CHAPTER 3

RESEARCH METHODOLOGY

3.1

Preparation of Poly aluminium chloride

The PAC will be prepared in laboratory by the slow base injection method. PAC

with OH/Al molar ratio (B) of 2.5 will be prepared in the laboratory at room
temperature by slow base injection. The procedure of the preparation of PAC is as
follows: 80 mL of 0.5 M AlCl3 solution will be titrated with 200 mL 0.5 M NaOH at a
rate of 0.5 mL/min. Please be noted that the concentration will be varied as follows; 0.5
M, 1.0 M, 1.5 M and 2.0 M. The method will allow the slow addition of base (NaOH)
into the AlCl3 solution via peristaltic pump. The mixture will be stirred continuously in
a mixer until no bubbles are formed and a clear solution should be obtained.

3.2

Sampling and Preservation of POME

Wastewater that will be used in this study is biologically treated POME obtained

from a palm oil mill industry in Kulai, Johor. For BOD determination, the sample must
be kept in a plastic or glass (preferably amber glass). Typical volume suggested during
sampling is 500mL. The container should be filled to exclude air. The transportation of
the sample is under ice, away from light. The maximum hold time is suggested 48
hours, but preferable to be analysed as soon as possible. Otherwise, refrigerate in the
dark (<6C) [16]. For COD determination, the containers suggested are of glass,
polytetrafluoroethylene (PTFE) or polyethylene. The typical volume during sampling is

100 mL with the container filled completely to exclude air. The sample must be
transported under ice and away from light. The sample is preferable to be analysed as
soon as possible. Otherwise, it needs to be preserved under acidic condition (pH <2)
with sulfuric acid or it can be frozen if polyethylene containers are used. The maximum
holding time for COD sample is 28 days. The storage of the sample should be done
under <6C in the dark. For both BOD and COD samples, glass containers are preferred
if the value is less than 5 mg/L [16].

3.3

Characterization of POME (COD, BOD, oil and grease)

In the determination of COD, the sample will be digested for two hours with

strong oxidizing agent, potassium dichromate. Prior to digestion, sulfuric acid reagent
(containing silver) and mercury sulfate are added, as catalyst and to complex chloride
interferences, respectively. Dilution of samples might be needed if the sample turns
green with the addition of sulfuric acid. The digested sample will then be analyzed using
HACH DR/4000.
For the determination of BOD, it is best to carry out as soon as possible after the
collection of the sample. The collected samples will be diluted with dilution water and
incubated for 5 days at 20C under dark condition. The dissolved oxygen will be
measured at initial and final days of incubation.
The oil and grease determination is carried out by rotary evaporation. The sample
will be extracted with organic solvent (hexane). It will be then analyzed fro the oil and
grease content via rotary evaporation.

3.4

Jar Tests

The optimization of the parameters including pH, coagulant dosage and PAC
speciation will be carried out using the jar tests. The jar tests will be carried as follows:
250 ml of wastewater (sample) will be transferred into a 1 L beaker. The temperature,
pH, turbidity and alkalinity of the sample must be recorded before the tests begin. Dose
each beaker with different amount of coagulant and stir at 160 rpm for 2 minutes.
Flocculation will be promoted at 40 rpm for 15 minutes. The mixture will be left to
settle for 30 minutes before being analysed for COD value and turbidity. Adjustment on
the pH of the coagulation will be done with the addition of either 1 M H 2SO4 or 1 M
NaOH prior to the addition of coagulant.

3.5

Speciation of PAC
Ferron assay will be used to determine the speciation of PAC. The determination

involves the following procedure: 20 L of Al solutions and 5.5 mL ferron colorimetric

solutions will be transferred into a 25 mL volumetric flask and will be diluted with
deionized distilled water to mark. The absorbance of the mixture will measured at
wavelength 370 nm immediately. The specified time of reaction will indicate the types
of Al species formed (monomeric Ala, polymeric Alb and colloidal Alc).
The ferron solutions will be prepared from three solutions, namely Reagent A,
Reagent B and Reagent C. Reagent A (0.2 % w/v) will be prepared by dissolving 2 g of
ferron (8-iodo-7-hydroxyquinoline-5-sulfonic acid) into 1000 mL of pre-boiled
deionized distilled water to ensure the absence of dissolved CO2. Reagent B (20 % w/v)
will be prepared by dissolving 200 g of sodium acetate (NaAc) into 1000 mL of
deionized distilled water. Reagent C (1:9, v/v) will be made up of 100 mL 37 % HCl in
900 mL deinoized distilled water [23].
3.6

Conceptual Framework

Literature Review
Project Write-up
Proposal Writing
Preparing PAC (slow base
injection method)

Aging of PAC (13 days)

PAC speciation
(ferron assay)

Preparing ferron
solutions (ferron,
NaAc, HCl, DDW)

Wastewater

Biologically treated
POME

Jar tests (coagualtion

performance)

BOD, COD, oil, grease

determination