Aim :- To perform the assay of calcium gluconate as per I.P.
Reference:-
Requirements :- Ammonia, Solochrome black-T indicator, disodium edetate, calcium chloride,
burette, pipette, conical flask, volumetric flask, funnel, glass rod etc
A) Preparation and standardization of EDTA solution (0.05M)
Principle:- This experiment is based on the complexometric titration. Indicator is added in calcium
chloride solution which result in the formation of Ca-Indicator complex.
CaCl2 + In- Ca-In
Calcium chloride indicator calcium-indicator complex
On titrating against disodium edetate the complex gives Ca to EDTA, which liberate blue coloured
indicator i.e. end point of reaction.
Ca-In + EDTA Ca-EDTA + In-
calcium-indicator complex disodium edetate Calcium-disodium Free indicator
edetate complex
Procedure :-
a) Preparation of reagents and solutions:-
1. Preparation of CaCl2 (0.05M):- dissolve 7.35g of calcium chloride in 700ml distilled
water and make upto 1000ml.
2. Ammonia (10 M) :- dissolve 75ml of strong ammonia solution to a volumetric flask
and make up to 100ml with distilled water.
3. Preparation of ammonia buffer (pH 10) :- dissolve 5.4g of ammonium chloride in 20
ml water, add 35 ml of 10 M ammonia and make up 100ml with distilled water.
4. Preparation of EDTA solution :- weigh accurately about 18.16 g of disodium edetate
and dissolve in 1000ml distilled water.
b) Titration:-
1. Clean and dry all glass ware as per standard laboratory procedure.
2. Take 10ml of CaCl2 solution by using pipette and transfer to a conical flask.
3. Add 5ml buffer solution to make it alkaline.
4. Add 2 drops Solochrome Black-T indicator.
5. Then fill the burette with EDTA solution.
6. Start titration with the EDTA solution with vigorous shaking of flask until reach the
endpoint.
7. Record the reading of burette.
8. Repeat the titration 3 times to get precise readings.
Observation Table:-
Sr. No. Content in flask Burette reading Volume of EDTA
solution used(ml)
Initial final
1. 10 ml CaCl2 solution + 5 ml
2. buffer solution
3.
Volume of EDTA used = F1 + F2 + F3 / 3 =
Calculation :-
M1V1 = M2V2
M2= V1M1 / V2
Where, M1 = molarity of CaCl2 solution
V1= volume of CaCl2 solution used(ml)
M2= molarity of EDTA solution
V2= volume of EDTA solution used(ml)
B) Performing assay of calcium gluconate
Principle :- this is based on the replacement complexometric titration. Magnesium forms complex
with Solochrome black T indicator which shows first colour.
Mg2+ + In- Mg-In
Magnesium ion indicator magnesium-indicator complex
Magnesium indicator complex is much more stable than calcium-indicator complex. On titration
against disodium edetate complex of calcium and disodium edetate is formed.
Ca+ + EDTA Ca-EDTA
Calcium ion disodium edetate calcium-disodium edetate complex
When calcium is totally consumed, nest drop of disodium edetate breaks the magnesium – indicator
complex and make complex with magnesium by liberating free indicator. End point is detected by
observing second colour at that time.
Mg-In + EDTA Mg-EDTA + In-
Magnesium-indicator magnesium disodium free indicator
Complex edetate complex
Procedure :-
A. Preparation of reagents and solutions:-
1. 0.05M MgSO4 solution:- 0.6gm of MgSO4 dissolve in 100 ml distilled water.
2. Strong ammonia-ammonium chloride solution :- mix 10 ml water with 20 ml strong
ammonia solution and saturate it with ammonium chloride.
B. Titration:-
1. About 0.5gm calcium gluconate dissolve in 50 ml of warm water. Allow to cool.
2. Add 5ml of 0.05 M magnesium sulphate.
3. Add 10 ml strong ammonia- ammonium chloride solution.
4. Add 2 drops of Solochrome black T indicator.
5. Fill the burette with disodium edetate solution.
6. Start titration with disodium edetate until reach the endpoint.
7. The endpoint shown by change in colour of solution.
8. Repeat titration 3 times to get precise reading.
9. Repeat the titration again using same procedure without calcium gluconate for blank
reading.
Observation table:-
Sr. No. Content in flask Burette reading Volume of EDTA
solution used(ml)
Initial final
1. 0.5g calcium gluconate in 50 ml
2. water + 5 ml MgSO4 + 10 ml
3. strong ammonia- ammonium
chloride solution
Calculation :-
Percentage purity = V * E * AM * 100 / W * RM
Where, V= volume of disodium edetate used (ml)
V= A – B
A = volume of EDTA used in titration with calcium gluconate
B = volume of EDTA used in titration without calcium gluconate
E= equivalent factor
AM = actual molarity
RM = required molarity
W = weight of sample (g)
Note :- Equivalent factor of calcium gluconate for 1 ml of 0.05 M disodium edetate is 0.02242.
Result :- The Strength of prepared EDTA solution was found to be ……………….M
The percentage purity of calcium gluconate was found to be………………….
