Practical 15 2023

PRACTICAL 15 : MEASURING DISSOLVED OXYGEN – THE
WINKLER METHOD
NAME :
CLASS :
DATE :
INTRODUCTION
The Winkler test is used to determine the concentration of dissolved oxygen in water
samples. Dissolved oxygen (D.O.) is widely used in water quality studies and routine
operation of water reclamation facilities. An excess of manganese(II) salt, iodide (I–) and
hydroxide (OH–) ions is added to a water sample causing a white precipitate of Mn(OH)2
to form.
__ MnSO4 + ___KOH ____Mn(OH)2 + ____K2SO4
This precipitate is then oxidized by the dissolved oxygen in the water sample into a
brown manganese(IV) precipitate, MnO(OH)2 .
____ Mn(OH)2 + ____O2 ____ MnO(OH)2
In the next step, a strong acid is added to acidify the solution. The Mn(SO4)2 formed by
the acid converts the iodide ions into iodine, itself being reduced back to manganese(II)
ions in an acidic medium.
___Mn(SO4)2 + ___ I–(aq) → ___Mn2+(aq) + ___I2(aq) + ___ SO42–(aq)
Thiosulfate is used, with a starch indicator, to titrate the iodine.
___ S2O32–(aq) + ___I2 → ___S4O62–(aq) + ___ I–(aq)
The amount of dissolved oxygen is directly proportional to the titration of iodine with a
thiosulfate solution.
From the above stoichiometric equations, we can find that:
___ mole of O2 → ___ moles of MnO(OH)2 → ___ mole of I2 → ___ mole of S2O32–
Therefore, after determining the number of moles of iodine produced, we can work out
the number of moles of oxygen molecules present in the original water sample. The
oxygen content is usually presented as mg/dm3.
1
Materials/chemicals required Apparatus required
● 3M Manganese(II) sulfate solution *2cm3 graduated pipet
● Alkali-iodide-azide solution *Conical flask (250 cm3)
● Concentrated sulphuric acid *Filter funnel + filter paper
● Starch solution *Reagent Bottle (300 cm3) + stopper
● 0.010M Sodium thiosulfate *25 cm3 Pipette + filler
solution *Burette + stand
PROCEDURES
Caution! Gloves have to be worn when handling alkali-iodide-azide and
concentrated sulphuric acid.
1. Carefully fill a 300- cm3 glass reagent stoppered bottle brim-full with sample
water.
2. Immediately add 2 cm3 of manganese(II) sulfate to the collection bottle by
inserting the calibrated pipette just below the surface of the liquid. (If the reagent
is added above the sample surface, you will introduce oxygen into the sample.)
Squeeze the pipette slowly so no bubbles are introduced via the pipette.
3. Add 2 cm3 of alkali-iodide-azide reagent in the same manner.
4. Stopper the bottle with care to be sure no air is introduced. Mix the sample by
inverting several times. Check for air bubbles; discard the sample and start over
if any are seen. If oxygen is present, a brownish-orange cloud of precipitate or
floc will appear. When this floc has settle to the bottom, mix the sample by
turning it upside down several times and let it settle again.
5. Add 2 cm3 of concentrated sulfuric acid via a pipette held just above the surface
of the sample. Carefully stopper and invert several times to dissolve the floc. (At
this point, the sample is "fixed" and can be stored for up to 8 hours if kept in a
cool, dark place.)
6. In a glass flask, titrate 25 cm3 of the sample with sodium thiosulfate to a pale
straw color. Titrate by slowly dropping titrant solution from a burette into the flask
and continually stirring or swirling the sample water.
7. Add 2 cm3 of starch solution so a blue color forms.
8. Continue slowly titrating until the sample turns clear. As this experiment reaches
the endpoint, it will take only one drop of the titrant to eliminate the blue color. Be
especially careful that each drop is fully mixed into the sample before adding the
next. It is sometimes helpful to hold the flask up to a white sheet of paper to
check for absence of the blue color.
9. Repeat the titration process for at least two times.
OBSERVATIONS AND RESULT:
2
Table 1:
Experiment Trial 1 2 3
Final volume / cm3 ( ± cm3)
Initial volume/ cm3 ( ± cm3)
Volume used/ cm3 ( ± cm3)
Questions:
1. Calculate the average volume of sodium thiosulphate used in the titration.
2. Calculate the number of moles of sodium thiosulphate used in the reaction.
3. What is the number of moles of iodine in the conical flask?
4. Determine the content of dissolved oxygen in the water sample in mg/dm3 ?
3
5. One of the factors that affect the amount of oxygen dissolved in water is salinity. What
are the other possible factors?
6. Why is starch solution not added prior to titration?

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PRACTICAL 15 : MEASURING DISSOLVED OXYGEN – THE

MnSO4 + _KOH Mn(OH)2 + K2SO4

Mn(OH)2 + O2 MnO(OH)2

_Mn(SO4)2 + _ I–(aq) → _Mn2+(aq) + _I2(aq) + ___ SO42–(aq)

Thiosulfate is used, with a starch indicator, to titrate the iodine.

_ S2O32–(aq) + _I2 → _S4O62–(aq) + _ I–(aq)

From the above stoichiometric equations, we can find that:

OBSERVATIONS AND RESULT:

1. Calculate the average volume of sodium thiosulphate used in the titration.

2. Calculate the number of moles of sodium thiosulphate used in the reaction.

3. What is the number of moles of iodine in the conical flask?

4. Determine the content of dissolved oxygen in the water sample in mg/dm3 ?

6. Why is starch solution not added prior to titration?

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