1.

0 PROBLEM STATEMENT
The purpose of using blank sample is to compensate for any error that may cause of the
presence of extraneous organic matter in the reagents.
2.0 AIM
To determine the organic oxidize able matters content of water samples.
3.0 METHODOLOGY
3.1 Sampling procedure
i.
Collect the sample in glass bottles, if possible. Use of plastic containers is
permissible if it is known that no organic contaminants are present in the
ii.

containers.
Biologically active samples should be tested as soon as possible. Samples
containing settle able material should be well mixed, preferably

iii.

homogenized, to permit removal of representative aliquots.

Samples should be preserved with sulphuric acid to a pH < 2 and
maintained at 4oC until analysis.

3.2 Sampling location (include type of sample, with photo or diagram)

Drain Water

3.3

Apparatus
1. Burette

2. Pipette

3. COD Vial

3.4

Equipment
1. COD Reflux System

3.5 Chemicals and reagent

i.
Standard potassium dichromate 0.01667M
1000ml distilled water
4.903g potassium dichromate (K2Cr2O7) dry 2 hour 150C
167ml acid sulphuric (H2SO4)
33.3g mercury sulphate (Hg S04)
ii.
Acid sulphuric reagent
5.5g silver sulphate (Ag SO4)
1kg acid sulphuric (H2 SO4)
iii.
Standard ferrous ammonium sulphate
39.2g ammonium iron II sulphate 6-Hydrate {Fe(NH4)2(SO4)2. 6H20}
20ml acid sulphuric (H2SO4)
1L distilled water
iv. Ferroin indicator
v.
3.6 Lab procedures
1. The substances must be added in COD Vial following the sequences below :
a. Place in COD Vial 1 and 2 with :
i. 1.5ml Potassium Dichromate Reagent
ii. 3.5ml Acid Sulphuric Reagent
NOTE : Mixture reflux thoroughly before applying heat to prevent
local heating of flask bottom and possible blowout of flask
contents
b. COD Vial No. 1 : 2.5ml sample
COD Vial No. 2 : 2.5ml distilled water
2. Entering the refluxing mixture at COD Reactor with temperature 150 for 2
hours. At a meantime, please proceed to Procedure no. 6.
3. After 2 hours, cool wash down the condenser with distilled water. Continue
cooling the condenser to room temperature.
4. Disconnect reflux condenser. Transfer the solution to the conical flask and
dilute the mixture up 150ml with distilled water. Added with 3 drops ferroin
indicator. Placed the magnetic bars and stir it with magnetic stirrer.

5. Titrate K2Cr2O7 with Ferrous Ammonium Sulfate (FAS). First and last
reading was noted in Table 2. Take as the end point of the titration the sharp
colour to blue-green. Stop titration, add 3 drops of Ferroin indicator.
Continue titration until the colour change to reddish brown that persist for 1
minute or longer. Stop titration and jot down the last reading in Table 2. Take
a precaution that the end point colour changes of titration is fast. Calculate
the volume of FAS used in titration Table 2.
6. Preparation of Standard Ferrous Ammonium Sulfate (FAS) titrant as below :
a. Dilute 5ml Potassium Dichromate K2Cr2O7 standard (0.01667M) with
10ml distilled water in the conical flask 250ml. swirl and mix slowly.
b. Slowly and carefully add 30ml conc H 2SO4 and cool. Refer to Figure 1,
titrate with the FAS titrant using 3 drops of ferroin indicator. First and last
Reading should be jot down in Table 1.
c. Take as the end point of the titration the first sharp colour change to bluegreen. Stop titration, add 3 drops of ferroin indicator. Continue titration
until color change to reddish brown that persists for 1 minute or longer.
d. Take precaution that the end point colour changes of titration is fast.
Jotted down the colume of FAS used in titration Table 1.

4.0 DATA
Table 1 : FAS Standard Titration Data :
Reading of buret/pipet
First Reading
Last Reading
Volume of FAS standard (ml)

Cone Flask (Standard) (ml)

0
16
16

Molarity of FAS solution = Volume 0.01667M K2Cr2)7 solution titrated, ml x 0.100

Volume FAS used in titration, ml
= 5 ml x 0.100
16
= 0.03125
*Note : The 0.1 is the Standard Potassium Dichromate solution, 0.01667M K 2Cr2O7
undergoes

a six-electron reduction; the equivalent concentration is 6 x 0.01667M or

0.100N
Table 2 : COD test Data Collections :

Normality of

Sample

FAS (N)

volume
(mL)
2.5

In

Volume of FAS used

the
original in the blank sample,

sample, b (mL)
First reading
Last reading

s (mL)

0
3.4
3.4

3.4
5.4
2.0

COD as mg O2/L = (A-B) x M x 8000

(ml) sample
= (3.4 2.0) x 0.031 x 8000
2.5
= 138.88 mg/l

5.0 ANALYSIS
1. Which volume is larger, in the blank sample or in the original sample.
The volume is larger in the original sample. The original sample has a large volume
due to the amount of organic and inorganic contaminant is higher.
2. How to obtain the normality of FAS equal 0.25N.
N1V1 = N2V2
0.25V1 = 0.1(5)
0.1 ( 5 )
V1 = 0.25 =2
Where :
N1 = Mol. of FAS (N)
N2 = Mol. of Standard Potassium Dichromate (N)
V1 = Vol. of FAS used (ml)
V2 = Vol. of Standard Potassium Dichromate used (ml)
To obtain the normality of FAS = 0.25N is by using 2ml of FAS.

3. If the original sample has to be diluted, how can you calculate the value of
COD.

The value will get in negative.

6.0 DISCUSSION
1. What is the purpose of using blank sample in this experiment
The purpose of using blank sample is to compensate for any error that may cause of
the presence of extraneous organic matter in the reagents. The blank sample is
produced by adding the reagents to an amount of distilled water. The result from
blank sample will be compared with the original, thus the compared result will be
used to calculate the COD value.
2. What is the objective of COD test and what is the different between COD and
BOD test
The objective of COD test is to determine the amount of organic pollutants found in
the water sample.
Differences of COD test and BOD test
Parameter
Oxidant used

COD test
227 Potassium

BOD test
Oxidation by microorganism

Most suitable use

Dichromate
Rapid and frequent monitoring

Modeling treatment plant

of treatment plant efficiency and

process and the effect of

water quality.

organic compounds on the

dissolved oxygen content of

Test completion time

Use

1 to 3 hours
Its been used for referring the

receiving water.
5 days for standard BOD test
Its been used to measure the

requirement of dissolve oxygen

consumption of oxygen by

for the oxidation of organic and

aquatic microorganism to

inorganic constituent both.

decompose or oxidize organic

matter.
3. Why the CODs value needs to be monitor for the polluted surface water such
as in lakes and rivers as well as for wastewater.
According to the value of COD, we may recognize the level pollution of the polluted
water. Thus, a few treatments can be done and action can be taken. For the ordinary
domestic sewage, it can able to be treated sewage treatment, meanwhile for water
that has a higher COD value, some specialized treatment might needed.
4. Give your opinion, if you need to compare the results of COD test to BOD and
permanganate value (test COD by using potassium permanganate, KMnO4)
tests.
From the history, Potassium permanganate is the strong oxidizing agent that can be
used for measuring chemical oxygen demand. But it is not very effective in
oxidizing all the organic matter present. Its effectiveness often much greater in
many cases of BOD. Thus, on my opinion, the COD value would be lower than
BOD value.
5. Why the value of COD increase when the amount of pollutant increased in
surface water.
Because the COD value is indicated in the amount of water dissolve oxygen
consumed by organic and inorganic contaminant in polluted water. Thus, the higher
the amount of contaminant, the higher the amount of water dissolve oxygen has been
consumed and the COD value will be increased.
6. Explain briefly the steps of COD measurement that you should follow during
this experiment.
Chemical oxygen demand (COD) is a measure of the capacity of water to consume
oxygen during the decomposition of organic matter and the oxidation of inorganic
chemicals such as ammonia and nitrite. COD measurements are commonly made on
samples of waste waters or of natural waters contaminated by domestic or industrial
wastes. Chemical oxygen demand is measured as a standardized laboratory assay in
which a closed water sample is incubated with a strong chemical oxidant under
specific condition of temperature and for a particular period of time. A commonly
used oxidant in COD assays is potassium dichromate (K2Cr2O7) which is used in

combination with boiling sulfuric acid (H2SO4). Because this chemical oxidant is
not specific to oxygen-consuming chemicals that are organic or inorganic, both of
these sources of oxygen demand are measured in a COD assay.
7. Briefly explain whether the value of COD obtain in this experiment are suitable
to be discharged to the stream.
The value of COD obtained in this experiment is 138.88 mg/l which has exceeded
the allowable limits in the Second Schedule in The Environment Protection Act 2002
that is 120mg/l, thus the waste water used in this test cannot be discharged to the
stream.

7.0 CONCLUSION
Chemical oxygen demand (COD) is used as a measure of oxygen requirement of
sample that is susceptible to oxidation by strong chemical oxidant. The COD value for
sample in this experiment was under range. Hence, we can conclude that this water
sample has long organic matter. Chemical Oxygen Demand is the total measurement of
all chemicals in the water that can be oxidized.
Error and precautions
However, during the experiment, some errors may occur due to the observer when
taking the reading of FAS titration from the burette.

1. The observer accidently late stopped the titration till the sample was completely
changed back its original (blue green) Thus, come precautions must be taken to
reduce the errors:
i.
Repeat the data collection by different observers and get its average value.
ii.
The observer must be more alert on the colour changes of the sample.
The experiment must be carried out carefully in order to get a more precise result.
8.0 REFERENCES

http://www.differencebetween.com/difference-between-bod-and-vs-cod/
http://www.envexp.com/technical/method-downloads/cod-method-410
http://www.slideshare.net/lovecantbpainted/chemical-oxygen-demand
http://civilengineerspk.com/environmental-engineering-2-experiments/exp-1chemical-oxygen-demand/