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14 views

Experiment

Uploaded by

almaahmad408
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
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Oxidation-Reduction titration : Bleach analysis

# Objective :
Determination of the percentage of a valuable Cl2 in a number of
commercial bleaching agent.

The determination of free chlorine in bleach is possible by a redox titration.


The most common and successful method involves taking the sample of
bleach converting the hypochlorite ion (ClO-) to iodine (I2) by the addition of
KI and then titrating the iodine with standardized sodium thiosulfate solution.

The ability of household bleach to remove stains is


related to the amount of oxidizing agent in it. The
oxidizing agent in “bleach” is sodium hypochlorite,
NaOCl , which dissociates in water as follows

NaOCl(aq) Na+(aq) + OCl-(aq)

Many commercial bleaches are simply solutions of


hypochlorite salts such as sodium hypochlorite
(NaOCl) or calcium hypochlorite (Ca(OCl)2) .
Hypochlorite ion reacts with excess iodide ion in the
presence of acid to generate an iodine solution:

OCl-(aq) + 2H+(aq) + 2I-(aq) I2(aq) + Cl-(aq) + H2O


The product is I2(aq) yellow when diluted and red-brown when
concentrated .

The liberated iodine solution can be titrated against sodium


thiosulfate solution using a freshly prepared starch solution as
indicator. The titration reaction may be represented by the
equation:
2S2O3-2(aq) + I2(aq) S4O6-2(aq) + 2I-(aq)

The amount of hypochlorite ion present in a solution of bleach


can be determined by an oxidation-reduction titration.
One of the best methods is the iodine-thiosulfate titration
procedure.
The iodide ion , (I-) , is easily oxidized by almost any oxidizing
agent.
In acid solution, hypochlorite ions oxidize iodide ions to form
iodine , (I2) .
The iodine that forms is then titrated with a standard solution
of sodium thiosulfate.
The analysis takes place in a series of steps :

a) Acidified iodide ion is added to hypochlorite ion solution


and the iodide is oxidized to iodine .

2H+(aq) + ClO-(aq) + 2I-(aq) Cl-(aq) + I2(aq) + H2O


b) Iodine is only slightly soluble in water, but it dissolves
very well in an aqueous solution of iodide ion, in which it
forms a complex ion called the triiodide ion.
Triiodide is a combination of a neutral (I2) molecule with
an (I-) ion.
The triiodide ion is yellow in dilute solution and dark red-
brown when concentrated.

I2(aq) + 2I-(aq) I3-(aq)

c) The triiodide is titrated with a standard solution of


thiosulfate ions, which reduces the iodine back to iodide
ions.

I3-(aq) + 2S2O3-2(aq) 3I-(aq) + S4O6-2(aq)

Materials :
1. Na2SO3 (0.1M) , (500ml) .
2. H₂SO4 solution .
3. Bleach solution .
4. Potassium iodide KI .
5. Starch solution .
6. Pipette .
7. Burette .
8. Conical flask .
9. Volumetric flask .
10. Beaker .
Procedure :
 Dilute the concentrated bleach Use a (5 ml) volumetric pipet
to measure (5 ml) of a commercial bleach solution into a
(100 ml) volumetric flask.
 Dilute to the mark with distilled water, stopper and mix well .
 Weigh out approximately (2 g) solid (KI) . This a large
excess over that which is needed.
 Oxidize the iodide ion with hypochlorite ion.
 Pipet (25 ml) of the dilute bleach into an Erlenmeyer flask .
 Add the solid (KI) and about (25 ml) distilled water.
 Swirl to dissolve the (KI) .
 Work in a fume hood and slowly, with swirling, add
approximately (2 ml) of (3 M) HCl .
 The solution should be dark yellow to red-brown from the
presence of the (I3-) complex ions.
 Titrate the iodine . Titrate with a standard (0.100 M) sodium
thiosulfate solution until the iodine color becomes light
yellow .
 Add one dropper of starch solution . The blue color of the
starch-iodine complex should appear.
 Continue to titrate until one drop of (Na2S2O3) solution
causes the blue color to disappear.
 Repeat the titration beginning with step 2 two more times .
A relation ship between sodium thiosulfate (Na2S2O3) and
Iodine (I2) from the ionic equation :

2S2O3-2(aq) + I2(aq) S4O6-2(aq) + 2I-(aq)

# of mole I2 = 0.5 (# of mole S2O3)


# of mole I2 = 0.5 (C * VT) S2O3

A relation ship between chloride (Cl2) and Iodine (I2) from the
ionic equation :

2H+(aq) + ClO-(aq) + 2I-(aq) Cl-(aq) + I2(aq) + H2O

# of mole Cl2 = # of mole I2


mass Cl2 = 0.5 (C * VT) S2O3 * M.wt (Cl2)

To find the mass of sample :

Mass of sample = Density bleach * 0.1 (Thinning agent) * V sample


Data :
Total
Volume of Initial Final Volume
Trial No Sample(ml) burette burette of Average
reading reading Titrant
used
1 25 0 16 16
15
2 25 22 36 14

Calculation :

%Cl2 = mass of Cl2 / mass of sample *100%

mass Cl2 = 0.5 (C * VT) S2O3 * M.wt (Cl2)

mass Cl2 = 0.5 (0.1 M * 0.015 L * 71 g/mol)


mass Cl2 = 0.05325 g

mass of sample = Density bleach * 0.1 (Thinning agent) * V sample

mass of sample = 1.084 g/ml * 0.1 * 25 ml


mass of sample = 2.71 g
%Cl2 = mass of Cl2 / mass of sample *100%

%Cl2 = 0.05325 g / 2.71 g * 100%


%Cl2 = 1.96 % (Experimental)

%Cl2 = M.wt (Cl2) / M.wt (NaOCl) * 5.25

%Cl2 = 71 / 74 * 5.25
%Cl2 = 5% (Theoretical)

Error = [ Exp – theo ] / theo * 100%

Error = [1.96 % - 5%] / 5% * 100%


Error = 60.8 %

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