Experiment No.

Pharmaceutical Chemistry-I (0806)

Experiment No. 3
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. 2. 3. Sodium bicarbonate. Potassium permanganate Magnesium trisilicate

2.0

Prior Concepts :Impurities, sources of impurities, types of impurities.

3.0

New Concepts: Principle

Proposition 1: Chemical Interaction Limit test for chloride depends upon the interaction of chlorides with silver nitrate in the presence of dilute nitric acid. Proposition 2: Precipitation/Opalescence Deposition of solid particle of chloride as silver chloride.

Proposition 3: Comparison of test sample with standard 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 Nesslers cylinders to draw inference. Proposition 4: Importance of limit tests: 1. 2. To find out the amount of harmful impurities. To find out the avoidable/unavoidable amount of impurities.

Chemical Reaction: Dilute HNO3 Cl+ AgNO3 (Soluble) AgCl (Precipitate) + NO-

(Soluble)

(Soluble)

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Pharmaceutical Chemistry-I (0806)

Experiment No. 3

General Concept Structure:

4.0

Learning Objectives:
4.1 Intellectual Skills:
1. To identify impurities in the given sample.

4.2

Motor Skills:
1. 2. To observe the turbidity /opalescence in Nesslers cylinder. To compare opalescence of test solution with standard solution.

5.0

Apparatus:
5.1 Materials:
A pair of Nesslers cylinder, Wooden stands, Glass rod, Pipette (10 ml, 25 ml) and Measuring cylinder (100 ml).

5.2

Chemicals:
Sodium bicarbonate, Potassium permanganate, Magnesium Trisilicate, 0.1 M Silver nitrate, dilute nitric acid and Sodium chloride, Chloride standard solution (25 ppm), distilled water and ethanol (95%).

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Experiment No. 3

Pharmaceutical Chemistry-I (0806)

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MAHARASHTRA STATE BOARD OF TECHNICAL EDUCATION

Pharmaceutical Chemistry-I (0806)

Experiment No. 3

7.0

Observations:
1. Opalescence produced by sodium bicarbonate test solution is .................................. (less/same/more) intense than that of standard solution. Opalescence produced by potassium permanganate test solution is ........................ (less/same/more) intense than that of standard solution. Opalescence produced by magnesium trisilicate test solution is ............................ .. (less/same/more) intense than that of standard solution.

2.

3.

8.0

Results:
1. 2. 3. The given sample of sodium bicarbonate..................................................... (complies/ does not comply) the limit test for chlorides as per the Indian Pharmacopoeia 1996. The given sample of potassium permanganate........................................... (complies/ does not comply) the limit test for chlorides as per the Indian Pharmacopoeia 1996. The given sample of magnesium trisilicate................................................. (complies/ does not comply) the limit test for chlorides as per the Indian Pharmacopoeia 1996.

9.0

Questions:
(Answer the following questions, Q. Q..Q.and Q.., Question Number to be allotted by teacher)
1. 2. 3. 4. 5. 6. 7. 8. 9. 10. State the meaning of the term opalescence. Write the principle of limit test for chlorides. State the chemical equation of chloride limit test. Give the reason for formation of opalescence. Write the procedure for preparation of standard solution for chloride limit test I.P. Write the procedure for preparation of sodium bicarbonate test solution for chloride limit test I.P. Write the procedure for preparation of potassium permanganate test solution for chloride limit test I.P. Write the procedure for preparation of magnesium trisilicate test solution for chloride limit test I.P. State the reason for use of silver nitrate in the chloride limit test. Why nitric acid is used in the chloride limit test give the reasons.

10.0 Reference:
Indian pharmacopoeia 1996

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Experiment No. 3

Pharmaceutical Chemistry-I (0806)

(Space for Answers)

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