Vous êtes sur la page 1sur 2

Chemical Oxigen Demand ( COD ) 1. Pipette 25 ml of potassium dichromate 0.1N into a round -bottomed flask of 250 ml or 500ml. 2.

Add slowly through a burette 30 ml of cont, swirl the flask at the time. 3. While the contents in the round-bottomed flask are still very hot, add slowly through a graduated pipette a suitable volume of effluent sample and swirl the flask all the time until the colour of the contents in the round-bottomed flask change of colour can be easily observed when compared with the blank which contains only the unreacted dichromate. 4. Add an amount of cone. Sulphuric acid equal to the volume of sample taken multiplied by 1.2. 5. Now, add 10 ml of silver sulphate solution and a few anti-bumping granules. Fix a suitable reflux condenser to the flask. Mix the solution well and boil it under reflux for at least 2 hours. 6. After 2 hours of boiling, allow the contents to cool down for about hour and wash the inside of the reflux with some distillated water. Cool the flask further in running water. 7. Before starting to titrate, add distillated water equal to 3 times its original voume. Add a few (56) drops of indicator . 8. Swirl the flask and titrate against ferrous sulphate solution (0.1) until the colour changes to reddish brown, that is the end point. The end point is fairly sharp. Carry out a blank determination.

Calculation: C.O.D. (mg/l) = (a-b) xC x 8000 Volume of sample taken

Where a = ml FeSO4 (0.1N) used for blank B = ml FeSO4 (0.1N) used for sample C = Normality of FeSO4 0.1N.

Dissolved Oxigen (DO) 1. To the sample as collected in a 250-300 ml bottles add 2 ml manganese sulphate solution followed by 2 ml alkali-iodida-azide solution, well below the surface of the liquid stopper with care to exclude air bubbles and mix by inverting several times. 2. When precipitate settles, leaving a clear supernatant above the manganese hydroxide floc, shake again. 3. When settling has produced at least 100 ml of clear supernate, carefully remove the stopper and ammediately add 2 ml conc. H2SO4 by allowing the acid to run down the neck of the bottle, restopper, and mix by gentle inversion until dissolution is complete. 4. The iodine should be uniformly distributed throughout the bottle before decanting the amount needed for titration. This should correspond to 200 ml of the original sample after correction for the loss of sample by displacement with the reagents has been made. Thus, when a total of 4 ml (2 ml each) of the MnSO4 and alkali-iodide-azide solution is added to a 300 ml bottle, the volume taken for titration should be 200 x 300/(300-4) = 203 ml. 5. Titrate with 0.025N thiosulphate solution to a pale straw colour. Add 1-2 ml freshly prepared starch solution and continue the titrationnto the first disappearance of the blue colour.

Calculation Because 1 ml of 0.025N sodium thiosulphate titrant is equivalent to 0.2 mg D.O., each ml of sodium thiosulphate titrant used is equivalent to 1 mg/1 D.O. If volume equal to 200 ml of original sample is titrated.