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1.1COD Method

This document provides instructions for determining chemical oxygen demand (COD) using the closed reflux titrimetric method. COD is a measure of the amount of organic compounds in a sample that can be oxidized by a strong chemical oxidant. The method involves adding a sample to a vial with potassium dichromate and sulfuric acid, heating to digest organic compounds, then titrating the digested solution with ferrous ammonium sulfate and measuring the amount needed to reach the endpoint color change. By comparing the titrant volume used for samples versus a blank, and making calculations using the titrant molarity, the COD level of the original sample in mg O2/L can be determined. This provides a quantitative

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38 views2 pages

1.1COD Method

This document provides instructions for determining chemical oxygen demand (COD) using the closed reflux titrimetric method. COD is a measure of the amount of organic compounds in a sample that can be oxidized by a strong chemical oxidant. The method involves adding a sample to a vial with potassium dichromate and sulfuric acid, heating to digest organic compounds, then titrating the digested solution with ferrous ammonium sulfate and measuring the amount needed to reach the endpoint color change. By comparing the titrant volume used for samples versus a blank, and making calculations using the titrant molarity, the COD level of the original sample in mg O2/L can be determined. This provides a quantitative

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UNIVERSITI PUTRA MALAYSIA (UPM)

FACULTY OF ENGINEERING
DEPARTMENT OF CIVIL ENGINEERING
WATER AND ENVIRONMENTAL ENGINEERING UNIT

WATER AND WASTEWATER ENGINEERING (ECV 3405)

Chemical Oxygen Demand (COD)

Introduction:

Chemical oxygen demand (COD) is used as a measure of oxygen requirement of a sample that is susceptible to
oxidation by strong chemical oxidant. The dichromate reflux method is preferred over procedures using other
oxidants (e.g. potassium permanganate) because of its superior oxidizing ability, applicability to a wide variety
of samples and ease of manipulation. Oxidation of most organic compounds is 95-100% of the theoretical
value. In this laboratory, closed reflux method is used. This method is more economical in the use of metallic
salt reagents, but required homogenization of samples containing suspended solid to obtain reproducible result.

Objective: i) To determine the COD level of the samples given using Closed Reflux Titrimetric
Method.

Apparatus: 1. 10 ml vial
2. COD reactor
3. Measuring cylinder
4. Beaker
5. Pipette
6. Burette with retort stand

Preparation of reagent and solutions:

1. Sulfuric acid Reagent

Add Ag2SO4 reagent or technical crystal powder, to conc. H2SO4 at the rate 5.5g Ag2SO4/ kg H2SO4.
Let stand 1 to 2d to dissolve. Mix.

2. Ferrous ammonium sulfate (FAS) titrant, 0.10M

Dissolved 39.2g Fe (NH4)2(SO4)2.6H2O in distilled water. Add 20mL conc. H2SO4, cool and dilute to
1000mL

3. Ferroin indicator

Readily purchased

4. Potassium dichromate (K2Cr2O7) digestion solution, 0.01667M

Add to about 500ml distilled water, 4.903 g K2Cr2O7, primary standard grade, previously dried at
150°C for 2h, 167 mL conc H2SO4 and 33.3 g HgSO4. Dissolve, cool to room temperature, and dilute to
1000mL

Methodology:

A. Sample and reagent preparation

1. Rinse vials and caps with 20% H2SO4 before use.


1. Prepare 3 vials for each sample and additional 3 vials for blank.
2. Into each vial, firstly pipette 2.5 ml sample respectively and for the blank, replace 2.5 ml sample with
2.5 ml distilled water. Dilute samples few times if necessary.
3. Secondly, pipette 1.5 ml of K2Cr2O7 into each vial and mix gently.
4. Thirdly, pipette 3.5 ml H2SO4 reagent into each vial. Cap the vial and tighten the cap. Mix gently.
The vial will be hot after the reagents mixed together.
5. Place the vials in the COD reactor at 150oC for 2 hours.
6. After 2 hours (digestion complete), take the vials out and cool to room temperature.

B. Titration

1. Transfer sample carefully from the vial into 50 or 100 ml beaker.


2. Add 1 – 2 drops of ferroin indicator into the beaker. Mix gently.
3. Titrate the sample in the beaker with FAS titrant until the color change from yellow to reddish-brown
(end-point).
4. Record the volume of FAS titrant used for each titration.

Calculation:

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


ml sample

where A = ml FAS used for blank


B = ml FAS used for sample
M = molarity of FAS = 0.1 M

Results:
Refer slide for further instruction

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