Experiment I

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Experiment no-

Date:

Estimation of Hardness of Water by Complexometric method


using EDTA

Aim: To estimate the total hardness of water by Complexometric method using


EDTA.
Apparatus required:
1. Weighing bottle
2. Volumetric flask
3. Beaker
4. Burette
5. Pipette
6. Conical flask
7. Wash bottle
Reagents required:
1. MgSO4·7H2O (Epsom salt)
2. Disodium salt of Ethylene di amine tetra aceticacid
3. Eriochrome Black-T (EBT) indicator
4. Buffer (NH4OH +NH4Cl)

Principle:
Ca2+(aq) and Mg2+(aq) ions that causes hardness in water can be determined by
complexometric titration with a chelating agent, ethylene diamine tetra acetic acid
(EDTA), usually in the form of disodium salt.

Addition of Eriochrome Black-T indicator to the hard water at pH range 9–10


forms wine red coloured unstable complex with Ca2+ and Mg2+ ions of the sample
water. The unstable wine red colour complex forms a colourless stable complex with
EDTA and liberates the blue coloured EBT indicator.

Ca2+ / Mg2+ + EBT pH 9-10 [Ca- EBT] / [Mg-EBT]


Wine red colour complex
(Unstable )

[Ca- EBT] / [Mg-EBT] + EDTA pH 9-10 [Ca- EDTA] / [Mg-EDTA] + EBT


Colourless complex Blue
(stable )

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Engineering Chemistry Lab

Procedure:
Step- 1: Preparation of standard MgSO4·7H2O solution

· Weigh the given MgSO4·7H2O salt using weighing balance and


transfer into aclean 100 ml volumetric flask.

· Dissolve the transferred salt in the distilled water and make up the
solution up to the mark.

· Shake the volumetric flask for a while to get uniform concentration.


Calculations:

Weight of MgSO4·7H2O salt + weighing bottle (W1) = …………..


Weight of empty weighing bottle (W2) = ………….
Weight of MgSO4·7H2O salt transferred (W1-W2) = …………

Weight of salt 1000


Normality of MgSO4·7H2O = X
Equivalent weight of salt 100

(Equivalent Weight of MgSO4 .7H2O is 123)

Step- 2: Standardization of EDTA solution

• Pipette out 20ml of Standard MgSO4·7H2O solution into a clean 250 ml


conical flask.
• Add 2 ml of buffer (NH4OH+NH4Cl) to maintain pH between 9–10.
• Add 2–3 drops of Eriochrome Black-T indicator, the solution then turns
to wine red.
• Fill the burette with EDTA solution and adjust to zero, then fix it to the
burette stand.
• Now titrate the above MgSO4·7H2O solution against EDTA solution till
the wine-red solution turns to blue which is the end point of the titration.
• Note down the burette reading and repeat the titration for concurrent
values.

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Observations and Calculations:

Burette reading (ml) Volume of EDTA


Volume of MgSO4· 7H2O Initial Final solution run
S.No solution ( ml)
down (ml)

N1 V1= N2V2

N1 = Normality of MgSO 4·7H2O solution =

V1 = Volume of MgSO4·7H2O solution = N2

= Normality of EDTA solution =

V2 = Volume of EDTA solution =

N1 V1
Normality of EDTA solution (N2) = =
V2

STEP- 3: Estimation of total hardness of the given water samples


• Pipette out 20ml water sample-1 into a clean 250 ml conical flask.
• Add 2 ml of buffer (NH4OH+NH4Cl) to maintain pH between 9–10.
• Add 2–3 drops of Eriochrome Black-T indicator then solution turns
to wine red in colour.
• Fill the burette with EDTA solution and adjust to zero then fix it into
the burette stand.
• Now titrate the above water sample against EDTA solution till the
wine-red solution turns to blue which is the end point of the titration.
• Note down the burette reading and repeat the titration with water
sample-2.

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Engineering Chemistry Lab

Observations and Calculations:

Burette reading Volume of EDTA


Volume of water solution run down
sample ( ml) Initial Final (ml)

Sample-1 (V3)

Sample-2 (V4)

Total hardness expressed as CaCO3 equivalents


Normality of EDTA x Volume of EDTA x 50 x1000
=
Volume of water sample

N2 x Volume of EDTA(V3) x 50 x1000


Sample-1 =
Volume of water sample

N2 x Volume of EDTA(V4) x 50 x1000


Sample–2 =
Volume of water sample

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Precautions:
1. All the glassware must be washed with distilled water.
2. All the reagents must be prepared freshly with distilled water.
3. Discard the buffer solution if it is turbid.
4. Avoid skin contact with chemicals.

Result:

Amount of total hardness present in the given Reported Given % Error

Water sample 1

Water sample 2

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Engineering Chemistry Lab

POGIL ACTIVITY

I. Title: Estimation of Hardness of Water by Complexometric method using EDTA


II. Learning Objectives:
i. To determine the hardness of water samples by complexometric titration.
ii. To compare the amount of hardness in the given water samples.

III. Critical thinking Questions:

1. Name the titration involved in this experiment?

a) Precipitation titration b) Complexometric titration c) Acid -Base titration d)


Redox titration
2. What is the colour change at the end point?
a) blue to wine red b) wine red to blue c) red to blue d) blue to pink

3. The type and composition of the buffer used in the titration is.
a) Acidic buffer (HCl + NH4Cl) b) Basic buffer (NH4OH+ NH4Cl)
c) Acidic buffer (HCl + NaOH) d) Basic buffer (NaOH+NaCl)

4. What is the hardness range of hard water?


a) 0 – 70 ppm b) 70 – 150 ppm c) 150 – 300 ppm d) 300 above
5. At what favorable pH range, complexes are formed.
a) 6-7 b) 7-8 c) 9-10 d) 8-9

6. Write the unstable complex formed in the reactions ------------------------ --.


7. Temporary hardness is estimated by------------------------------ method.
8. Hardness of water is expressed in ------------------------------------units.
9. -------------------is the primary standard used in the hardness experiment.
10. The indicator used in the determination of hardness of water by EDTA method
is ----------- --.
11. Why natural water should not be fed into boilers?
12. Soft water is not fit for drinking. Justify
13. Blue color is formed at the end point. Give reason
14. Suggest another method for estimating the amount of hardness in water sample.
15. What are the permissible and desirable limits of hard water?

IV. Research Applications:


What is the information obtained by performing this experiment and its utility in
various fields of water technology? (200 words)
Hints:

1) What happens if hard water is used in various industries?


2) With special reference to steam generation in boilers.

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