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Experiment 5

This experiment aims to determine the concentration of dissolved oxygen in a water sample using a standard sodium thiosulfate solution. Manganese hydroxide is used as an oxygen carrier to facilitate the reaction between dissolved oxygen and potassium iodide. Excess iodine is then titrated with sodium thiosulfate using starch indicator. The volume of sodium thiosulfate used is then used to calculate the parts per million of dissolved oxygen in the original water sample. Proper shaking and addition of reagents is required to ensure an accurate measurement.

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42 views12 pages

Experiment 5

This experiment aims to determine the concentration of dissolved oxygen in a water sample using a standard sodium thiosulfate solution. Manganese hydroxide is used as an oxygen carrier to facilitate the reaction between dissolved oxygen and potassium iodide. Excess iodine is then titrated with sodium thiosulfate using starch indicator. The volume of sodium thiosulfate used is then used to calculate the parts per million of dissolved oxygen in the original water sample. Proper shaking and addition of reagents is required to ensure an accurate measurement.

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Experiment No.

4
Objective: To determine the concentration of
dissolved oxygen from the given water sample
using standard N/40 Na2S2O3 solution
Reagent required: Potassium iodide solution (10%), N/40
Hypo solution (Na2S2O3), Starch solution (freshly
prepared).

Apparatus required: Burette, Pipette, Measuring flask,


Glass rod
Theory
• The experiment is based on the oxidation of Potassium
Iodide by dissolved oxygen. The liberated iodine is
titrated against a standard sodium thiosulphate solution
using starch as final indicator. Since, oxygen dissolved
in water remains present in molecular state; it is not
capable of reacting with potassium iodide. An oxygen
carrier such as manganese hydroxide is, therefore used
to bring about the reaction. Manganese hydroxide is
produced in situ by the action of potassium hydroxide
and manganous sulphate.
Structure of Starch
Starch is used as an indicator in iodometric titration.
Starch is a viable indicator in the titration process
because it turns deep dark blue when iodine is present
in a solution. When starch is heated in water, decom-
position occurs and beta-amylose is produced.
Beta-amylose with iodine, resulting in a dark blue
color change.
Reactions Involved:

MnSO4 + 2KOH Mn(OH)2 + K2SO4


2Mn(OH)2 + O2 2MnO2(dark brown ppt)
2MnO2 + H2SO4 MnSO4 + H2O + [O]
2KI + H2SO4 + [O] K2SO4 + H2O + I2
I2 + Na2S2O3 2NaI + Na 2S4O6(Sodium
tetrathionate)
Starch + I2 Blue colour complex
• Azide modification is used to remove substances like
nitrites, sulphides etc. which liberate iodine from
potassium iodide to dissolve oxygen. For example the
interference of nitrite is overcome by adding sodium
azide (NaN3) and H2SO4 shown as below:
NaN3 +H+ N3H + Na+
N3H + NO2- + H+ N2 + 2 H2O +N2O
Procedure:
• Take 50 ml water sample in iodometric flask; avoiding as far as possible,
contact with air.
• Immediately add 1ml of manganese sulphate solution from the burette
and add 1ml of alkaline iodide from the other burette.
• Insert the stopper and shake several times.
• Allow the precipitate to settle half way and mix again. Repeat this process
of shaking and settling at least three times.
• Add 1ml of conc. sulfuric acid. Insert the stopper and shake again.
• Allow the yellow solution to stand for 5 mins.
• Withdraw 50 ml of the solution. Titrate it against the standard N/40 sodium
thiosulphate solution till the colour of the solution becomes faint yellow.
• At this stage add few drops of starch solution. The colour turns to deep
blue due to the formation of starch-iodide.
• Continue the titration till the solution becomes colourless.
Observations:
• Volume of water for each titration = 50 ml
• Volume of N/40 thiosulphate solution = 44.5 (V) ml
Calculations:
50 ml of water sample ≈ V ml of N/40 Na2S2O3 solution
Normality = V/50× 40
Strength = V × 8/50 × 40gm of O2/litre
V × 8/50 × 40 × 1000 ppm

Amount of dissolved oxygen = .........ppm

Result: Dissolved oxygen = ........ppm


Precautions:
1) The solution in the iodide flask should be shaken
carefully while keeping the thumb on the lid.
2) The solution should be well shaken before each aliquot
is withdrawn for titration.
3) The solution in the iodine flask should not be sucked
into the pippete with the mouth.

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