Dissolved oxygen

Aim: To determine the dissolved oxygen in the given water sample by Iodometric method.

Apparatus: BOD bottle, pipette, conical flask, Dropper, Measuring cylinder.

Reagent: 1. Manganese sulphate solution

2. Alkali iodide azide solution
3. Conc. Sulphuric acid
4. 0.025N sodium thiosulphate solution
5. 2% starch solution
6. water sample

Principle:
Dissolved oxygen levels depends upon the physical, chemical, biological activities in
the water bodies. The analysis of oxygen plays a key role in water pollution control activities
and treatment process.

MnSO4 + 2NaOH Mn(OH)2 + Na2SO4

DO in the sample rapidly oxidize an equivalent amount of dispersed Mn2+ precipitate

to higher valent Manganese (IV) oxide hydroxide floc. Which has the formula MnO(OH) 2

2Mn2+ + O2 + 4OH 2MnO(OH)2

In the presence of Iodide ion and in acidic medium Mn4+ reduced back to divalent Mn2+
thus liberating I2 .

Mn4+ + 2I ‾ + 4OH Mn2+ + I2

Thus liberated iodine is stoichiometrically equivalent to the dissolved oxygen in the

sample. Librated iodine is titrated against standard solution of Na2S2O3 or phenyl arsine oxide
using starch indicator to a colourless end point.

2Na2S2O3 + I2 2Na2S4O6 + 2NaI

Starch solution is preferred as indicator in iodometric titration. Although iodine itself

has, a perceptible colour at a concentration of 5 X 10 -6M. It cannot serve as its own indicator
because the environmental samples are often dirty and not so clear. Starch is composed of
macromolecular components , α- amylose and 𝞫-amylose. The former reacts irreversibly with
iodine to for the red adduct. 𝞫-amylose on the other hand reacts with iodine forming a deep
blue complex, because this reaction is reversible, 𝞫-amylose is an excellent choice for
indicator. 𝞫-amylose is polymer of thousands glucose molecules. It has a helical structure in to
which iodine is incorporated as I5.

When sodium thiosulphate is slowly added to the deep blue solution of starch iodine
complex, the reducing agent takes away iodine from the helix. At the end point, when all iodine
is lost, the solution becomes colourless.
Procedure:

1. Take 300ml DO bottle & filled completely with sample of water, stopper immediately
to avoid contact with air.
2. Add 2ml MnSO4 & 2ml of Alkali iodide azide solution to it.
3. Mix thoroughly by inverting bottles 4 to 5 times makes the precipitate settle.
4. Add 2 ml of conc.H2SO4 re-stopper & de-precipitate by shaking.
5. Now the total volume becomes 300ml. Take 203 ml sample in conical flask for
titration.
6. Add 2 to 4 drops of starch indicator to it & titrate against 0.025N Na2S2O3 solution.
7. End point of titration from blue to colourless.

Observations:

1. Solution in burette: 0.025N Na2S2O3 solution.

2. Solution in pipette: 203 ml sample water.
3. Indicator: starch indicator
4. End point: Blue to colourless
5. C.B.R.: (A) --------ml

Observation Table:

Sr. No. Vol. of water Vol. of 0.025 N. Na2S2O3 Avg/ Mean Vol. of 0.025N
taken (ml) required (ml) Na2S2O3 sol. required (A)

v1 v2

Calculation:
A = -------ml of titrant (Na2S2O3)
N = Normality of Na2S2O3

𝐴 × 𝑁
DO = × 8000
𝑀𝑙 𝑜𝑓 𝑠𝑎𝑚𝑝𝑙𝑒

Result: The amount of dissolved oxygen in the given water sample is-----------mg/lit.
Aim: To determine the dissolved oxygen in the given water sample by Iodometric method.

Solutions:

1. MnSO4 Solution: Dissolve 400 gm of MnSO4 or 480 gm of MnSO4.4H2O in

distilled water and make up to 1 L. This solution should not give volour with
acidified potassium Iodide and starch.
2. N/20 Sodium Thiosulphate: Dissolve 12.41 gm of AR sodium thiosulphate
pentahydrate (Na20S2O3.5H2O) in 1L or distilled water. This solution may be
rpreserved by adding 3 drops of chloroform.
3. 0.025 N sodium thiosulphate: Standard sodium thiosulphate solution (0.025N):
6.025 gm sodium thiosulphate pentahydrate (Na2S2O3.5H2O) is dissolved
in distilled water and either 1.5 ml of 6N sodium hydroxide solution or 0.4 gm solid
sodium hydroxide is added and diluted to 1000 ml.
4. Conc. H2SO4: as per need or solution becomes clear.
5. Alkaline Iodide azide reagent. : Dissolve 500 gm of NaOH and 150 gm of KI in
distilled water. Add 10 gm of NaN3 in 40 ml distilled water. Dilute to 1 L. This
solution should not give colour with starch on dilution and acidification.
6. Starch solution: prepare fresh paste of 0.5 gm starch with distilled water and pour
this in to 100 ml of boiling distilled water while stirring. Continue boiling for few
minutes and cooll .
7. Solid KI free from Iodate