Calcium Analysis by EDTA.22

KIBABII UNIVERSITY
FACULYTY OF SCIENCE
DEPARTMENT OF SCIENCE, TECHNOLOGY AND ENGINEERING
SCH 350 ENVIRONMENTAL CHEMISTRY
CALCIUM ANALYSIS BY EDTA TITRATION
INTRODUCTION
Calcium Analysis by EDTA Titration
One of the factors that establish the quality of a water supply is its degree of hardness. The
hardness of water is defined in terms of its content of calcium and magnesium ions. Since an
analysis does not distinguish between Ca2+ and Mg2+, and since most hardness is caused by
carbonate deposits in the earth, hardness is usually reported as total parts per million(ppm)
calcium carbonate by weight. A water supply with a hardness of 100 ppm would contain the
equivalent of 100 grams of CaCO3 in 1 million grams of water or 0.1 gram in one liter of water.
In the days when soap was more commonly used for washing clothes, and when people bathed
in tubs instead of using showers, water hardness was more often directly observed than it is
now, since Ca2+ and Mg2+ form insoluble salts with soaps and make a scum that sticks to clothes
or to the bath tub. Detergents have the distinct advantage of being effective in hard water, and
this is really what allowed them to displace soaps for laundry purposes. Calcium in water will be
analyzed this week by EDTA titration and next week by atomic absorption analysis and the
results compared.
In this experiment you will standardize a solution of EDTA by titration against a standard
solution made from calcium carbonate, CaCO3. You will then use the EDTA solution to
determine the hardness of an unknown water sample. Since both EDTA and Ca2+ are both
colorless, it is necessary to use a rather special indicator to detect the end point of the titration.
The indicator you will employ is called Eriochrome Black T or simply Black T indicator, which
forms a rather stable wine-red complex, MgIn- with the magnesium ion. A tiny amount of this
complex will be present in the solution during the titration. As EDTA is added, it will complex
free Ca2+ and Mg2+ ions leaving the MgIn- complex alone until essentially all of the calcium and
magnesium has been converted to chelates. At this point, the EDTA concentration will increase
sufficiently to displace Mg2+ from the indicator complex; the indicator reverts to an acid form,
which is sky blue, and this establishes the end point of the titration.
The titration is carried out at a pH of 10, in an NH3-NH4+ buffer, which keeps the EDTA (H4Y)
mainly in the half-neutralized form, H2Y2-, where it complexes the Group IIA ions very well but
does not tend to react as readily with other cations such as Fe 3+ that might be present as
impurities in the water. Taking H4Y and H3In as the formulas for EDTA and Eriochrome Black T
respectively, the equations for the reactions that occur during the titration are as follows:
main reactions H2Y2-(aq)+Ca2+(aq)→CaY2-(aq)+2 H+(aq)

H2Y2-(aq)+Mg2+(aq)→MgY2-(aq)+2 H+(aq), at end point
H2Y2-(aq)+MgIn-(aq)→MgY2-(aq)+HIn2-(aq)+ H+(aq)
wine red sky blue
A little magnesium ion is already present in the solutions you will be using to form the initial red
complex with the indicator. This experiment requires that you recall the concepts of
stoichiometry, molarity and dilutions. You may need to refresh your memory before you begin
the prestudy and the experiment.
EXPERIMENTAL PROCEDURE
(a) Standardization of EDTA stock solution
Obtain a 50 mL buret, a 250 mL volumetric flask and 25 and 50 mL pipets.
1 .Using weighing paper, accurately weigh 0.3120 g of CaCO3. Transfer it quantitatively to a 250
mL beaker. (That is, make sure that every bit of the CaCO3 gets from the paper into the beaker.)
2. Add 25 mL of distilled water to the beaker and then slowly, about 20 drops of 12 M HCl.
(CAUTION: 12M HCl will burn flesh and clothing.) If the solution is not clear add a few
drops more of the HCl. Cover the beaker with a watch glass and allow the reaction to proceed
until all of the solid carbonate has dissolved.
3. Heat the solution until it just begins to boil. (Be sure not to be confused by the evolution of
CO2 which occurs with the boiling.) Carefully transfer the solution, using a clean funnel, to the
250 mL volumetric flask. Rinse the beaker several times with small portions of distilled water
and transfer each portion to the flask through the funnel. Rinse the funnel several times also. All
of the Ca2+ originally in the beaker should now be in the volumetric flask; the solution is one of
slightly acidic CaCl2.
4. Fill the volumetric flask with distilled water, adding the last few mL a drop at a time with your
wash bottle or an eye dropper. When the bottom of the meniscus is just even with the horizontal
mark on the flask, stopper the flask and mix the solution thoroughly by inverting the flask at least
a dozen times and shaking at intervals over a period of five minutes. Clean your buret
thoroughly.
5. Draw about 300 mL of the stock EDTA solution from the carboy into a clean, dry beaker.
Rinse the buret with 5 mL of the solution three times. Make sure the tip of the buret is full before
continuing with the titration. Don’t forget to check the tip for air bubbles.
6. Pipet 25 mL portions of your Ca2+ solution from the volumetric flask into two clean but not
necessarily dry 250 mL Erlenmeyer flasks. To each flask add 5 mL of the pH10 buffer and 2
drops of indicator. The initial color should be red and the endpoint color blue with no purple tint
to it. Reference solutions will be available for color comparison.
Be sure to read the burette to 0.01 mL.
7. Refill the burette, read it, and titrate the second solution. Do a third titration if there is poor
agreement between the first two. Use your best two values in your calculations.
(NB. If the volume of EDTA required in the first titration is low due to the fact that the water is
not very hard, increase the volume of the water sample.)
Calculate the molarity of the stock EDTA solution.
(b) Analysis of unknown water sample
Your instructor will furnish you with a sample of water for hardness analysis. Since the
concentration of Ca2+ is probably lower than that in the standard calcium solution you prepared,
pipet 50 mL of the water sample into two clean 250 mL Erlenmeyer flasks. As before, add 2
drops of indicator and 5 mL of pH10 buffer and titrate to a blue endpoint.
Questions
1. Work out the average titre volume.

2. Determine the number of moles of EDTA that reacted.
3. How many moles of Ca2+ were used?
4. Calculate the hardness of water in ppm CaCO3 .

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KIBABII UNIVERSITY

main reactions H2Y2-(aq)+Ca2+(aq)→CaY2-(aq)+2 H+(aq)

(a) Standardization of EDTA stock solution

Obtain a 50 mL buret, a 250 mL volumetric flask and 25 and 50 mL pipets.

(b) Analysis of unknown water sample

1. Work out the average titre volume.

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