Experiment No - 06
Aim :To determine the strength of free chlorine in given water sample.
Given standard N/40 copper sulphate (CuSO4) solution to standardize
sodium thiosulfate solution
Apparatus Required :
Burette, Pipette, Measuring flask, glass rod
Chemicals Required:
Potassium iodide solution (10%), N/40 Hypo solution (Na2S2O3), starch
solution (freshly prepared).
APPARATUS NEEDED FOR TITRATION
Theory:
Chlorine is widely used for disinfection of potable and municipal water
supplied to remove bacteria, fungus and other pathogenic micro – organisms,
and for deodorization, since it is a powerful oxidizing agent and is cheaply
available. Chlorination is done with the help of bleaching powder or chlorine
gas or chlorine dissolved in water in the form of concentrated solution or with
chloramines. The sterilizing action of chlorine is supposed to be due to its
reaction with water producing hypochlorous acid and nascent oxygen both of
which have powerful germicidal properties.
CaCOCl2 + H2O Ca(OH)2 + Cl2
Cl2 + H2O HOCl + HCl
HOCl HCl + (O)
(Hypochlorous acid) (nascent oxygen)
HOCl + germs germs are killed
However, excess of free chlorine in drinking water is undesirable, as it is not only
unpleasant for drinking, but is also injurious for human metabolism. Hence, the amount of
free chlorine in municipal water is estimated prior to the domestic supply so as to make
necessary adjustment in dose range accordingly. The principle involved in the estimation of
free chlorine in water is that when a measured quantity is treated with excess of potassium
iodide, the free chlorine present in the water oxidizes the corresponding amount of
potassium iodide to iodine. The liberated iodine is estimated by titrating against standard
hypo solution, using starch as indicator.
Cl2 + 2KI > 2KCl + I2
I2 + Na2S2O3 > Na2S4O6 + 2NaI
Sodium thiosulphate > Sodium tetrathionate
I2+ Starch indicator > Blue colour
Procedure:
Part I: Standardization of hypo solution with given copper sulphate solution
Take 10 ml of given copper sulphate solution (CuSO4) from pipette in conical flask.
Add 1 ml of potassium iodide (KI) solution and titrate with the hypo solution till faint
yellow colour develops. At this point, add 1-2 drop of starch as indicator. The solution
will turn blue in colour. Titrate further with hypo to colourless as end point. Note the
concordant volume of hypo solution as V mL.
Part II : Titration of given water sample with hypo solution:
Take 10 ml of given water sample from pipette in a conical flask. Add 1 ml
of potassium iodide (KI) solution and titrate with the hypo solution till faint
yellow colour develops. At this point, add 1-2 drop of starch as indicator.
The solutionT will turn blue in colour. Titrate further with hypo to colourless
as end point. Note the concordant volume of hypo solution as V mL.
Observation:
Table 1: Titration of hypo solution versus given CuSO4 solution Indicator – Starch; End
point – Blue to colourless
S.No Vol. Of Burrette Volume of Concordant
CuSO4 readings hypo reading V(ml)
solution (ml) solution (ml)
Initial Final
Table 2: Titration of hypo solution versus given CuSO4 solution
Indicator – Starch; End point – Blue to colourless
S.No Volume of
water sample
Burette Volume of Concordant
readings (ml)
readings hypo used
(ml) (ml)
Initial Final
Calculations:
Part I: Titration of hypo solution versus given CuSO4 solution
Normality of CuSO4 solution (N1) = N/40
Volume of CuSO4 solution (V1) = 10 ml
Normality of hypo solution (N2) = ?
Volume of hypo solution (V2) = burette reading
N1 V1 = N2 V2 will give the normality of hypo solution (N2)
Part II: Titration of hypo solution versus given CuSO4 solution
Volume of water sample taken for each titration (V3) = 10 mL
Normality of water sample (equivalent to dissolved chlorine) (N3) = ?
Normality of hypo solution (N2) = ?
Volume of hypo solution (V2) = burette reading
N2 V2 = N3 V3 will give the normality of water sample (N3)
Total chlorine residuals = N3 × Equivalent wt of chlorine (35.5) g/l
Convert g/l into ppm.
Result: Amount of total residual chlorine in a given sample of water = .............
ppm
Precautions:
1. The solution being unstable should be titrated immediately after its
preparation.
2. The solution should be well shaken before each aliquot is withdrawn for
titration.
3. Chlorine vapours being harmful, the solution should not be sucked into
the pipette with the mouth.
