CHAPTER III

RESEARCH METHODOLOGY

This Chapter presents the research design, methods and procedures

of the study.

RESEARCH DESIGN

This study used the experimental method of research in the extraction of

biodiesel from Rambutan seed oil. Method of extraction of Rambutan seed oil was

Soaking Extraction Method using n-hexane. Method of converting Biodiesel (B100) and

Biodiesel Blend (B2) from Rambutan seed oil is Base-Catalyzed Transesterification

using methanol as the alcohol and sodium hydroxide as the catalyst. The physical

properties such as Density and Kinematic Viscosity; Thermal Properties such as

Distillation, Flash point and Pour point; and Chemical properties such as Cetane were

determined. The study of Physical, Thermal and Chemical properties of the expected

biodiesel and biodiesel blend products will be compared to the Philippine National

Standard for Coco methyl Ester.

EXPERIMENTAL PROCEDURE

A. COLLECTION AND PREPARATION OF RAW MATERIALS

The Rambutan fruits was gathered from Tinga, Batangas and

transported to Batangas State University Main Campus II, Golden Country

Homes Subdivision, Brgy. Alangilan, Batangas City. The Chemicals that was

used in this experimental study is n-Hexane for soaking extraction; methanol and

sodium Hydroxide for the Base-Catalyzed Transesterification process. The neat

automotive diesel oil was used as a base diesel for biodiesel formulated blend.

B. PREPARATION OF RAMBUTAN SEEDS

Production and Evaluation of Biodiesel from Rambutan Chapter III
(Nephelium lappaceum) Seed Oil Research Methodology
Aguila, A.M.,Arellano, J.C.M., Panganiban, K.D.D.

The seeds was removed from the fruit manually. The seeds obtained

was grinded into small particles using a Mortar and Pestle or Blender and dried in

the oven at 70C for 1 hour to reduce its moisture content and then weight.
C. EXTRACTION OF OIL
For the extraction of Rambutan seeds, three varying days for the

soaking method is considered. Below is the procedure of the extraction done and

respective variation which is primarily based on the actual equipment available in

Analytical Laboratory at the Batangas State University Main II.

Soaking Extraction:

1. The samples will be weight on the electrical balance to fill up a container

that could hold four hundred (400) grams of fine dried grinded seeds.
2. For every 400g of seed grains per container equates an 800mL of n-

hexane where it must be soaked for three (3) varying days.

3. After soaking to the varied time, wet seed grains will then be filtered and

pressed to accumulate extract.

4. Extracted liquid shall be placed in a rotary shaker at 70C until extract

solution has no trace of n-hexane.

Table 5. Matrix of Trial Variations for Soaking Extraction

Run No. Time Amount of Fine Grain Seeds Solvent

(days) (g) (mL)
1 4 400 800
2 5 400 800
3 6 400 800

Oil Yield Percentage

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Production and Evaluation of Biodiesel from Rambutan Chapter III
(Nephelium lappaceum) Seed Oil Research Methodology
Aguila, A.M.,Arellano, J.C.M., Panganiban, K.D.D.

weight of oil (grams)

oil yeild content = x 100
weight of seed used (grams)
Equation 1. Percent Oil Yield Content

D. CHARACTERIZATION OF EXTRACTED OIL

The extracted oil was then characterized. The properties that were

determined were Density, Fatty Acid Profile, Free Fatty Acid, Moisture and

Volatile Matter and Saponification value. The Procedures in characterizing the

extracted oil were provided by the laboratory were the oil was characterized.
Density (Pycnometer Method)
The exact amount of sample was transferred to a pycnometer bottle

and was brought to a specified temperature and weighed using analytical

balance reading was taken.

Fatty Acid Profile (AOAC No 940.28) and Free Fatty Acid Content (AOAC No

963.22)
The fatty acid content of the extracted oil was characterized by a gas

chromatography according to AOAC No 940.28 and the free fatty acid content

according to AOAC No 963.22.

Moisture and Volatile Matter (AOAC No 926.12)
The Moisture and Volatile Matter of the extracted oil was characterized according

to AOAC No 926.12.
Saponification value (AOAC 950.16)
The Saponification value of the extracted oil was characterized according to

AOAC No 950.16.

E. BIODIESEL PRODUCTION
After oil extraction, filtration and removal of all water content of the oil,

Base catalyzed transesterification will be conducted to convert the triglycerides of

the oil to biodiesel. In this process, 500 mL of Rambutan seed oil will be

measured and heated to 55 C until all solid fats melt.

A solution of 500 mL methanol and 7 grams of Sodium Hydroxide

(NaoH) which will served as the catalyst will be added to the oil. The mixture will

then agitated for 2 hours to homogenize the mixture. After the agitation, it will be

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Production and Evaluation of Biodiesel from Rambutan Chapter III
(Nephelium lappaceum) Seed Oil Research Methodology
Aguila, A.M.,Arellano, J.C.M., Panganiban, K.D.D.

transferred to a close container and then the mixture will allow to settle for 24

hours.
Separation of Biodiesel and Glycerin
After settling, two phase solution will obtain with Rambutan seed

Biodiesel at the top and the gylcerin at the bottom. It will then be separated using

decantation. The obtain Rambutan Biodiesel still contained small amount of

methanol and glycerin so it will be purified by washing.

Rinsing/Washing Methyl Ester
Warm water will be added to the Separatory funnel. Stir slightly so it will

allow to settle. The water will cleanly separate from the methyl esters, the water

will be drained out from the bottom. This process will be repeated until the water

reach pH level 6-7 and no soap bubble will appear on it. If the liquid remaining is

cloudy, there is water being retained in the fuel, and it was to be reheated slowly

up to 100 C to evaporate out the water. Any white substance at the bottom or any

bubbles forming at the surface is a sign of soaps and was removed or liquid was

re-washed. The clean methyl ester is a version of biodiesel.

Biodiesel Yield Percentage
Volume of Biodiesel produced(mL)
Biodiesel yeild content = x 100
Volume of oil taken( mL)
Equation 2. Percent Biodiesel Yield Content
F. BLENDING OF BIODIESEL
1. Diesel 98%, Rambutan seed Biodiesel 2% (B2)
Washed biodiesel from Rambutan seed oil will blended with

net automotive diesel oil (ADO) in 98:2 ratio (Diesel 98%, Rambutan

seed Biodiesel 2%) using 980 ml of neat ADO and 20 ml of Rambutan

seed Biodiesel.
G. ANALYSIS OF BIODIESEL PROPERTIES
The different properties of the Rambutan seed Biodiesel

(Rambutan Methyl Ester) will be analyzed according to standard test

methods.
Density (ASTM D4052)

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Production and Evaluation of Biodiesel from Rambutan Chapter III
(Nephelium lappaceum) Seed Oil Research Methodology
Aguila, A.M.,Arellano, J.C.M., Panganiban, K.D.D.

A small of volume (approximately 0.7 mL) of liquid sample is

introduced into as oscillating sample tube and the change in oscillating

frequency caused by the change in the mass of the tube is used in

conjunction with the calibration data to determined the density sample.

Kinematic Viscosity (ASTM D4455)
The time is measured for a fixed volume of liquid to flow under

gravity through capillary tube of a calibrated viscometer under a

reproducible driving force and at a closely controlled and known

temperature. The kinematic viscosity is the product of the measured flow

time and the calibration constant of the viscometer.

Calculation:
V= C x t
Equation 3. Kinematic Viscosity
Where:
V- Kinematic viscosity, mm^2/s
C- Calibration constant of the viscometer, (mm^2/s)/s
t- mean flow time, s
Distillation (ASTM D86)
Based on its composition, vapor pressure, expected IBP or

expected EP, or combination thereof, the sample is place in one of five

groups. Apparatus arrangement, condenser temperature and other

operational variables are defined by the group in which the sample falls.

A 100-mL specimen of the sample is distilled under prescribed

conditions for the group in which the sample falls. The distillation is

performed in a laboratory batch distillation unit at ambient pressure under

condition that are designed to provide approximately one theoretical plate

fractionation. Systematic observation o (f temperature readings and

volume of condensate are made depending on the needs of the user of

the data. The volume of the residue and losses are also recorded.

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Production and Evaluation of Biodiesel from Rambutan Chapter III
(Nephelium lappaceum) Seed Oil Research Methodology
Aguila, A.M.,Arellano, J.C.M., Panganiban, K.D.D.

Flash Point (ASTM D93)

A specimen is tested at a slow constant rate which continual

stirring in a brass test cup of specified dimensions with cover of specified

dimensions. The test cup is ignited directly at regular intervals with

simultaneous interruption of the stirring. The flash point is the lowest liquid

temperature at which application of the ignition sources causes the vapor

of the specimen of the sample to ignite.

Pour Point (ASTM D97)
After preliminary heating, the sample is cooled at a specified rate

and examined at intervals of 3 C for flow characteristics. The lowest

temperature at which movement of the specimen is observed is recorded

as the pour point.

Cetane Number (ASTM D7437)
Two correlation in SI units have been established between the

ASTM cetane number and the density and 10%, 50% and 90% distillation

recovery temperatures of the fuel. This procedure has been developed for

diesel fuels meeting the requirements of Specification D975 Grades 1-D

Low Sulfur, No.1-D, 2-D and 4-D. the relationship is given by the following

equation.

CCI=45.2+ ( 0.0892 ) ( T 10 N )+ [ 0.131+ ( 0.901 )( B ) ] [ T 10 N ]+ [ 0.0523( 0.420 )( B ) ] [T 90 N ] + [ 0.00049 ] [

Equation 4. Cetane Number

Where
CCl = Calculated Cetane Index by Four Variable Equation
D = Density at 15 C, g/mL determined by Test Methods D 1298 or D 4042
DN = D 0.85,
B = [ e^ (-3.5)(DN)] 1
T10 = 10 % recovery temperature, C determined by Test Method D 86

and corrected to standard barometric pressure,

H. EVALUATION OF RESULTS

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Production and Evaluation of Biodiesel from Rambutan Chapter III
(Nephelium lappaceum) Seed Oil Research Methodology
Aguila, A.M.,Arellano, J.C.M., Panganiban, K.D.D.

Base on the data that will be obtained, results will be evaluate to

determine the Physical, Thermal and Chemical properties of the Biodiesel

and Biodiesel Blends, also there will be a Statistical Treatment which is

the Independent t-test to be use to determine whether the results will have

a tendency to go over the limit of the Philippine National Standards for

Coco Methyl Ester.

I. APPLICATION
The blended biodiesel will be evaluated in performance in terms

of its emission and combustion through the Standard Emission and

Combustion Testing Procedures of the testing facility. With the aid of

testing laboratory engines, emission and combustion results of the

produced biodiesel and formulated biodiesel blend will be compared with

the available commercialized diesel in the market.

Gathering of Rambutan Seeds from Batangas Public

Market

Washing, Grinding and Drying at 70 C for 1 hour of

Rambutan Seeds

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Production and Evaluation of Biodiesel from Rambutan Chapter III
(Nephelium lappaceum) Seed Oil Research Methodology
Aguila, A.M.,Arellano, J.C.M., Panganiban, K.D.D.

Soaking Extraction of Oil from Rambutan seeds using

n-Hexane as solvent

Suction Filtration of Extracted Rambutan Seed Oil

using vacuum pump

Evaporation of Water Content in Rambutan Seed oil

using Rota-Vap

Base Catalyzed Transesterification of Rambutan seed

oil using 400 mL Methanol and 14 grams of NaOH

Separation of Rambutan seed Biodiesel and Gylcerin

using Separatory Funnel

Washing/Rinsing of Rambutan seed Biodiesel with

warm water

Blending of Rambutan seed Biodiesel with Automotive

Diesel Engine to formulate (B1, B2, & B5)

Characterization of Physical, Thermal and Chemical Properties

of Rambutan seed Biodiesel and Rambutan seed oil Biodiesel
Blends

Engine Emission Test and Engine Combustion Test for

Rambutan seed Biodiesel Blends

Figure 9. Schematic Diagram of Biodiesel Production & Evaluation

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