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Assay of Calcium gluconate IP Pharmaceutical Analysis I Practical


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 determine per cent content of Calcium gluconate in a given sample

Principle

Calcium gluconate can be assayed using complexometric titrations of Ca2+ ions using EDTA as a sequestering (chelating) agent which results in the formation of a relatively stable complex. However, Mordant-Black II which is used as an indicator does not give distinct colour change. Hence, calcium ions are not directly titrated against disodium EDTA. Rather a displacement or replacement type of titration is used or performed wherein, a known volume of 0.05M magnesium sulphate solution is added (5ml) which acts as a displacing agent.

Magnesium ions displace calcium ions from the calcium indicator complex and form a more stable Mg indicator complex. But this complex is less stable than the Mg-EDTA complex. Relative stability of different complexes decreases in following order: Ca-EDTA > Mg-EDTA > Mg-In > Ca-In. Initially when both calcium and magnesium ions are present in the solution and when the indicator is added it forms complex with Mg as Mg-In is stronger than Ca-In complex and imparts a pink colour to the solution. When titration commences added EDTA forms a complex with calcium ions as a Ca-EDTA complex is stronger than the Mg-EDTA complex. when all the calcium ions are complexed than free Mg++ forms complex with EDTA and endpoint is reached then Mg-In complex breaks liberating free Mg+2 and In- which forms complex with EDTA and free In- imparts a blue colour to the solution. The ammonia solution buffers the solution at pH 10

Standard

Calcium gluconate (mol. wt.: 448.4) contains not less than 98.5% and not more than 102.0% of C12H22CaO14, H2O.

Procedure

Preparation of 0.1M disodium edetate solution

Dissolve ______ g of disodium edetate in sufficient water to produce 1000ml

  1. Standardization of 0.1M disodium edetate solution

Weigh accurately about 0.8 g of granulated zinc dissolve by gentle warming in 12 ml of dil. Hydrochloric acid and 0.1ml of bromine water. Boil to remove excess bromine, cool and add sufficient water to produce 200ml. pipette 20 ml of the resulting solution into a flask and nearly neutralize with 2M sodium hydroxide. Dilute to about 150ml with water add sufficient ammonia buffer pH 10.0 to dissolve the precipitate and add 5ml in excess. Add 50mg of mordant black II mixture and titrate with the disodium edetate solution until the solution turns green.

  • Assay of calcium gluconate

Weigh 0.5 g and dissolve in 50 ml of warm water; cool, add 5.0 ml of 0.05 M magnesium sulphate and 10 ml of strong ammonia solution and titrate with 0.05 M disodium edetate using mordant black II mixture as an indicator. Carry out a blank titration.

Reference

Indian Pharmacopoeia 2014; Vol. II; Pg. No. 1253-1254.


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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F Y B Pharm Sem-IF Y B Pharm Sem-II
BP101T Human Anatomy and Physiology I TheoryBP201T Human Anatomy and Physiology II – Theory
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F Y D Pharm & S Y D Pharm Notes, Books, Syllabus, PDF, Videos

First Year D PharmSecond Year D Pharm
ER20-11T Pharmaceutics TheoryER20-21T Pharmacology Theory
ER20-11P Pharmaceutics PracticalER20-21P Pharmacology Practical
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Suggested Readings:

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  • BP108P Pharmaceutical Analysis I Practical
  • BP701T. INSTRUMENTAL METHODS OF ANALYSIS Theory

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B Pharmacy Notes (Subjectwise/Topicwise)

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  • Disease
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  • Ellicium Solution Freshers Job
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