INTRODUCTION
Dissolved oxygen levels in natural
and wastewater depends on physical chemical and biochemical activities in the
water body. Analysis for dissolved oxygen is the key test in water pollution
and waste treatment process control. A dissolved oxygen level of 0-8 ppm is
normal and supports aquatic life.
METHODS FOR ESTIMATION:
1. lodometric method
2. Membrane electrode method
3. Azide modification method
4. Permanganate method
5. Alum flocculation method
6. CuSO4 sulfuric acid
modification method
AZIDE MODIFICATION METHOD PRINCIPLE:
lodometric test is most precise and
reliable titrimetric procedure for dissolved oxygen analysis. It is based on
addition of divalent manganese solution followed by addition of strong alkali
azides. An equivalent amount of dispersed divalent manganous hydroxide
precipitates to hydroxide of higher valency state (Mn+3). If no O2
is present, white precipitates of Mn(OH)2 are formed. But in
the presence of O2,, divalent (Mn+2) is oxidized to Mn+4
i.e., MnO2. In the presence of iodine ions in acidic solution,
oxidized manganese reverts to divalent state (Mn+2) with liberation
of I2 equivalent to original dissolved oxygen content. The liberated
I2 is then titrated with standard solution of thiosulfate.
REAGENTS:
· MnSO4 solution: Dissolve
480gm MnS04.4H2O or 400 gm MnSO4.2H2O
or 364 gm MnSO4.H2O in distilled water and make volume up
to 1 liter.
· Alkali iodide azide reagent: dissolve
700gm KOH, 150 gm KI and 10 gm NaN3 in 1000 ml of distilled water.
· Concentrated sulfuric acid
· Starch solution: 2% starch solution.
· Standard sodium thiosulfate titrant:
Dissolve 6.205 gm Na2S2O3.5H2O in
distilled water and 1.5 ml 6N NaOH or 0.4 gm solid NaOH and make total volume
to 1000 ml.
PROCEDURE:
· To the sample collected in 250/300 ml
bottle add 1 ml MnSO4 solution followed by 1 ml alkali azide
reagent.
· Stopper the bottle to exclude air
bubbles and mix by inverting the bottle.
· Allow the precipitates to settle
sufficiently.
· Add 2 ml concentrated H2SO4
and shake the bottle so that the precipitates dissolve.
· Take 200 ml from it and add 1-2 drops
of starch.
· Titrate with 0.025 M Na2S2O3
solution until the blue color disappears.
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