DO Rimu Mam

Experiment Name: Determination of dissolved oxygen (DO) in supplied water sample.
Dissolved Oxygen (DO) is a water quality parameter that is very important in secondary treatment
processes. DO levels represent the amount of oxygen that is dissolved and dispersed throughout a
water sample. Bacteria and microorganisms use dissolved oxygen to break down organic material,
therefore reducing concentrations of dissolved oxygen. In wastewater treatment, microorganisms are
added in flocs to aerobically digest and remove biodegradable substances. As a result, efficient
treatment relies on microorganism health and dissolved oxygen concentration. Evaluating dissolved
oxygen is also very important in industrial settings for numerous processes. For instance, sewage
treatment plants rely on the decomposition of solids by bacteria. When DO levels are low, the
bacteria that’s needed to complete this process will stop, which results in the decomposition stopping
until DO levels are restored. When dissolved oxygen levels are too high within sewage treatment
plants, too much energy will be effectively wasted, which makes for an inefficient process. For
boilers in industrial settings, low DO levels are necessary to avoid the buildup of scale and corrosion.
When the amount of scale increases inside a boiler, the heat transfer process within the system will
become increasingly inefficient. Measuring the concentration of dissolved oxygen is important
with such applications as live fish transport, corrosion control, wastewater treatment, and fish
farming. Dissolved Oxygen (DO) levels in natural and wastewaters are dependent on the physical,
chemical and biochemical activities prevailing in the water body. The analysis of DO is a key test in
water pollution control activities and waste treatment process control. Dissolved oxygen is supplied
to a lake from two main sources: plant and algae photosynthesis and diffusion from the atmosphere.
Iodometric determination of DO is based on oxidation of potassium iodide. The liberated iodine is
titrated against standard hypo solution using starch as a final indicator. Since oxygen in water is in
molecular state and not capable to react with KI, an oxygen carrier manganese hydroxide is used to
bring about the reaction between KI and O2 .Manganous hydroxide is produced by the action of
potassium hydroxide and Manganese Sulphate.
Chemical reaction: 2KOH + MnSO4 → Mn(OH)2 + K 2 SO4
2Mn(OH)2 + O2 → 2MnO (OH)2
2MnO(OH)2 + 2H2SO4 +4I- → 2MnSO4 +4H2 O +2I2
2I2 + 4Na2 S2 O3 → 4NaI + 2Na2 S4 O6 (Sodium tetrathionate)
Starch + I2 → Starch iodide complex (Blue in color)
The Azide Modification with the Winkler Method for DO Determination
This modification is used because of presence of nitrite ions in wastewater. This occurs in effluents
from wastewater treatment plants employing biological processes, in river water and in incubated BOD
samples. It does not oxidize Mn2+ but doses oxidize I- to I2 under acidic conditions. When the reduced
form of nitrite (N2O2) is oxidized by oxygen, it is converted to NO2 - again, establishing the cycle again
that can result in erroneous results, far in excess of amounts that would be expected.
2NO2- +2I- +4H+ = I2 + N2O2 + 2H2O………(a)
N2O2 + 0.5 O2 +H2O = 2NO2 - +2H+ ………..(b)
When interference from nitrites is present, it is impossible to obtain a permanent end point. As soon as
the blue color of the starch indicator has been discharged, the nitrites formed by the reaction (b) reacts
with more iodide ions to produce I2 and the blue color of the starch indicator will return. The nitrite
interference is easily overcome with use of sodium azide (NaN3), which is incorporated in the alkali-KI
reagent. When sulfuric acid is added, following reactions happen:
NaN3 + H+ = HN3 +Na+ …………. (c)
HN3 +NO2- + H+= N2 +N2O+H2O ……(d)
Reagents:
1. Manganous sulfate solution 2. Sodium hydroxide (NaOH) 3. Potassium iodide solution
4. 0.025N sodium thiosulfate 5. Starch solution (indicator) 6. Concentrated sulfuric acid
7. Sodium Azide (NaN3)
Chemicals:
Manganous sulphate solution: Dissolve 36.4 g manganous sulphate (MnSO4) in 100 mL distilled water.
Alkaline‐iodide‐azide solution: Required chemicals are: Sodium hydroxide, potassium iodide and
sodium azide. Dissolve 50 g sodium hydroxide in 100 mL distilled water. Allow to stand for some days,
during which any carbonate present sinks to the bottom. Siphon off all of the clear liquid, add 15 g
potassium iodide, stir until the complete dissolve.
Take 4 g sodium azide into a volumetric flask, pour the NaOH+KI solution, make up to 100 mL with
distilled water. Store in a plastic container.
Starch indicator: Weight 0.5 g of soluble starch and dilute it with 100 mL of boiled distilled water.
Sodium thiosulphate (0.025 N): Required chemicals are sodium thiosulphate and Sodium hydroxide.
Dissolve 3.012 g of sodium thiosulphate and 0.2 g of NaOH to 500 mL with distilled water.
Procedure: Dissolved oxygen (DO) is determined according to the following procedure:
1. Add 1 mL of manganous sulfate solution to the BOD bottle by means of pipette, dipping in end of the
pipette just below the surface of the water.
2. Add 1 mL of alkaline potassium iodide solution to the BOD bottle in a similar manner.
3. Insert the stopper and mix by inverting the bottle several times.
4. Allow the "precipitates" to settle halfway and mix again.
5. Again allow the "precipitates" to settle halfway.
6. Add 1 mL of concentrated sulfuric acid. Immediately insert the stopper and mix as before.
7. Allow the solution to stand at least 5 minutes.
8. Withdraw 100 mL of solution into an Erlenmeyer flask and immediately add 0.025N sodium
thiosulfate drop by drop from a burette until the yellow color almost disappears.
9. Add about 1 mL of starch solution and continue the addition of the thiosulfate solution until the blue
color just disappears. Record the ml. of thiosulfate solution used (disregard any return of the blue color).
Calculation:
Dissolved oxygen (mg/L) = (mL of titrant × normality of sodium thiosulphate ×8 × 1000)/ V2 (V1-V)/V1
Here, V1= volume of DO bottles
V2= Volume of titrant
V= volume of manganese -sulphate and alkali-iodide-azide solution added, in mL

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Experiment Name: Determination of dissolved oxygen (DO) in supplied water sample.

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