EXPERIMENT No.

Object: To determine the amount of total permanent and temporary hardness of given sample of hard water
by EDTA titration method.

Apparatus required: 50 ml Burette, 20 ml Pipette, 250 ml Conical flask, 100 ml Beaker, 250 ml beaker,
Glass funnel, etc.

Reagents: EDTA solution, Standard CaCO3 solution, Eriochrome Black–T indicator, Buffer solution.

Theory: Eriochrome Black-T (E.B.T) is used as an indicator to detect the end point. EBT forms unstable,
wine-red colored complexes with Ca2+ and Mg2+ ions present in hard water sample. When EDTA (Ethylene
diamine tetra acetic acid) is added to water, the metal ions Ca 2+ and Mg2+ forms colorless stable complexes
with EDTA. When all the metal ions react with EDTA and the metal ions in EBT complex are removed by
EDTA, the indicator is set free. Therefore, the colour changes from wine red to steel blue. To maintain the
pH of the solution at 9-10, buffer solution (NH4Cl + NH4OH) is used. The metal-EDTA complex is stable at
pH= 9-10. The end point is change from wine red to steel blue.
PROCEDURE:

Titration-I Standardization of EDTA (Std. Hard water Vs EDTA)

(i) Pipette out 20 ml of standard hard water into a conical flask.
(ii) Add 5 ml of buffer solution and few drops of Eriochrome Black-T. The indicator, which is steel blue
colour, would acquire a wine-red color.
(iii) Titrate with EDTA solution taken in the burette, till the wine red color changes to steel blue which is the
end point. Let the burette reading of EDTA be V2 ml.

S.No. Volume of Hard Burette Reading (ml) Volume of EDTA (ml) Concordant value (ml)
water (ml)
Initial Final
1. 20 0.00 19.6 19.6
2. 20 0.00 19.5 19.5 19.5
3. 20 0.00 19.4 19.4

Volume of Std. Hard water, V1 = 20 ml

Strength of Std. Hard water, N1 = 0.01 N
Volume of EDTA solution, V2 = 19.5 ml
So, Strength of EDTA solution, N2 = V1N1/V2
20 x 0.01
= = 0.0102 N
19.5

Titration-II Determination of Total hardness (Std. EDTA Vs Water sample)

Repeat the above titration method for sample hard water instead of standard hard water. Let the
burette reading of EDTA be V2 ml.
S.No. Volume of Hard Burette Reading (ml) Volume of Std. Concordant value (ml)
water sample EDTA (ml)
Initial Final
(ml)
1. 20 0.00 12.5 12.5
2. 20 0.00 12.7 12.7 12.5
3. 20 0.00 12.4 12.4

Volume of Std. EDTA, V1 = 12.5 ml

Strength of Std. EDTA, N1 = 0.0102 N
Volume of Hard water sample, V2 = 20 ml
So, Strength of Hard water sample, N2 = V1N1/V2
12.5 x 0.0102
= = 0.0063 N
20

Total Hardness = Strength of Hard water x Eq. Wt of CaCO3 x 1000

= 0.0063 x 50 x 1000
= 315 ppm
So, Total Hardness in given sample = 315 ppm
Titration-III Determination of Permanent hardness (Sample Hard water Vs EDTA)
Take 100 ml of sample hard water in 250 ml beaker. Boil it to remove temporary hardness to about
half of this volume and cool to room temperature. Filter through filter paper to remove insoluble CaCO3 and
MgCO3. Make up the volume to the original 100 ml by adding distilled water. Now pipette out 20 ml of this
solution into a clean conical flask. Then repeat the process of titration steps as mentioned above. Let the
burette reading of EDTA be V2 ml.

S.No. Volume of Hard Burette Reading (ml) Volume of Std. Concordant value (ml)
water sample EDTA (ml)
Initial Final
(ml)
1. 20 0.00 6.2 6.2
2. 20 0.00 6.4 6.4 6.2
3. 20 0.00 6.0 6.0

Volume of Std. EDTA, V1 = 12.5 ml

Strength of Std. EDTA, N1 = 0.0102 N
Volume of Hard water sample, V2 = 20 ml
So, Strength of Hard water sample, N2 = V1N1/V2
6.2 x 0.0102
= = 0.0031 N
20

Permanent Hardness = Strength of Hard water x Eq. Wt of CaCO3 x 1000

= 0.0031 x 50 x 1000
= 155 ppm

So, Permanent Hardness in given sample = 155 ppm

Total Hardness = Temporary Hardness + Permanent Hardness

So, Temporary hardness = Permanent Hardness - Temporary Hardness

= 315-155 = 160 ppm

Results:
(i) Amount of Total Hardness of the given sample of water = 315 ppm
(ii) Amount of Permanent Hardness of the given sample of water = 155 ppm
(iii) Amount of Temporary Hardness of the given sample of water = 160 ppm
 EXPERIMENT No. 2

Object: Determination of acetic acid in commercial vinegar using NaOH.

Apparatus required: 50mL beaker, 100 ml volumetric flask (with cap), 50 ml burette, 10 ml pipette,
Titration apparatus, etc.

Chemical required: Phenolphthalein indicator solution, distilled water, 0.1N oxalic acid, 0.1N NaOH
solution, sample of commercial vinegar, etc.

Theory: vinegar is 4-10% acetic acid and it is neutralized by titrating with standard NaOH solution. The
reaction between acetic acid and NaOH is given below:

CH3COOH + NaOH → CH3COONa + H2O

PROCEDURE:

Preparation of 100 ml, 0.1N oxalic acid solution:

Molecular weight of oxalic acid = 126
Equivalent weight of oxalic acid = 63

0.1 x 63 x 100
Wt. of oxalic acid = = 0.63 g
1000
Dissolved 0.63 g oxalic acid in 50ml of distilled water and transferred it in to 100 ml volumetric
flask and make up the volume 100 ml.

Titration-I Standardization of NaOH (Std. Oxalic acid Vs NaOH)

(i) Pipette out 10 ml of standard oxalic acid into a conical flask.
(ii) Add 2 or 3 drops of Phenolphthalein indicator.
(iii) Titrate with NaOH solution taken in the burette, till the colourless solution changes to pink colour which
is the end point. Repeat the titration to get concordant readings. Let the burette reading of NaOH be V2 ml.

S.No. Volume of oxalic Burette Reading (ml) Volume of NaOH (ml) Concordant value (ml)
acid (ml)
Initial Final
1. 10 0.00 10 10
2. 10 0.00 9 9 10
3. 10 0.00 11 11

Volume of Std. Oxalic acid, V1 = 10 ml

Strength of Std. Oxalic acid, N1 = 0.1 N
Volume of NaOH solution, V2 = 10 ml
So, Strength of NaOH solution, N2 = V1N1/V2
10 x 0.1
= = 0.1 N
10
Titration-II Determination of strength of vinegar (Standardized NaOH Vs Vinegar)
(i) Pipette out 10 ml of diluted vinegar sample into a conical flask.
(ii) Add 2 or 3 drops of Phenolphthalein indicator.
(iii) Titrate with NaOH solution taken in the burette, till the colourless solution changes to pink colour which
is the end point. Repeat the titration to get concordant readings. Let the burette reading of NaOH be V2 ml.

S.No. Volume of dil. Burette Reading (ml) Volume of NaOH (ml) Concordant value (ml)
vinegar (ml)
Initial Final
1. 10 0.00 13 13
2. 10 0.00 15 15 14
3. 10 0.00 14 14

Volume of Standardized NaOH, V2 = 14 ml

Strength of Standardized NaOH, N2 = 0.1 N
Volume of diluted Vinegar, V3 = 10 ml
So, Strength of diluted Vinegar, N3 = V2N2/V3
14 x 0.1
= = 0.14 N
10

Equivalent weight of Acetic acid = 60

60 x 0.14 x 10
Since, W g of acetic acid present in 10 ml diluted vinegar = = 0.084 g
1000

So, Acetic acid present in 100 ml diluted vinegar = 10 W g = 10 x 0.084 = 0.840 g

10 W x 100
Percentage of acetic acid in commercial vinegar = = 8.40 %
10

Results: 8.40 % of acetic acid in given commercial vinegar sample.

 EXPERIMENT No. 3

Object: Estimate the amount of oxalic acid present in the whole of the given solution, being supplied with
Ferrous Sulphate crystals and approximately N/20 KMnO4 solution.
Chemicals: N/20 N Potassium permanganate given oxalic acid solution, dilute (5N) H2SO4.
Apparatus: Volumetric flask (250 ml), conical flask, beaker, burette, pipette, funnel, etc.
Indicator: Potassium permanganate (self indicator)
Theory: Estimation is based on the reaction between KMnO4 and Oxalic acid. KMnO4 oxidizes oxalic acid
in the presence of acid and while hot.
2 KMnO4 + 3 H2SO4 → K2SO4 + 2MnSO4 + 3H2O + 5 [O]
FeSO4.7H2O + H2SO4 [O] → Fe2(SO4)3 + 8H2O
H2C2O4.2H2O + [O] → 2CO2 + 3H2O
Equivalent weight of oxalic acid = 63
Equivalent weight of Ferrous Sulphate = 278
The above reaction proceeds slowly at room temperature but at 60 – 70 °C quantitative oxidation
takes place. As soon as the oxidation of oxalic acid is complete, addition of a drop of KMnO 4 produces a
permanent pink colour in the solution, indicating the end point. In this titration no need of indicator as
KMnO4 itself acts as an indicator.
Procedure:
Titration I: Standardization of KMnO4 (Std. FeSO4 Vs KMnO4)
(i) Approximately 3.5 g of Ferrous Sulphate is weighed and transferred into a 250 ml standard flask. It is
then dissolved in distilled water to which 10 ml of dil.H2SO4 has been added and made up to the mark.
(ii) 20 ml of the standard Ferrous Sulphate solution is pipette out into a clean conical flask and 20 ml of dil.
H2SO4 is added.
(iii) This solution is titrated against the KMnO4 solution taken in the burette. The end point is the appearance
of the permanent pink colour. The titration is repeated for concordant values.

S.No. Volume of Ferrous Burette Reading (ml) Volume of KMnO4 Concordant value
Sulphate (ml) solution (ml) (ml)
Initial Final
1. 20 0.00 20 20
2. 20 0.00 19 19 20
3. 20 0.00 21 21

Volume of Std. Ferrous Sulphate solution, V1 = 20 ml

Strength of Std. Ferrous Sulphate solution, N1 = 0.05 N
Volume of KMnO4 solution, V2 = 20 ml
So, Strength KMnO4 solution, N2 = V1N1/V2
20 x 0.05
= = 0.05 N
20
Titration II: Estimation of Oxalic acid (Given Oxalic acid Vs KMnO4)
(i) Approximately 3.5 g of Ferrous Sulphate is weighed and transferred into a 250 ml standard flask. It is
then dissolved in distilled water to which 10 ml of dil.H2SO4 has been added and made up to the mark.
(ii) 20 ml of the standard Ferrous Sulphate solution is pipette out into a clean conical flask and 20 ml of dil.
H2SO4 is added.
(iii) This solution is titrated against the KMnO4 solution taken in the burette. The end point is the appearance
of the permanent pink colour. The titration is repeated for concordant values.

S.No. Volume of Oxalic Burette Reading (ml) Volume of KMnO4 Concordant value
acid (ml) solution (ml) (ml)
Initial Final
1. 20 0.00 10 20
2. 20 0.00 11 19 10.5
3. 20 0.00 10.5 21

Volume of Standardized. KMnO4 solution, V1 = 10.5 ml

Strength of Standardized. KMnO4 solution, N1 = 0.05 N
Volume of Oxalic acid solution, V2 = 20 ml
So, Strength Oxalic acid solution, N2 = V1N1/V2
10.5 x 0.05
= = 0.026 N
20

The amount of Oxalic acid present in 20 ml solution = Strength of Oxalic acid x Eq. wt. of Oxalic acid
= 0.026 x 63
=

Results: The amount of Oxalic acid present in the whole of the given solution = 0.060 g