Environmental Engineering Laboratory

By: Ngoc Thuan Le

Chemical Oxygen Demand (COD) - Mn

Apparatus: COD-300ml refluxing flask, condenser with cooling system.

Before doing experiments, turn on water bath
Procedure:
1. Place 100ml of sample in a 300ml refluxing flask.
2. Very slowly add 10ml of H2SO4 : water (1:2),
3. Add 1g Ag2SO4 (less than 1g is possible) -- mixing well to dissolve. Wait for 5 mins,
solution will become milky color.
4. Add 10ml of KMnO4 0.025N and mix.
5. Attach flask to condenser and turn on cooling water system, boiling for 30 minutes
Caution: Mix flux mixture thoroughly before applying heat to prevent local heating of flask
bottom and a possible blowout of flask contents
6. Disconnect reflux condenser, add 10ml sodium oxalate Na2C2O4 0.025N (수산나트 륨).
7. Titrate with solution of KMnO4 0.025N from a burette, with a magnetic bar. During the
titration, keep temperature of solution around 60-80oC.
Maximum COD can be measured around 10mg/l.
Prepare 1 blank sample with distilled water.
Caculation: (b − a ) × f ×1000 × 0.2
COD ( mgO / L) =
V
a. volume of KMnO4 0.025N used for blank.
b. volume of KMnO4 0.025N used for sample.
f. factor.
V. Volume of sample (ml).
Factor:
- Place 100ml in refluxing flask, add 10 ml H2SO4 (1+2), 10ml Na2C2O4 0.025N, warming at
60-80oC. Titrate the mixture with KMnO4 0.025N, record a ml.
- Place 100ml in refluxing flask, add 10 ml H2SO4 (1+2), warming at 60-80oC. Titrate the
10
mixture with KMnO4 0.025N, record b ml. f =
( a − b)
Reagents:
- KMnO4 0.025N: 158.3 g/mol. Standard solution 0.02M (0.1N) ~ 3.161g, dilute 4 times before
using.
- H2SO4 1:2, 1V H2SO4: 2V dW.
- Ag2SO4, crystals or powder.
- Na2C2O4 0.025N (0.0125M): Dissolve 1.675g Na2C2O4 primary standard grade, in water and dilute
to 1000ml.
(Stock solution: Na2C2O4 0.25N (0.125M): Dissolve 16.75g Na2C2O4 primary standard grade, in
water and dilute to 1000ml, dilute 10 times before using)