IV.

DESIGN AND METHODOLOGY

Apparatus washing
and drying

Preparation
of water
sample and
digestion

Data
gathering with
colorimeter

Clean up

In the experiment, the Chemical Oxygen Demand (COD) of the water sample was determined
under specific conditions of oxidizing agent, temperature, and, time via colorimetric method.
Apparatus washing and drying
The researchers checked borrowed the apparatuses needed for the experiment from the
laboratory custodian, Sir Francisco Pascua. The apparatus used for the experiment such as the
beaker and stirring rod were rinsed with distilled water then wiped with clean dry cloth;
however, the pipette used for drawing out the water sample was hung upside down to let the
water drip out of its opening. The digester vessels were washed with an acid solution to prevent
contamination.
Preparation of water sample and desiccation
Standard potassium dichromate digestion solution
4.903 grams of potassium dichromate was dried at 150C for two hours. The dried
potassium dichromate was diluted to 500 mL distilled water. To the solution, 167 mL of
concentrated H2SO4 was added followed by 33.3 grams of HgSO4. The mixture was thoroughly
stirred then cooled to room temperature. After cooling, the solution was diluted to 1000 mL.
Sulfuric acid reagent
Ag2SO4 was added to a concentrated H2SO4 solution at a rate of 5.5 g Ag2SO4/kg
H2SO4. The mixture was left to stand for a day or two until Ag2SO4 has dissolved into the sulfuric
acid. The mixture was mixed thoroughly.
A volume of the mixture of the sulfuric acid reagent and standard potassium dichromate
digestion solution was poured into two digester vessels and the vessels left on a test tube rack.

The digester was preheated to 150C and a plastic shield was placed in front of the
digester. The 500 mL beaker was filled with the water sample up to its mark and the water
sample was stirred for 2 continuous minutes with a stirring rod. From the homogenized water
sample solution, 2 mL was drawn with the use of a pipette and the 2 mL was poured into a
digester vessel. The cap of the vessel was closed tightly and the outside of the vessel was wiped
with a clean paper towel. The cap of the vial was held then inverted several times until the
contents were thoroughly mixed. The digester vessel was placed back into the test tube rack. The
second digester bottle was also added with 2 mL of the water sample drawn out from the
homogenized water sample in the 500 mL beaker. The digester vial was tightly capped and its
outside surface wiped off with a clean paper towel then inverted. Both digester vessel were put
inside the digester and heated for two hours. After two hours, the digester was powered off and
the vials left to cool for about 30 minutes. After cooling, a vessel was taken out of the digester
and inverted a few times before placing it on a rack for further cooling. The second vessel was
taken out of the digester and inverted then placed beside the first vessel on the tube rack.
Data gathering with colorimeter
The COD of the water sample was measured with a colorimeter. The colorimeter was first
calibrated before any measuring was done. The calibration of the colorimeter was done by
placing the vial of the calibrating liquid into the sample compartment afterwhich the cover was
placed over the colorimeter. The zero switch was pressed until the screen showed zero reading.
Next, the colorimeter was uncovered and the vial with calibrating liquid was replaced with the
first vial filled with the water sample and the sulfuric acid reagent. The read button was pressed
and the result shown in the screen was recorded.
The colorimeter was again calibrated with the calibrating liquid after removing the first
vessel with the sample. After calibrating, the second digester vessel was placed in the colorimeter
and the COD level was read and recorded.
Clean up
The contents of the digester vessel were disposed properly and the apparatus used were
washed with soap and water then rinsed again with distilled water. The digester was check to be
powered off and its socket unplugged. The colorimeter was put box into its box and the table
countertop wiped with a dry cloth.
Computation
The obtained value of COD from the colorimeter was taken as an average value using the
equation below and the mean value of COD was used to interpret the result of the study.
EQUATION EQUATION EQUATION