Short Procedures

Estimation of total, permanent and temporary hardness by EDTA method

Aim

To determine the amount of total, temporary and permanent hardness in the given sample of
water by EDTA method

Principle

The estimation is based on the complexometric titration. The basic principle is complexing agent
forms stable complex with the ions (Ca2+, mg2+) present in the sample hard water.
PH = 8 – 10
Ca2+ / Mg2+ + EBT [EBT-Ca2+ / Mg2+ ]
In water less stable complex
Wine red colour
PH = 8 – 10
[ EBT-Ca / Mg ] + EDTA
2+ 2+
[EDTA-Ca2+ / Mg2+ ] + EBT
Less stable complex colourless more steel blue colour
Wine red colour stable complex

Procedure

Titration1: Sample water Vs standard EDTA solution

S.No Content Observation

1 Pipette Solution
2 Burette Solution
3 Indicator
4 pH
5 Buffer
6 End Point
20 ml Sample Water
EDTA Solution
2 drops of Eriochrome black -T
9-11
2-3 ml Ammonium Buffer (NH4OH &
NH4Cl)
Wine red to steel blue colour

Titration II: Boiled sample water Vs EDTA solution

S.No Content Observation

1 Pipette Solution
2 Burette Solution
3 Indicator
4 pH
5 Buffer
6 End Point
20 ml Sample Water
EDTA Solution
2 drops of Eriochrome black -T
9-11
2-3 ml Ammonium Buffer (NH4OH &
NH4Cl)
Wine red to steel blue colour

Molecular weight of disodium salt of EDTA = 372

 Estimation of copper in brass by EDTA method

Aim

To estimate the amount copper present in the given brass solution.A standard solution of zinc
sulphate of strength 0.1N and approximately N/10 solution of EDTA is given.

Principle

Fast Sulphon Black-F is the sodium salt of 1-hydroxy-8-(2-hydroxy-naphthylazo)-2-

(sulphonaphthylazo)-3,6-disulphonic acid. The colour reaction seems virtually specific for copper
ions. In ammonical solution it forms complexes with copper and nickel. In the direct titration of
copper in ammonical solution, the colour change at the end point is from pale blue to bright green

Procedure

Titration1: Zinc sulphate Vs standard EDTA solution.

S.No Content Observation

1 Pipette Solution
2 Burette Solution
3 Indicator
4 pH
5 Buffer
6 End Point
Standard zinc sulphate solution
EDTA Solution
2 drops of Erichrome black -T
9-11
2-3 ml Ammonium Buffer (NH4OH &
NH4Cl)
Wine red to steel blue colour

Titration II : Brass solution Vs EDTA solution

S.No Content Observation

1 Pipette Solution Brass solution
2 Burette Solution EDTA Solution
3 Indicator 2 drops of Fast Sulphon Black-F
4 pH 9-11
2-3 ml Ammonium Buffer (NH4OH &
5 Buffer
NH4Cl)
6 End Point Light blue to dark green

Molecular weight of disodium salt of EDTA = 372

2
 Determination of dissolved oxygen of water by Winkler’s method

Aim

To estimate the amount of dissolved oxygen in the given sample.

Principle

Oxygen dissolves in water to the extent of 7-9 mgs/lit at a temperature range of 25-35 C. The
estimation of dissolved oxygen in water is useful in studying corrosion effects of boiler feed water
and in studying water pollution. The amount of dissolved oxygen in water is estimated using
Winkler’s reagent (potassium bromide + potassium bromate). Water sample is collected carefully
avoiding aeration / deeration in ground stopper flask. Initially Manganous sulphate and alkali-
iodide reagents are added and the reactions occur as follows

2Mn2+ + 2OH- MnO (OH)  (White)

MnO(OH)2 + ½ O2 MnO(OH)2  (yellow brown)

The precipitate dissolves in concentrated sulphuric acid liberating iodine and the liberated iodine
is titrated against Na2S2O3.


MnO(OH)2 + 2 H2SO4 Mn(SO4)2 + 3H2O

Mn(SO4)2 + 2KI MnSO4 + K2SO4 + I2

2Na2S2O3 + I3 Na2S4O6 + 2 NaI

Procedure

Titration1: K2Cr2O7 Vs Na2S2O3

S.No Content Observation

1 Pipette Solution
2 Burette Solution
3 Indicator
4 End Point
20ml potassium Dichromate + 5ml of H2SO4
+ 50ml of 5% KI
Sodium thiosulphate Solution
Starch
Blue colour to Light Green Colour

Titration II : Water sample Vs Standard sodium Thiosulphate

S.No Content Observation

1 Pipette Solution
2 Burette Solution
3 Indicator
6 End Point
100ml sample water + 2ml MnSo4 +2ml of
Conc. H2SO4
Sodium thiosulphate Solution
Starch
Disappearance of Blue colour

Equivalent weight of oxygen =8

Equivalent weight of potassium dichromate = 49
Equivalent weight of Sodium thiosulphate Solution = 248
3
 Estimation of chloride in water by Argentometric method

Aim

To estimate the amount of chloride in a given sample with standard sodium chloride solution of
strength 0.1N.

Principle

The estimation is based on precipitation reaction. The reacting constituents from precipitate is the
basic principle

AgNO 3 + NaCl AgCl ↓ + NaNO 3

ppt.

Procedure

Titration I : Standard sodium chloride Vs Silver nitrate solution

S.No Content Observation

1 Pipette Solution 20 ml Standard NaCl solution
2 Burette Solution Silver nitrate solution
3 Indicator Potassium chromate
4 End Point Reddish brown tinge ppt.

Titration –II : Water sample Vs AgNO3 solution

S.No Content Observation

1 Pipette Solution 20 ml water sample
2 Burette Solution Silver nitrate solution
3 Indicator Potassium chromate
4 End Point Reddish brown tinge ppt.

Equivalent weight of Cl– = 35.5

4
 Estimation of alkalinity in water by indicator method

Aim

To determine the different types of alkalinity and to estimate their amount present in the given
sample of water

Principles

Alkalinity of water is capacity to neutralize the acid alkalinity can be determined by the
neutralization of sample water by H2SO4 by using phenolphthalein and methyl orange indicator

OH- + H+ H 2O
CO3 2-
+ H+ HCO3 -
HCO3 + H+
-
H2CO3

Procedure

Titration I : Sample water Vs H2SO4 solution

S.No Content Observation

1 Pipette Solution 100 ml Sample Water
2 Burette Solution H2SO4 Solution (0.02N)
3 Indicator Phenolphthalein
4 End Point Disappearance of pink colour

Titration II : The above conical flask content Vs H 2So4 solution

S.No Content Observation

5 Indicator Methyl orange
6 End Point Appearance of pale pink colour

Equivalent weight of H2SO4 = 49

5
 Determination of molecular weight of polymer by viscometer method
Aim

To determine the molecular weight of the given polymer of Ostwald”s Viscometer method.

Procedure
Preparation of polymer solution

S.No Content Observation

0.5% of polymer solution in benzene (or)
1 Standard solution Toulene
0.1%, 0.2%, 0.3% and 0.4% of polymer
2 Make up Solution
Solution

S.No Content Observation

Measuring jar
1 15 (or) 17ml of solvent containing polymer
Solution
Rubber bulb , measuring jar and Oswald’s
2 Apparatus Viscometer
Flow times for polymer solutions of different
3 Determination
concentrations.

Apparatus

Model Graph
The following graph is obtained by plotting reduced viscosity need against concentration of
polymer solution.

red

[]
X

C
6
 Conductometric titration of strong acid with strong base
Conductometric Titration of Strong acid Vs Strong base (HCl Vs NaOH)

Aim

To determine the amount of hydrochloric acid present in the whole of the given solution by
conductometric titration using sodium hydroxide of 0.1N.

Principle

The change in conductance takes place at the basic principle of conductometric titration.

HCl + NaOH NaCl + H2O

Procedure

Hydrochloric acid Vs Sodium hydroxide

S.No Content Observation

1 Pipette Solution 40 ml of made up HCl solution

2 Burette Solution NaOH solution (0.5ml by each addition)

3 Instrument Conductivity meter

4 Equivalent point Sudden increase of conductance

5 Equivalent weight of NaOH 40

Model Graph

The following graph is obtained by plotting conductance against volume of NaOH.

Y
A C

HCl
NaOH

Conductance
End point
B

Vol of NaOH

7
 Estimation of mixture of acids by conductometry

Aim

To determine the amount of hydrochloric acid and acetic acid present in the mixture of the given
solution by conductometric titration using sodium hydroxide of 0.1N.

Principle

The change in conductance takes place at the basic principle of conductometric titration.

HCl + NaOH NaCl + H2O

Procedure

Hydrochloric acid Vs Sodium hydroxide

S.No Content Observation

1 Pipette Solution 40 ml of made up hydrochloric and acetic acid solution
2 Burette Solution NaOH solution (0.5ml by each addition)
3 Instrument Conductivity meter
4 Equivalent weight of Hcl 36.5
Equivalent weight of
5 60.05
Acetic acid

Model Graph

The following graph is obtained by plotting conductance against volume of NaOH.

y
A D

Conductance
C
B

Vol of NaOH

8
 Estimation of ferrous iron by potentiometer titration

Aim

To determine the amount of ferrous iron present in the given solution using potassium dichromate
by using potentiometer.

Principle

The change in emf takes place at the end point is the basic principle of potentiometer titration.

6 Fe2+ + Cr2O72-+ 14 H+ 6 Fe3+ + 2Cr3+ + 7H2O

Procedure

S.No Content Observation

1 Pipette Solution 40 ml of Fe2+ ions + 10ml of dilute H2SO4
2 Burette Solution K2Cr2O7 (0.5ml by each addition)
3 Instrument Potentiometer
4 Electrode Platinum electrode, standard calomel electrode
5 Equivalent weight of ferrous 55.84
iron

Model Graph -I

A graph is obtained by plotting emf against volume of K 2Cr2O7.

Y

emf

End point
X

Vol of K 2Cr2O7
Model Graph -II
A graph is obtained by plotting DE/DV against volume of K2Cr2O7.

E

V

End point
X

Vol of K2Cr2O7

9
 Estimation of hydrochloric acid by pH- metry

Aim

To estimate the amount of hydrochloric acid present in the whole of the given solution using
standard sodium hydroxide.

Principle

The pH of the solution varies with concentration of H + ion

pH = -log [H+]

S.No Content Observation

1 Pipette Solution
2 Burette Solution
3 Instrument
4 Electrode
5 Equivalent weight of HCl
40 ml of made up HCl solution
NaOH solution (0.5ml by each addition)
pH meter
Combined electrode (pH electrode and standard
calomel electrode)
36.5

Model Graph 1

pH

End point
X

Vol of NaOH

Model Graph 2

The graph is obtained by plotting pH /V against volume of NaOH added.
Y

pH

V

X
Vol of NaOH

10
 Determination of the iron content by spectrophotometry

Aim

To estimate the amount of iron present in the given sample using spectrophotometer.

Principle

It involves the measurement of intensity of light absorbed by a sample. According to Beer-

Lambert’s law. Absorbance is given by

log (I/Io) =  c l = A

Procedure

Preparation of standard Iron (III) solution

S.No Content Observation

1 Stock Solution 100ppm iron (III) solution
2 Standard solution 2,4,6,8 and 10 ppm iron (III) solution
3 Reagents (i) 5ml 5N Nitric acid
(ii) 5 ml 10% ammonium Thiocyanate
Making of sample iron (III) solution

S.No Content Observation

1 Sample Solution Unknown amount of iron (III) solution
To make up sample solution in 100ml
2 Made up sample solution
standard flask
(i) 5ml 5N Nitric acid
3 Reagents
(ii) 5 ml 10% ammonium Thiocyanate
Standardization of spectrophotometer

S.No Content Observation

1 Standardazing solution Distilled water
2 Wavelength 480nm
3 Absorbance (or) Transmitance Zero (or) 100%
Block Diagram

The Block Diagram of the spectrometer is as follows

11
Estimation of iron (III) solution

Measure the absorbance of all iron III solution at 480nm

Model Graph

A graph is obtained by plotting absorbance against strength of iron solution.

Absorbance of
unknown solution

Absorbance

Strength of iron

12
 Estimation of Chromium in Waste Water

Aim

To estimate the amount of chromium present in whole of the given waste water solution.

Principle

The ferrous ammonium sulphate solution is used for the standardization of link potassium
permanganate solution. The chromium content is determined by the addition of excess of
standard ferrous ammonium sulphate solution to the known volume of tannery waste and the
excess FAS (unreacted) is titrated against standard potassium permanganate. Here redox
reaction takes place. Ferrous ion gets oxidized [ Fe 2+  Fe3+] and chromium ion get reduced
[Cr(vi)  Cr(iii)] in acidic medium.

Cr2O72- + 6Fe2+ + 14H+ 2Cr3+ + 6Fe3+ +7H2O

Procedure

Titration I : Standard Ferrous Ammonium Sulphate Vs Potassium Permanganate

S.No Content Observation

1 Pipette Solution 20 ml Ferrous ammonium sulphate solution

2 Burette Solution Potassium permanganate solution

3 Reagents added to conical flask One test tube full of sulphuric acid

4 Indicator Self
5 End Point Appearance of pale pink colour

Titration II : Tannery waste solution Vs Standard KMnO4 solution

S.No Content Observation

1 Pipette Solution
2 Burette Solution
3 Reagents added to conical
flask
4 Indicator
5 End Point
20 ml of made up tannery waste solution
Standard Potassium permanganate solution
20ml of Ferrous ammonium sulphate solution and
One test tube full of sulphuric acid
Self
Appearance of pale pink colour

Equivalent weight of Cr3+ = 17.3

13