Assay of Calcium gluconate by complexometry

Aim
To determine per cent content of Calcium gluconate in a given sample / To perform the
assay of calcium gluconate
Principle
Calcium gluconate can be assayed using complexometric titrations of Ca 2+ 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 a 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 the 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 a 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 0.05 M disodium edetate (C10H14Na2O8,2H2O) solution
Molar mass: 372.24 g/mol
372.24gm disodium edetate -----------------------1M-----------------------1000 mL
37.224gm disodium edetate -----------------------0.1 M---------------------1000 mL
3.72244 gm disodium edetate --------------------- 0.1 M---------------------100 mL
3.7224 gm/2 disodium edetate --------------------- 0.1 M/2---------------------100 mL
1.8612 gm disodium edetate --------------------- 0.05 M ---------------------100 mL

Dissolve 1.8612 gm of disodium edetate in sufficient water to produce 100ml

Preparation of 0.05 M Calcium chloride solution
Molar mass: 110.98 g/mol
110.98 gm Calcium chloride--------------------1 M--------------------- 1000 mL
11.098 gm Calcium chloride--------------------0.1 M--------------------- 1000 mL
1.1098/2 gm Calcium chloride--------------------0.1 M/2--------------------- 100 mL
0.55 gm Calcium chloride--------------------0.05 M------------------------- 100 mL
Dissolve 0.55 gm Calcium chloride in sufficient water to produce 100ml
Preparation of 10 M Ammonia solution
 Take 75 ml of strong ammonia and dissolve in 100 ml of water.

Preparation of Ammonia buffer:

Take 35 ml Ammonia solution (10 M) and 5.4 gm Ammonium chloride in 20 ml water and
then dissolve them in 100 ml water.
Preparation of 0.05 M Magnesium sulphate
Molar mass: 120.366 gm/mol
120.36 gm Magnesium sulphate --------------------1 M--------------------- 1000 mL
12.036 gm Magnesium sulphate --------------------0.1 M--------------------- 1000 mL
1.2036/2 gm Magnesium sulphate --------------------0.1 M/2--------------------- 100 mL
0.6 gm Magnesium sulphate --------------------0.05 M------------------------- 100 mL
Dissolve 0.6 gm Magnesium sulphate in sufficient water to produce 100ml

Standardization of 0.1M disodium edetate solution

Take 10 ml calcium chloride into the conical flask and add 5 ml Ammonia buffer two drops of
mordant black T or Solo Chrome black T indicator and start titrating with 0.05 molar EDTA.

Assay of calcium gluconate

Weigh 0.5 g calcium gluconate 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-ammonium chloride solution
and titrate with 0.05 M disodium edetate using mordant black II mixture as an indicator.
Carry out a blank titration.

Percentage purity can be determined by the following formula.

Titre value x Equivalent wt factor x Normality of NaOH(actual)
%= ----------------------------------------------------------------------- x100
Weigh of sample x Normality of titrant (expected)

REPORT: The percentage purity of the given sample of calcium gluconate is……101%