Calcium Ion Concentration Determination via EDTA Titration

EDTA titrations forms complexes with metal ions, such that: Y 4 + Ca2+  CaY-2. In this case,

Standardization of 0.01 M EDTA solution:

Mass of CaCO3 used: 0.5 g

Standard Ca2+ Solution Sample A Sample B Sample C

Volume of Ca2+ (mL) 25 mL 25 mL 25 mL
Molarity of Ca2+ 0.01 M 0.01 M 0.01 M
Volume of EDTA (mL) 1000 mL 1000 mL 1000 mL
Molarity of EDTA 0.01 M 0.01 M 0.01 M

The procedure was

Analysis of calcium unknown:

Mass of CaCO3 used: 0.1 g

Ca2+ Unknown Sample A Sample B Sample C

Volume of Ca2+ unknown
250 mL 250 mL 250 mL
(mL)
26.5 mL 26.2 mL 26.4 mL
Volume of EDTA (mL)
Average volume of EDTA (mL): 26.3 mL
M
0.009 M  0.01 M 0.009 M  0.01 M 0.009 M  0.01 M
Ca2+ ion (mol/L)
concentration ppm
400000000 ppm 400000000 ppm 400000000 ppm
(mg/L)
%Ca determination (w/w) 0.04% 0.04% 0.04%

Analysis of eggshell:
Mass of eggshell used: 0.01997 g
 CALCIUM ION CONCENTRATION DETERMINATION VIA EDTA TITRATION

Calcium ion concentration and %Ca determination: Results and Observations

STANDARDIZATION
Mean
Volume of Molarity of Volume of Molarity of
Sample No. Molarity of
Ca2+ Ca2+ EDTA EDTA
EDTA
1 250 mL 0.02 M 26.5 mL 0.0189 M
2 250 mL 0.02 M 26.2 mL 0.0191 M 0.0190 M
3 250 mL 0.02 M 26.4 mL 0.0189 M

DETERMINATION OF UNKNOWN CONCENTRATION AND %m/m

Mass of
Volume of Molarity of Molarity of
Trial No. original %m/m of Ca2+
EDTA EDTA Ca2+
sample
1 26.5 mL 0.0189 M 0.5 g 1.88% 0.02 M
2 26.2 mL 0.0191 M 0.5 g 1.90% 0.02 M
3 26.4 mL 0.0189 M 0.5 g 1.89% 0.02 M
 End Point Detection Methods: Fajans

Results:

Samples 1, 2, and 3 showed accurate and precise results that proved to be repeatable and
reproducible. With similar reactions, the concentrations of all three samples are 3.33%. A mass of
1.5 g of chloride sample with 2-3 drops of dichlorofluorescein indicator was titrated with AgNO3. The
appearance of persistent pink color was achieved when 45.00 mL of AgNO3 was added to the
chloride solution as shown in the table 1 below.

Calculated
Volume of AgNO3
Sample No. Mass of Chloride concentration of
added
chloride ion (%w/v)
Sample 1 1.5 g 45.00 mL 3.33%
Sample 2 1.5 g 45.00 mL 3.33%
Sample 3 1.5 g 45.00 mL 3.33%

Thus, the reaction of AgNO3 and Cl is represented as:

AgNO3(aq) + Cl(aq)  AgCl(s) + NO3(aq)
Ag+ + NO3 + Cl  AgCl + NO3
Ag+(aq) + Cl(aq)  AgCl(s)

The anionic dye, dichlorofluorescein, is added to the analyte’s solution. Before the endpoint,
the precipitate of AgCl has a negative surface charge due to the adsorption of excess Cl . Due to the
fact that dichlorofluorescein also carries a negative charge, it is repelled by the precipitate and
remains in solution where it has a greenish-yellow color. After the endpoint, the surface of the
precipitate carries a positive surface charge due to the adsorption of excess Ag +. Dichlorofluorescein
now adsorbs to the precipitate surface where its color is pink. This change in the indicator’s color
signals the endpoint, where:

Before the equivalence point:
At equivalence point:
After the equivalence point:
Addition of Ag+ to Cl leads to the formation of colloidal AgCl.
All Ag+ ions have been consumed.
Anion dyes adsorbed on the AgCl surface and excess Ag+ react with
dichlorofluorescein, producing pink precipitate.