Eng Chem Lab manual

EXPERIMENT NO: 2
ESTIMATION OF HARDNESS OF WATER BY COMPLEXOMETRIC METHOD
USING EDTA

AIM: To determine the total hardness of water by EDTA method.

APPARATUS: Standard Flask, Pipette, Burette, Conical Flask, Beakers, Weighing Bottle,
Funnel
CHEMICALS REQUIRED: Epsom Salt (MgSO4 .7H2O), EDTA (Ethylene Diamine Tetra
Acetic acid) solution, EBT indicator (Eriochrome black-T), Buffer solution (NH4Cl+ NH4OH)
(pH= 9-10) & Hard water sample.

PRINCIPLE:
The hardness of water is generally due to the presence of calcium and magnesium ions in water.
The chlorides, nitrates and sulphates of calcium & magnesium are responsible for permanent
hardness, while bicarbonates of calcium & magnesium are the cause of temporary hardness.
EDTA forms a stable complex of Ca-EDTA or Mg-EDTA with hardness causing ions of Ca
and Mg present in hard water at pH= 9-10 (fixed using buffer). EBT is used as the indicator to
detect the completion of the reaction. When a small amount of EBT is added to hard water
sample, it reacts with Mg2+ or Ca2+ to produce wine red coloured solution due to the formation
of a complex. This wine red coloured solution is titrated with EDTA till the colour of the
solution changes blue, as EBT is released free in the solution and the stable Mg-EDTA or Ca-
EDTA complex is formed. End point is determined by the change in colour from wine red to
blue.
pH= 9-10
2+
M + EBT --------→ M-EBT complex (wine red colour)
Hard water Blue (Less stable)

pH= 9-10
M-EBT complex + EDTA --------→ M –EDTA complex + EBT
More stable, (colourless) (blue)

(Here M+2 = Ca+2 or Mg+2)

1
Eng Chem Lab manual

M = Ca2+, Mg2+

Fig.1. EDTA complexing agent

a M-EDTA2- complex
Fig.2. M

Procedure: It consists of 3 parts

parts:

PART – I: Preparation of standard Epsom salt (MgSO4.7H2O) Solution:

Weigh out accurately the given Epsom salt (MgSO4.7H2O) and transfer it into clean 100 ml
standard flask using a funnel. Dissolve the substance in minimum quantity of distilled water and
make it up to the mark with distilled water. Shake the solution thoroughly for uniform
concentration.
PART – II: Standardization of EDTA solution using standard
sta Epsom salt solution:
Fill burette with EDTA solution till the mark ‘0’. Next, ppipette
ipette out 20ml of Epsom salt solution
into a clean conical flask and add 5 ml of buffer solution (mixture of NH4OH + NH4Cl) followed
by 4 to 5 drops of EBT-indicator.
indicator. Titrate
Titrate this solution against the EDTA solution taken in the
burette, until the wine red color of the solution turns blue (end point). Repeat the titration for at
least two concurrent titre values.
PART – III: Estimation of Total hardness of water:
Pipette out 20 ml of the given hard water sample into a clean conical flask and add 5 ml of the
buffer solution (NH4OH + NH4Cl) followed by 4 to 5 drops of EBT indicator. Titrate this
solution against the standardized EDTA solution, until the wine red colour changes
chang blue (end
point). Repeat the titration for at least two concurrent titre values.

2
Eng Chem Lab manual

CALCULATIONS AND TABLES:

PART – I: Preparation of standard Epsom salt (MgSO4.7H2O) Solution:
Weight of the weighing bottle + Epsom salt (W1) = -------------- gms
Weight of the empty weighing bottle (W2) = ------------- gms
Weight of the Epsom salt (W1 – W2) = ----------------- gms
Eqv. wt of Epsom salt =123
Volume of the solution = 100 ml
୛ଵି୛ଶ ଵ଴଴଴
Normality of Epsom salt solution. (N1) = x
ଵଶଷ ଵ଴଴

= ---------
= --------- N

PART – II: Standardization of EDTA solution using standard MgSO4.7H20 solution:

S.No Volume of Epsom Burette readings Volume of EDTA

salt Pipette out (ml) Initial Final required (ml) (Final-Intial)
1 20
2 20
3 20

Epsom salt solution EDTA solution

Normality of Epsom salt sol.(N1) =------ N Normality of EDTA sol.(N2) =----- N
Volume of Epsom salt sol. (V1)= -------ml Volume of EDTA sol. (V2) =------ml

Normality of EDTA solution (N2) = N1V1

V2
= -------------

= ----------- N
PART – III: Estimation of Total hardness of water:

S.No Volume of Hard Water Burette readings Volume of EDTA

Pipette out (ml) Initial Final required (ml) (final-intial)
1 20
2 20
3 20

3
Eng Chem Lab manual

EDTA Solution
Normality of EDTA solution (N2) = ------ N (from Part-II)
Volume of EDTA solution (V2′) = Burette reading from Part-III (ml);
Hard water
Normality of hard water (N3) =------- N
Volume of hard water (V3) = 20 ml

Normality of hard water (N3) = N2 V2′

V3

= ----------- N

Total hardness of water in terms of CaCO3 equivalents = N3 x 50 x 1000 mg/lit

= ---------------- mg/lit or ppm

RESULT:

1) Normality of EDTA solution (N2) =--------------N

2) Normality of Hard Water (N3) = ------------- N
3) Total hardness of water in terms of CaCO3 equivalents =---------------- ppm

Viva – Questions

1. Mention the various units of hardness of water.

2. What are the chemical substances responsible for temporary and permanent hardness of
water?
3. Why carbonate hardness is temporary?
4. Non-carbonate hardness cannot be removed easily. Give the reason.
5. Write the chemical reactions taking place between hardness causing ions & EDTA.
6. Define buffer solution. Why basic buffer is added to hard water during titration.
7. Why this method of estimation is known as Complexometric method?
8. What is the indicator used in this method? Draw its chemical structure.
9. What are the colour observed with metal indicator complex and metal EDTA complex.
10. Draw the structure of Na2EDTA and Ca-EDTA.
11. What are the gram molecular and gram equivalent weights of Epsom salt (MgSO4.7H2O)
and Calcium Carbonate?
12. Calculate the weight of MgSO4.7H2O required to prepare 100 ml of 0.01N solution?