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PROGRAMME : HENCE
COURSE : CE308
LECTURER : DR S. Misi
DATE : 12/10/18
To measure the oxygen demand of a water sample by titration with FAS solution.
THEORY
COD is an indicative measure of the amount of oxygen that can be consumed by reactions in a
measured solution. It is commonly expressed in mass of oxygen consumed over volume of
solution which in SI units is milligrams per litre (mg/L). A COD test can be used to easily
quantify the amount of organics in water. The most common application of COD is in
quantifying the amount of oxidizable pollutants found in surface water (e.g. lakes and rivers)
or wastewater. COD is useful in terms of water quality by providing a metric to determine the
effect an effluent will have on the receiving body, much like biochemical oxygen demand (BOD)
MATERIALS
Sterile bottles, Sterile 10ml pipettes, Automatic Zero burettes, rubber bulb and conical
flasks,Ferrous Ammonium Sulphate, Silver Sulphate, Calcium Chloride (CaCl2), Sodium
Hydrogen Carbonate (NaHCO3) and Potassium Dichromate.
METHOD
1. The C.O.D. digester was turned on and pre-heated to 1500C. Care was taken when handling
the top of the digester as it was very hot.
2. The samples were accurately diluted by pipetting, using a safety pipette filler, sample
volumes of 5 ml and 10ml were measured into a graduated flask and the volume made up
with pure water. Dilution factors of 10 and 5 were selected respectively. The COD value
of the dilutions should be between 20 and 300 mg/L.
3. Digestion vials were labelled near the top, with sample number and corresponding dilution
factors.
4. The cap was removed from the digestion vial and then it was placed on the rack provided.
5. The following solutions were then pipetted into the vial in order using a safety pipette filler:
.i 0.5mls of 20% Mercuric Sulphate Solution
.ii 1.0mls of 0.125N Potassium Dichromate Solution-Accurately.
.iii 2.0mls of diluted sample- Accurately.
A blank in which 2mls of pure water replaces the 2mls of sample was then also prepared. All
samples and blanks were done in duplicate.
6. The vial was then held with the rubber sleeve provided and then safely holding it away
from the face 2 ml of Silver Sulphate in Concentrated Sulphuric Acid were pipetted using
a safety pipette filler.
Precautions taken:
.i The Silver Sulphate in Concentrated Sulphuric acid is a very heavy solution and may
tend to leak out if the safety pipette filler is not attached properly. Care was therefore
taken to ensure that the drops did not drop onto any clothing. The solution is very
corrosive and could potentially cause severe burns.
.ii Wet tissues were used to wipe off any excess solution from the outside of the pipette.
Dry tissues were not suitable as they wipe very badly and may ignite.
.iii The addition of a concentrated acid to water results in the production of a lot heat
therefore caution should be taken.
7. The top of the vial was then replaced and tightened using a special tightening tool
provided.
8. With the vial still in the rubber sleeve it was then shaken to mix.
.i Mixing the solution resulted in the production of a lot of heat careful handling
was essential to prevent spillages and burns.
9. The Hot vial was then placed in the pre-heated digester and the safety screen placed
over the reactor and then digested for 2 hours.
10. After 2 hours the vials from the reactor were then replaced and cooled to room
temperature.
11. The vial top was then removed carefully and a mini-bar follower and 3 drops of Ferroin
indicator added.
12. The excess Dichromate was then titrated against the standard 0.025N Ferrous
Ammonium Sulphate solution to end point. The color changes observed in sequence
were as follows. At first the color was green, it then changed to blue, grey and then 1
13. or 2 drops after the grey the color changed to red. This was the end point.
RESULTS:
Where:
b is the volume of FAS used in the blank sample
s is the volume of FAS in the original sample
n is the normality of FAS
Volume Of Dilution Final Burette Initial Burette C.O.D
Sample Sample Taken Factor Reading Reading Titre (Mg/L)
Blank - - 0.9 8.0 7.1 -
Borehole 20 1 23.2 29.7 6.5 3
River 20 1 42.7 45.3 2.6 22.5
DISCUSSION
The COD Test results shown above indicate the presence of organic matter in the water which
were oxidized by the Potassium Dichromate. Sample. River water has a relatively high amount
of COD which indicates possibility of self-cleaning of the water say in the river after storms.
Borehole water has the lowest and is suitable for drinking since it is within limits recommended
by W.H.O.
CONCLUSION
According to (Burton, et al., 2003), it is key to note that even though the C.O.D test can be
regard as an indirect method in establishing the amount of organic substances in water it usually
results in higher values of oxygen demand being obtained and this is because Potassium
Dichromate is a very strong oxidizing agent it will also oxidize other substances in the water that
would not normally be oxidized naturally.
1. TITLE
OBJECTIVE
THEORY
BOD is the amount of dissolved oxygen needed (i.e. demanded) by aerobic biological organisms
to break down organic material present in a given water sample at certain temperature over a
specific time period. The BOD value is most commonly expressed in milligrams of oxygen
consumed per litre of sample during 5 days of incubation at 20 °C and is often used as a
surrogate of the degree of organic pollution of water.
MATERIALS
250ml glass bottles with glass stoppers (preferably special BOD bottles), Incubator at 37oC or
20oC, Phosphate Buffer, Magnesium Sulphate, Calcium Chloride, Sulphuric Acid, Sodium
Hydroxide, Standard Titration glassware including burettes and conical flasks.
METHOD
1. The water sample was added to a 250ml BOD bottle. The bottle was completely filled
with water with no air bubbles trapped under the stopper. A duplicate and blank were
made for each sample and the procedure done as exact as possible.
2. All sample bottles were placed in a plastic tray before adding the chemical reagents. The
pipette fillers provided were used.
3. 2ml of Manganese Sulphate solution was added with a pipette well below the liquid
4. surface.
5. 2ml of alkaline iodide solution was added IMMEDIATELY to the water surface using a
pipette.
6. The bottle stopper was replaced carefully allowing surplus liquid to overflow into the tray
while avoiding trapping any air bubbles under the stopper.
7. The stoppered bottle was inverted several times to mix the components and the brown
precipitate formed was allowed to settle within the lower third of the bottle.
8. The stoppered bottle was inverted to mix again. The precipitate formed was allowed to
settle to within the lower third of the bottle.
9. 4ml of 1:1 Sulphuric Acid was added and the stopper was replaced carefully. The
contents were shaken until all the precipitate had dissolved, forming a clear brownish
solution.
10. A 200ml portion of the solution was measured using a measuring cylinder and was
poured into a conical flask.
11. The 200ml aliquot was titrated with 0.0125N sodium thiosulphate until the solution
became pale yellow in colour. A small amount of the soluble starch indicator powder was
added until a deep blue solution was formed. Sodium thiosulphate continued to be added
drop by drop until solution became colourless which was the endpoint.
12. The volume of the thiosulphate solution used for the sample and the blank was recorded
and the calculation of dissolved oxygen is as follows.
CONCLUSION
The initial dissolved oxygen measurements need to be conducted promptly to ensure that no
consumption occurs and its less than 6mg/L.
References
Burton, F., Stensel, D. & Tchobanoglous, G., 2003. Wastewater Engineering Treatment and Reuse. 4th ed. London:
McGrawHill.