QUANTITATIVE

DETERMINATION
OF
DISSOLVED OXYGEN CONTENT BY WINKLER
REDOX TITRATION
P. OGI1
1

INSTITUTE OF KAGWAPUHAN, COLLEGE OF GOOD-LOOKING ONES

UNIVERSITY OF THE PHILIPPINES, DILIMAN, QUEZON CITY 1101, PHILIPPINES
DATE SUBMITTED:
DATE PERFORMED:

RDR
1.

Give the pertinent chemical equations and stoichiometry in the

Na 2 S2 O3 .

I O3 =6 mol S 2 O3

standardization of
1 mol

+ 3 H 2 O
+ 3 I 3
+ 6 H
+8 I
I O3
+ I 2
I
I 3
2
+S4 O6
2 2 I
I 2 +2 S 2 O3
2. Explain the purpose of the addition of

H 2 SO 4

and excess

KI

during

standardization and why the it was added to the solution in that

specific order.

H 2 SO 4

was added in particular order to have an acidic environment in the

reaction. This would lead the reaction of iodate to take place. Addition of
used to form

I3

as shown in the reaction below. [2]

KI

was

+ 3 H 2 O
+ 3 I 3
+ 6 H
+8 I
I O3

3. Give the pertinent chemical equations and stoichiometry in the sample

analysis.
1 mol

O2 = 4 mol

S 2 O3

Mn(OH )2

2++2 OH
Mn
Mn(OH )2 +O 2 + H 2 O Mn(OH )3
4. Explain stepwise how

I3

was produced from the dissolved

O2

in

water sample. Explain briefly why the reagents are added in a definite
sequence.
5. Give the reason why starch was used as an indicator in this analysis
and why it was added towards the end of the titration.
Starch was used as an indicator because of hydrolysis that starch can undergo to
amylose and amylopectin according to the following reaction. [3]

Starch Amylose + Amylopectin

It was added towards the end of titration in order to prevent the stabilization of the

I 2 starch

complex. When

I2

is introduced to starch,

I2

will be encaged

within the helical structure of starch which makes it difficult to achieve the
endpoint. [2]
6. How is the analysis (iodometric process) different from an iodimetric
one?
The difference of iodomeric method and iodimetric method is the used titrant and
analyte. In iodometric redox method, sodium thiosulfate is the titrant and iodine is
the analyte. For iodimetric redox method, iodine is the titrant and sodium
thiosulfate is the analyte which is the reverse of iodometric method. [2]

7. From the calculated ppm

O2

in water sample, identify the degree of

water pollution and ability of water sample source to sustain aquatic

life.
The calculated values of

ppmO 2 in three different trials were 2.98, 2.84, and

2.98. The average value was 2.93

ppm O2 . The table below shows the relationship

between DO content and water quality which the water quality can be identified
from the experimental values.
Table 1. Relationship of DO Content in

DO Content ( ppmO2 ) , 20
8-9
7-11

ppm O2 and water quality

Water quality

Clean, good water

Ideal for stream fishes including cold water
fishes
Slightly polluted
Moderately polluted, can sustain life on
warm fishes
Highly polluted
Cannot sustain life

6.7-7.9
4.5-6.6
Below 4.5
0-2

Therefore, the water quality from the experimental values is highly polluted.
8. Predict the effect, if any, of each of the following on the DO oxygen
content obtained:
a. The water sample is made to stand overnight before analysis.
The water sample may contain organisms that could perform cellular respiration
and photosynthesis which the effect on oxygen is indeterminate.
b.

MnSO4

is added and the solution made to stand for an hour before

the alkaline

KI

solution is added.

Manganese is light sensitive which will undergo reduction. This would have a
decrease on the volume of titrant which the calculated dissolved oxygen to
decrease as well. [2]
9. What are the possible sources of errors and their effect on the
calculated parameters?
One possible source of error is personal error during solution preparation and in
preparation of sample. Solution preparation is crucial for the experiment that it
affects the entire experiment because it affects the concentration which affects the
volume of the titrant. If the sample preparation was not prepared under standard
operating procedures, the dissolved oxygen content may be affected and cause
discrepancy for the experiment. Method error is another possible for this experiment
since some reaction may be incomplete that would affect the dissolved oxygen

content. Indeterminate error may also arise in this experiment which could affect
experimental values.[1]
Additional Questions:
1. Account for the addition of sodium carbonate in titrant preparation.
Because sodium thiosulfate decomposes in acidic environment as shown in
the reaction below, addition of sodium carbonate stabilizes sodium thiosulfate. [2]

+ S(s )+ H 2 O(l )

+ SO 2(g )

+2 H (aq)
S2 O3(aq)

2. Why the titrant was prepared on the Day 2 of the experiment, unlike
others?
The titrant was prepared on the Day 2 to ensure that the water used in the
experiment was freshly boiled. If the titrant was prepared on day 1,

CO2

may

dissolve which makes the solution acidic and promotes disproportionation of

S 2 O3

[2]
3.

Give the side reactions that may happen if the reagent addition was
not sequential.

Formation of

HIO 3 in addition of sulfuric acid before potassium:

+ HIO 3
+ H
IO3

Addition of sulfuric acid before potassium iodide may cause the molarity of
thiosulfate to increase while its volume decreases. This would also lead to an
increase in the calculated oxygen content because

HIO 3 is a weak acid which

means the dissociation of ions is incomplete. Furthermore, some parts

IO3

will be

titrated. [2]
4.

Account for the delay of the reaction in standardization, especially if

the red solution was not titrated immediately.
Because the decomposition of

I3

is slow which delays the reaction. If the

red solution was not titrated immediately, the

I2

encaged within the helical

structure of starch will make it difficult to achieve the endpoint. [2]

REFERENCES

[1] Skoog, West, Holler, Crouch. Fundamentals of Analytical Chemistry. 9th ed.
Belmont: Brooks/Cole, 2014. 87-89, 391. Print.
[2] Harris, Daniel. Qualitative Chemical Analysis. 8th ed. New York: W. H. Freeman,
2010. 130, 347-356. Print.
[3] Campbell, Mary, Farrell, Shawn. Biochemistry. 7th ed. Belmont: Brooks/Cole,
2012. 469-470. Print.