Limit Test of Iron Pharmaceutical Analysis I Practical, Lab Manual, PDF
Pharmaceutical Analysis I Practical: Limit test for (1) Chloride (2) Sulphate (3) Iron (4) Arsenic Preparation and standardisation of (1) Sodium hydroxide (2) Sulphuric acid (3) Sodium thiosulfate (4) Potassium permanganate (5) Ceric ammonium sulphate Assay (1) Ammonium chloride (2) Ferrous sulphate(3) Copper sulphate (4) Calcium gluconate (5) Hydrogen peroxide (6) Sodium benzoate (7) Sodium Chloride Determination of Normality (1) Conductometric titration of strong acid against a strong base (2) Conductometric titration of strong acid and weak acid against a strong base (3) Potentiometric titration
Aim
To observe limits for iron impurities
Principle
The limit test for iron is based on the formation of purple colour by the reaction of iron (II) with thioglycolic acid in presence of citric acid and ammonia. The intensity of colour produced in the test solution is compared against the standard solution containing a known amount of iron. The purple colour is of iron thioglycollate complex
Procedure
Label two Nessler’s cylinders as Standard and Test and follow the procedure
Standard solution
Pipette out 2 ml of standard iron solution
Add 20 ml of distilled water
Add 2 ml of 20% solution of iron-free citric acid
Add 0.1 ml of thioglycolic acid Make the solution alkaline with ammonia buffer
Make up the volume to 50 ml with distilled water and allow to stand for 5 min
Test solution
Pipette out 2 ml of test iron solution Add 20 ml of distilled water
Add 2 ml of 20% solution of iron-free citric acid
Add 0.1 ml of thioglycolic acid
Make the solution alkaline with ammonia buffer
Make up the volume to 50 ml with distilled water and allow to stand for 5 min
Compare the colour intensities produced in standard and test solutions and report your result.
Reference
Indian Pharmacopoeia, ,2007, Volume 1, Pg No. 72
Limit test Chlorides, Sulphate, Iron, Heavy metals * Identification tests for Anions and Cations * Prep. & std Sodium Hydroxide, Potassium Permanganate * Assay Ferrous sulphate, Calcium gluconate, Sodium chloride, Ascorbic acid, Ibuprofen * Determination of Melting point & Boiling point * Preparation Benzoic acid from Benzamide, Picric acid from Phenol * Identification & purity test Aspirin, Caffeine
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