium Sulphate,

Barium Sulphate Reagent (barium chloride, alcohol, potassium sulphate), Distilled Water

Theory:

Procedure :

Limit Test for Chloride

Test Solution Standard Solution

1. 1g of substance is dissolved in water. 1. 1ml of 0.05845%w/v solution of sodium


2. 1ml of nitric acid is added. chloride.
3. The solution was diluted to 50ml in Nessler 2. 1ml of nitric acid is added.
Cylinder. 3. The solution was diluted to 50ml in
4. 1ml of silver nitrate solution is added. Nessler Cylinder.
5. Turbidity is produced. 4. 1ml of silver nitrate solution is added.
5. Turbidity is produced.

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Limit Test for Sulphate

Test Solution Standard Solution

1. 1g of substance is taken in Nessler cylinder. 1. 1ml of 0.1089%w/v solution of


2. 2ml of HCl was added and solution was potassium sulphate is taken.
diluted to 45ml. 2. 2ml of HCl was added and solution was
3. 5ml of solution of barium sulphate reagent diluted to 45ml.
was added. 3. 5ml of solution of barium sulphate
4. Turbidity is produced reagent was added.
4. Turbidity is produced

Result:

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Experiment No. 7

Object: To perform modified limit test of Chloride and Sulphate.

References:

1) “Indian Pharmacopoeia” , Published by the Controller of Publications, Ministry of


Health and Family Welfare, Government of India, New Delhi, Page no.

2) Chatwal G. R , “Pharmaceutical Chemistry Inorganic”, Himalaya Publishing House


5th edition , Vol-I, New Delhi, page no.

Chemicals: Dil. Nitric Acid, Silver Nitrate, Barium Chloride, Acetic Acid, Potassium
Sulphate, ethanol, Distilled Water

Theory:

Procedure:

Limit Test for Chloride

Test Solution Standard Solution

1. Dissolve specified quantity of substance under 1. 10ml of 25ppm of NaCl solution + 5ml
examination in water. water.
2. Transfer the solution to nessler’s cylinder. 2. Transfer the sol. to nessler’s cylinder.
3. Add 10ml of dil. Nitric acid. 3. Add 10 ml of dil. Nitric acid.
4. Dilute to 50ml with water(volume makeup). 4. Dilute to 50ml with water(volume
5. Add 1ml of 0.1M silver nitrate. makeup).
6. Stir immediately with glass rod. 5. Add 1ml of 0.1M silver nitrate.
7. Allow to stand for 5 min. protect from light. 6. Stir immediately with glass rod.
8. Turbidity produced. 7. Allow to stand for 5 min. protect from

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light.
8.Turbidity produced.

Limit Test for Sulphate

Test Solution Standard Solution

1. 1ml of 25% Barium Chloride in nessler’s 1. 1ml of 25% Barium Chloride in nessler’s
cylinder + 1.5 ethanolic sulphate standard cylinder + 1.5 ethanolic sulphate
sol. standard sol.
2. Mix and allow to stand for 1 min. 2. Mix and allow to stand for 1 min.
3. Add 15ml of sample solution. 3.Add 15ml of sulphate standard sol.(10ppm)
4. Add 0.15ml of 5M acetic acid. 4. Add 0.15ml of 5M acetic acid.
5. Makeup the volume upto 50ml with water. 5. Makeup the volume upto 50ml with water.
6. Stir immediately with glass rod. 6. Stir immediately with glass rod.
7. Allow to stand for 5min. 7. Allow to stand for 5min.
8. Turbidity 8. Turbidity

Result:

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Experiment No. 8

Object: To perform limit test of iron.

References:

1) “Indian Pharmacopoeia” , Published by the Controller of Publications, Ministry of


Health and Family Welfare, Government of India, New Delhi, Page no.

2) Chatwal G. R , “Pharmaceutical Chemistry Inorganic”, Himalaya Publishing House


5th edition , Vol-I, New Delhi, page no.

Chemicals: Acetic Acid, Thioglycolic acid, Ammonia Solution, Distilled Water

Theory:

Procedure:

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Test Solution Standard Solution

1. Sample + 40ml of water + 2ml of 20% 1. 2ml of standard sol. + 40ml of water + 2ml of
W/V iron free citric acid + 0.1ml of 20% W/V of iron free citric acid + 0.1ml of
thioglycollic acid. thioglucollic acid.
2. Transfer it in nessler’s cylinder. 2. Transfer it in nessler’s cylinder.
3. Mix the sol. Then solution is made 3. Mix the sol.
alkaline with ammonia. 4. The solution is made alkaline with ammonia.
4. Make up the volume upto 50ml with 5. Make up the volume upto 50ml with water.
water. 6. Allow to stand for 5 mins.
5. Allow to stand for 5mins 7. Colour produced.
6. Colour produced.

Result:

Experiment No. 9

Object: To perform limit test of heavy metal.

References:

1) “Indian Pharmacopoeia” , Published by the Controller of Publications, Ministry of


Health and Family Welfare, Government of India, New Delhi, Page no.

2) Chatwal G. R , “Pharmaceutical Chemistry Inorganic”, Himalaya Publishing House


5th edition , Vol-I, New Delhi, page no.

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Chemicals: Lead Solution, dil. Acetic acid or ammonia solution, hydrogen sulphide gas,

sulphuric acid, dil. Nitric acid, hydrochloric acid, sodium hydroxide, sodium sulphide,

thioacetamide, Distilled Water

Theory:

Procedure:

Method A

Test Solution Standard Solution

1. Dissolve specified quantity of 1. 1ml of standard lead so.(20ppm

substance in water to produce 25ml in lead) in nessler cylinder. Dil. To

nessler cylinder. 25ml with water.

2. Adjust the ph between 3 and 4 with 2. Adjust the ph between 3 and 4

dil. Acetic acid or dil. Ammonia sol. with dil. Acetic acid or dil.

3. Dil. To 35ml with water and mix. Ammonia sol.

4. Add 10ml of freshly prepared 3. Dil. To 35ml with water and mix.

hydrogen sulphide sol. 4. Add 10ml of freshly prepared

5. Mix and dil. To 50ml with water. hydrogen sulphide sol.

6. Allow to stand for 5 mins 5. Mix and dil. To 50ml with water.

7. Colour produced 6. Allow to stand for 5 mins

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7. Colour produced

Method B

Standard Solution Test Solution

1. 1ml of standard lead solution(20ppm) in 1. Weigh the substance as specified in


nessler cylinder. the individual monograph in a
2. dil to 25ml with water. crucible
3. Adjust the ph between 3 and 4 with dil. 2. Wet the sample by adding sufficient
Acetic acid or dil. Ammonia sol. sulphuric acid.
4. Dil. To 35ml with water and mix. 3. Ignite at low temp. to charring.
5. Add 10ml of freshly prepared hydrogen 4. To the charred mass add 2ml of nitric
sulphide solution. acid and 5drops of sulphuric acid
6. Mix and dil. To 50ml with water 5. Heat until white fumes are no longer
7. Allow to stand for 5 mins. evolved.
8. Colour produced. 6. Ignite at 500-6000C until the carbon is
completely burned off.
7. Cool and add 4ml of dil. Hcl
8. Heat on water bath for 15mins.
9. Evaporate to dryness or water bath.
10. Moisten the residue with 1 drop of hcl
+ 10ml of hot water.
11. Digest for 2mins.
12. Make the sol. Just alkaline to the
litmus paper by dropwise addition of
ammonia sol.
13. Dil. To 25ml with water
14. Adjust the ph between 3 and 4 with
dil. Acetic acid.
15. Filter rinse the crucible and filter with
10ml of water.
16. Combine the filtrate and washing to
nessler cylinder.
17. Dil. To 35ml with water.
18. Mix
19. Add 10 ml of freshly Add 10ml of
freshly prepared hydrogen sulphide

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solution.
20. Mix and dil. To 50ml with water
21. Allow to stand for 5 mins.
22. Colour produced.

Method C

Standard Solution Test Solution

1. 1ml of standard lead sol. 1. Dissolve the specified quantity of


(20ppm) in nesler cylinder + 5ml of 2. Dil. To 50ml with water and mix.
sodium hydroxide sol. 3. Add 5 drops of sodium sulphide sol.
2. Dil. To 50ml with water and 4. Mix and allow to stand for 5 mins.
mix. 5. Colour produced.
3. Add 5 drops of sodium
sulphide sol.
4. Mix and allow to stand for 5
mins.
5. Colour produced.

Method D

Standard Solution Test Solution

1. 10ML of standard sol. (1ppm lead) or


standard sol. (2ppm lead) 1. 12ml of sample sol.
2. Add 2ml of acetate buffer(ph 3.5) 2. Add 2ml of acetate buffer(ph
3. Mix 3.5)

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4. 1.2 ml of thioacetamide reagent. 3. Mix


5. Allow to stand for 2mins. 4. 1.2 ml of thioacetamide reagent.
6. Colour produced. 5. Allow to stand for 2mins.
6. Colour produced

Result:

Experiment No. 10

Object: To perform limit test of lead. References:

1) “Indian Pharmacopoeia” , Published by the Controller of Publications, Ministry of


Health and Family Welfare, Government of India, New Delhi, Page no.

2) Chatwal G. R , “Pharmaceutical Chemistry Inorganic”, Himalaya Publishing House


5th edition , Vol-I, New Delhi, page no.

Chemicals: Potassium cyanide, dithizone, nitric acid, Distilled Water

Theory:

Procedure:

Test Solution Standard Solution

1. Standard lead sol.(1ppm lead)+ 6ml of


1. Sample + 6ml of ammonium nitrate ammonium nitrate sol. And 2ml
sol. And 2ml hydroxyl amine hydroxyl amine hydrochloride.
hydrochloride. 2. Add 2 frops of phenol red sol.
2. Add 2 frops of phenol red sol. 3. Make the sol. Alkaline by adding strong

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3. Make the sol. Alkaline by adding ammonia sol.


strong ammonia sol. 4. Add 2ml of potassium cyanide sol.
4. Add 2ml of potassium cyanide sol. 5. Immediately extract sol. With 5ml
5. Immediately extract sol. With 5ml portion of dithizone extraction sol., until
portion of dithizone extraction sol., it becomes green in colour.
until it becomes green in colour. 6. Combine the dithizone extract and
6. Combine the dithizone extract and transfer to second separator.
transfer to second separator. 7. Shake the combined dithizone extract for
7. Shake the combined dithizone extract 30secs. With 30ml of 1% v/v nitirc acid
for 30secs. With 30ml of 1% v/v nitirc sol.
acid sol. 8. Discard the chloroform layer
8. Discard the chloroform layer 9. To the nitric acid sol. Add 5ml of
9. To the nitric acid sol. Add 5ml of dithizone standard sol.
dithizone standard sol. 10. Shake for 30secs.
10. Shake for 30secs. 11. Violet colour produced.
11. Violet colour produced.

Result:

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Experiment No. 11

Object: To perform limit test of arsenic.

References:

1) “Indian Pharmacopoeia” , Published by the Controller of Publications, Ministry of


Health and Family Welfare, Government of India, New Delhi, Page no.

2) Chatwal G. R , “Pharmaceutical Chemistry Inorganic”, Himalaya Publishing House


5th edition , Vol-I, New Delhi, page no.

Chemicals: Potassium Iodide, zinc, mercuric chloride paper, arsenic solution.

Theory:

Procedure:

Test solution Standard solution

1. Take sample into a conical flask or 1. Add 1ml of arsenic standard sol

bottle. (10ppm) into a bottle or conical

2. Add 5ml of 1M potassium Iodide and flask.

10gm of Zinc. 2. Add 5ml of 1M potassium Iodide

3. Dil. To 50ml with water. and 10gm of Zinc.

4. Immediately immerse the flask in a 3. Dil. To 50ml with water.

water bath. 4. Immediately immerse the flask in

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5. After 40mins stain produced on a water bath.

mercuric chloride paper. 5. After 40mins stain produced on

mercuric chloride paper.

Result:

Experiment No. 12

Object: To determine the swelling power of Bentonite .

References:

1) “Indian Pharmacopoeia” , Published by the Controller of Publications, Ministry of


Health and Family Welfare, Government of India, New Delhi, Page no.

2) Chatwal G. R , “Pharmaceutical Chemistry Inorganic”, Himalaya Publishing House


5th edition , Vol-I, New Delhi, page no.

Chemicals: Bentonite, sodium lauryl sulphate, Distilled Water

Theory:

Procedure:

1. Add 2.0 g in twenty portions at intervals of 2 minutes to 100 ml of a 1 per cent w/v

solution of sodium lauryl sulphate in a 100-ml graduated cylinder about 3 cm in

diameter.2.

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2. Allow each portion to settle before adding the next and let it stand for 2 hours. 3.

3. The apparent volume of the sediment at the bottom of the cylinder is not less than 24

ml.

Result:

Experiment No.13

Object: To determine the neutralizing capacity of aluminium hydroxide gel.

References:

1) “Indian Pharmacopoeia” , Published by the Controller of Publications, Ministry of


Health and Family Welfare, Government of India, New Delhi, Page no.

2) Chatwal G. R , “Pharmaceutical Chemistry Inorganic”, Himalaya Publishing House


5th edition , Vol-I, New Delhi, page no.

Chemicals: Aluminium Hydroxide, Hydrochloric acid, Sodium Hydroxide, Distilled Wate

Theory:

Procedure:

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1. Disperse 5.0 g in 100 ml of water, heat to 37°, add 100.0 ml of 0.1 M hydrochloric

acid previously heated to 37°and stir continuously, maintaining the temperature at

37°; the pH of the solution, at 37°, after 10, 15 and 20 minutes, is not less than 1.8,

2.3 and 3.0 respectively and at no time is more than 4.5.

2. Add 10.0 ml of 0.5 M hydrochloric acid previously heated to 37°, stir continuously

for 1 hour maintaining the temperature at 37° and titrate with 0.1 M sodium hydroxide

to pH 3.5. Not more than 50.0 ml of 0.1 M sodium hydroxide is required.

Result:

Experiment No.14

Object: To determine potassium iodate and iodine in iodine solution.

References:

1) “Indian Pharmacopoeia” , Published by the Controller of Publications, Ministry of


Health and Family Welfare, Government of India, New Delhi, Page no.

2) Chatwal G. R , “Pharmaceutical Chemistry Inorganic”, Himalaya Publishing House


5th edition , Vol-I, New Delhi, page no.

Chemicals: Potassium Iodide, Conc. Hydrochloric Acid, Chloroform, amaranth, sodium

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thiosulphate, Distilled Water

Theory:

Procedure:

A. Preparation and standardization of Potassium Iodate solution

1. Weigh accurately 0.5g of potassium iodate in iodine flask, dissolve in 50ml of water and

60ml of concentrated HCl and 5ml of chloroform.

2. Titrate with potassium iodate solution until the purple color disappears from the

chloroform layer.

3. Near the end point add the reagents and swirl vigorously between additions.

B. Assay of Iodine Solution

1. Pipette out 10ml of sample solution into a conical flask, dilute with 20ml of water and

titrate with 0.1 N sodium thiosulphate solution until the solution becomes colorless.

2. Pipette out another 10ml of sample solution into a conical flask, dilute with 30ml of water

and add 50ml of concentrated HCl, and titrate with 0.05M potassium iodate solution.

3. The solution becomes brown due to liberation of iodine. Continue the titration until the

solution becomes lighter.

4. Add 1ml of amaranth solution and continue the titration until the red color becomes pale

yellow.

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Result :

Experiment No. 15

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Object: To prepare Boric Acid.

References:

1) “Indian Pharmacopoeia” , Published by the Controller of Publications, Ministry of


Health and Family Welfare, Government of India, New Delhi, Page no.

2) Chatwal G. R , “Pharmaceutical Chemistry Inorganic”, Himalaya Publishing House


5th edition , Vol-I, New Delhi, page no.

Chemicals: Dil. Sulphuric Acid, Borax, Distilled Water

Theory:

Procedure:

1. 15ml of dil. H2SO4 was taken in a beaker.

2. 15gm of borax was dissolved in 40ml of distilled water and boil.

3. Dil. H2SO4 was added to hot sol. Of borax.

4. Hot sol. was cooled

5. Ppt. of boric acid is filtered and dried.

Result:

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Experiment No. 16

Object: To prepare Potash Alum

References:

1) “Indian Pharmacopoeia” , Published by the Controller of Publications, Ministry of


Health and Family Welfare, Government of India, New Delhi, Page no.

2) Chatwal G. R , “Pharmaceutical Chemistry Inorganic”, Himalaya Publishing House


5th edition , Vol-I, New Delhi, page no.

Chemicals: Potassium Sulphate, Aluminium Sulphate, Distilled Water

Theory:

Procedure:

1. Solution of potassium sulphate is prepared in water.

2. Equimolar solution of aluminium sulphate is prepared andboiled.

3. When the solution is concentrated and cooled.

4. The crystals of potash alum seperates out.

Result :

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Experiment No. 17

Object: To prepare Ferrous Sulphate

References:

1) “Indian Pharmacopoeia” , Published by the Controller of Publications, Ministry of


Health and Family Welfare, Government of India, New Delhi, Page no.

2) Chatwal G. R , “Pharmaceutical Chemistry Inorganic”, Himalaya Publishing House


5th edition , Vol-I, New Delhi, page no.

Chemicals: Iron, Dil. Sulphuric acid, Distilled Water

Theory:

Procedure:

1. Dissolve 5gm of iron dust in 30ml of dilute sulphuric acid.

2. After the effervescence ceases the liquid is filtered.

3. The filterate is concentrated and cooled.

4. The green crystals are separated by filteration.

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5. The crystal obtained was dried.

Result:

Page 29

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