Experiment 5

OXIDATION REDUCTION
TITRATION IODOMETRY

IODOMETRY
- a method of volumetric analysis
- an application of iodine chemistry to
redox titrations
- iodines appearance or disappearance
determines endpoint
- effective method in determining
chlorine concentration in water

REDOX TITRATION
In a redox (reduction-oxidation)
titration, an oxidizing agent is used to
titrate a reducing agent or vice versa.
The reducing agent donates electrons
and becomes oxidized, while the
oxidizing agent gains electrons and is
reduced.

IODOMETRY
- An excess of iodide is used to
quantitatively reduce a chemical
specie while simultaneously forming
iodine, and the iodine is subsequently
titrated with thiosulfate.

- Iodine is used as an intermediate. It

is produced but is later consumed.

IODIMETRY
- Iodine is used as titrant for
oxidizable analyte.

PROCEDURE
A. Preparation of 0.1 M Na2S2O3 solution
Dissolve 12.4 g
of Sodium
thiosulfate in
100 ml Pre-

Dilute
to 500
ml

Add 0.2 g of
Sodium
Carbonate

boiled d H2O
Na2S2O3 is standardized as
it will serve as the titrant
for the experiment. It is
chosen because of its
unique quantitative
reaction with iodine.

Prevents oxidation of thiosulfate

into sulfite ions and sulfate into
elemental sulfur
S2O32- + H+ HSO3- + S(s)

Store in a
reagent
bottle

PROCEDURE
A. Standardization of 0.1 M Na2S2O3 solution
Place 0.10 + 0.05 g of
pure dry potassium
dichromate in three
500 ml erlenmeyer
flask

K2Cr2O7 will be
the primary
standard used. It
is chosen because
it liberates iodine
(I2) when added
with excess KI

Add 50 ml
carbon
dioxidefree water

Add 4 ml
of 1:2
Sulfuric
Acid

Add 5g of
KI
dissolved
in 5 ml
H2 O

Cover with
watch glass
and let is
stand for 3
minutes

H2SO4 is added so that pH will be less than 4. If more basic than

this, reaction might not proceed completely and instantaneously.

Cr2O7 + 6I- + 14H+ 2Cr3+ + 3I2 +

7H20
Brown solution
produced due to
brown color of I2

PROCEDURE
A. Standardization of 0.1 M Na2S2O3 solution
Dilute solution with
50 ml with carbon
dioxide-free water

Titrate with
thiosulfate solution
until brown color
of Iodine turns to
near colorless

Iodide was first produced through

titration so that the amount of iodine in
the solution will be decreased. If starch is
immediately added in the solution
containing a large amount of iodine, a
starch-iodine complex will form which
may not easily break up and a recurring
end point will be observed.

I2 + 2S2032- 2I- +
2S4 0
Oxidation
Half
6
Reaction22S
S4062- +
203
Reduction
2e-Half Reaction
I2 + 2e- 2I-

The solution becomes colorless as

iodide (I-) which is colorless is
produced.

PROCEDURE

A. Preparation of 0.1 M Na2S2O3 solution

Add 5 ml
Starch
Solution
The starch used was freshly
prepared because it reacts
photochemically.

Continue
titration until
the blue color
turns to
emerald green
(or aqua blue)

Upon addition of starch,

the remaining iodine in the
initially titrated solution
will react with it to form a
blue starch-iodine complex
creating a blue solution
from an almost colorless
solution.

PROCEDURE
B. Preparation of Starch Indicator
Dissolve 0.5
starch in 5 ml
carbon
dioxide-free
H2O

Add to 100 ml
boiling water

Let it boil for 2

minutes

RESULTS
TRIAL

Weight of
K2Cr2O7
(g)

Volume of
Molarity
Na2S2O3
of Na2S2O3
(mL)

0.0948 g

20.20 mL

0.09120 M

0.1072 g

22.00 mL

0.09938 M

0.0980 g

19.88 mL

0.1005 M

0.1035 g

21.35 mL

0.09887 M

0.1022 g

21.01 mL

0.09921 M

Average Molarity of Na2S2O3 :

0.09784 M
Standard Deviation: 3.764 x 10-3

SAMPLE COMPUTATION
FOR THE CONVERSION FACTOR:
1 mol K2Cr2O7 x
(3 mol I2)
mol S2O32(1 mol K-2Cr2O7) +

(2 mol S2O32-)

=6

mol3+
I2 )
Cr2O7 + 6I + 14H (12Cr
+ 3I2 +
I2 + 2S27H
032-20 2I- +
Therefore,
S4062-the conversion factor is
1 mol K2Cr2O7: 6 mol S2O32-

FOR TRIAL 1:
0.0948 g K2Cr2O7
S2O32-)

(1 mol K2Cr2O7 )

(249.2 g K2Cr2O7)
0.02120 L

(6 mol
= 0.09120
(1 mol K2Cr2O7)M S2O32-

CONCLUSIONS AND RECOMMENDATIONS

Different household bleaches vary in strengths. The
experiment used the method of iodometry in determining
the amount of sodium hypochlorite in household bleaches.
Iodometry is an application of iodine chemistry to redox
titration. In the process, an excess of iodide is used to
quantitatively
reduce
a
chemical
specie
while
simultaneously
forming
iodine,
and the
iodine
is
subsequently titrated with thiosulfate. This is different from
iodimetry wherein iodine is used as titrant for oxidizable
analyte. The accepted value for the weight per volume
percent concentration of sodium hypochlorite in household
bleaches ranges from 3%-6%. Errors could be due to
improper handling of reagents and careless use of
apparatuses such as the analytical balance.
It is recommended that the thiosulfate solution be
standardized against other oxidizing agent, such as KIO 3 or
KBrO3. With potassium dichromate, the green color of the