Chapter four

Experimental Part
4-1 Research methodology steps:

Research Methodology Workflow:

Step 1: Procurement of Waste Vegetable Oil Samples

The research process commenced with the collection of waste vegetable oil (WVO)
samples from a diverse range of sources, including restaurants, cafeterias, and
households. This step ensured the availability of the necessary feedstock for the
biodiesel production process.

Step 2: Filtration and Purification of WVO Samples

The collected WVO samples underwent a thorough filtration process to remove any
remaining cooking impurities and contaminants. This purification step was crucial to
prepare the oil for the subsequent transesterification reaction.

Step 3: Analysis of WVO Properties

The purified WVO samples were analyzed to determine their acidity levels and free
fatty acid content. This assessment provided the necessary information to select the
most appropriate transesterification method for the biodiesel production.

Step 4: Selection of Transesterification Method

Based on the low free fatty acid content identified in the previous step, the base-
catalyzed transesterification method was chosen as the preferred approach. This
selection was made to avoid the occurrence of saponification reactions during the
transesterification process.

Step 5: Biodiesel Production via Base-Catalyzed Transesterification

The waste vegetable oil was then converted into biodiesel through the base-catalyzed
transesterification reaction. This chemical process involved the conversion of the oil's
triglycerides into fatty acid methyl esters (biodiesel).
Step 6: Biodiesel Purification and Washing

The produced biodiesel underwent a wet washing process to remove any remaining
impurities or byproducts, ensuring the purity and quality of the final fuel.

Step 7: Optimization of Process Parameters

Experiments were conducted to analyze and study the factors that influence biodiesel
yield and the conversion of the treated oil, such as concentration, temperature, and
catalyst composition. This step aimed to optimize the biodiesel production process for
maximum efficiency.

Step 8: Analytical Testing of Biodiesel

The final biodiesel product was subjected to comprehensive analytical testing to

assess its physical properties and compare them with literature data, as well as the
specifications of conventional petroleum-based diesel fuels.
This detailed research methodology outlined a systematic approach to converting
waste vegetable oil into high-quality biodiesel, with a focus on optimizing the key
process parameters and ensuring the final product's compliance with industry
standards

4-2 Rationale for Choosing Base-Catalyzed Transesterification

1. The tested waste vegetable oil (WVO) samples had a low acid content (low free
fatty acid content), making the base-catalyzed transesterification method a suitable
choice for their conversion into biodiesel. This method is well-suited for feedstocks
with low free fatty acid levels.
2. The base-catalyzed transesterification process is a relatively simple and
straightforward procedure, which aligns well with the available laboratory capabilities
and resources at the research facility.

4-3 Experimental Methods for Determining Free Fatty Acid Content

There are two common approaches to estimate the free fatty acid content in the treated
waste vegetable oil:
1. Saponification Test: During the esterification process, the free fatty acid content
can be determined by conducting a saponification test on the oil sample.
2. Titration Method: The oil-alcohol mixture can be titrated with drops of sodium
hydroxide in the presence of phenolphthalein indicator. The pink color change
indicates the endpoint, where all the free fatty acids have reacted, allowing the
quantification of the free fatty acid content.

4-4 Safety Precautions during the Experiment

To ensure a safe experimental environment, the following personal protective
equipment (PPE) and safety measures should be implemented:
1. Safety glasses must be worn to protect the eyes.
2. Safety gloves must be worn to protect the hands.
3. A face mask must be worn to prevent inhalation of any hazardous vapors or
particles.
4. A lab coat must be worn to protect the clothing and body.
5. A fire extinguisher must be readily available in the laboratory as a precaution
against potential fire accidents.

4-5 Laboratory Equipment and Apparatus

The equipment and apparatus required for the laboratory-scale production of biodiesel
include:
- Magnetic stirrer
- Electrical heater
- Separating funnel
- Conical flask
- Thermometer
- Ring stand
- Utility clamp
- Weighing balance
- Burette
- Graduated cylinder
- Bottle wash
- Test tubes
- Spatula
- Beakers
- Filter paper for the filtration of waste vegetable oil

4-6 Experimental Materials

The materials required for the biodiesel production process include:
- Methanol
- Sodium hydroxide
- Potassium hydroxide
- Sunflower oil (as a representative waste vegetable oil)
- Distilled water
- Phenolphthalein (as an indicator)
This comprehensive overview provides detailed information on the rationale behind
the selected transesterification method, the experimental techniques for determining
free fatty acid content, the necessary safety precautions, the required laboratory
equipment and apparatus, as well as the consumable materials needed for the
biodiesel production process.

4-7 Experimental Procedures:

4-7-1 Collection of wasted vegetable oils

Waste vegetable oil, specifically sunflower oil from restaurants, is collected and
labeled as a sample, as illustrated in Figure 4-1.
 Figure (4.1) Oil Sample

4-7-2 Treatment of wasted vegetable oil samples

First, vegetable oil waste samples are filtered using filter paper. Next, it is heated to
110°C to remove any remaining traces of water, as shown in Figure 4-2.
Figure (4.2)
Figure (4.3) Oil Sample
Figure (4.4) Oil Sample
Figure (4.5) Oil Sample
Figure (4.6) Oil Sample
Figure (4.7) Oil Sample
Figure (4.8) Oil Sample
Figure (4.9) Oil Sample
Figure (4.10) Oil Sample
Figure (4.11) Oil Sample
Figure (4.12) Oil Sample
Figure (4.13) Oil Sample
Figure (4.14) Oil Sample
 Chapter five
Results and Discussion
: The effect of different temperature on the reaction 5-1

To measure the effect of temperature, 100 ml of five samples of waste Sun flower oil and 1gm
of sodium hydroxide catalyst were taken to react with 20 ml of alcohol (methanol) at five
different temperatures (40, 50, 60, 65, 70) 0C. where Table 5-1 presents the outcome for
temperature effect at different temperatures.

:Amount of methanol for 100 ml of WVO -

Molecular weight of triglycerides from waste vegetable oil = 870 gm/mol

Molecular weight of methanol = 32 gm/mol

:For calculation of molar ratio from the reaction equation -

:For 1:3 molar ratio

WVO + 3 Alcohol −−−→ Biodiesel + glycerol

react with
gm WVO 3×32 gm Alcohol 870
−−−−−−−→

gm WVO −−−→ M Alcohol 89.74

89.74∗3∗32
M= =9.9gm
870

:Find the amount of unreacted methanol -

The amount of alcohol entered was 15.51 gm (20 ml)

Unreacted Alcohol = 15.51 – 9.9 = 5.61 gm

- Sample Calculation for yield:

Quantity of WVO taken = 89.74 gm

Quantity of biodiesel produced = 80.4 gm

Yield=(Quantity of biodiesel produced/Quantity of wvo

taken)

*100 = (80.4/89.74) *100

= 89.6 %
 .Table 5-1: The effect of temperature on the biodiesel and glycerol productivity

Sample Sample Sample Sample Sample

NaOH(1) Sun NaOH(2) Sun NaOH(3) Sun NaOH(4) Sun NaOH(4) Sun
flower oil flower oil flower oil flower oil flower oil
at 40 0 C at 50 0 C at 60 0 C at 65 0 C at 70 0 C
WVO inlet 100 100 100 100 100
volume
(ml)
WVO inlet 88.2 88.1 89.74 88.15 88.65
Mass
(gm)
Biodiesel 58.2 62.9 80.4 67.8 65.65
Mass
(gm)
Glycerin 30.42 25.35 15.6 23 23.5
Mass(gm)
Inlet 15.75 15.83 15.51 15.7 15.1
alcohol
Mass (gm)
Inlet 20 20 20 20 20
alcohol
Volume
(ml)
Reacted 9.73 9.72 9.9 9.72 9.78
alcohol
mass (gm)
Unreacted 6.02 6.11 5.61 5.98 5.32
alcohol
mass (gm)

itcaer eht no serutarepmet tcefE

%59 %06.98
%09
%58
%08 %00.77
%00.47
%57 %04.17
%07 %00.66
%56
dleiY

%06
%55
%05
03 53 04 54 05 55 06 56 07 57 08
serutarepmeT

Figure 5-1: The effect of different temperatures on the reaction yield

Through laboratory experiments to find out the optimum temperature for the
reaction, it was found that the temperature of 60 0C gives the best biodiesel
yield. This effect of temperature on biodiesel yield was showed in figure 5-1.
Through experiments to find out the best temperature for a reaction, it was found
that the best temperature is 60 0C.

: The effect of different temperature on the reaction 5-2

To measure the effect of temperature, 100 ml of five samples of waste Sun flower oil
and 1gm of potassium hydroxide catalyst were taken to react with 20 ml of alcohol
(methanol) at five different temperatures (40, 50, 60, 65, 70) 0C. where Table 5-2
.presents the outcome for temperature effect at different temperatures
:Amount of methanol for 100 ml of WVO -
Molecular weight of triglycerides from waste vegetable oil = 870 gm/mol
Molecular weight of methanol = 32 gm/mol
:For calculation of molar ratio from the reaction equation -
:For 1:3 molar ratio
WVO + 3 Alcohol −−−→ Biodiesel + glycerol
react with
gm WVO 3×32 gm Alcohol 870
−−−−−−−→
gm WVO −−−→ M Alcohol 88.1
88.1∗3∗32
M= =9.72gm
870

:Find the amount of unreacted methanol -

The amount of alcohol entered was 15.8 gm (20 ml)
Unreacted Alcohol = 15.8 – 9.72 = 6.08 gm
- Sample Calculation for yield:
Quantity of WVO taken = 88.1 gm
Quantity of biodiesel produced = 66.1 gm
Yield=(Quantity of biodiesel produced/Quantity of wvo
taken)
*100 = (66.1/88.1) *100 = 75 %
 .Table 5-2: The effect of temperature on the biodiesel and glycerol productivity

Sample Sample Sample Sample Sample

KOH(1) Sun KOH(2) Sun KOH(3) Sun KOH(4) Sun KOH(4) Sun
flower oil flower oil flower oil flower oil flower oil
at 40 0 C at 50 0 C at 60 0 C at 65 0 C at 70 0 C
WVO inlet 100 100 100 100 100
volume (ml)
WVO inlet 88.2 88.25 88.1 88.3 88.6
Mass (gm)
Biodiesel Mass 54.7 60.9 66.1 65.2 63.5
(gm)
Glycerin 36.4 24.35 21.4 23.2 23.8
Mass(gm)
Inlet alcohol 15.83 15.75 15.8 15.75 15.6
Mass (gm)
Inlet alcohol 20 20 20 20 20
Volume (ml)
Reacted 9.73 9.73 9.72 9.74 9.77
alcohol mass
(gm)
Unreacted 6.1 6.01 6.08 6.01 5.83
alcohol mass
(gm)

itcaer eht no serutarepmet tcefE

%08
%57
%57 %47
%27
%96
%07

%56 %26
dleiY

%06

%55

%05
03 53 04 54 05 55 06 56 07 57 08
serutarepmeT

Figure 5-2: The effect of different temperatures on the reaction yield

Through laboratory experiments to find out the optimum temperature for the
reaction, it was found that the temperature of 60 0C gives the best biodiesel
yield. This effect of temperature on biodiesel yield was showed in figure 5-2.
Through experiments to find out the best temperature for a reaction, it was found
that the best temperature is 60 0C.
: Effect of the catalyst formula on productivity 5-3
To measure the effect of the catalyst combination on the yield of biodiesel, two samples were
taken consisting of 100 ml of waste sun flower oil and 20 ml of methanol and a reaction
temperature of 60 0C, and a catalyst was used for each sample. Table 5-3 shows the effect of
catalyst formulation on biodiesel and glycerol productivity. The outcome of this effect was
reveled in figure 5-3 at which it was found out that the use of NaOH catalyst gives higher
biodiesel yield than KOH catalyst.

.Table 5-3: The effect of catalyst formula on the biodiesel and glycerol productivity

Sample NaOH(1) Sample KOH(2)

Sun flower oil Sun flower oil
at 60 0 C , at time (60min) at 60 0 C , at time (60 min)
WVO inlet volume (ml) 100 100

WVO inlet Mass (gm) 89.74 88.1

Biodiesel Mass (gm) 80.4 66.1

Glycerin Mass(gm) 15.6 21.4

Inlet alcohol Mass (gm) 15.51 15.8

Inlet alcohol Volume (ml) 20 20

Reacted alcohol mass (gm) 9.7 9.72

Unreacted alcohol mass 6.1 6.08

(gm)
wt gnisu dleiy leseidoiB

%09

%00.09

%00.58
% 57
dleiY

%00.08

%00.57

%00.07

%00.56
HOaN HOK
stsylataC

Figure 5-3: The effect of the catalyst formula on the reaction yield.

: The effect of different time on the reaction 5-4

To measure the effect of time, 100 ml of five samples of waste Sun flower oil and 1gm of
sodium hydroxide catalyst were taken to react with 20 ml of alcohol (methanol) at five
different times (30, 45, 60, 75, 90) min. where Table 5-4 presents the outcome for time effect
.at different times
.Table 5-4: The effect of reaction time on the biodiesel and glycerol productivity

Sample Sample Sample Sample Sample

NaOH(1) Sun NaOH(2) Sun NaOH(3) Sun NaOH(4) Sun NaOH(4) Sun
flower oil flower oil flower oil flower oil flower oil
at 30 min at 45 min at 60 min at 75 min at 90 min
WVO inlet 100 100 100 100 100
volume (ml)
WVO inlet 88.15 88.25 89.74 88.1 88.2
Mass (gm)
Biodiesel 64.35 69.85 80.4 63.6 50.05
Mass (gm)
Glycerin 26 22 15.6 30.05 33.6
Mass(gm)
Inlet alcohol 15.7 15.55 15.51 15.65 15.2
Mass (gm)
Inlet alcohol 20 20 20 20 20
Volume (ml)
Reacted 9.72 9.73 9.9 9.72 9.73
alcohol mass
(gm)
Unreacted 5.98 5.82 5.61 5.93 5.47
alcohol mass
(gm)
y noitcaer eht no emit tceffE
%59 %06.98
%09
%58 %51.97
%08
%00.37 %02.27
%57
%07
%56
dleiY

%06 %57.65
%55
%05
02 03 04 05 06 07 08 09

)nim( emiT

Figure 5-4: The effect of reaction time on the reaction yield.

Through laboratory experiments to find out the optimum time for the reaction, it was found
that the time of 60 mine gives the best biodiesel yield. This effect of time on biodiesel yield
was showed in figure 5-4. Through experiments to find out the best time for a reaction, it was
.found that the best time is 60 min

: The effect of Agitation on the reaction :5-5

To measure the effect of Agitation, 100 ml of four samples of waste Sun flower oil and 1gm
of sodium hydroxide catalyst were taken to react with 20 ml of alcohol (methanol) at four
different Agitations (2, 3, 4, 5) Rpm. where Table 5-4 presents the outcome for Agitation
.effect at different Agitations
.Table 5-5: The effect of Agitation on the biodiesel and glycerol productivity

Sample Sample Sample Sample

NaOH(1) Sun NaOH(1) Sun NaOH(2) Sun NaOH(3) Sun
flower oil flower oil flower oil flower oil
at (2 Rpm) at (3 Rpm) at (4 Rpm) at (5 Rpm)
WVO inlet volume 100 100 100 100
(ml)
WVO inlet Mass 88.15 88.1 89.74 88.25
(gm)
Biodiesel Mass 70 71.5 80.4 72.1
(gm)
Glycerin Mass(gm) 21.7 21.5 15.6 21.1

Inlet alcohol Mass 15.85 15.75 15.51 15.65

(gm)
Inlet alcohol 20 20 20 20
Volume (ml)
Reacted alcohol 9.72 9.72 9.9 9.73
mass (gm)
Unreacted alcohol 6.13 6.03 5.61 5.92
mass (gm)
eiy noitcaer eht no noitaitgA tceffE
%00.59
%06.98
%00.09

%00.58
%01.18 %06.18
%04.97
%00.08
dleiY

%00.57

%00.07
5.1 2 5.2 3 5.3 4 5.4 5 5.5 6
)mpR( noitaitgA

Figure 5-5: The effect of Agitation on the reaction yield.

Through laboratory experiments to find out the optimum Agitation for the reaction, it was
found that the Agitation of 4 Rpm gives the best biodiesel yield. This effect of Agitation on
biodiesel yield was showed in figure 5-5. Through experiments to find out the best Agitation
.for a reaction, it was found that the best Agitation is 4 Rpm

: The effect of Catalyst Concentration on biodiesel yield 5-6

To measure the effect of Catalyst Concentration, 100 ml of five samples of waste Sun flower
oil and 1gm of sodium hydroxide catalyst were taken to react with 20 ml of alcohol
(methanol) at five different Catalyst Concentration (0.5, 0.75, 1, 1.25, 1.5) gram. where Table
5-6 presents the outcome for Catalyst Concentration effect at different Catalyst
.Concentration
.Table 5-6: The effect of Catalyst Concentration on the biodiesel and glycerol productivity

Sample Sample Sample Sample Sample

NaOH(1) Sun NaOH(2) Sun NaOH(3) Sun NaOH(4) Sun NaOH(4) Sun
flower oil flower oil flower oil flower oil flower oil
at 0.5 gm at 0.75 gm at 1 gm at 1.25 gm at 1.5 gm
WVO inlet 100 100 100 100 100
volume (ml)
WVO inlet 88.35 88.2 89.74 88.1 88.35
Mass (gm)
Biodiesel 76.85 78.1 80.4 69.4 45.7
Mass (gm)
Glycerin 18 17 15.6 25 34.95
Mass(gm)
Inlet alcohol 15.8 15.75 15.51 15.7 15.75
Mass (gm)
Inlet alcohol 20 20 20 20 20
Volume (ml)
Reacted 9.74 9.73 9.9 9.72 9.74
alcohol mass
(gm)
Unreacted 6.06 6.02 5.61 5.98 6.01
 alcohol mass
(gm)

artnecnoc tsylatac tceffE

%00.001
%89.68 %05.88 %06.98
%00.09
%77.87
%00.08
%00.07
%00.06 %27.15
dleiY

%00.05
%00.04
2.0 4.0 6.0 8.0 1 2.1 4.1 6.1
mg )%tw( noitartnecnoc tsylataC

Figure 5-6: The effect of Catalyst Concentration on the reaction yield.

Through laboratory experiments to find out the optimum Catalyst Concentration for the
reaction, it was found that the Catalyst Concentration of 1 gram gives the best biodiesel yield.
This effect of Catalyst Concentration on biodiesel yield was showed in figure 5-6. Through
experiments to find out the best Catalyst Concentration for a reaction, it was found that the
.best Catalyst Concentration is 1 gram

: Effect of reactants volume ratio on biodiesel yield 5-7

Five samples of waste sun flower oil were taken in different volumes (90, 70,100, 90 and 50)
ml for a reaction with (10, 10, 20, 30, and 50) ml, respectively, with reactant volume ratio of
(9:1, 7:1, 5:1, 3:1, 1:1), respectively, of methanol at a temperature of 60 0C , using 1 gram of
sodium hydroxide catalyst the effect of volume reactants ration on biodiesel and glycols
productivity was presented in table 5-7. the outcome of this effect was shown in figure 5-7 at
which it was revealed that the best of volume ratio (5:1) to give the height biodiesel yield of
about 89.6% . in addition, it was found that the increase of alcohol quantity against oil
.quantity may not help to improve the biodiesel yield

.Table 5-7: The effect of Reactants Volume Ratio on the biodiesel and glycerol productivity

Sample Sample Sample Sample Sample

NaOH(1) Sun NaOH(1) Sun NaOH(2) Sun NaOH(3) Sun NaOH(4) Sun
flower oil flower oil flower oil flower oil flower oil
At (9:1) At (7:1) at (5:1) at (3:1) at (1:1)
WVO inlet 90 70 100 90 50
volume (ml)
WVO inlet Mass 78.2 61.7 89.74 78.8 43.38
(gm)
Biodiesel Mass 50.1 47.7 80.4 65.68 9.85
(gm)
Glycerin 28.9 17.85 15.6 19.7 59.3
Mass(gm)
Inlet alcohol 8.65 8.25 15.51 23.9 39.4
Mass (gm)
 Inlet alcohol 10 10 20 30 50
Volume (ml)
Reacted alcohol 8.6 6.81 9.9 8.69 4.78
mass (gm)
Unreacted 0.05 1.44 5.61 15.21 34.61
alcohol mass
(gm)

ht nehw leseidoib fo dleiY

degnahc %06.98
%53.38
%00.09 %03.77
%00.08
%00.46
%00.07
%00.06
%00.05
%00.04 %07.22
dleiY

%00.03
%00.02
%00.01
%00.0
10:1 10:3 10:5 10:7 10:9

Figure 5-7 The effect of reactants volume ratio on the reaction yield.

. Table 5-7 : Physical properties of biodiesel produced

METHOD Name of Diesel ASTM UNIT Sample Sample Sample

properties Petroleum[109] standard (1) (2) (3)
biodiesel[110]
ASTM D Kinematic 5-2 5.0 – 3.5 mm.sq/sec 4.8 5.9 5.82
445 Viscosity at
40 0C
ASTM D Density at 0.838 0.90 – 0.84 g/cm3 0.8886 0.9026 0.8946
4052 15.0 0C
API 27.67 25.199 26.6
0
ASTM D Flash 80 - 55 180 - 100 C 174 165 175
93 point C 0
0
ASTM D Clold Point C 4 3 3
2500
0
ASTM D Pour Point C 6- 0 2-
97
ASTM D Total Max 0.1 PPM 0.7 0.1 0.8
7963 Sulpher
ASTM D Mg PPM 0 0 0
7963
ASTM D Ca PPM 1.9 4.3 3.5
7963
ASTM D Heating Min 10600 K.Cal / Kg 10742. 10690. 10720.
4868 Value 705 04 235
ASTM D .Acid No Max 0.1 Mg KOH/gr 0.1286 0.4708 0.2884
974
METHOD Name of Diesel ASTM UNIT Sample Sample Sample
properties Petroleum[109] standard (4) 10% (5) 20% (6) Sun
biodiesel[110] biodiesel biodiesel flower
oil
ASTM D Kinematic 5-2 5.0 – 3.5 mm.sq/sec 4.4 4.6 49.98
445 Viscosity at
40 0C
ASTM D Density at 0.838 0.90 – 0.84 g/cm3 0.8532 0.8538 0.9389
4052 15.0 0C
API 34.27 34.15 19.13
Cetan index 51.9 51.95 ---
:Distillation --- --- --- ---
0
I.B.P C 175.5 176.8
0
% 10 C 252.4 254.1
0
% 50 C 300.8 302.0
0
% 90 C 354 356
0
F.B.P C 372 373
@ .Rec % 88.1 87.5
0
C 350
0
ASTM D Flash 80 - 55 180 - 100 C 76 78 254
93 point C 0
0
ASTM D Clold Point C 0.0 0.0 ---
2500
 0
ASTM D Pour Point C 9- 9- 12-
97
ASTM D Total Max 0.1 %Wt 0.0419 0.0375 0.0006
7963 Sulpher 2
ASTM D Heating Min 10600 K.Cal / Kg 10867. 10865.9 10051.
4868 Value 6 4 5
ASTM D .Acid No Max 0.1 Mg KOH/ gr 0.0270 0.0372 ---
974

: Conclusions
In the fourth chapter, the research methodology for this project was presented. The most
important materials, equipment and devices needed to conduct this experiment were
presented. Experimental steps for producing biodiesel from WVO at different operating
temperatures, different volumetric ratios of reactants, and different oil source are shown.

In the fifth chapter, the best temperature that gave the highest productivity was reached
experimentally, which was 60 degrees Celsius, the best time that gave the highest
productivity was 60 minutes, and the best stirring that gave the maximum amount of stirring
was 4 Rpm revolutions per minute. And the best motivator. NaOH was compared with KOH,
and the best catalyst concentration was 1 g and the best oil:methanol volumetric ratio, which
gave the maximum yield for biodiesel production. 5:1 In addition, it was found that the
physical properties of the experimentally produced biodiesel were similar to ASTM
specifications.