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EDITION:
TECHNOLOGY
LABORATORY: CIVIL 2
REVISION NO:
ENGINEERING TECHNOLOGY
FEB
EXPERIMENT: CHEMICAL EFFECTIVE DATE:
2015
OXYGEN DEMAND (COD)
AMENDMENT DATE:
1
FACULTY : ENGINEERING
EDITION:
TECHNOLOGY
LABORATORY: CIVIL 2
REVISION NO:
ENGINEERING TECHNOLOGY
FEB
EXPERIMENT: CHEMICAL EFFECTIVE DATE:
2015
OXYGEN DEMAND (COD)
AMENDMENT DATE:
I hereby declare that I have prepared this report with my own efforts. I also admit to
not accept or provide any assistance in preparing this report and anything that is
in it is true.
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1.0 OBJECTIVES
a) To determine the chemical oxygen demand (COD) in water/wastewater
sample.
b) To compare the laboratory result between influent and effluent of
water/wastewater sample.
2.0LEARNING OUTCOMES
At the end of this course students are able to:
a) Understand the concept of chemical oxygen demand in a given
water/wastewater sample.
b) Identify the principle of dichromate reflux and reactor digestion methods to
determine COD.
c) Evaluate the water parameter quality in domestic wastewater sample and
water supply.
d) Identify problems and use their generic skill to solve problems.
e) Develop their ability to work in group.
3.0INTRODUCTION
The principle of this experiment is to completely oxidize the organic
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4.0INSTRUMENTS /APPARATUS / CHEMICAL / REAGENTS
4.1 Chemicals / Reagents
4.4. Closed Reflux, Titrimetric Method (Prepared by Technician)
Caution: In carrying out the following procedures, use proper safety
beaker.
(iii) A tray of ice is placed on a magnetic stirrer in the fume
cupboard.
(iv) Both beakers are transferred to the fume cupboard; the 1
litre beaker is put into the ice tray and a stirrer bar is
added.
(v) Approx. 500ml of distilled water is added to the 1 litre
stirring continuously.
(viii) The mixture is allowed to cool to room temperature, and
volumetric flask, rinsing the beaker into the flask until all
invert to mix.
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(xi) The contents of the flask are transferred into the correct
catalyst reagent):
(i) 22. 5 g of silver sulphate is weighed out into a 250 ml
beaker.
(ii) A full 2.5 L bottle of concentrated sulphuric acid is
from acid.
(v) Any remaining silver sulphate in the beaker or on the
water.
(vi) The solution is left in a safe cupboard for 24 hours, and
glass rod.
(iii) 25 ml of conc. sulphuric acid is measured out using the
measuring cylinder.
(iv) The acid is poured into the beaker very slowly, whilst
stirring.
(v) Ensure that all the FAS has dissolved.
(vi) The beaker is allowed to reach room temperature
(vii) The solution is poured into a 1 litre volumetric flask via a
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Note: The deterioration of FAS can be decreased if it is stored in a dark
bottle.
i) COD digestion reagent vials with all premixed reagents included (e.g.
Hach COD digestion vial low range and COD digestion vial high
range)
digestion vessels
iii) Pipettes (10, 25 and 50 mL)
iv) Burette (50 mL), burette stand and clamp
v) Analytical balance
vi) Spatula
vii) Volumetric flask
viii) Magnetic stirrer and stirring bars
ix) Measuring cylinder
x) Beakers
xi) Conical flask
digestion vessels.
ii) Spectrophotometer (DR 6000)
iii) COD digestion reagent vials
iv) Test tube rack
v) Wipe tissue
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5 PROCEDURE
5.1 Closed Reflux, Titrimetric Method
5.1.1. Standardization of FAS solution : The ferrous ammonium
procedure:
(i). The clean burette is prepared. The clean burette is rinsed with
FAS three (3) times) prior to fill it in with FAS.
(ii). 5 ml of digestion reagent is dispensed into a beaker and
catalyst.
(iv). 2 drops of ferroin indicator is added and titrated with FAS
(v). The initial and the final reading of FAS (titre) is recorded and
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5.1.2. Digestion
(i) The digestion block is turned on after checking that it is clear
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(AT THIS POINT THE TUBE CONTENTS WILL UNDERGO
and the tube is capped very tightly. Hold the tube by the cap
5.1.3 Titration
(i) The contents of a digestion tube are poured into a clean 100 ml
conical flask. The tube into the flask is rinsed twice with
samples = B ml. The initial and the final reading of FAS are
5.2.1 Digestion
appropriate range.
(iii) The vial is held at a 45o angle. Pipette 2.0 mL (for low range)
with deionised water and the vial is wiped clean with paper
towel.
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(v) The vial is held by the cap and over a sink and inverted gently
several times to mix the contents. The vial is placed in the
2.0 mL (for low range) and 0.2 mL (for high range) deionised
COD reactor
DR6000 spectrophotometer.
(ii) Select programme: 430 COD LR or 435 COD HR. Touch start.
(iii) Clean the outside of the vial with a wipe tissue to remove
sample cell holder. Results will appear in mg/L COD and record
6 RESULTS CALCULATIONS
6.1 Results
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Table 6.1: FAS standard titration (Closed Reflux, Titration method)
Table 6.3: Volume of FAS required for Sample (Closed Reflux, Titration
method)
Type of Sample:
Blank Sample 1
0.0 122.0
6.2 Calculations
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Where: A = volume of FAS used for blank, mL
diluted)
7.8
= 141 mg/L
7 ANALYSIS
From the result, the volume of FAS required for FAS standardization
(T) and the volume of FAS used for blank (A) and sample (B) in closed reflux,
titration method are used to calculate the COD value of the sample in mg/L.
The burette readings are taken as final reading of table 6.1, 6.2 and 6.3 when
the colour of the contents changed from yellow to red. The value of A, B and T
is calculated by using the final reading minus the initial reading of the
burette reading. The value of COD is calculated by using the formula given
and it is 141 mg/L. The result obtained from the closed reflux, colorimetric
8 DISCUSSIONS
The COD test is used widely to estimate the amount of organic matter
oxidant (in this case, dichromate). When wastewater contains only readily
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available organic bacterial food and no toxic matter, the COD test results
than titrimetric method. For colorimetric method, the chromium (III) ion in
cooled. The excess chromium (III) ion shows how much chromic was use by
error that may result because of the presence of extraneous organic matter in
the reagents.
There are few results obtained from the experiment because the vials
stuck in the COD reactor that caused by unclean of vials surface. The result
of the titrimetric method and colorimetric method are different with the value
of 122 mg/L and 141mg/L. This difference may happen when titrate the
sample with FAS solution until it changes to red colour. In addition, it will be
a large difference in the result although the reading obtained from titration
has a difference about 0.1ml. The value of COD got from this experiment was
122mg/L and 141mg/L and under low range of COD (<150mg/L). Based on
Environment, the COD values above the 100mg/L are class V and useless for
9 ADVANCED QUESTIONS
1. What will happen to the COD value if HgSO4 is not added?
Chlorine will not be separated out of the sample effluent and the value of
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The purpose of running a blank is to compensate for any error that may
reagents.
4. Summarize the method and write the chemical reactions involved and
following day. Describe two ways by which the sample can be preserved.
keeping samples in ice. Keeping samples in ice until they are submitted to
the laboratory will preserve them well enough for most tests. It is
necessary to preserve the sample because it can retard the chemical and
10 CONCLUSION
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Chemical oxygen demand (COD) is used as a measure of oxygen
oxidant. The COD value for sample in this experiment under low range and it
water sample has high organic matter. Lastly, COD is the total measurement of
The vial must be cleaned and removed all tags on the vials surface
before putting in to the COD reactor and the tags should be putting on the
cap of vial. This should be considered a precaution during carry out the
experiment. The parallax error should be avoided when taking the reading of
the burette.
12 REFERENCES
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Prepared by/Disediakan oleh : Approved by/Disahkan oleh :
Signature/Tandatangan : Signature/Tandatangan :
Name/Nama : DR. NOR HASLINA HASHIM Name/Nama : DR. SURAYA HANI ADNAN
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