DCC40172: Structure, Hydraulics and Water Quality Laboratory

CIVIL ENGINEERING DEPARTMENT

POLITEKNIK PORT DICKSON
Km 14, Jalan Pantai, 71050 Si Rusa, Port Dickson, Negeri Sembilan
Tel : 06-662 2000 / 2111 Faxs : 06-662 2026 / 2027

WATER QUALITY LABSHEET

EXPERIMENT 2 - CHEMICAL OXYGEN DEMAND (COD)
A. OBJECTIVES

1. To determine the chemical oxygen demand of the given wastewater samples.

B. THEORY

The chemical oxygen demand (COD) is the amount of oxygen consumed to completely chemically
oxidize the organic water constituents to inorganic end products. COD is an important, rapidly measured
variable for the approximate determination of the organic matter content of water samples. Some water
samples may contain substances that are difficult to oxidize. In these cases, because of incomplete
oxidation under the given test methods, COD values may be a poor measure of the theoretical oxygen
demand. It should also be noted that the significance of the COD value depends on the composition of
the water studied. 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 wide variety of samples, and ease of manipulation.
Oxidation of most organic compounds is 95 -100% the theoretical value.

C. APPARATUS & MATERIAL

1. 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.
2. Burette.
3. Pipette
4. COD vial
5. Reagent;
i) Standard potassium dichromate 0.016667 M
 1000ml distilled water
 4.903 g potassium dichromate (K2 Cr2 O7) dry 2 hours 150o C
 167 mL acid sulphuric (H2 SO4)
 33.3 g mercury sulphate (Hg SO4)

ii) Sulphuric acid reagent

 5.5g silver sulphate (Ag SO4)
 1kg acid sulphuric (H2 SO4).

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iii) Standard ferrous ammonium sulphate

 39.2g ammonium iron II sulphate 6-Hydrate {Fe (NH4)2(SO4)2. 6H20}
 20mL acid sulphuric (H2 SO4)
 1L distilled water 0.) IV.

iv) Ferroin indicator

D. PROCEDURE

Sampling Procedure

1. The sample is collected in plastic container that is known no organic contamination in the container.
2. The sample is tested biologically.
3. Sample is preserved with sulphuric acid to a pH value < 2

Laboratory Procedures

1. The substances were added in COD vial by followed the sequences below;
a) Placed in COD vial 1 and 2 with;
 mL Potassium Dichromate Reagent
 mL Acid Sulphuric Reagent

b) COD vial no.1: 2.5 mL sample

COD vial no.2: 2.5 mL distilled water

2. Refluxing mixture placed at COD Reactor with temperature 1500C for 1 hour.
3. After 1 hour, cool down the condenser with distilled water. Cooling down process continued to room
temperature.
4. Disconnect reflux condenser. The solution transferred to the conical flask and mixed up with 150ml
distilled water. Added with 3 drops of ferroin indicator.
5. Titrated K2 Cr2 O7 with Ferrous Ammonium Sulfate (FAS). The initial and final reading recorded.
The titration stopped when colour changed into reddish brown.

Titration Test

1. 5mL Postassium Dichromate K2 Cr2 O7 solution (0.01667 M) diluted with 10 mL of distilled water
into 250 mL conical flask. Swirled and mixed slowly.
2. 30 mL of concentrated acid sulfuric H2SO4 was added slowly and carefully. Titrated with FAS titrant
using 3 drops of ferroin indicator. The titration is stopped immediately when the colour changed
into reddish brown.
3. Initial and final reading was recorded.

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 DCC40172: Structure, Hydraulics and Water Quality Laboratory

E. DATA / RESULTS

Table 1 - FAS standard titration data;

Reading of buret / pipette Cone flask (Standard)

First reading
Last reading
Volume of FAS (mL)

Compute the molarity of FAS by using the given formula;

𝑉𝑜𝑙𝑢𝑚𝑒 0.1667𝑀 𝐾2 𝐶𝑟2 𝑂7 𝑠𝑜𝑙𝑢𝑡𝑖𝑜𝑛 𝑡𝑖𝑡𝑟𝑎𝑡𝑒𝑑, 𝑚𝑙

𝑀𝑜𝑙𝑎𝑟𝑖𝑡𝑦 𝑜𝑓 𝐹𝐴𝑆 𝑠𝑜𝑙𝑢𝑡𝑖𝑜𝑛 = 𝑥 0.100
𝑉𝑜𝑙𝑢𝑚𝑒 𝐹𝐴𝑆 𝑢𝑠𝑒𝑑 𝑖𝑛 𝑡𝑖𝑡𝑟𝑎𝑡𝑖𝑜𝑛, 𝑚𝑙

Table 2 - COD test data collections;

Volume of FAS used

Normality of FAS Sample volume In the original In the blank
(𝑵) (𝒎𝑳) sample, B sample, A
(𝒎𝑳) (𝒎𝑳)

Compute the COD concentration in mg/L for the sample by using the given formula;

𝒎𝒈 (𝑨 − 𝑩) 𝒙 𝑴 𝒙 𝟖𝟎𝟎𝟎
𝑪𝑶𝑫 𝒂𝒔 =
𝑳 (𝒎𝑳) 𝒔𝒂𝒎𝒑𝒍𝒆

F. CALCULATION

G. DISCUSSION

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

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

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H. CONCLUSION

I. REFERENCES

J. APPENDIX

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