CHAPTER 3

RESEARCH METHODOLOGY

The research regarding biodiesel production using in situ

transesterification will apply subsequent process available to purify the

yield obtained from rubber seeds. Concomitantly, three variables will be

study in order to facilitate the procedure of optimizing the biodiesel yield.

3. 1 Location of Study

Laboratory of Faculty of Chemical Engineering, University of Technology

Mara Shah Alam

3.2 Material

The rubber seeds are obtained from rubber plantation of Malaysia Rubber
Board

3.3 Chemical

Potassium hydroxide (KOH), methanol

3.4 Method

3.4.1 Sampling procedure

Rubber trees yield 3-seeded ellipsoidal capsules, each capsule with three

seeds. Rubber seeds are ellipsoidal, variable i n size, 2 .5-3 cm long,

mottled brown, lustrous, weighing 2-4 g each. The capsules of the seeds

are spread over the ground in plantation. The seeds were collected from a

plantation and dried under the sun about 3 hours to remove the remaining

moisture, then, the shell and kernels were separated by breaking the

capsule. The kernels were dried in the oven for about 24 hours to remove
the remaining moisture. The kernal were immediately ground using food

processing machine (blender) in order to weaken and rupture the cell,

subsequently, the ground rubber seed was taken into the oven overnight

at 104oC in order to deactivate the remaining enzyme as well to remove

the moisture and then sieved using 300, 350, and 400 m opening

screens. Finally, three different size fractions were obtained 150 m (0-

300 m), 325 m (300-350 m), and 375 m (350-400 m). After drying,

the moisture content of the kernels was determined using halogen

moisture content analyzer and also after the water is removed from the

seeds by evaporation using furnace, and in both cases it was found to be

1.5 %. The oil content of the kernels was determined through soxhlet

extraction using hexane as a solvent for 4-5 h.

3.4.2 Transesterification

This method is according to AbdulKadir et. al (2014) with slight

modification. Methanol and the KOH catalyst were mixed in a three neck

round bottom flask connected to a reflux condenser and heated until

catalyst completely dissolved. Then, 10 g of the ground rubber seeds

sample was added into the mixture and the blend was heated at 60 C

and at atmospheric pressure for 120 min at 500 rpm stirring speed. The

product was filtered using Whatman filter paper and poured into the

separating funnel to separate the excess of alcohol. The reaction was

repeated to study the effect of rubber seeds to methanol mass ratio,

reaction period, and catalyst loading on the FAME yield. The experiment

was divided into three stages. The first stage (preliminary study) was

carried out to obtain reaction time for in situ processing. In this step,
response variable was analyzed on density and viscosity. The experiment

was done at KOH 3g and ratio of raw material to methanol (1:6) and every

15 minutes was analyzed until constants condition. In the second stage,

the experiment was investigated with catalyst concentration of KOH about

1, 2, 3, and 4 (g). The experiment was done in variable ratio of raw

material to methanol (1:6) and 120 minutes reaction time. In the third

stage, the experiment was conducted about effect of ratio of raw material

to methanol i.e; 1:4, 1:5, 1:6, and 1:7 (w:v). The FAMEs analysis was

quantified by Agilent Technologies 7890A Gas Chromatography equipped

with Flame Ionization Detector (GC-FID) with standard capillary column

(30 m by 320 m by 0.25 mm). Automatic injection sampler by Agilent

was used. Methyl heptadecanoate (0.630 mg internal standard) was

dissolved in 1 m L hexane to prepare the standard solution. Approximately

100 mg crude methyl ester was dissolved in 1 mL standard solution for

GC-FID analysis. About 1 L sample was injected into the GC at an oven

temperature of 210 C with helium as the carrier gas. The GC oven was

programmed at 210 C, isothermally for 15 min. Then, the FAMEs content

and the FAME yield were calculated.

The FAME yield was calculated using the following expression:

Moil phase Xfame

100
FAME Yield = Mseed Xoil F

Moil phase = Mass of oil phase after transesterification (g)

XFAME = Mass fraction of FAME in oil phase

Mseed = mass of seeds (g)

Xoil = Mass fraction of oil in seeds

F = 3MWFAME / MWoil (MW = molecular weight)

3.5 Expected outcome

From this experiment, the rubber seed are able to produce significance

amount of biodiesel yield with respect to three treated variables such as

rubber seed to methanol mass ratio, reaction temperature and catalyst

concentration associated with FAME yield.