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Formal Report Experiment 8

This document describes the Winkler method for determining the dissolved oxygen content in water samples. Key steps include fixing the oxygen content by adding manganese sulfate and an alkaline iodide-azide solution. This allows manganese to oxidize from Mn2+ to Mn3+, oxidizing iodide to iodine. The generated iodine is then titrated with a standardized sodium thiosulfate solution. The endpoint is detected by a color change from starch-iodine complex formation. The methodology involves standardizing the thiosulfate solution, then collecting and treating a water sample to fix its oxygen content before titrating and calculating the dissolved oxygen concentration.

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yay
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533 views

Formal Report Experiment 8

This document describes the Winkler method for determining the dissolved oxygen content in water samples. Key steps include fixing the oxygen content by adding manganese sulfate and an alkaline iodide-azide solution. This allows manganese to oxidize from Mn2+ to Mn3+, oxidizing iodide to iodine. The generated iodine is then titrated with a standardized sodium thiosulfate solution. The endpoint is detected by a color change from starch-iodine complex formation. The methodology involves standardizing the thiosulfate solution, then collecting and treating a water sample to fix its oxygen content before titrating and calculating the dissolved oxygen concentration.

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yay
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© © All Rights Reserved
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You are on page 1/ 4

QUANTITATIVE DETERMINATION OF

DISSOLVED OXYGEN CONTENT BY WINKLER


REDOX TITRATION
W. YBAEZ
NATIONAL INSTITUTE OF MOLECULAR BIOLOGY AND BIOTECHNOLOGY, COLLEGE OF SCIENCE
UNIVERSITY OF THE PHILIPPINES, DILIMAN, QUEZON CITY 1101, PHILIPPINES
DATE SUBMITTED: 23 FEBRUARY 2016
DATE PERFORMED: 18 FEBRUARY 2016

ABSTRACT

INTRODUCTION
The dissolved oxygen (DO) content in
water is an important index in the
consideration
of
water
suitability.
Sufficient concentration of DO is critical
for the survival of most aquatic life, as
well as in waste water treatment. It is a
key parameter for characterizing natural
and wastewaters and for assessing the
state of the environment in general.[1]
The Winkler method is a premier and
classical method for the determination of
DO content in water sample. A sample of
water is collected in such a way that its
exposure to the atmosphere is minimized.
This is because exposure might alter the
level of dissolve O2. To fix the DO content
of the water sample, it is treated with a
solution of MnSO4, and then added with
and then with a solution of NaOH and KI
(hereafter referred to as alkaline iodide
azide).[2]
The basis of this method is the
quantitative oxidation of Mn2+ to Mn3+ by

dissolved O2 in the water sample. Then,


the trivalent Mn oxidizes I- to I2 in a
subsequent redox reaction; the amount of
I2 generated is determined by the titration
with a standard S2O32- solution. The
endpoint is determined by the color
change brought by the formation of a
starch-triiodide complex.[3]
The objectives of the experiment was to
perform the water sampling and
pretreatment techniques accurately, to
calculate the DO content of the water
sample, and to discuss the chemistry
behind the Winkler method for dissolved
oxygen determination.[4]
METHODOLOGY
Firstly, the solutions prepared for the
experiment were 25.0mL of 4.0M MnSO4,
25.0mL of alkaline iodide azide, 250.0mL
of 0.125M stock Na2S2O3, 50.0mL 0.5M
H2SO4, and freshly prepared starch
solution. Then, 250.0mL of 0.0125M

Page 1 of 3

standard Na2S2O3 solution was prepared


from the stock Na2S2O3 solution.
For
the
standardization
of
the
Na2S2O3solution, 0.1500g KIO3 powder
was weighed and subsequently dissolved
into a 50mL beaker. The contents were
transferred to 100-mL volumetric flask
and bulked to mark. Three 10.00mL
aliquots were transferred each into 250-mL
Erlenmeyer flasks, diluted with 20.0mL
distilled water and added with 1.0g KI
and 10.0mL of 0.5M H2SO4. The solution
was then titrated with standard Na 2CO3
until pale yellow colour is observed. Until
then, 1.0mL of the starch solution was
added to the analyte. Titration was
continued until the disappearance of the
blue colour. The procedure was repeated
for the other two flasks.
For the analysis of the water sample, a
glass bottle covered with aluminium foil
was filled to the brim with pond water. It
was added with 0.5mL MnSO4 solution
and 0.5mL alkaline iodide azide solution,
taking care to avoid inclusion of air
bubbles. The sample was then mixed and
the formation of a brown precipitate was
observed. The sample was added with
2.0mL concentrated H3PO4, again taking
care to avoid the inclusion of air bubbles.
The sample was mixed, and left to stand
for 10 minutes. 50mL aliquot of the
sample was transferred into a 250mL
Erlenmeyer flask and titrated with
standard Na2CO3 solution until pale
yellow colour was observed. 1.0mL of the
starch solution was added to the analyte
and titration was continued until the
disappearance of the blue colour. The
analysis was performed in triplicate.

RESULTS AND DISCUSSION


The Na2S2O3 solution is not stable and is
therefore standardized against a primary
standard, IO3- to become an effective
titrant. During the standardization, the
comproportionation
redox
reaction
between IO3 and I occurs as seen in (1).[5]

+ 3 H 2 O(1)
+ 3 I 3
+6 H
+8 I
IO 3
The reaction in (1) yields I3- which is then
titrated with S2O32-, as seen in (2).

2(2)
+ S 4 O 6
2 3 I
+ 2 S2 O3
I 3
Therefore, integrating reactions (1) and
(2), we get a stoichiometric ratio of 1 mol
IO3- is to 6 moles of S2O32- (see Appendix C
for the dimensional analysis).
Before the standardization of the
thiosulfate solution with IO 3-, excess KI
and H2SO4 was added to the solution
containing the primary standard, in that
specific order. KI was added for the
comproportionation reaction to occur.
H2SO4 is added to create an acidic
environment for the reaction, enabling it
to occur. It is important to add KI before
sulfuric acid since the H+ ions released
from H2SO4 will react with the IO 3- in the
solution to form iodic acid. HIO3 is a weak
acid, and its formation from its
constituents in solution is highly probable.

Page 2 of 3

2++ I 2+ 4 H 2 O

+ 2 Mn

+6 H
2 MnO (OH )+2 I

The formation of HIO3 will cause errors in


the calculated molarity of Na2SO3, and
subsequently, the DO, to increase.[3]
The analysis of the water sample occurred
after the standardization of the thiosulfate
solution. In the water sampling, while
taking water from the sample source, the
bottle was capped underwater to avoid the
inclusion of air bubbles. This is because
the inclusion of air bubbles would
increase the DO in the water sample from
which dissolved from the air. The bottle
was also covered with aluminum
beforehand


I 3

I 2+ I

2
+ S 4 O 6
2 3 I
+ 2 S2 O3
I 3
2

+ S 4 O6
+ starch 3 I
I 3

The importance of adding the sulfuric acid


before KI crystals is because the acid
separates the free iodine from the iodate.
Solubilizing the free iodine comes after
the addition of excess KI.[6]

2
+ S 4 O 6
2 3 I
+ 2 S2 O3
I 3
Mn(OH )2
2++2 OH
Mn
4 Mn (OH )2 +O2+ 2 H 2 O 4 Mn (OH )3
or

4 Mn (OH )2 +O 2 4 MnO (OH )+2 H 2 O


2+ + I 2+6 H 2 O
+ 2 Mn
+6 H
2 Mn (OH )3 +2 I

SUMMARY AND CONCLUSIONS

REFERENCES
[1]

Helm, I., Jalukse, L., and Leito, I. (2012).


Report on method for improved, gravimetric

Page 3 of 3

Winkler
titration.
Retrieve
from [4]
https://sisu.ut.ee/sites/default/files/me
asurement/files/g_winkler_report_28061
3.pdf, on March 23, 2016

Analytical Chemistry Group. (2013).


Analytical Chemistry Lab Manual.
Quezon City: University of the Philippines
Institute of Chemistry

[2]

Harvey, D. (2000). Modern Analytical [5]


Chemistry. (1st Edition). (pp. 345-346). The
McGraw-Hill Companies.

[3]

Bell, S. & Johnson, R. (1997). Determination


of Dissolved Oxygen by Winkler Titration.
Bermuda Biological Station For Reasearch,
Inc. pp. 29-30

University
of
Malaya.
(n.d.).
Department of Chemistry, Faculty of
Science.
Retrieved
from
http://www.kimia.um.edu.my/images/
kimia/lab%20manual/level
%202/Experiment%20SCES2441AnalisisLevel2.pdf, on April 10, 2016

Page 4 of 3

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