Laboratory Manual in PHARMACEUTICAL ANALYSIS 1

PRELAB
Exercise 11 Assay of Calcium Chloride
5

Name: Unlayao, Diana Mae Date Submitted:

Group No.:5 Score:

OBJECTIVE/s: At the end of this exercise, the student should be able to determine the purity of
of the raw material Calcium chloride using the volumetric complexation method
of analysis.

Principle Involved

 Calcium Chloride is assayed using volumetric complexation analysis using 0.5M EDTA solution
as the titrant and hydroxynapthol blue as the indicator producing clear/light blue endpoint.

Reaction/s Involved

 EDTA + CaCl2 CaEDTA + Cl2

Official USP/NF Requirement

 Calcium Chloride contains an amount of CaCl 2 equivalent to not less than 99.0 percent and not more
than 107.0 percent of CaCl2·2H2O.

Materials: Calcium chlroride

3N HCl solution
Hydroxynaphthol blue
1 N Sodium hydroxide
0.05 M Edetate disodium VS

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ASSAY PROCEDURE:
1. Transfer about 1 g of Calcium Chloride, accurately weighed, to a 250-mL beaker, and
dissolve in a mixture of water and 3 N hydrochloric acid (100:5).
2. Transfer the solution to a 250-mL volumetric flask, dilute with water to volume, and mix.
3. Pipet 50 mL of the solution into a suitable container, add 100 mL of water, 15 mL of 1 N
sodium hydroxide, and 300 mg of hydroxyl naphthol blue, and titrate with 0.05 M edetate
disodium VS until the solution is deep blue in color.

Each mL of 0.05 M edetate disodium is equivalent to7.351 mg of CaCl 2•2H2O.

Formula for the Calculation of Percent Purity:

%Purity= VolEDTA ×M×MW×100

Wt.ofsample

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Questions/Problems

1. What is the role of sodium hydroxide solution in the titration?

 Sodium hydroxide reacted to alkalinize and stabilize Ca-EDTA complex and prevent Mg2+ ion
which maybe present as contaminant.

2. What is the percentage of calcium (Ca) in fruits using 5.0-g sample consuming 12.5 mL of
0.0565 M EDTA? Each mL of 0.05 M EDTA is equivalent to 2.002 mg of calcium.

%Ca= V×M×MW×100
Sx

0.0125L×0.0565 mol L ×40.08 g mol ×100

5g
=0.57%

%Ca=V×MF×t iter×100
Sx
MF= 0. 0565M
0. 05M
=1. 13
12. 5mL×1. 13×2. 002 mg/ mL ×100
5000mg
=0. 57%

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3. A 200-mg sample of pure calcium carbonate was acidified and dissolved in 500 mL of
solution. A 50-mL sample required 25.0 mL of an EDTA solution for titration. Find the
molarity of the EDTA solution.

MWCaCO3 = 100. 09g/ mol

Ca=40. 08
C=12.02
O=16x3=48

=100. 09 g mol

M EDTA= Wt .
V×MW

0. 2g
0. 025L×100. 09 g/mol

=0. 0799 or 0. 08M

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