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CYCLE - I Experiment-2

TOTAL, PERMANENT AND TEMPORARY HARDNESS OF WATER -


DETERMINATION BY EDTA METHOD

Experiment No.: 2 Date:25/07/2016

Principle:
Hardness of water is due to the presence of calcium and magnesium salts in water. Ehtylene
diamine tetraacetic acid (EDTA) forms complexes with a large number of cations including
Ca2+ and Mg2+ ions depending upon pH of the solution. Hence, it is possible to determine the
total hardness of water using EDTA solution. EDTA in the form of its sodium salt (H 2Y2-) is
more often used in place of EDTA in complexometric titration for estimation of metal ions
because pure EDTA (H4Y) is sparingly soluble in water. EDTA has six binding sites (the
four carboxylate groups and the two amino groups) providing six pairs of electrons. The
resulting metal-ligand complex, in which EDTA forms a cage-like structure around the
metal ion, is very stable at specific pH. All metal-EDTA complexes have a 1:1
stoichiometry. The H2Y2- form complexes with metal ions as follows.
M + H2Y2- MY2- + 2H+ (1)

where, M is Ca2+ and Mg2+ present in water. Reaction (1) can be carried out quantitatively at
pH of 10 using Eriochrome Black T (EBT) indicator. EBT forms a wine-red complex with
M2+ ions which is relatively less stable than the metal-EDTA complex. On titration EDTA
first reacts with free M2+ ions and then with the metal-EBT indicator complex. The end point
of the reaction is change of colour from wine red to steel blue.

Requirements

Reagents and solutions: Standard hard water (0.001M), EDTA solution (0.001M), EBT
indicator, hard water sample and NH3-NH4Cl buffer solution.

Apparatus: Burette, pipette, conical flask, standard flask and burette stand
Procedure
Titration I - Standardization of EDTA
Pipette out 20 mL of the standard calcium ion solution (0.01N) into a clean 250 mL conical flask.
Add one full test tube of ammonia buffer (NH 4OH NH4Cl) solution to maintain the pH around
10. Add three drops of Eriochrome Black T (EBT) indicator and titrate the solution against
EDTA solution taken in the burette. The end point is change of color from wine red to steel blue.
Repeat the titration for concordant titre values. Let V1 be the volume of EDTA consumed.

Titration II - Estimation of Total Hardness


Pipette out 20 mL of the given sample of hard water into a clean conical flask. Add one test tube
full of ammonia buffer (NH4OH NH4Cl) solution and three drops of Eriochrome BlackT
(EBT) indicator. Titrate this mixture against standardized EDTA solution taken in the burette.
The end point is the change of color from wine red to steel blue. Repeat the titration for
concordant titre value. Let V2 be the volume of EDTA consumed.

Titration III - Estimation of Permanent Hardness


Transfer 100 mL of the given sample water into a beaker and boil it gently for 20 minutes. Cool
and filter it through a filter paper directly into a 100 mL standard flask. Make the solution with
distilled water upto the mark and mix well. Pipette out 20 mL of this solution into a clean 250
mL conical flask. Add one full test tube of ammonia buffer and three drops of EBT indicator.
Titrate this mixture against standardized EDTA solution taken in the burette. The end point is
change of color from wine red to steel blue. Repeat the titration for concordant titre value. Let
V3 be the volume of EDTA consumed.
OBSERVATION AND CALCULATIONS
Titration I - Standardization of Ethylene diamine tetraacetic aciddisodium salt (EDTA)
Burette: EDTA solution
Conical Flask: 20 mL of Standard hard water (SHW) + one test tube of buffer solution + 2 drops
of EBT. End point: wine-red to steel blue

Volume of Standard Burette reading (mL) Volume of EDTA


S. No.
hard water (mL) Initial Final (V1, mL)
1 20 0 19.8 19.8
2 20 19.8 39.5 19.7
3 20 0 19.8 19.8
Concordant titre value 19.8

20mL of Standard hard water = 19.8 mL of EDTA


20 x 1mg of CaCO3 = 19.8 mL of EDTA
1mL of EDTA = (20/V1) mg of CaCO3eqvt.
= (20/19.8) mg of CaCO3eqvt.
Titration II - Estimation of total hardness
Burette: standardized EDTA solution
Conical Flask: 20 mL of HW + one test tube buffer solution + 2 drops of EBT

S. No. Volume of Standard Burette reading (mL) Volume of EDTA


hard water (mL)
Initial Final (V2, mL)
1 20 0 7.2 7.2
2 20 0 7.2 7.2
Concordant titre value 7.2
20mL of given hard water = 7.2 mL of EDTA
= V2 X 20/V1 mg of CaCO3eqvt.
= 7.2* (20/19.8)

V2 X 20 X 1000
1000mL of given hard = mg of CaCO3eqvt
V1 X 20

V2 X 1000
= mg / L
V1

Total Hardness = V2X 1000 ppm = (7.2*1000)/19.8 ppm =363.63 ppm


V1

Titration III - Estimation of Permanent hardness


Burette: Standardized EDTA solution

Conical Flask: 20 mL of boiled and cooled sample water + one test tube buffer solution + 2 drops
of EBT

End point: wine-red to steel blue

S. No. Volume of standard hard Burette reading (mL) Volume of EDTA


water (mL)
Initial Final (V3, mL)
1 20 0 4.6 4.6
2 20 0 4.5 4.5
3 20 0 4.5 4.5
Concordant titre value 4.5

20mL of given boiled hard water = 4.5 mL of EDTA


V3 X 20
= mg of CaCO3eqvt.
V1
= (4.5*20)/19.8 mg of CaCO3eqvt

V3 X 20 X 1000
1000 mL of given boiled hard water = mg of CaCO3eqvt.
V1 X 20

= V3 X 1000 mg / L or ppm
V1
= (4.5*1000)/19.8 ppm

Permanent hardness= (V3/V1)*1000 ppm; = (4.5/19.8)*1000 ppm = 227.27 ppm

Temporary hardness = Total hardness Permanent hardness

= V2 V3 X 1000 ppm.
V1 V1

V2 V3
= V1 X 1000 ppm.
= 136.36 ppm Result:

The hardness of the given sample of hard water is


Total hardness = 363.63 ppm
Permanent hardness = 227.27 ppm
Temporary hardness = 136.36 ppm

Evaluation of result

Sample Experimental Actual Value Percentage of Marks


number value error awarded