Dissolved Oxygen

DISSOLVED OXYGEN
AIM
To determine the dissolved oxygen (DO) present in the given sample.
APPARATUS
Pipette, Burette, conical flask, Measuring cylinder, BOD Bottle
REAGENTS
Manganous sulphate solution, Alkali iodide sodium azide solution, Conc. Sulphuric acid
(H2SO4), Starch indicator solution, 0.025 N Sodium thiosulfate (Na2S2O3.5H2O).
THEORY
The D.O. determination measures the amount of dissolved (or free) oxygen present in water
or wastewater. All living organisms depend on oxygen to maintain metabolic processes that
produce energy for growth and reproduction. All gases are soluble in water to some extent.
Aerobic bacteria and aquatic life such as fish must have DO to survive.
Aerobic wastewater treatment processes use aerobic and facultative bacteria to break down
the organic compounds found in wastewater into more stable products that will not harm the
receiving waters. Wastewater treatment facilities such as lagoons or ponds, trickling filters
and activated sludge plants depend on these aerobic bacteria to treat sewage.
Winklers Method
Most of the modern method of determining D.O. depends on reaction that release the amount
of oxygen originally present with subsequent measurement of the amount of iodine released
by means of standard solution of reducing agent. This method is known as the Winklers
method and its modifications use for the determination of D.O.
Sodium thiosulphate is the reducing agent commonly used & starch solution is used as the
indicator. All reactions are Redox reaction, Starch indicator absorbs iodine from dilute
solutions to produce brilliant blue colour and return to colourless when all iodine is reduced
to iodide.
2Na2S2O3.5H2O + I2 Na2S4O6 + 2NaI + 10H2O
2S2O32- + I2 S4O62- + 2I2The reactions involved in Winkler procedure are as follows:
Mn2+ + 2OH- Mn(OH)2(s)
(White Precipitate)
If no oxygen is present, a pure white precipitate of Mn(OH) 2(s) forms when MnSO4 and the
alkali-iodide reagent are added to the sample, if oxygen is present in the sample, then some of
the Mn(II) is oxidized to Mn(IV) and precipitates as a brown hydrated hydrated oxide. The
reaction is as follows:
Mn2+ + 2OH- + O2 MnO2(s) + H2O
(Brown Precipitate)
The oxidation of Mn(II) to MnO 2 called fixation of oxygen. After all oxygen forms floc,
H2SO4 is added, under low pH condition MnO2 oxidizes I- to free iodine (I2),
MnO2(s) + 2I- + 4H- Mn2+ + I2 + 2H2O
Sample is now ready for the titration with sodium thopsulphate.
Electrometric Meter Method
Since there are many models and manufacturers of DO meters and probes, this manual will
not describe the operating procedures for all meters. For best results, follow the
manufacturers instruction for operation of meters and probes.
Condensation may collect on the membrane. This will interfere with the readings. Shake off
excess water and gently blot dry with a laboratory tissue. The membrane must be stretched
tightly across the probe and will not work correctly if air bubbles are present in the probe
underneath the membrane. Be sure that the O ring holding the membrane to the probe fits
securely.
Allow the instrument to warm up for at least 15 minutes before taking the first reading of the
day. Leave the instrument on between measurements. This will eliminate the need for warm
up periods between tests.
Calibrate at least once per day. Distilled or deionized water, and not effluent, should be used
for the probe calibration. Always stir the sample while taking a reading.
PROCEDURE
Modified Winkler Method
1. Collect the sample to be tested in a 300 mL BOD bottle taking special care to avoid
adding air to the liquid being collected. Fill bottle completely and add stopper.
2. Remove bottle stopper and add 2 mL of the manganous sulfate solution at the surface of
the liquid.
3. Add 2 mL of the alkaline potassium iodide sodium azide solution at the surface of the
liquid.
4. Replace the stopper, avoid trapping air bubbles and shake well by inverting the bottle
several times. Repeat shaking after floc has settled halfway. Allow floc to settle a
second time.
5. Add 2 mL of concentrated sulfuric acid by allowing the acid to run down the neck of the
bottle above the surface of the liquid.
6. Restopper, rinse the top of the bottle to remove any acid and shake well until the
precipitate has dissolved.
7. Titrate a volume of treated sample which corresponds to 200 mL of the original sample.
This corrects for the loss of some sample during the addition of reagents. This volume
calculated using the formula:
mL of sample to titrate = 200 x [300/(300-2)] = 201 mL

8. Pour 201 mL of sample from the BOD bottle into an Erlenmeyer flask.
9. Add a small quantity (approximately 2 mL) of starch indicator. If no blue color
develops, there is zero dissolved oxygen. If a blue color develops, proceed to step 10.
10. Titrate with 0.0250 N sodium thiosulfate.
INTERFERENCES
In the determination of DO by the Winkler method, there are various materials which cause
interferences, including iron salts, organic matter, excessive suspended matter, sulfide, sulfur
dioxide, residual chlorine, chromium, cyanide, and certain oxidizing and reducing agents. If
Nitrite is present in sample, it is impossible to obtain a permanent end point because it does
oxidize I- to I2.
Interference of nitrite is removed by addition of sodium azide (NaN3).
RESULT

Dissolved Oxygen

Uploaded by

Copyright:

Available Formats

Dissolved Oxygen

Uploaded by

Document Information

Original Description:

Copyright

Available Formats

Share this document

Share or Embed Document

Sharing Options

Did you find this document useful?

Is this content inappropriate?

Copyright:

Available Formats

Dissolved Oxygen

Uploaded by

Copyright:

Available Formats

DISSOLVED OXYGEN

Mn2+ + 2OH- + O2 MnO2(s) + H2O

mL of sample to titrate = 200 x [300/(300-2)] = 201 mL

You might also like