Cod
Cod
Cod
1.0 INTRODUCTION
The COD (Chemical Oxygen Demand) test is commonly used to indirectly measure
the amount of organic compound in water. Most applications of COD determine the
amount of organic pollutants found in surface water like lakes and rivers. COD also
represents the amount of chemically digestible organics (food). COD measures all
organics that were biochemically digestible as well as all the organics that can be digested
by heat and sulfuric acid. It is used in the same applications as BOD. COD has the
advantage over BOD in that the analysis can be completed within a few hours whereas
BOD requires 5 days. The major drawback of the COD test is the presence of hazardous
chemicals and toxic waste disposal.
2.0 OBJECTIVE
To measure the effectiveness of waste water sample (usually industrial waste water)
through the oxidation and reduction reaction
Ferrous ion reacts with dichromate ion as in Eqn. 2. The oxidation process ended with
dichromate reduction:
O2 + 4e + 4H+ = 2H2O
5.0 PROCEDURES
1. The substances must be added in Erlenmeyer flask following the sequences below:
a. Erlenmeyer flask no. 1 : 10 mL of asid asetic (C2H5COOH) sample.
Erlenmeyer flask no. 2 : 10 mL distilled water as a blank.
b. Placed in beaker 1 and 2 with:
i. 3 glass boiling beads – act as a antibumping
ii. HgSO4– 0.4g
iii. 0.0417M K2Cr2O7 – 10 mL
iv. Acid sulphuric reagent H2SO4 (contain Ag2SO4)- 30 mL
Laboratory 1: CHEMICAL OXYGEN DEMAND(COD) 2013
c. The beaker is placed at the fume hood. H2SO4 is added slowly. Mixing to
avoid possible loss of volatile materials. Continued swirling and mixing while
adding sulphuric acid reagent.
CAUTION: Mix reflux mixture thoroughly before applying heat to prevent local
heating of flask bottom and a possible blowout of flask contents.
2. Flask is attached to condenser and turn on cooling water. Open end of condenser is
covered with a small beaker to prevent foreign material from entering refluxing
mixture and reflux for 2 hours. At a meantime, please proceed to procedure no. 6.
3. After 2 hours, cool wash down the condenser with distilled water. Continue cooling
the condenser to room temperature.
4. Reflux condenser is disconnected. The solution is transferred to the cone flask and the
mixture is diluted up to 150 mL with distilled water. Added with 3 drops of ferroin
indicator. Place the magnetic bars and stir it with magnetic stirrer.
5. Titrate K2Cr2O7 with ferrous ammonium sulphate (FAS). First and last reading should
be jot down in Table 2. Take as the end point of the titration the first sharp colour
change to blue-green. Stop titration, add 3 drops of ferroin indicator. Continue
titration until the colour change to reddish brown that persists for 1 minute or longer.
Stop titration and jot down the last reading in Table 2. Take a precaution that the end
point colour changes of titration is fast. Calculate the volume of FAS used in titration
in Table 2.
6. Preparation of Standard ferrous ammonium sulfate (FAS) titrant as follows:
a. Dilute 10 mL K2Cr2O7 standard (0.0417 M) to about 100 mL with adding 90
mL distilled water in the cone flask 250 mL. Swirl and mix slowly.
b. Slowly and carefully add 30 mL conc H2SO4 and cool. Refer to Figure 1,
titrate with the FAS titrant using 3 drops of ferroin indicator. First and last
reading should be jot down in Table 1.
c. Take as the end point of the titration the first sharp colour change to blue-
green. Stop titration, add 3 drops of ferroin indicator. Continue titration until
the colour change to reddish brown that persists for 1 minute or longer.
d. Take a precaution that the end point colour changes of titration is fast. Jotted
down the volume of FAS used in titration in Table 1.
Laboratory 1: CHEMICAL OXYGEN DEMAND(COD) 2013
Fill the both of the Erlenmeyer cones with distill water up to 150 mL.
Laboratory 1: CHEMICAL OXYGEN DEMAND(COD) 2013
= 0.248
.
Range of normality of FAS is 0.23 < (N) < 0.27
Hence, the result is 0.248 so it is included in the range, 0.23 < 0.248 < 0.27.
Reading of burette / pipette (A ) Cone flask 1 (Sample) (B) Cone flask 2 (Blank)
First Reading 18.1mL 7.5mL
Last Reading 27.9mL 17.6mL
Volume of FAS standard (mL) 9.8mL 10.1mL
(B – A) X NFAS X 8000
COD as mg O2/L =
mL sample
Where:
Notes: The 8000 multiplier is to express the results in units of milligrams per liter of oxygen
since 1 liter contains 1000 mL and the equivalent weight of oxygen is 6.
= 60.734mg/L