First Year Experiment 1 - 4

Pharmaceutical Chemistry ER20-12P
Class F.Y.D.Pharm
Experiment No. 1
1.0 Title:
Limit test for chloride
(To perform and report the limit test for chloride on the given samples as per Indian
Pharmacopoeia)
1. Sodium bicarbonate.
2. Potassium permanganate.
3. Magnesium trisilicate.
2.0 Prior concepts: -

Impurities, sources of impurities, types of impurities.
3.0 New concepts: Principle

Limit test for chloride depends upon the interaction of chlorides with silver inpresence
of dilute nitric acid.Deposition of solid particle of chloride as silver chloride.Chloride
as impurity is present in very small quantities. In the chemical interaction the
precipitation of silver chloride appears as opalescence. It is compared under uniform
conditions of illumination with standard opalescence in Nessler’s cylinders to draw
inference.
Importance of limit tests:

1. To find out the amount of harmful impurities.
2. To find out the avoidable/unavoidable amount of impurities.
Chemical Reaction:
Cl⁻ + AgNO3 Dilute HNO3 AgCl + NO⁻3
(Soluble)(Soluble) (Precipitate) (Soluble)
4.0 Apparatus:
Materials:
A pair of Nessler cylinder, Wooden stands, Glass rod, Pipette (10 ml, 25ml) andMeasuring
cylinder (100ml).
Chemicals:
Sodium bicarbonate, Potassium permanganate, Magnesium Trisilicate, 0.1M Silver nitrate,
dilute nitric acid and Sodium chloride, Chloride standard solution (25 ppm), distilled water
and ethanol (95%).
Dr.D.Y.Patil Institute of Pharmacy, Akurdi, Pune. 1

Class F.Y.D.Pharm
5.0 Stepwise Procedure:

Standard Solution Test solution of Test solution of Test solution of
sodium bicarbonate Pottasium magnesium
Permaganate trisilicate
1. Take 10 ml of 1. Weigh accurately 1. Weigh accurately 1. Weigh accurately
chloride solution in 1.25 g of sodium 1.50 g of Pottasium 2.0g of magnesium
labeled Nesslers bicarbonate permanganate Trisilicate and
Cylinder 2.dissolve it in 15 ml solution and transfer transfer it in 250ml
2. Add 5ml of distilled of distilled water in a it in 250 ml conical conical flask
water labeled Nesslers flask 3. Add 12 ml of
3. Add 10 ml of dilute cylinder 2. Add 50 ml of distilled water , allow
nitric acid and mix 3. Add 2ml of dilute distilled water, heat to cool , filter to
well nitric acid and mix on water bath obtain clear solution
4. Dilute to 50 ml with well 3. Add gradually 6 4. Dilute the filtrate
distilled water 4. Dilute to 50 ml ml of ethanol and to 20 ml with
5. Add 1ml of 0.1 M with distilled water cool distilled water
silver nitrate solution 5. Add 1ml of 0.1 M 4. Dilute to 60 ml 5. Take 0.5 ml of
6. Stir immediately silver nitrate solution with distilled water above solution in
with glass rod and 6. Stir immediately and filter, the filtrate labeled Nesslers
allow to stand for 5 with glass rod and is colourless cylinder (T)
minute protect from allow to stand for 5 5. Take 40 ml of 6. Dilute 50 ml with
light minute above filtrate in a distilled water
7. Compare the labeled Nesslers 7. Add 1ml of 0.1 M
opalescence produced cylinder (T) silver nitrate solution
with that of standard 6. Add 10 ml of 8. Stir & keep for 5
solution dilute nitric acid min.
7. Add 1ml of 0.1 M 9. Compare the
silver nitrate solution opalescence
8. Stir 7 allow to produced with that of
stand for 5 min. standard solution
9. Compare the
opalescence
produced with that of
standard solution
6.0 Observation:
1. Opalescence produced by sodium bicarbonate test solution is ……………(less/same/more)
intense than that of standard solution.
2. Opalescence produced by Pottasium permagnate test solution is …………( less/same/more)
3. Opalescence produced by magnesium trisilicate test solution is …………(less/same/more)

Class F.Y.D.Pharm
7.0 Results:
1. The given sample of sodium bicarbonate …………………………… (complies/ does not
complies) the limit test for chlorides as per the Indian Pharmacopoeia 1996.
2. The given sample of potassium permanganate ……………………… (complies/does not
3. The given sample of magnesium trisilicate …………………………(complies/ does not
8.0 Questions:
(Answer the following question, Q)
1. State the meaning of the term opalescence.
2. Write the principle of limit test for chlorides.
3. State the chemical equation of chloride limit test.
4. State the reason for use of silver nitrate in the chloride limit test.
5. Why nitric acid is used in the chloride limit test give the reasons.
Space for Writing Answer

Class F.Y.D.Pharm

Class F.Y.D.Pharm
Experiment No. 2
1.0 Title:
Limit test for sulphate.
(To perform and report the limit test for sulphate on the given samples as per Indian
Pharmacopoeia).
1. Purified water.
2. Sodium bicarbonate.
3. Calcium gluconate.

Opalescence, Impurities, Supersaturation Parts per millions.

Limit test for sulphate depends upon the interaction of soluble sulphate with barium
chloride in presence of alcohol and potassium sulphate. Deposition of solid particles
of sulphate as barium sulphate.The opalescence/turbidity produced by sample under
test is compared with standard sample opalescence/turbidity against the dark
background.
Note: (barium chloride, alcohol and a small amount of potassium sulphate is used for this
purpose; alcohol prevents supersaturation and potassium sulphate increases sensitivity
of the test by giving ionic concentration in the reagent which just exceeds the
solubility product of barium sulphate.)
Chemical Reaction:
BaCl2 + SO2-4 BaSO4 + 2Cl⁻
4.0 Apparatus:
Materials:
A pair of Nessler cylinder, Wooden stands, Glass rod, Pipette (10 ml, 25ml) and
Measuring cylinder (100ml).
Chemicals:
Sodium bicarbonate, Calcium gluconate, Purified water, Alcohol, Barium sulphate,
Ethanolic sulphated standard solution (10 ppm SO4), 5M acetic acid, Barium chloride and
2M hydrochloric acid.

Class F.Y.D.Pharm

Purified water sodium bicarbonate Calsium Gluconate
1. Take 1 ml of 25% 1. Take 10 ml of 1. Take 1 ml of 25% 1. To 1ml 25 % w/v

solution of barium purified water in a solution of Barium solution of barium
chloride in labeled labeled Nesslers chloride in a labeled chloride in a labeled
Nesslers Cylinder cylinder Nesslers cylinder Nesslers cylinder
2. Add 1.5ml of 2.Add 0.1ml of 2M 2. Add 1.5 ml of 2. Add 1.5 ml of
ethanolic sulphate hydrochloric acid ethanolic sulphate ethanolic sulphate
standard solution Mix 3. Add 0.1ml of standard solution Mix standard solution Mix
an stand for 1 min. 25%w/v barium and allow to stand for and allow to stand for
3. Add 0.15 ml of chloride solution 1 min. 1 min.
acetic acid and mix 4. Observe 3. Weigh accurately 3. Weigh accurately
well appearance of 1.0g of sodium 1.0g of calcium
4. Add sufficient water solution for 1 hr. bicarbonate and add to gluconate and add to
to produce 50 ml nesslers cylinder nesslers cylinder
5. Stir immediately 4. Add 10 ml distilled 4. Dissolve it by
with glass rod and water neutralize with adding 15 ml of
allow to stand for 5 HCl and dilute to 15 distilled water
minute protect from ml with distilled water 5. Add 0.15ml of 5M
light 5. Add 0.15 ml of 5M acetic acid
acetic acid. 6. Add sufficient
6. Add Sufficient water to produce
water 50 ml stir & 50ml Stir & keep for
allow to stand 5 min 5 min.
7. Compare the 7. Compare the
opalescence produced opalescence produced
with that of standard with that of standard
solution solution
6.0 Observation:
1. There is ………………… (Change/no change) in appearance of test solution of purified
water after 1 hour.
2. Opalescence produced by sodium bicarbonate test solution is ……………
(less/same/more) intense than that of standard solution.
3. Opalescence produced by calcium gluconate test solution is …..………………
(less/same/more) intense than that of standard solution.

Class F.Y.D.Pharm
7.0 Results:
1. The given sample of purified water ………………………………. (complies/ does not
complies) the limit test for sulphate as per the Indian Pharmacopoeia 1996.
2. The given sample of sodium bicarbonate ………………………………. (complies/ does
not complies) the limit test for sulphate as per the Indian Pharmacopoeia 1996.
3. The given sample of calcium gluconate ………………………………. (complies/ does
not complies) the limit test for Sulphate as per the Indian Pharmacopoeia 1996.
8.0 Questions:
(Answer the following question)
1. State the meaning of the term impurities as applicable to drug.
2. Define supersaturation.
3. Write the procedure for preparation of standardsolution for the test of sulphate
impurities.
4. Write the procedure for preparation of testsolution of purified water for test of
sulphate impurities.
5. Write the procedure for preparation of test solution of sodium bicarbonate for test of
6. Write the procedure for preparation of test solution of calcium gluconate for test of
7. State the use of barium chloride and alcohol in limit test of sulphate.
Space of writing answer

Class F.Y.D.Pharm

Class F.Y.D.Pharm

Class F.Y.D.Pharm
Experiment No. 3
1.0 Title:
Limit test for Iron.
(To perform and report the limit test for Iron on the given samples as per Indian
Pharmacopoeia).
1. Zinc sulphate.
2. Sodium chloride.
3. Magnesium sulphate.

Limit test, sources of iron impurities, colour intensity.

Limit test for iron based upon the chemical reaction of iron in ammonical solution in
Presence of iron free citric acid with thioglycollic acid, it form ferrous thioglycolate
Complex. A purple colour is formed due to formation of ferrous thioglycolate complex.
The original state of iron is unimportant as thioglycollic acid reduces ferric (fe3+) to
Ferrous (fe2+). This test is very sensitive making use of 20% citric acid, which forms,
complex with other metal ion, eliminates interference of other metal ion.The colour
produced by sample under test is compared with the coloured produced by the
standard solution.
Note: (purple colour is developed only in alkaline medium, so ammonia solution is used,
but ammonia solution forms precipitate with iron, therefore citric acid is added to form
ammonium citrate buffer which stabilizes ferrous thioglycolate complex).
Chemical Reaction:

Class F.Y.D.Pharm
4.0 Apparatus:
Materials:
A pair of Nessler cylinder, Wooden stands, Glass rod, Pipette (1 ml, 2ml and 10 ml) and
Measuring Cylinder (100ml), White tile, Glass beaker, analytical weighing balance and
weight box.
Chemicals:
Standard solution of iron (20 ppm Fe), 20% w/v iron free citric acid, thioglycollic acid,zinc
sulphate, sodium chloride, magnesium sulphate, iron free ammonia and distilled water.
Standard solution Test solution for Test solution for Test solution for
zinc sulphate sodium chloride magnesium
sulphate
1. Take 2.0 ml of 1. Weigh accurately 1. Weigh accurately 1. Weigh accurately
iron standard 2.5 g of zinc 2g of sodium 5g of magnesium
solution (20ppm Fe) sulphate and chloride and sulphate and
in labelled dissolved in dissolve in 20 ml of dissolve in sufficient
Nesslers cylinder. sufficient carbon water in a labelled carbon dioxide-free
2. Add 2ml of a 20% dioxide free water to Nesslers cylinder water to 50ml in a
w/v solution of iron- produce 50 ml in a (T). beaker. Take 2ml of
free citric acid. beaker. Take 2.0 ml 2. Add2 ml of a 20% solution in a labelled
3. And add 0.1 ml of of solution and w/v solution of iron Nesslers cylinder
thioglycollic acid, diluted to 10ml with free citric add. (T).
mix well, make water in a labelled 3. And add 0.1 ml of 2. Add 2ml of a 20%
alkaline with iron Nesslers Cylinder thioglycollic acid, w/v solution of iron-
free ammonia (T). mix well and make free citric acid.
solution. 2. Add 2ml of a alkaline with Iron – 3. Add 0.1 ml of
4. Dilute to 50 ml 20%w/v solution of free ammonia thioglycollic acid,
with water and allow iron-free citric acid. solution. mix well and make
to stand for 5 3. And add 0.1 ml of 4. Dilute to 50ml alkaline with iron
minutes. thioglycollic acid, with water and allow free ammonia
mix well and make to stand for 5 min. solution.
alkaline with iron 5.View the colour 4. Dilute to 50ml
free ammonia intensity against with water and allow
solution. while background to stand for 5 min.
4. Dilute to 50ml and compare with 5. View the colour
with water and allow that of standard intensity against
to stand for 5 min. while background
and compare with
that of standard.

Class F.Y.D.Pharm
6.0 Observation:
1. The color intensity produced in Zinc Sulphate sol. is ……………… (Less/same/more)
than the color intensity produced in standard solution.
2. The color intensity produced in Sodium chloride sol. is ……………… (Less/same/more)
than the color intensity produced in standard solution
3. The color intensity produced in Magnesium solution is ……………… (Less/same/more)
7.0 Results:
1. The given sample of Zinc Sulphate ………………………………. (Complies/ does not
complies) the limit test for Iron as per the Indian Pharmacopoeia 1996.
2. The given sample of Sodium Chloride …………………………… (Complies/ does not
3. The given sample of Dextrose ………………………………. (Complies/ does not
9.0 Questions:
1. What is the principle limit test for iron.
2. Why ammonia solution and citric acid solution are used in iron limit test?
3. Why deep reddish purple colour is developed in iron limit test?
4. Write the procedure for preparation of sodium chloride test solution.
5. How to observe the colour intensity?

Class F.Y.D.Pharm

Class F.Y.D.Pharm

Class F.Y.D.Pharm
Experiment No. 4
1.0 Title:
Limit test for Heavy Metals.
(To perform and report the limit test for Heavy metals on the given samples as per
Indian Pharmacopoeia).
1. Sodium chloride
2. Potassium iodide
3. Dextrose.

Sources of impurities, colloidal state, metal impurities

Limit test for heavy metal is based upon the reaction between hydrogen sulphide and
certain heavy metals such as lead, iron, copper, nickel, cobalt and bismuth resulting in the
formation of sulphides of the respective metals in presence of dilute acetic acid. The
sulphides so formed are distributed in a colloidal state and produce brownish coloured
solution. Comparison of sample with standard.The intensity of colour produced in test is
compared with intensity of colour produced in standard solution.
Chemical Reaction:
M + H2S Dil.Acetic MS + 2H+
Metals Hydrogen sulphide Sulphide of metals
4.0 Apparatus:
Materials:
A pair of Nessler cylinder, Wooden stands, Glass rod, Pipette (10 ml, 25ml) and
Measuring cylinder (100ml).
Chemicals:
Lead standard solution (20 ppm Pb), dilute acetic acid, dilute ammonia solution, freshly
prepared Hydrogen Sulphide solution, distilled water, sodium chloride, Potassium iodide
and dextrose.

Class F.Y.D.Pharm
Sodium Chloride Pottasium Iodide Dextrose
1.In to a 50 ml labeled 1. Accurately weigh 1. Accurately weigh 1. Accurately weigh

Nesslers cylinder (S) 4g of sodium chloride 2g of potassium iodide 4g of dextrose and
Pipette 1.0 ml of lead and add to labeled and add to labeled dissolve in 10 ml
standard solution (20 Nesslers cylinder (T). Nesslers cylinder (T) . water in a labeled
ppm Pb). 2. Add 2 ml of dilute 2. Add 2 ml of dilute Nesslers cylinder
2. Dilute with distilled acetic acid and mix acetic acid and mix 2. Add 2 ml of dilute
water to 25 mi. well ,then add well, then add acetic acid and mix
3. Adjust the pH with sufficient water to sufficient water to well, then add
dilute acetic acid or produce 25 ml. produce 25 ml. sufficient water to
dilute ammonia 3. Adjust the pH with 3. Adjust the pH with produce 25 ml
solution in between 3.0 dilute acetic acid or dilute acetic acid or 3. Adjust the pH with
to 40. dilute ammonia dilute ammonia dilute acetic acid or
4. Dilute with solution in between solution in between dilute ammonia
distilledwater about 35 3.0 to 4.0. 3.0 to 4.0. solution in between
ml and mix with glass 4. Dilute with water 4. Dilute with water to 3.0 to 4.0
rod. to 35 ml and mix 35 ml and mix well. 4. Dilute with water
5. Add 10 mi of well. 5. Add 10 ml of to 35 ml and mix
freshly prepared 5. Add 10 ml of freshly prepared well.
hydrogen sulphide freshly prepared hydrogen sulphide 5. Add 10 ml of
solution. hydrogen sulphide sólution. freshly prepared
6. Mix and dilute to 50 solution. 6. Mix and dilute to 50 hydrogen sulphide
ml with water. 6. Mix and dilute to ml with water. solution.
7. Allow to stand for 5 50 ml with water. 7. Allow to stand for 5 6. Mix and dilute to
minutes. 7. Allow to stand for minutes. 50 ml with water.
5 minutes. 7. Allow to stand for
5 minutes.
6.0 Observation:
1. The color intensity produced in Sodium chloride sol. is ………………(less/same/more)
than the color intensity produced in standard solution.
2. The color intensity produced in Potassium Iodide sol. is ……………… (less/same/more)
3. The color intensity produced in Dextrose solution is ………………….(less/same/more)

Class F.Y.D.Pharm
7.0 Results:
1. The given sample of Sodium chloride ………………………………. (Complies/ does
not complies) the limit test for heavy metals as per the Indian Pharmacopoeia 1996.
2. The given sample of Potassium Iodide ………………………………. (Complies/ does
not complies) the limit test for heavy metals as per the Indian Pharmacopoeia 1996.
3. The given sample of Dextrose ………………………………. (Complies/ does not
complies) the limit test for heavy metals as per the Indian Pharmacopoeia 1996.
8.0 Questions:
1. Why limit test for heavy metals is performed?
2. Write the procedure for preparation of standard solution for limit test for heavy
metals.
3. Write the principle involved in the limit test for heavy metals.
4. Write the procedure for preparation of test solution of sodium chloride.
i. Dilute acetic acid
iiDilute ammonia solution
iii. Freshly prepared solution of hydrogen sulphides.
5. Is it possible to replace hydrogen sulphides solution by any other means? Justify with
example.

Class F.Y.D.Pharm

Class F.Y.D.Pharm

Class F.Y.D.Pharm

First Year Experiment 1 - 4

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First Year Experiment 1 - 4

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Pharmaceutical Chemistry ER20-12P

2.0 Prior concepts: -

3.0 New concepts: Principle

Importance of limit tests:

Dr.D.Y.Patil Institute of Pharmacy, Akurdi, Pune. 1

5.0 Stepwise Procedure:

Dr.D.Y.Patil Institute of Pharmacy, Akurdi, Pune. 2

Space for Writing Answer

Dr.D.Y.Patil Institute of Pharmacy, Akurdi, Pune. 3

Dr.D.Y.Patil Institute of Pharmacy, Akurdi, Pune. 4

2.0 Prior concepts: -

3.0 New concepts: Principle

Dr.D.Y.Patil Institute of Pharmacy, Akurdi, Pune. 5

5.0 Stepwise Procedure:

1. Take 1 ml of 25% 1. Take 10 ml of 1. Take 1 ml of 25% 1. To 1ml 25 % w/v

Dr.D.Y.Patil Institute of Pharmacy, Akurdi, Pune. 6

Space of writing answer

Dr.D.Y.Patil Institute of Pharmacy, Akurdi, Pune. 7

Dr.D.Y.Patil Institute of Pharmacy, Akurdi, Pune. 8

Dr.D.Y.Patil Institute of Pharmacy, Akurdi, Pune. 9

2.0 Prior concepts: -

3.0 New concepts: Principle

Dr.D.Y.Patil Institute of Pharmacy, Akurdi, Pune. 10

Dr.D.Y.Patil Institute of Pharmacy, Akurdi, Pune. 11

Space of writing answer

Dr.D.Y.Patil Institute of Pharmacy, Akurdi, Pune. 12

Dr.D.Y.Patil Institute of Pharmacy, Akurdi, Pune. 13

Dr.D.Y.Patil Institute of Pharmacy, Akurdi, Pune. 14

2.0 Prior concepts: -

3.0 New concepts: Principle

Dr.D.Y.Patil Institute of Pharmacy, Akurdi, Pune. 15

1.In to a 50 ml labeled 1. Accurately weigh 1. Accurately weigh 1. Accurately weigh

Dr.D.Y.Patil Institute of Pharmacy, Akurdi, Pune. 16

Space of writing answer

Dr.D.Y.Patil Institute of Pharmacy, Akurdi, Pune. 17

Dr.D.Y.Patil Institute of Pharmacy, Akurdi, Pune. 18

Dr.D.Y.Patil Institute of Pharmacy, Akurdi, Pune. 19

Dr.D.Y.Patil Institute of Pharmacy, Akurdi, Pune. 20

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