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1.

0 INTRODUCTION

COD or Chemical Oxygen Demand is the total measurement of all chemicals in


the water that can be oxidized. COD is used as a measurement of pollutants in
natural and waste waters to assess the strength of discharged waste such as
sewage and industrial effluent waters. It is normally measured in both municipal
and industrial wastewater treatment plants and gives an indication of the
efficiency of the treatment process. The dichromate reflux method is preferred
over procedures using other oxidants because of superior oxidizing ability,
applicability to a with wide variety of samples, and ease of manipulation.
Oxidation of most organic compounds is 95-100% the theoretical value.

Most types of organic matter are oxidized by a boiling mixture of chromic and
sulfuric acids. A sample is refluxed in strongly acid solutions with a known
excess of potassium dichromate (K2Cr2O7). After dilution the remaining
unreduced K2Cr2O7 is titrated with ferrous ammonium sulphate to determine the
amount of K2Cr2O7 consumed and oxidizable organic matter is calculated in
terms of oxygen equivalent. Keep ratios of reagent weights, volumes and
strengths constant when sample volumes other than 50 ml are used. The standard
2 hours reflux time may be reduced if it has been shown that a shorter period
yields the same results

2.0 EQUIPMENT

a. COD Reflux System – consisting Erlenmeyer flask (250 mL or 500 mL) with
ground glass 24/40 neck and 300-mm jacket Liebig West, or equivalent condenser
with 24/40 ground-glass joint, and a hot plate having sufficient power to produce
at least 1.4 W/cm2 of heating surface.
b. Burette
c. Pipette
d. Glass beads
e. Magnetic stirrer bars
f. Chemical required : - Standard potassium dichromate (K2Cr2O7) 0.04167N
-Sulfuric acid (H2SO4)
-Ferrous ammonium sulfate (FAS)
-[Fe(NH4)2(SO4)2
-Ferro in indicator (ferrous ammonium sulfate)
-Dilution water

2.1 REAGENT
a. Standard potassium dichromate (K2C2O7) solution (0.04167 M) : (Prepare
By the technician; dissolve 12.259 g K2Cr2O7, primary standard grade,
previously dried at 150°C for 2 hours in distilled water and dilute to 1000
mL). Notes: This reagent undergoes a six-electron reduction reaction; the
equivalent concentration is 6 X 0.04167M or 0.2500N.
b. Mercuric sulfate (Hg SO4)
c. Sulfuric acid reagent: (Prepare by the technician: Add Ag2SO4, reagent or
technical grade, crystals or powder, to concentration H2SO4 at the rate of
5.5 g Ag2SO4 /kg H2 SO4. Mix) phenanthroline monohydrate and 695 mg
FeSO4·7H2O in distilled water and dilute to 100 mL. This indicator solution
may be purchased already prepared).
b.Standard ferrous ammonium sulfate or FAS (Fe (NH4)2(SO4)2 solution
(0.25 M) titrant.
3.0 PROCEDURE

3.1 FAS Test


a. Measured 10 mL of standard potassium dichromate, 30 mL of sulfuric
acid and 20 mL of diluted water and add them together in refluxing flask.
b. Make sure added the solution in the fume chamber.

c. The solution must be cooled first with the flow water before continue the
experiment.
d. Added the solution with 3 drops of Ferro in indicator.

e. Put magnetic stirrer into the refluxing flask and the solution was swirled
slowly while adding ferrous ammonium into the solution until the
solution changed to light green color.

c.Added some 3 drops of the Ferro in indicator again into solution and stir
again the solution with ferrous ammonium until the solution became
reddish brick.
d. Take the initial and final reading at the burette.
3.2 Reflux Test
a. Measured 20 mL of sample, 10mL standard potassium dichromate, 30
mL of sulfuric acid and add them together in refluxing flask.
b. Make sure added the solution in the fume chamber.
c. Heat the solution in 1 hour.

d. Cooled the solution in room temperature.


e. Rinsed the condenser with dilution water.
f. Added the dilution water into refluxing flask until at 150mL.
e. Added the solution with 2 to 3 drops of Ferro in indicator.
f. Put magnetic stirrer into the refluxing flask and the solution was
swirled slowly while adding ferrous ammonium into the solution until the
solution changed to light green color.
g. Added some 3 drops of the Ferro in indicator again into solution and
stir again the solution with ferrous ammonium until the solution
became reddish brick.

h. Take the initial and final reading at the burette.

4.0 DATA AND CALCULATION

FAS Result

Reading of Cone Flask


Burette (standard)
First Reading 0
Last Reading 10.5
Volume of FAS 10.5
standard (mL)

Table 1: FAS standard titration data


Volume of FAS standard (mL) = 10.5 – 0
= 10.5 mL
Compute the molarity for the FAS standard using formula:

10 mL

= 0.23 < N < 0.28 …ok!!

Reflux Result

Sample (Cone Flask B) Blank (Cone Flask A)

DATA: DATA :

First Reading 11.0 First Reading 20.0


Last Reading 20.8 Last Reading 30.0
Volume Reading 9.8 Volume Reading 10.0

CALCULATION : CALCULATION :
B = 9.8 A = 10.0

Table 2: Sample and Blank titration data

COD CALCULATION:

= 38.1 mg/l

DISCUSSION

1. What is the purpose of using blank sample in the experiment?

a. The main reason for using the blank sample is to control the volume of
organic material in the sample. COD was carried out to measure the
oxygen demand of organic compounds in a sample of water, and we have
to ensure there were no accidentally outside organic materials added to the
sample to be measured. A blank sample is created by adding the reagents
to a volume of distilled water. Both water and blank sample will be
compared. The oxygen demand for the blank sample is subtracted from the
COD for the original sample to ensure the true measurement of organic
matter.

2. What is the objective of COD test and what is the different between COD and
BOD test
a. Chemical oxygen demand (COD) is an indicative measure of the amount
of oxygen that can be consumed by reactions in a measured solution. COD
is the amount of oxygen required to chemically breakdown the pollutants
whereas BOD is the amount of oxygen required to do this biologically
through micro-organisms. There is a strong correlation between COD and
BOD; however COD analysis is a much faster and more accurate method.

3. Why the COD’s value needs to be monitor for the polluted surface water such as
in lakes and rivers as well as for wastewater.

a. Chemical Oxygen Demand is an important water quality parameter


because, similar to BOD, it provides an index to assess the effect
discharged wastewater will have on the receiving environment. Higher
COD levels mean a greater amount of oxidizable organic material in the
sample, which will reduce dissolved oxygen (DO) levels. A reduction in
DO can lead to anaerobic conditions, which is deleterious to higher
aquatic life forms. The COD test is often used as an alternate to BOD due
to shorter length of testing time.

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.

a. As with COD, the use of an oxidizing agent and acidic conditions is


designed to accelerate the chemical and microbial oxidation of organic
material that occurs in natural waters. It cannot be used as a definitive
measure of theoretical oxygen demand or the total organic content as
many compounds are only partially oxidized during the test and therefore
the full COD test is preferable where possible. Permanganate values can
be used directly to quantify water quality or can be converted to provide
an estimate of the COD, BOD or TOC values.

5. Why the value of COD increase when the amount of pollutant increased in
surface water.

a. the chemical oxygen demand (COD) test is commonly used to indirectly


measure the amount of organic compounds in water. Most applications of
COD determine the amount of organic pollutants found in surface water
(e.g. lakes and rivers) or wastewater, making COD a useful measure of
water quality. It is expressed in milligrams per liter (mg/L) also referred to
as ppm (parts per million), which indicates the mass of oxygen consumed
per liter of solution.

6. Explain briefly the steps of COD measurement that you should follow during this
experiment.
FAS Test

a. Make sure added the solution in the fume chamber


b. The solution must be cooled first with the flow water before continue the
experiment
c. Added the solution with 3 drops of Ferro in indicator
d. Put magnetic stirrer into the refluxing flask and the solution was swirled
slowly while adding ferrous ammonium into the solution until the solution
changed to light green color
e. Added some 3 drops of the Ferro in indicator again into solution and stir
again the solution with ferrous ammonium until the solution became
reddish brick
f. Take the initial and final reading at the burette

Reflux Test

a. Make sure added the solution in the fume chamber.


b. Heat the solution in 1 hour
c. Cooled the solution in room temperature.
d. Rinsed the condenser with dilution water.
e. Added the dilution water into refluxing flask until at 150mL.
i. Added the solution with 2 to 3 drops of Ferro in indicator.
j. Put magnetic stirrer into the refluxing flask and the solution was
swirled slowly while adding ferrous ammonium into the solution until the
solution changed to light green color
k. Added some 3 drops of the Ferro in indicator again into solution and
stir again the solution with ferrous ammonium until the solution became
reddish brick
l. Take the initial and final reading at the burette

7. Briefly explain whether the value of COD obtain in this experiment are suitable to
be discharged to the stream.

a. As a conclusion, from the value of COD is 38.1 mg/L that we get from the
experiment was successful because the value of normality of FAS (n) is
0.238 was in the range that required
APPENDIX

REFERENCES

Hammer, MarkJ. (2001)”Water and Waste water Technology Fourth Edition” New
Terzey: Prentice Hall

Master, Gelbert M (1998) “ Introduction to Environmental Engineering and Science”


New Terzey : Prentice Hall

Davis Cornwell (2008) “Introduction to Environmental Engineering” Fourth Edition,


New York:Mc Graw Hill

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