Pharmaceutical Analysis - 1
Unit 1
B. Pharm I Semester
UNIT-I
1. Pharmaceutical analysis- Definition and scope
i. Different techniques of analysis
ii. Methods of expressing concentration
iii. Primary and secondary standards.
iv. Preparation and standardization of various molar and normal solutions-
Oxalic acid, sodium hydroxide, hydrochloric acid, sodium thiosulphate,
sulphuric acid, potassium permanganate and ceric ammonium sulphate.
2. Errors: Sources of errors, types of errors, methods of minimizing errors,
accuracy, precision and significant figures.
3. Pharmacopoeia, Sources of impurities in medicinal agents, limit tests.
Notes Prepared by: Mr. Aamir Malik (Assistant Professor, HIMT College of Pharmacy)
Pharmaceutical Analysis - 1
Unit 1
B. Pharm I Semester
Topic: Limit Test
Limit Test:
These are the semi-quantitative test which are used to identify the impurities
present in a substance are in a certain limit or not.
Limit = a range of value or amount that is likely to be present in a substance.
Test = to examine or to investigate.
They are used to check the purity of the substances.
These test are generally evaluated by comparing the turbidity/opalescence,
colour intensity between the standard and test sample.
Importance of limit test:
Detect the amount of impurities present in the sample.
Make the difference between avoidable and unavoidable impurities.
It help in finding out the harmful substances in the sample.
Notes Prepared by: Mr. Aamir Malik (Assistant Professor, HIMT College of Pharmacy)
Pharmaceutical Analysis - 1
Unit 1
B. Pharm I Semester
Limit test for chloride:
Principle:
Limit test of chloride is based on the reaction of chloride ion (Cl-) present in
the sample with silver nitrate in presence of dilute nitric acid to form silver
chloride.
dil. HNO3 NO3-
Cl- + AgNO3 AgCl +
Present in Appears as
sample Precipitate
The silver chloride formed in the reaction is appears as precipitate/insoluble
substance and shows the turbidity in the solution.
Higher the amount of chloride ion (Cl-) present in the sample, higher the
turbidity of the solution.
Procedure:
Test sample Standard compound (25 ppm Cl- )
Specific weight of compound is dissolved in Take 1ml standard solution of chloride in Nessler
water or solution is prepared as directed in cylinder
the pharmacopoeia and transferred in Nessler
cylinder
Add 10 ml of nitric acid Add 10 ml of nitric acid
Dilute to 50ml in Nessler cylinder Dilute to 50ml in Nessler cylinder
Add 1ml of AgNO3 solution Add 1ml of AgNO3 solution
Keep aside for 5 min Keep aside for 5 min
Observe the Opalescence/Turbidity Observe the Opalescence/Turbidity
Standard chloride solution:
5ml of 0.0824 % W/V solution of sodium chloride in 100 ml of water.
Observation:
The turbidity produce in sample and standard solution is compared.
If turbidity produces in sample solution is less than the standard solution,
then sample passed the limit test of chloride.
If turbidity produces in sample solution is greater than the standard solution,
the sample did not passed the limit test of chloride.
Notes Prepared by: Mr. Aamir Malik (Assistant Professor, HIMT College of Pharmacy)
Pharmaceutical Analysis - 1
Unit 1
B. Pharm I Semester
Notes Prepared by: Mr. Aamir Malik (Assistant Professor, HIMT College of Pharmacy)
Pharmaceutical Analysis - 1
Unit 1
B. Pharm I Semester
Limit Test of Sulphate:
Principle:
Limit test of sulphate is based on the reaction of sulphate ion (SO42-) with
barium chloride in presence of dilute hydrochloride acid to form barium
sulphate (BaSO4).
dil. HCl Cl-
SO42- + BaCl2 BaSO4 +
Present in Appears as
sample Precipitate
The barium sulphate (BaSO4) formed in the reaction is appeared
precipitate/insoluble substance and shows the turbidity in the solution.
Higher the amount of sulphate ion (SO42-) present in the sample, higher the
turbidity of the solution.
Procedure:
Test sample Standard compound (10 ppm SO4 2-)
Specific weight of compound is dissolved Take 1ml of 0.1089 % W/V solution of
in water or solution is prepared as potassium sulphate in Nessler cylinder
directed in the pharmacopoeia and
transferred in Nessler cylinder
Add 2ml of dilute hydrochloric acid Add 2ml of dilute hydrochloric acid
Dilute to 45 ml in Nessler cylinder Dilute to 45 ml in Nessler cylinder
Add 5ml of barium sulphate reagent Add 5ml of barium sulphate reagent
Keep aside for 5 min Keep aside for 5 min
Observe the Turbidity Observe the Turbidity
Preparation of Barium Sulphate Reagent:
Add 15ml of 0.05M Barium Chloride solution to the mixture of 55ml water,
and 20 ml ethanol.
Then add 5 ml of 0.0181% w/v potassium sulphate (K2SO4) solution and
make the volume up to 100ml with distilled water.
Preparation of ethanolic sulphate standard solution (10 ppm SO4 2-):
Dissolve 1 part of a 0.181% w/v solution of potassium sulphate in 100 parts of ethanol
(30%).
Preparation of sulphate standard solution (10 ppm SO4 2-):
Notes Prepared by: Mr. Aamir Malik (Assistant Professor, HIMT College of Pharmacy)
Pharmaceutical Analysis - 1
Unit 1
B. Pharm I Semester
Dissolve 1 part of a 0.181% w/v solution of potassium sulphate in 100 parts of
distilled water.
Observation:
The turbidity produce in sample and standard solution is compared.
If turbidity produces in sample solution is less than the standard solution,
then sample passed the limit test of chloride.
If turbidity produces in sample solution is greater than the standard solution,
the sample did not passed the limit test of sulphate.
Notes Prepared by: Mr. Aamir Malik (Assistant Professor, HIMT College of Pharmacy)
