FACULTY OF APPLIED SCIENCES

B. Sc. (Hons.) ENVIRONMENTAL TECHNOLOGY

EVT577

WASTEWATER TECHNOLOGY

EXPERIMENT 3: CHEMICAL OXYGEN DEMAND (COD)

NAME STUDENT ID

NOR IFTIHA BINTI ABDUL AZIZ 2022991399

PREPARED FOR

DR. NURUL NADIAH BINTI MOHD FIRDAUS HUM

DATE OF LABORATORY

11th APRIL 2023

DATE OF SUBMISSION

18th APRIL 2023

TITLE

EXPERIMENT 3: CHEMICAL OXYGEN DEMANDS (COD)

OBJECTIVE

To determine the concentration of Chemical Oxygen Demand (COD) in the wastewater

sample.

INTRODUCTION

Chemical Oxygen Demand (COD) commonly used to determine the oxygen content and
needed in the water when it oxidized by a strong chemical oxidant. Besides that, there are two
methods in determination of COD which are Dichromate Reflux Method (Open Reflux) and
Reactor Digestion Method (Close Reflux). Potassium dichromate, K2Cr2O7 is used as oxidizing
agent in order to determine COD in the water or wastewater sample for this experiment. Then,
the another of oxidizing agent also can be as potassium permanganate, KMnO4. Dichromate
has been known because it can oxidize organic matter about 95% - 100%. The chemical
reaction is shown as below:

Figure 1: Chemical Reaction for Reflux Process.

The open reflux method is suitable for a wide range of wastes where a large sample size
is preferred. Due to a higher oxidizing ability dichromate reflux method is more suitable rather
than other procedures that using other oxidants whereas potassium permanganate. While,
closed reflux method is more economical in the use of metallic salt reagents and generate
smaller quantities of hazardous waste, but require homogenization of samples containing
suspended solids to obtain reproducible results. For this experiment, we only conduct the
method of open reflux for knowing the concentration of chemical oxygen demand.
PROCEDURE

Method I: Dichromate (Open Reflux)

1. 50 ml of wastewater sample was placed in refluxing flask. The blank was prepared
using 50 ml of deionised water.
2. 5 to 7 glass boiling beads was added.
3. 1 g of mercuric sulphate (HgSO4) and 5 ml of concentrated sulphuric acid-silver
sulphate solution was added and mixed until the HgSO4 was in solution.
4. 25 ml of 0.25 N potassium dichromate (K2Cr2O7) was accurately added and mixed.
5. An additional 70 ml of concentrated sulphuric acid-silver sulphate solution was added
while mixing.
6. After through mixing, the flask was attached to reflux condenser and heat was applied
for 2 hours.
7. A reagent blank containing 50 ml of deionized water was treated with the same
reagent. FAS solution was standardized while waiting 2 hours of digestion.
8. After 2 hours reflux, the apparatus was cooled to room temperature. The interior of the
condenser and the flask was washed down twice with approximately 25 ml portions of
distilled water.
9. 4 to 5 drops of Ferroin indicator and magnetic stirring bar was added.
10. The flasks were placed on a magnetic stirrer and was rapidly titrated with 0.1 N ferrous
aluminium sulphate to the first red-brown endpoint.
RESULTS

Sample Volume of titrant used (mL) COD (mg/L)

Blank 62.1

Standard 26.0 153.84

Wastewater 61.1

Table 1: The value of titrant used (mL) and COD (mg/L)

CALCULATIONS

(𝑚𝐿 𝐾2𝐶𝑟2𝑂7) (0.25)

Normality (N) = 𝑚𝐿 𝐹𝐴𝑆 𝑟𝑒𝑞𝑢𝑖𝑟𝑒𝑑

(100 𝑚𝐿) (0.25)

Normality (N) = 26 𝑚𝐿

= 0.9615 N

(𝑎−𝑏)(𝑁) ×8000
COD (mg/L) =
𝑆𝑎𝑚𝑝𝑙𝑒 𝑆𝑖𝑧𝑒 (𝑚𝐿)

Where, a = mL of FAS used for blank

b = mL of FAS used for sample

N = normality of FAS titrant

COD for wastewater sample:

(62.1 𝑚𝐿−61.1 𝑚𝐿) (0.9615 𝑁) ×8000

COD (mg/L) = 50 𝑚𝐿

= 153.84 mg/L
DISCUSSIONS

The Chemical Oxygen Demand (COD) test was used very widely to estimate the amount
organic matter in wastewater. It is a measurement of the oxygen similar of the materials
present in the wastewater that are subject to oxidation by a strong chemical oxidant. Other
than that, COD was used as a measurement of pollutants in natural and wastewater to access
the strength of discharged waste like sewage and industrial effluent waters. It was normally
measured in both municipal and industrial wastewater treatment plants and gives an indication
of the efficiency of the treatment process.

For this experiment which was open reflux, most types of organic matter were being
oxidized through a boiling mixture of chromic and sulphuric acids. A sample was refluxed in
strongly acid solution with a known excess of potassium dichromate, K2Cr2O7. The COD test
only takes 2 hours in order to obtain the results. Besides that, the FAS solution also was being
standardized by diluted standard potassium dichromate with distilled water, concentrated
sulphuric acid and titrate with FAS titrant. After 2 hours, the apparatus was cooled and 4 to 5
drops of Ferroin indicator was added. Last, flasks (samples and flask) were placed on
magnetic stirrer and titrated with 0.1 N ferrous ammonium sulphate until first red-brown
endpoint.

From the experiment, we get a value of normality of FAS which was 0.9615 N. From that
value, the COD reading (mg/L) could be obtained for wastewater sample whereas 153.84
mg/L. In this experiment, the concentration of COD value was higher for this wastewater
sample. According to the Classes in Malaysian Water Quality Index for Chemical Oxygen
Demand, this sample was at level V (> 100). It could be said, higher COD levels mean a
greater amount of oxidizable organic material in the sample, which will reduce dissolved
oxygen (DO) levels. Mostly, a reduction in DO could lead to anaerobic conditions and can
affect the aquatic life forms.

Table 2: Classes in Malaysian Water Quality Index for Chemical Oxygen Demand
 There were some errors and precautions that should be alert in this experiment. Firstly,
the wastewater sample was not shaken properly before run the experiment. Hence, the
samples sometimes were not being cooled enough, so this would affect our result. The titration
process was not conduct in the right way might contamination the data also. Moreover, for
precautions, the wastewater sample and the other reagents in the bottle should be shaken
first before pipette. Next, during reflux process we must be more careful in order to avoid any
injuries. Lastly, all of us must wear the lab coat and gloves especially when handling any of
acid solution.

CONCLUSION

In the conclusion, it could be said that the concentration of chemical oxygen demand
(COD) was successfully achieved. The normality of FAS have obtained to be 0.9615 N and
from FAS, the calculation of COD could make to get the result for sample. From the calculation
of open reflux method, were obtain 153.84 mg/L for COD value.

REFERENCES

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What is chemical oxygen demand (COD)? (2021, December 15). Scientific and Medical
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