Standard Operating Procedure (SOP) for The Effectiveness of Palm Oil Mill Effluent

(POME) Treatment Using Cockle Shell and Coconut Shell Activated Carbon as an
Adsorbent.

Purpose: This study aims to assess the effectiveness of combining Cockle Shell and Coconut
Shell Activated Carbon in treating POME. The objectives of the study are as follows:

i) To characterize Cockle Shell and Coconut Shell Activated Carbon.

ii) To determine the optimal dosage of the Cockle Shell and Coconut Shell Activated Carbon
combination for removing Suspended Solids (SS), Color, Biological Oxygen Demand (BOD),
and Chemical Oxygen Demand (COD).

iii) To ascertain the optimal conditions for parameter removal, including pH value, adsorbent
dosage, and contact time for Cockle Shell and Coconut Shell Activated Carbon.

Scope: This study involves the preparation and evaluation of mixed media for the removal of
Suspended Solids (SS), Color, Biological Oxygen Demand (BOD), and Chemical Oxygen
Demand (COD) from POME. The investigation is limited to samples of POME collected from
palm oil mill industries. Two different materials, namely Cockle Shell and Coconut Shell
Activated Carbon, will be utilized. The focus will be on determining the optimal environmental
parameters, including pH, adsorbent dosage, and contact time.
Analytical method

Chemical Oxygen Demand (COD)

APPARATUS

1. Tube rack
2. Culture tube with cap
3. Reflux apparatus which is Erlenmeyer flask
4. Condenser and hot plate
5. Magnetic stirrer
6. Burette
7. Burette stand
8. White porcelain evaporating dish

REAGENTS

9. Standard potassium dichromate solution (K₂Cr₂O₇)

10. Sulfuric acid reagent (H₂SO₄)
11. Ferroin indicator solution
12. Standard ferrous ammonium sulfate (FAS)
13. Mercuric sulfate (HgSO₄).

PROCEDURE

For reactor digestion procedure

1. 100mL of sample was poured in a blender and blended for 30 seconds or until
homogenized. (For samples with a large number of solids, increase the homogenization
time. If the sample does not contain suspended solids, skip the next step.)
2. The homogenized sample was poured into a 250mL beaker and stirred with a magnetic
stir plate.
3. (Sample preparation) the cap was removed from a vial for the selected range. Hold the
vial at an angle of 45 degrees. a clean pipette was used to add 2.00 mL of sample to the
vial. For 250–15,000 mg/L vials and a TenSette Pipet was used to add 0.20 mL of
sample to the vial.
 4. (blank preparation) the cap was removed from a second vial for the selected range. Hold
the vial at an angle of 45 degrees. Use a clean pipet to add 2.00 mL of deionized water
to the vial. For 250–15,000 mg/L vials and a TenSette Pipet was used to add 0.20 mL
of deionized water to the vial.
5. The vials were closed tightly, rinsed with water and wiped with a clean paper towel.
6. The vials should be held by the cap, over a sink, and inverted gently several times to
mix. The vials get very hot during mixing.
7. The vials were inserted into the preheated DRB200 reactor and the lid was closed. The
vials were heated for 2 hours. After that, set the reactor power to off and let the vials
cool in the reactor for approximately 20 minutes to 120 degrees or less. Then, each vial
should be inverted several times while it is still warm.
8. The vials were placed in a tube rack to cool to room temperature.

For colorimetric procedure

1. The blank sample cell needs to be cleaned.

2. The blank was inserted into the cell holder.
3. Press ZERO, the display shows 0 or 0.0mg/L COD.
4. Clean the prepared sample cell.
5. The prepared sample was inserted into the cell holder and press READ and write down
the results in mg/L COD. If using High Range Plus COD digestion reagent vials,
multiply the result by 10. For the most accurate results with samples near 1500 or
15,000 mg/L COD
6. Repeat the analysis with a diluted sample.
Biochemical Oxygen Demand (BOD)

APPARATUS

1. DO meter,
2. 300 mL BOD bottles,
3. Incubator that capable of maintaining 20 +/- 1°C
4. 250 ml graduated cylinders
5. 100 ml graduated cylinders
6. 25 ml measuring pipettes
7. 10 ml measuring pipettes
8. 100 ml beaker
9. 1000 ml beaker
10. 250 ml Erlenmeyer flask
11. burette graduated to 0.1 ml
12. dilution water bottle
13. pipette bulb equipment for pH measurements
14. magnetic stirrer
PROCEDURE

1. The sample water was filled 300mL in BOD bottles to be tested or dilution whether
distilled or
2. deionized water and various amounts of the wastewater sample are added to reflect
different dilutions.

3. One of the bottles was filled only with dilution water as a control of DO meter, which
4. used to measure the initial dissolved oxygen concentration (mg/L) in each bottle, at
least 8.0mg/L.
5. Each bottle was placed into a dark incubator at 20°C for five days.
6. Final dissolved oxygen concentration (mg/L) was measured after five days (± 3 hours)
by using the DO meter, which ideally will be a reduction of at least 4.0 mg/L.
7. The final DO reading then subtracted from the initial DO reading and the result is the
BOD concentration (mg/L).
8. If the wastewater sample requires dilution, the BOD concentration reading is multiplied
by the dilution factor.
Dissolved Oxygen (DO)

APPARATUS

1. Dissolved oxygen probe meter

2. distilled water
3. 250 ml beaker
4. water sample

PROCEDURE

1. Switch on the probe meter and rinse with distilled water.

2. Pour 100 ml water sample in a beaker.
3. Soak the DO probe in the first water sample and wait until the meter shows the reading.
4. To ensure a constant flow of water across the membrane, the probe was gently stirred
in the water sample.
5. Record the reading.
6. Then repeat the same procedure, starting with a rinse probe using distilled water.
Acidic and Alkaline (pH)

APPARATUS

1. pH meter
2. pH electrodes
3. distilled water
4. 250 ml beaker

PROCEDURE

1. Allow the temperature of the sample to equilibrate to room temperature.

2. Fill the disposable cap or beaker with an aliquot of the sample. As soon as the electrode
emerges from the sample, the depth of the sample should cover the junction spot on the
electrode.
3. The electrode should be placed into the sample and stirred gently with a magnetic stirrer
and stirring bar or by hand.
4. Record the reading.
5. Wipe excess water off the electrode using a kimwipe after rinsing with DI water.
6. As in step 5, rinse and blot dry the electrode after measuring the samples.
7. The electrode should be stored in the electrode storage solution until it is next used. In
the case of electrode storage solutions, they are either “pH electrode storage solutions”
or buffer solutions with a pH of 7.00.
Total Suspended Solid (TSS)

APPARATUS

1. Evaporating dish
2. Oven
3. Dessicator
4. 5 cm diameter of porcelain crucible
5. 100ml measuring cylinder
6. 10 ml pipette
7. Steam bath which was preheated at 100°C
8. Buchner flask and funnel
9. 12.5 cm glass fiber filter disk
10. Analytical balance

PROCEDURE

1. Drying the filter paper in the oven for 15 minutes was followed by cooling it in a
desiccator and weighing the sample.
2. Using gentle suction, 10 mL of water sample was pipetted onto the center of the filter
disk in a Buchner flask.
3. After thoroughly shaking the sample, 10 ml were pipetted into the filter using a
volumetric pipette.
4. The filter paper was dried for at least one hour at temperatures ranging from 103 to
105degrees Celsius.
5. After removing the filter paper, it was placed in a desiccator to cool. We weighed the
sample after it had cooled to the suitable temperature. Every piece of data was
thoroughly documented.