Experimental Sept9

PAMANTASAN NG LUNGSOD NG MAYNILA
University of the City of Manila

College of Engineering and Technology
Department of Chemical Engineering
EXPERIMENTAL
STUDY
INTRODUCTION
The experimental method is the scientific approach of research that proves whether
or not it is feasible to produce propylene glycol using guyabano seeds. Laboratory set-
up for the experimentations was done and operating conditions from other researchers
were used as the basis to devise the most appropriate conditions in producing
propylene glycol.
The raw material (guyabano seeds) were obtained from RJ-Sun Tropical Herbs and
Fruits located in Purok 6, Dologon, Maramag, Bukidnon. Pretreatment was done
including dehulling (to obtain the seed kernel), drying (to achieve the optimal moisture
content for oil yield), size reduction and sieving. Parameters such as drying time, drying
temperature, and grinding time were varied to obtain the best operating conditions.
Afterward, the ground seed kernels were subjected to solvent extraction to obtain
the oil needed in the succeeding processes. The resulting mixture, the miscella which is
oil and solvent mixture, and the cake (ground seed kernels) were separated through
filtration. Then, the recovered miscella had undergone a distillation process to separate
the oil from the solvent. To achieve the optimum yield of oil, parameters such as solvent
type, mass ratio of solvent to ground seed kernels, extraction time and temperature
were varied.
The recovered oil was reacted with methanol and an alkali solution as a catalyst
which then produces methyl ester and glycerol. Variation of parameters such as
reaction time, temperature and type of catalyst determined the optimum yield of
glycerol.
Finally, the produced glycerol was reacted with copper to produce acetol through
dehydration, and then hydrogen gas is added to produce propylene glycol. Different
analysis and testing was done to determine the product’s properties as compared to
standard and commercially available ones.
Hydrogenolysis of Glycerol Derived from Guyabano (Annona muricata) Seeds for

EXPERIMENTAL
the Production of Propylene Glycol 32
Dionisio, C.P., Fulugan, C.L., Redublo, A.P., Saya, D.S. STUDY
OBJECTIVES OF THE EXPERIMENTAL STUDY
A. General Objectives
The main objective of the experimental study to produce propylene glycol that
conforms to the standard properties shown in Table 4.1.
Table 4.1 Standard and Exiting Properties

Property Standard1 Existing2
Appearance colorless clear and colorless
Boiling Point (ºC) 188 185
Specific Gravity @ 25 ºC (g/mL) 1.036 1.036
Refractive Index [20 ºC] 1.432 1.433
2950-2800 [C-H alkanes]
FTIR Peak Value (cm-1)
650-600 [alkynes]
Source: 1 Cefic - European Chemical Industry Council
2 Alyson’s Chemical Enterprises, Inc.
3 IR Absorptions for Representative Functional Groups
B. Specific Objectives
To identify the optimum operating conditions for the preparation and conditioning
of guyabano seeds which includes drying and size reduction;
To determine the parameters that will produce the highest conversion of

guyabano seed oil to propylene glycol through variation the different parameters
such as type of reagents, ratio, temperature and time of reaction;
To calculate the percent yield of each processes involved such as, solvent
extraction, distillation, transesterification, dehydration and hydrogenation;
To identify the equivalent unit operation and equipment of each laboratory

process and apparatus.

EXPERIMENTAL
EXPERIMENTAL STUDY
The experimental method of the study focused on performing the process in a

laboratory scale set-up. The experiment consisted the following:
I. Preparation and Conditioning of Raw Material
1. Dehulling
2. Drying
3. Size Reduction & Sieving
II. Conversion Process
1. Solvent Extraction of Ground Seed Kernel

2. Distillation of Miscella
3. Base-Catalyzed Transesterification of Extracted Oil
4. Hydrogenolysis of Glycerol
III. Testing Procedures
1. Oil and moisture content of the Guyabano seeds

2. Final Product Properties

EXPERIMENTAL
RAW MATERIAL, REAGENTS AND APPARATUS
Raw Material
The guyabano seeds were gathered from RJ-Sun Tropical Herbs and Fruits
located in Purok 6, Dologon, Maramag, Bukidnon through Ms. Jonnamei Tolomoro
Lozano.
Figure 4.1. Collection of Raw Material
Prior to the experimentation proper, the oil content and moisture content of the
guyabano seeds that were collected were tested. The composition of the raw material is
summarized in Table 4.2.
Table 4.2 Composition of Guyabano Seed

Composition Percent Content (%)
Oil 35.0
Moisture 33.63
Source: Adamson University Testing Research and Development Center (AdUTRDC)

EXPERIMENTAL
Reagents
The reagents used in the experimentation are summarized in Table 4.3 shown
below. The reagents were purchased from Alyson’s Chemicals Enterprises Inc, located
at 1425 Gregorio Araneta Avenue, Quezon City and RB Chemodities in Bambang,
Manila.
Table 4.3. Reagents and their Corresponding Properties
Reagent Process Chemical Structure Function Properties
Isopropanol
Boiling point: 82.6 °C

Solvent Density: 786 kg/m³
Solvent
Extraction Molar mass: 60.1 g/mol
Melting point: -89 °C
Methanol
Boiling point: 64.7 °C

Trans-
Molar mass: 32.04 g/mol
esterification Solvent
Density: 792 kg/m³
Melting point: -97.6 °C
Sodium
Hydroxide
Molar mass: 40.0 g/mol
Trans-
Catalyst Density: 2.13 g/cm³
esterification
Melting point: 323 °C

EXPERIMENTAL
Laboratory Apparatus
The laboratory apparatus with their corresponding description are presented in

Table 4.4.
Table 4.4. List of Laboratory Apparatus
Laboratory Apparatus Description

Mortar and Pestle
Used to dehull the guyabano seeds

in order to obtain the guyabano seed
kernels
Beaker
Container used for measuring,

stirring, mixing and heating liquids
Analytical Balance
A digital instrument that is used to

measure the mass of an object in S.I
unit (grams)
Oven
Used for drying the guyabano seed

kernels

EXPERIMENTAL
Blender
Used to reduce the particle size of

the dried guyabano seed kernels
Sieve
Used to separate the finer particles
from coarse particles after reducing
the size of the guyabano seed
kernels
Hot Plate
Electrically-powered device used for

heating
Stirring Rod
Used to stir chemicals and liquids
Thermometer
Used to measure temperature
Filter Paper
A piece of porous paper used for

filtering miscella from the cake

EXPERIMENTAL
Funnel
Used to efficiently transfer liquids
from one container to another with
small opening and hold the filter
paper during filtration
Switch
Used to on/off the distillation set-up
Thermostat
Used to maintain or adjust the

temperature to the desired set point
Pump
Used to supply cooling water to the

condenser for the distillation set-up
Condenser
Used for liquefying recovered solvent

EXPERIMENTAL
Erlenmeyer Flask
Used to measure, mix, and store

liquid and suitable for heating liquids
Stopwatch
Used to measure the amount of time

elapsed from a particular time when
it is activated
Vials
Used to store liquids and reagents
Syringe
Used to transfer small volume of

liquids from one container to another

EXPERIMENTAL
EXPERIMENTAL PROCEDURE
PREPARATION AND CONDITIONING OF RAW MATERIAL
I. Dehulling of Guyabano Seeds
Dehulling is the removal of the outer layer of the seed called seed coat by using
mortar and pestle. Fasakin, A., et.al (2008) stated that guyabano seed coats does not
contain any oil, thus it will not be utilized in this study. Furthermore, dehulling must be
done prior to any unit operations and processes in the production to expose the
guyabano seed kernel which contains oil needed in the succeeding processes (Akande,
F.B., et.al., 2016).
Guyabano Seeds Guyabano Kernels

Figure 4.2. Dehulling of Guyabano Seeds
Determination of Mass Ratio of Guyabano Seed and Seed Kernel
The mass ratio of the seed and the seed kernel were determined in order to
know the approximate weight of the kernel with every seed collected.
Materials and Apparatus
Material Apparatus
analytical balance
guyabano seeds Mortar
Pestle

EXPERIMENTAL
Objective
To determine the mass ratio of the seed kernel with respect to the seed.
Hypothesis
The seed kernels and seeds have a definite mass ratio.
Procedure
1. Weigh 500 g of guyabano seeds.

2. Dehull the seeds using mortar and pestle.
3. Weigh the collected guyabano seed kernels.
4. Repeat the procedure for five trials.
Laboratory Set-Up
Guyabano Guyabano
seed Kernels
Analytical
Balance
Figure 4.3 Guyabano Seed-Kernel Mass Ratio Determination

EXPERIMENTAL
Data and Results
Table 4.5 Determination of Guyabano Seed-Kernel Mass Ratio
Trial Mass of Seeds (g) Mass of Kernel (g) Ratio (S:K)

1 500 386.2 0.7724
2 500 387.4 0.7748
3 500 384.4 0.7688
4 500 390.2 0.7804
5 500 383.8 0.7676
Analysis
Using the data in Table 4.5, the average weight of the guyabano seed kernel can
be computed:
386.2 + 387.4 + 384.4 + 390.2 + 383.8

𝑎𝑣𝑒𝑟𝑎𝑔𝑒 𝑚𝑎𝑠𝑠 𝑜𝑓 𝑘𝑒𝑟𝑛𝑒𝑙 (𝑔) =
5
𝑎𝑣𝑒𝑟𝑎𝑔𝑒 𝑚𝑎𝑠𝑠 𝑜𝑓 𝑘𝑒𝑟𝑛𝑒𝑙 (𝑔) = 𝟑𝟖𝟔. 𝟒𝟎𝒈
With the mass of seeds as 500g in each trial, the average ratio of seed to kernel
is,
500𝑔
𝑎𝑣𝑒𝑟𝑎𝑔𝑒 𝑟𝑎𝑡𝑖𝑜 (𝑆: 𝐾) = = 1.29 ≈ 𝟏. 𝟑𝟎
386.4𝑔
Conclusion
The ratio of seed to the seed kernel is 1.30:1. Therefore, almost seventy seven
percent (77%) of the mass of the guyabano seed is the mass of the guyabano kernel
inside it.

EXPERIMENTAL
II. Drying of the Guyabano Seed Kernels
Drying is the removal of excess moisture content of the raw material that will
consume process heat resulting to a lower yield in the succeeding process. Raghavan,
V. & Dev, S. (2012) also stated that drying is important because of ease of handling due
to reduction in bulk and reduction in handling costs, and dry biomaterials are less prone
to microbiological degradation in storage. Furthermore, low moisture content indicates
good shelf life for the oil (Etim, E., et.al., 2012). According to Okoro, C.K, et.al. (2013),
the moisture content of the guyabano seeds should be conditioned within the range of
8.48% to 15.99% in wet basis in order to achieve high oil yield. Furthermore, it was
stated that the optimum oil yield can be obtained at 8.48% moisture content.
Laborataory Set-Up
Oven
Dried Kernels
Guyabano
Kernel
Figure 4.4. Drying of Guyabano Kernels

EXPERIMENTAL
A. Determination of Optimum Drying Temperature of Guyabano Kernel
Basis for Variation: In a study by Onimawo, I.A. (2002) & Okoro, C.K., et.al.
(2013), the guyabano seeds were oven dried at 105⁰C to obtain 8.48% to
15.99% moisture content in wet basis for higher oil yield in extraction. The raw
material has an initial moisture content of 33.63% (AdUTRDC 17-0957, 2017).
Thus, the researchers used 85, 95, 105, 115, 125⁰C as trials for the experiment.
Material Apparatus
Analytical Balance
Guyabano Seed Kernels Oven
Stopwatch
Objective
To determine the optimum drying temperature of guyabano kernels.
Hypothesis
The moisture content of the guyabano seed kernels would be reduced

significantly from its initial moisture content
Procedure
1. Weigh five (5) sets of 386.4 g guyabano seed kernels.

2. Uniformly place one set on the oven set to 85⁰C, for 30 minutes.
3. Weigh the dried kernels.
4. Repeat procedures 2-4 with different drying temperature of: 95, 105, 115, 125⁰C.

EXPERIMENTAL
Data and Results
Table 4.6 Determination of Optimum Drying Temperature Results

Mass of Final
Temp Time Mass of Dried
Trial Kernels Moisture Observation
(⁰C) (min) Kernels (g)
(g) Content(%)1
No noticeable change
1 386.4 85 30 306.2 16.25
in appearance
No noticeable change
2 386.4 95 30 303.4 15.47
in appearance
Kernels started to
3 386.4 105 30 297.4 13.77 shrink and turned
light-brown
4 386.4 115 30 290.2 11.63 Kernels turned brown
Approximately 120g of
5 386.4 125 30 285.8 10.27
kernels were burnt
Souce: (1) IRRI
Analysis
It was observed that after drying at 85⁰C and 95⁰C, there is no noticeable change
in appearance of the kernels. On the other hand, drying at temperatures of 105⁰C,
115⁰C, and 125⁰C results to a final moisture content of 13.77%, 11.63% and 10.27%,
respectively. However, at 125⁰C, some of the kernels were already burnt.
Calculation
According to IRRI, the final moisture content after drying can be compute by:
100 − 𝑀𝐶𝑖
𝑊𝑓 = 𝑊𝑖 ∗ ( )
100 − 𝑀𝐶𝑓

EXPERIMENTAL
Re-arranging the formula,

100 − 𝑀𝐶𝑖
𝑀𝐶𝑓 = 100 − (𝑊𝑖 ) ( )
𝑊𝑓
Equation 1
where:
𝑊𝑓 = mass of kernel after drying (g)

𝑊𝑖 = mass of kernel before drying (g)
𝑀𝐶𝑓 = final moisture content (%)
𝑀𝐶𝑖 = initial moisture content (%)
Using equation 1 and data in Trial 4,

100 − 33.63
𝑀𝐶𝑓 = 100 − (386.4) ( )
290.2
𝑴𝑪𝒇 = 𝟏𝟏. 𝟔𝟑%
The final moisture content of guyabano kernel after drying at 115⁰C is 11.63%,
which falls within the desirable range of 8.48% to 15.99% necessary to achieve
maximum oil yield.
Conclusion
Therefore, guyabano kernels will be subjected to drying temperature of 115⁰C
prior to succeeding processes to attain high oil yield.

EXPERIMENTAL
B. Determination of Optimum Drying Time of Guyabano Seed Kernel
Basis for Variation: In a study by Onimawo, I.A. (2002) & Okoro, C.K., et.al.
(2013), to determine the moisture content loss, the guyabano seeds were oven
dried at 105⁰C and continuous weighing was carried out until steady weight was
achieved.
Material Apparatus
Analytical Balance
Guyabano Seed Kernels Oven
Stopwatch
Objective
To determine the optimum drying time of guyabano kernels until constant weight
was achieved.
Hypothesis
The moisture content of the guyabano seed kernels would be reduced

significantly from its initial moisture content
Procedure
1. Weigh three (3) sets of 386.4g guyabano seed kernels.

2. Uniformly place each set on the oven set to 115⁰C
3. Weigh the sample every 10 minutes.
4. Continue drying until constant weight has been reached.

EXPERIMENTAL
Data and Results
Table 4.7 Determination of Optimum Drying Time Results
Mass of Elapsed time for drying (min) Final

Trial Kernels Moisture
(g) 10 20 30 40 50 60 Content(%)1
1 386.4 346.6 316.4 293.6 287.8 282.4 282.4 9.19

2 386.4 349.4 316.2 295.8 289.2 281.4 280.8 8.67
3 386.4 342.2 319.8 296.6 286.4 282.2 282.0 9.06
Souce: (1) IRRI
Analysis
It was observed that the mass of dried guyabano kernels between 50 and 60
minutes for trial 1 remained constant with a final mass of 282.4g, while at trial 3, the
final mass after 60 minutes is 282.0g, with a minimal difference of 0.2g from 50-minute
drying; and at trial 2, there was a minimal difference of 0.6g. Generally, there is an
insignificant difference of the results for 50 and 60 minutes drying time.
Using equation 1 and data in Trial 1,
100 − 33.63
𝑀𝐶𝑓 = 100 − (386.4) ( )
282.4
𝑴𝑪𝒇 = 𝟗. 𝟏𝟗%
The final moisture content of guyabano kernel after drying is 9.19% which falls
within the desirable range of 8.48% to 15.99% necessary to achieve high oil yield. At 50
minutes, the guyabano kernels achieved its equilibrium moisture content.
Conclusion
Therefore, guyabano kernels will be subjected to drying at 115⁰C for 50 minutes
prior to succeeding processes to attain maximum oil yield.

EXPERIMENTAL
III. Size Reduction of Guyabano Seed Kernel
Size reduction is a process of reducing large solid unit masses to small unit
masses, coarse particles or fine particles, which leads to increase of surface area
(Archana, K., et.al., 2013) The dried kernels were immediately size reduced in order to
rupture the cell and expose more surface area necessary for the next processes. In
addition to that, it also makes handling easier in the subsequent processing steps.
According to the study by Santoso, H., et.al (2013), the smaller the seed particle
size, the higher the oil yield can be obtained. Oboh, I., et.al (2008) stated that a particle
size of 0.25 to 0.5 mm is recommended for guyabano seeds to react more quickly and
will result to a higher rate of extraction. Furthermore, increasing the grinding time of the
material will result to a decrease in particle size, Samuel, D., et.al (2013) mentioned that
maximum yield was obtained at 5 minutes of grinding.
The bulk density of the guyabano seeds, kernel, and ground kernel were also
determined.
Laborataory Set-Up Sieve Tray

Mesh 35
Blender
Dried Ground
Kernels Kernels
Figure 4.5. Size Reduction and Sieving Process

EXPERIMENTAL
A. Determination of Grinding Time
Basis for Variation: Santoso, H., et.al (2013) stated that the smaller the seed
particle size, the higher the oil yield can be obtained. In a study by Samuel, D.,
et.al (2013), it was revealed that a maximum oil yield was obtained at 5 minutes
of grinding.

Material Apparatus
Blender & Spatula
Analytical Balance
Dried Guyabano Kernels
Stopwatch
Sieve Tray
Objective
To grind the guyabano seed kernel to a particle size within the range of 0.25 mm
to 0.50 mm to attain a higher oil yield.
Hypothesis
The guyabano seed kernel will be successfully ground resulting to a particle size
falling within the range of 0.25 mm to 0.50 mm with minimal losses.
Procedure
1. Place 282.4 g of dried guyabano kernels in a blender.

2. Grind the kernels for 3 minutes.
3. Let the ground kernels pass through ASTM Mesh 35
4. Weigh the ground kernels that pass through the sieve.
5. Repeat procedures with different time: 4, 5, 6, 7 min.

EXPERIMENTAL
Data and Results

Table 4.8 Size Reduction Results
Mass of Mass of
Mass of Dried Time % Retained
Trial Ground Retained
Kernels (g) (min) in Sieve
Kernels (g) in Sieve
1 282.4 3 271.6 10.8 3.82
2 282.4 4 275.4 7.0 2.48
3 282.4 5 278.6 3.8 1.35
4 282.4 6 280.0 2.4 0.85
5 282.4 7 280.8 1.2 0.42
Analysis
It was observed that after grinding process, some of the particles are left at the
sieve tray. The highest mass of ground kernels recovered was obtained after 6 minutes
of grinding with 0.85% retained in the sieve tray. At 7 minutes grinding time, it was
observed that some of the particles turned to dust.
Using data in Trial 1,
𝑚𝑎𝑠𝑠 𝑏𝑒𝑓𝑜𝑟𝑒 𝑔𝑟𝑖𝑛𝑑𝑖𝑛𝑔 − 𝑚𝑎𝑠𝑠 𝑎𝑓𝑡𝑒𝑟 𝑔𝑟𝑖𝑛𝑑𝑖𝑛𝑔

%𝑅𝑒𝑡𝑎𝑖𝑛𝑒𝑑 = ∗ 100
𝑚𝑎𝑠𝑠 𝑏𝑒𝑓𝑜𝑟𝑒 𝑔𝑟𝑖𝑛𝑑𝑖𝑛𝑔
Equation 3
282.4𝑔 − 271.6𝑔
%𝑅𝑒𝑡𝑎𝑖𝑛𝑒𝑑 = = 𝟑. 𝟖𝟐%
282.4
Conclusion
Most of the ground kernels (99.15%) pass though the sieve with mesh 35 while
the percent retained is 0.85% after 6 minutes of grinding.

EXPERIMENTAL
B. Determination of Bulk Density

For the design of some equipment, bulk density of the material is needed. Bulk
density is the mass of the particles divided by the volume they occupy that includes the
space between the particles (ASTM D5004, 2001).
The bulk density of the sample can be calculated using,
𝑊𝑠
𝑝𝑏 = Equation 4
𝑉
Where:
𝑝𝑏 - bulk density of the sample (g/cm3);
𝑊𝑠 – weight of the sample (g);
v - the volume of container (cm3)
Laboratory Set-Up
Guyabano Seeds Guyabano Kernels Ground Kernel
Figure 4.6 Bulk Density Determination

EXPERIMENTAL
Material Apparatus
Guyabano seeds & kernels, Analytical balance
ground kernel 1L beaker
Objective
To determine the bulk density of guyabano seeds, kernel and ground kernel.
Hypothesis
The bulk density of guyabano seeds, kernel and ground kernel will be dependent
on its weight and volume.
Procedure
1. Place the guyabano seeds, kernel and ground kernel in a 1-L beaker until it is
fully occupied.
2. Weigh the samples.
3. Repeat for five trials.
4. Calculate the bulk density using the gathered data.
Data and Results

B.1. Bulk Density of Guyabano Seeds
Table 4.9 Bulk Density of Guyabano Seeds Results
Trial Mass of Seeds (g) Bulk Density (g/cm3)

1 463.4 0.4634
2 465.6 0.4656
3 462.8 0.4628
4 468.2 0.4682
5 460.4 0.4604
Average Bulk Density 0.4641

EXPERIMENTAL
Analysis
Using equation 3 and data from trial 1,
𝑊𝑠
𝑝𝑏 =
𝑉
463.4𝑔 𝒈
𝑝𝑏 = = 𝟎. 𝟒𝟔𝟑𝟒
1000𝑐𝑚3 𝒄𝒎𝟑
Computing for the average bulk density,
0.4634 + 0.4656 + 0.4628 + 0.4682 + 0.4604 𝒈

𝑝𝑎𝑣𝑒 = = 0.4641 ≈ 𝟎. 𝟒𝟔
5 𝒄𝒎𝟑
B.2. Bulk Density of Guyabano Seed Kernels

Table 4.10 Bulk Density of Guyabano Kernels Results
Trial Mass of Kernels (g) Bulk Density (g/cm3)

1 536.6 0.5366
2 530.2 0.5302
3 533.8 0.5338
4 539.2 0.5392
5 537.4 0.5374
Analysis
𝑊𝑠
𝑝𝑏 =
𝑉
536.6𝑔 𝒈
𝑝𝑏 = = 𝟎. 𝟓𝟑𝟔𝟔
1000𝑐𝑚3 𝒄𝒎𝟑
EXPERIMENTAL

0.5366 + 0.5302 + 0.5338 + 0.5392 + 0.5374 𝒈
𝑝𝑎𝑣𝑒 = = 0.5354 ≈ 𝟎. 𝟓𝟒
5 𝒄𝒎𝟑
B.3. Bulk Density of Ground Kernels

Table 4.11 Bulk Density of Ground Kernels Results
Trial Mass of Ground Kernels (g) Bulk Density (g/cm3)

1 410.6 0.4106
2 408.4 0.4084
3 415.2 0.4152
4 411.4 0.4114
5 412.2 0.4122
Analysis
𝑊𝑠
𝑝𝑏 =
𝑉
410.6𝑔 𝒈
𝑝𝑏 = = 𝟎. 𝟒𝟏𝟎𝟔
1000𝑐𝑚3 𝒄𝒎𝟑

0.4106 + 0.4084 + 0.4152 + 0.4114 + 0.4122 𝒈
𝑝𝑎𝑣𝑒 = = 0.4116 ≈ 𝟎. 𝟒𝟏
5 𝒄𝒎𝟑
Conclusion
Therefore, the bulk density of guyabano seeds, kernels and ground kernels are
0.46 g/cm3, 0.54 g/cm3, and 0.41 g/cm3 respectively.

EXPERIMENTAL
IV. Solvent Extraction of Ground Kernel

Solvent extraction is a technique widely used by researchers for the extraction of
oils from different plant oil seeds due to it cost effectiveness, simplicity, remarkable
reduction in solvent volume and short time needed for the extraction (Olawale, O.,
2016). According to the testing conducted by Adamson University Testing, Research,
and Development Center, the oil content of the guyabano seed kernel is 35% on wet
basis.
Laboratory Set-Up
Mixture
Cake
Ground
Hot Plate Filtration
Kernel
Miscella
Figure 4.7. Solvent Extraction and Filtration Process

EXPERIMENTAL
A. Determination of Type of Solvent for Extraction
Basis for Variation: In a study conducted by Dhoot (2011), different solvents of

different nature were used to extract oil, using the same extraction conditions.
Some of the solvents used by Dhoot was hexane, chloroform, and various
alcohols. With this, the researchers opted for solvents of different functional
groups, namely: chloroform, hexane, isopropanol, petroleum ether, and acetone.
Material Apparatus
Ground kernels Beaker
Chloroform, Hexane, Isopropanol, Hotplate
Petroleum Ether, Acetone2 Thermometer
Objective
To determine the best solvent to use for extraction of oil from ground guyabano
kernels.
Hypothesis
The best solvent that will give the highest amount of oil extracted is hexane
Procedure
1. Weigh three (3) sets of 280 g of ground guyabano kernels in a beaker

2. Add 840 mL of chloroform (Basis: 1:3), stir the mixture, and cover with foil
3. Place the beakers on the hotplate set at 45°C for 1 hour
4. Filter and distill the mixture to recover the oil and solvent
5. Repeat the procedure for hexane, petroleum ether, acetone, and isopropanol

EXPERIMENTAL
Data and Results
Table 4.12 Solvent for Extraction Results for Chloroform

Mass of Volume of
Mass of Oil
Trial Ground Solvent % Oil Yield Observation
(g)
Kernels (g) (mL)
The mixture turned a
1 280 840 78.2 57.82 shade darker compared
to other set-ups
to other set-ups
to other set-ups
Analysis
The average amount of oil extracted is computed as,

78.2 + 82.0 + 81.2
𝑎𝑣𝑒𝑟𝑎𝑔𝑒 𝑜𝑖𝑙 𝑎𝑚𝑜𝑢𝑛𝑡 = = 𝟖𝟎. 𝟒𝟕𝒈
3
The % oil yield is computed using the formula,

𝑎𝑐𝑡𝑢𝑎𝑙 𝑦𝑖𝑒𝑙𝑑
% 𝑦𝑖𝑒𝑙𝑑 = × 100%
𝑡ℎ𝑒𝑜𝑟𝑒𝑡𝑖𝑐𝑎𝑙 𝑦𝑖𝑒𝑙𝑑
The theoretical oil yield according to AdUTRDC is,

𝑇ℎ𝑒𝑜𝑟𝑒𝑡𝑖𝑐𝑎𝑙 𝑌𝑖𝑒𝑙𝑑 = 𝑀𝑎𝑠𝑠 𝑜𝑓 𝑘𝑒𝑟𝑛𝑒𝑙𝑠 × % 𝑂𝑖𝑙 𝑐𝑜𝑛𝑡𝑒𝑛𝑡 Equation 5
𝑇ℎ𝑒𝑜𝑟𝑒𝑡𝑖𝑐𝑎𝑙 𝑌𝑖𝑒𝑙𝑑 = 386.4𝑔 × 0.35
𝑇ℎ𝑒𝑜𝑟𝑒𝑡𝑖𝑐𝑎𝑙 𝑌𝑖𝑒𝑙𝑑 = 𝟏𝟑𝟓. 𝟐𝟒𝒈
Computing for the % oil yield using equation 5,
80.47
% 𝑦𝑖𝑒𝑙𝑑 = × 100% = 𝟓𝟗. 𝟓𝟎%
135.24𝑔
It was observed that chloroform extracted an average amount of 80.47g of oil
which represents 59.50% of oil from the ground kernels.

EXPERIMENTAL
Table 4.13 Solvent for Extraction Results for Hexane

Mass of Volume of
Mass of Oil
(g)
Kernels (g) (mL)
The miscella is
1 280 840 86.8 64.18 homogenous and has a
dark yellow color
The miscella is
dark yellow color
The miscella is
dark yellow color
Analysis

86.8 + 86.0 + 88.6
𝑎𝑣𝑒𝑟𝑎𝑔𝑒 𝑜𝑖𝑙 𝑎𝑚𝑜𝑢𝑛𝑡. = = 𝟖𝟕. 𝟏𝟑𝒈
3
% 𝑦𝑖𝑒𝑙𝑑 = × 100%


87.13
% 𝑦𝑖𝑒𝑙𝑑 = × 100% = 𝟔𝟒. 𝟒𝟑%
135.24𝑔
It was observed that hexane extracted an average amount of 87.13g of oil which
represents 64.43% of oil from the ground kernels.

EXPERIMENTAL
Table 4.14 Solvent for Extraction Results for Isopropanol

Mass of Volume of
Mass of Oil
(g)
Kernels (g) (mL)
The miscella is
dark yellow color
The miscella is
dark yellow color
The miscella is
dark yellow color
Analysis

89.6 + 88.8 + 91.4
𝑎𝑣𝑒𝑟𝑎𝑔𝑒 𝑜𝑖𝑙 𝑎𝑚𝑜𝑢𝑛𝑡 = = 𝟖𝟗. 𝟗𝟑𝒈
3
% 𝑦𝑖𝑒𝑙𝑑 = × 100%


89.93
% 𝑦𝑖𝑒𝑙𝑑 = × 100% = 𝟔𝟔. 𝟓𝟎%
135.24𝑔
It was observed that isopropanol extracted an average amount of 89.93g of oil

which represents 66.50% of oil from the ground kernels.

EXPERIMENTAL
Table 4.15 Solvent for Extraction Results for Petroleum Ether

Mass of Volume of
Mass of Oil
(g)
Kernels (g) (mL)
The miscella is
dark yellow color
The miscella is
dark yellow color
The miscella is
dark yellow color
Analysis

72.8 + 72.6 + 73.4
𝑎𝑣𝑒𝑟𝑎𝑔𝑒 𝑜𝑖𝑙 𝑎𝑚𝑜𝑢𝑛𝑡 = = 𝟕𝟐. 𝟗𝟑𝒈
3
% 𝑦𝑖𝑒𝑙𝑑 = × 100%


72.93
% 𝑦𝑖𝑒𝑙𝑑 = × 100% = 𝟓𝟑. 𝟗𝟑%
135.24𝑔
It was observed that petroleum ether extracted an average amount of 72.93g of

oil which represents 53.93% of oil from the ground kernels.

EXPERIMENTAL
Table 4.16 Solvent for Extraction Results for Acetone

Mass of Volume of
Mass of Oil
(g)
Kernels (g) (mL)
The miscella is
dark yellow color
The miscella is
dark yellow color
The miscella is
dark yellow color
Analysis

70.8 + 69.8 + 69.0
𝑎𝑣𝑒𝑟𝑎𝑔𝑒 𝑜𝑖𝑙 𝑎𝑚𝑜𝑢𝑛𝑡. = = 𝟔𝟗. 𝟖𝟕
3
% 𝑦𝑖𝑒𝑙𝑑 = × 100%


69.87
% 𝑦𝑖𝑒𝑙𝑑 = × 100% = 𝟓𝟏. 𝟔𝟔%
135.24𝑔
It was observed that acetone extracted an average amount of 69.87g of oil which
represents 51.66% of oil from the ground kernels.

EXPERIMENTAL
Table 4.16 Determination of Best Solvent for Solvent Extraction

Mass of
Volume of
Ground Type of Mass of % Oil
Trial Solvent Observation
Kernels Solvent Oil (g) Yield
(mL)
(g)
1 280 Chloroform 840 80.47 59.50 shade darker compared
to other set-ups
The miscella is
2 280 Hexane 840 87.13 64.43 homogenous and has a
dark yellow color
The miscella is
3 280 Isopropanol 840 89.93 66.50 homogenous and has a
dark yellow color
The miscella is
Petroleum
Ether
dark yellow color
The miscella is
3 280 Acetone 840 69.87 51.66 homogenous and has a
dark yellow color
Analysis
It was observed that isopropanol extracted the most amount of oil from the
ground guyabano kernels at 66.50% oil yield. In contrast, acetone extracted the least
amount of oil at 53.93% oil yield. The theoretical oil yield was based on the test
conducted by the Adamson University Testing, Research, and Development Center.
Conclusion
At 66.50% oil yield, isopropanol is the best solvent to use in the extraction of oil
from the ground guyabano kernels.

EXPERIMENTAL
B. Determination of the Mass Ratio of Ground Guyabano Kernel to Solvent
Basis for Variation: In a study conducted by Dhoot (2011), different solid to

solvent ratios are used such as 1:5, 1:10, 1:15 w/v. the researchers chose the
ratio 1:5 as basis since the deviation of the amount extracted in relation to the
increased ratio is low. Henceforth, the researchers used the ratios 1:3, 1:4, 1:5,
1:6, 1:7, as trials for the experiment.
Material Apparatus
Beakers
Ground Guyabano Kernel Analytical Balance
Isopropanol Hotplate
Thermometer
Objective
To determine the optimum mass ratio of ground guyabano kernel to solvent that
would result to highest amount of extracted oil.
Hypothesis
The higher the amount of solvent used for every amount of ground kernel, the
higher the yield of oil extracted.
Procedure
1. Weigh five (5) sets of 280 g of ground guyabano kernels in a beaker

2. Add 840 mL of isopropanol, stir the mixture and cover the beaker with foil
3. Place the beakers on the hotplate then set at 45°C for 1 hour.
4. Filter and distill the mixture to recover the oil and the solvent
5. Repeat procedure for 1120mL, 1400 mL, 1680mL, and 1960mL of isopropanol

EXPERIMENTAL
Data and Results
Table 4.13 Determination of Mass Ratio of Ground Kernels to Solvent

Mass of Volume of Mass Ratio
Mass of
Trial Ground Isopropanol (Kernel: % Oil Yield
Oil (g)
Kernels (g) (mL) Solvent)
1 280 840 1:3 92.2 68.18
2 280 1120 1:4 105.8 78.23
3 280 1400 1:5 121.4 89.77
4 280 1680 1:6 122.6 90.65
5 280 1960 1:7 123.0 90.95
Analysis
It was observed that the trial with the highest oil yield was the fifth trial with 1:7
w/v ratio of solids to solvent at 90.95%. However, it was also observed that the
deviation of the yield from the third and fourth trial ratio is low, at only 0.88% and 0.3%
difference, respectively.
The theoretical oil yield was based on the test conducted by the Adamson
University Testing, Research, and Development Center.

121.4𝑔
% 𝑦𝑖𝑒𝑙𝑑 = × 100%
135.24𝑔
% 𝑦𝑖𝑒𝑙𝑑 = 𝟖𝟗. 𝟕𝟕%
Conclusion
Therefore, the best ratio of guyabano seed kernels to solvent is 1:5 w/v.

EXPERIMENTAL
C. Determination of Optimum Extraction Temperature
Temperature is the most important parameter for solvent extraction specifically in

case of oil extraction as it affects the quality of oil.
Basis for Variation: In a study conducted by Dhoot (2011), it was stated that at
temperatures greater than 45°C, solvents’ solubility increases. Henceforth, the
researchers will temperatures greater than 45°C, specifically, 60°C, 75°C, 90°C.
Material Apparatus
Beakers
Ground Guyabano Kernel Analytical Balance
Thermometer
Objective
To determine the best temperature of extraction of guyabano seed oil
Hypothesis
Higher temperature would yield higher extracted oil.
Procedure
1. Weigh three (3) sets of 280 g of ground guyabano kernels in a beaker

2. Add 1400 mL of isopropanol, stir the mixture, and cover the beaker with foil
3. Place the beaker on a hotplate set at 60°C for 1 hour
5. Repeat procedure for temperatures 75°C and 90°C

EXPERIMENTAL
Data and Results
Table 4.14 Determination of Extraction Temperature Results
Mass of Mass
Ground Ratio Temp Mass of Oil % Oil
Trial Observation
Kernels (kernel: (⁰C) (g) Yield
(g) solvent)
The mixture does not boil,

1 280 1:5 60 121.8 90.39 and significant amount of
oil was recovered.
The mixture does not boil,

2 280 1:5 75 124.2 92.17
thus oil yield is higher.
Rapid boiling and
vaporization was
3 280 1:5 90 126.8 94.10 observed. Approximately
400mL of solvent
vaporized.
Analysis
It was observed that the trial with the highest oil yield was the third trial with a
temperature of extraction at 90⁰C yielding 94.10% of oil, however, although the
temperature set on the hotplate is at 90⁰C, the mixture remained constant at around
83⁰C since the boiling point of isopropanol is 82.6⁰C. Rapid boiling and vaporization of
solvent was observed, resulting to solvent loss. Thus, the researchers concluded that
the optimal temperature of extraction is at 75⁰C.
The % yield is computed using the formula,

EXPERIMENTAL
% 𝑦𝑖𝑒𝑙𝑑 = × 100%

𝑇ℎ𝑒𝑜𝑟𝑒𝑡𝑖𝑐𝑎𝑙 𝑌𝑖𝑒𝑙𝑑 = 𝑀𝑎𝑠𝑠 𝑜𝑓 𝑘𝑒𝑟𝑛𝑒𝑙𝑠 × % 𝑂𝑖𝑙 𝑐𝑜𝑛𝑡𝑒𝑛𝑡
𝑇ℎ𝑒𝑜𝑟𝑒𝑡𝑖𝑐𝑎𝑙 𝑌𝑖𝑒𝑙𝑑 = 385𝑔 × 0.35
𝑇ℎ𝑒𝑜𝑟𝑒𝑡𝑖𝑐𝑎𝑙 𝑌𝑖𝑒𝑙𝑑 = 𝟏𝟑𝟒. 𝟕𝟓𝒈

124.2𝑔
% 𝑦𝑖𝑒𝑙𝑑 = × 100%
134.75𝑔
% 𝑦𝑖𝑒𝑙𝑑 = 𝟗𝟐. 𝟏𝟕%
Conclusion
The best temperature of extraction is 75⁰C with a yield of 92.17%
D. Determination of Optimum Extraction Time
Basis for Variation: In a study conducted by Dhoot (2011), the longest

extraction time of the guyabano seed kernels in the extractor is 180 minutes.
Henceforth, the researchers will trial use 1, 2, 3, 4, and 5 hr as trials.

Material Apparatus
Beakers
Ground Guyabano Kernels Analytical Balance
Thermometer
Objective
EXPERIMENTAL
To determine the optimum time of extraction of guyabano seed oil
Hypothesis
Longer time of extraction would yield higher percentage of oil extracted.
Procedure
1. Weigh five (3) sets of 280 g of ground guyabano kernels in a beaker

2. Add 1400 mL of isopropanol, stir the mixture, and cover the beaker with foil
3. Place the beakers on the hotplate set at 75°C for 1 hour
5. Repeat procedures for times 2, 3, 4, and 5 hours
Data and Results
Table 4.15 Determination of Optimal Extraction Time Results

Mass of
Mass Ratio
Ground Temp Time Mass of % Oil
Trial (kernel: Observation
Kernels (⁰C) (hr) Oil (g) Yield
solvent)
(g)
1 280 1:5 75 1 123.8 91.87 Oil yield is low.
Oil yield is higher
2 280 1:5 75 2 126.2 93.65
compared to trial 1
Oil yield has minimal
3 280 1:5 75 3 126.6 93.95
increment.
4 280 1:5 75 4 127.0 94.25
increment
5 280 1:5 75 5 127.2 94.40
increment
Analysis
EXPERIMENTAL
It was observed that the trial with the highest oil yield was the fifth trial with an
extraction time of 5 hours yielding 94.29% of oil. However, the deviation of the yield of
the 5-hour extraction to 2, 3, and 4 hours extraction is minimal. Moreover, first trial, has
a significantly lower yield in comparison to the succeeding trials. Thus, the researchers
concluded that the optimal extraction time is 2 hours.
The % yield is computed using the formula,
% 𝑦𝑖𝑒𝑙𝑑 = × 100%

𝑇ℎ𝑒𝑜𝑟𝑒𝑡𝑖𝑐𝑎𝑙 𝑌𝑖𝑒𝑙𝑑 = 𝑀𝑎𝑠𝑠 𝑜𝑓 𝑘𝑒𝑟𝑛𝑒𝑙𝑠 × % 𝑂𝑖𝑙 𝑐𝑜𝑛𝑡𝑒𝑛𝑡
𝑇ℎ𝑒𝑜𝑟𝑒𝑡𝑖𝑐𝑎𝑙 𝑌𝑖𝑒𝑙𝑑 = 385𝑔 × 0.35
𝑇ℎ𝑒𝑜𝑟𝑒𝑡𝑖𝑐𝑎𝑙 𝑌𝑖𝑒𝑙𝑑 = 𝟏𝟑𝟒. 𝟕𝟓𝒈

126.2𝑔
% 𝑦𝑖𝑒𝑙𝑑 = × 100%
134.75𝑔
% 𝑦𝑖𝑒𝑙𝑑 = 𝟗𝟑. 𝟔𝟓%
Conclusion
The optimal extraction time for the extraction of guyabano seed oil is 2 hours with
a yield of 93.65%

EXPERIMENTAL
V. Filtration and Distillation of Miscella
Distillation is a process of heating a solution to split up two or more components

resulting to an overhead distillate and bottoms (Zurich, 2014). In order to separate the
oil from solvent, the recovered miscella undergone distillation, as shown in Figure 4.8,
resulting to a bottom product of oil which is needed in the succeeding processes, while
the distillate is the solvent that vaporizes which will be condensed and collected.
Material Apparatus
Analytical balance Erlenmeyer flask
Thermometer Beaker
Miscella from solvent extraction
Iron stand Pump
process
Hotplate Condenser
Funnel Ring clamp
Objective
To separate the oil from the isopropanol solvent.
Hypothesis
The mixture of miscella and cake would be separated into oil, isopropanol, and
filter cake upon filtration and distillation

EXPERIMENTAL
Laboratory Set-Up
miscella condenser
thermostat
Hot plate Recovered isopropanol
Figure 4.8 Distillation of Isopropanol from Miscella
Procedure
1. Fix a piece of filter paper into a funnel and pour the mixture of miscella and
ground kernels
2. Place the filtered miscella in a 1-L Erlenmeyer flask
3. Attach the Erlenmeyer flask to the distillation set-up

EXPERIMENTAL
4. Set the hotplate to 75ºC and distill the miscella until recovery of isopropanol
slows considerably
Data and Results
Table 4.16 Filtration of Miscella Results
Mass of
Trial Miscella/Ground Mass of Miscella (g) Mass of Cake (g)
Kernel (g)
1 1368.4 1226.4 141.8

2 1365.8 1224.2 141.0
3 1370.0 1223.2 144.2
Table 4.17 Distillation of Miscella Results
Volume of
Mass of Mass of
Recovered % Solvent Isopropanol
Trial Miscella Recovered
Isopropanol Recovery Losses (mL)
(g) Oil (g)
(mL)
1 1226.4 127.2 1345 96.07 55

2 1224.2 126.4 1298 92.71 102
3 1223.2 126.8 1324 94.57 76

EXPERIMENTAL
Analysis
The ground kernels are leached of oil and has now no significant role in the
succeeding processs. Thus, the ground kernels are removed by filtration. The filtration
process is done prior to distillation.
Distillation is done to simultaneously recover the oil and to effectively recover the
solvent used in the extraction.
The average mass of miscella is computed as:
1226.4 + 1224.2 + 1223.2

𝐴𝑣𝑒𝑟𝑎𝑔𝑒 𝑚𝑎𝑠𝑠 𝑜𝑓 𝑚𝑖𝑠𝑐𝑒𝑙𝑙𝑎 =
3
𝑨𝒆𝒓𝒂𝒈𝒆 𝒎𝒂𝒔𝒔 𝒐𝒇 𝒎𝒊𝒔𝒄𝒆𝒍𝒍𝒂 = 𝟏𝟐𝟐𝟒. 𝟔𝒈
The average mass of cake computed as:
141.8 + 141.0 + 144.2

𝐴𝑣𝑒𝑟𝑎𝑔𝑒 𝑚𝑎𝑠𝑠 𝑜𝑓 𝑐𝑎𝑘𝑒 =
3
𝑨𝒆𝒓𝒂𝒈𝒆 𝒎𝒂𝒔𝒔 𝒐𝒇 𝒄𝒂𝒌𝒆 = 𝟏𝟒𝟐. 𝟑𝟑𝒈
To compute for the solvent losses, the volume of the recovered solvent is
deducted from the input solvent. The calculation goes as,
𝑆𝑜𝑙𝑣𝑒𝑛𝑡 𝐿𝑜𝑠𝑠𝑒𝑠 (𝑚𝐿) = 𝑖𝑛𝑝𝑢𝑡 𝑣𝑜𝑙𝑢𝑚𝑒 − 𝑟𝑒𝑐𝑜𝑣𝑒𝑟𝑒𝑑 𝑣𝑜𝑙𝑢𝑚𝑒
𝑆𝑜𝑙𝑣𝑒𝑛𝑡 𝐿𝑜𝑠𝑠𝑒𝑠 (𝑚𝐿) = 1400𝑚𝐿 − 1345𝑚𝐿
𝑆𝑜𝑙𝑣𝑒𝑛𝑡 𝐿𝑜𝑠𝑠𝑒𝑠 (𝑚𝐿) = 𝟓𝟓𝒎𝑳
The average % solvent recovery can be computed as,
96.07% + 92.71% + 94.57%

𝐴𝑣𝑒𝑟𝑎𝑔𝑒 % 𝑠𝑜𝑙𝑣𝑒𝑛𝑡 𝑟𝑒𝑐𝑜𝑣𝑒𝑟𝑦 =
3
𝐴𝑣𝑒𝑟𝑎𝑔𝑒 % 𝑠𝑜𝑙𝑣𝑒𝑛𝑡 𝑟𝑒𝑐𝑜𝑣𝑒𝑟𝑦 = 𝟗𝟒. 𝟒𝟓%

EXPERIMENTAL
Similarly, the average solvent loss can be computed as,
55𝑚𝐿 + 102𝑚𝐿 + 76𝑚𝐿

𝐴𝑣𝑒𝑟𝑎𝑔𝑒 𝑆𝑜𝑙𝑣𝑒𝑛𝑡 𝐿𝑜𝑠𝑠 =
3
𝐴𝑣𝑒𝑟𝑎𝑔𝑒 𝑆𝑜𝑙𝑣𝑒𝑛𝑡 𝐿𝑜𝑠𝑠 = 𝟕𝟔. 𝟔𝟕𝒎𝑳
Conclusion
The average percentage of solvent loss is 94.45% which can be quantified as the
average volume of solvent lost at 76.67mL. Hence, solvent loss is inevitable.
VI. Base-Catalyzed Transesterification
Transesterification is an equilibrium reaction and occurs essentially by mixing the

reactants. In the transesterification of the vegetable oils, triglyceride reacts with an
alcohol in the presence of a strong acid or base, producing a mixture of fatty acid alkyl
esters and glycerol. The stoichiometric reaction needs 1 mol of a triglyceride and 3 mol
of an alcohol. However, an excess of alcohol is favored to increase the yield of alkyl
esters and to allow their better separation from the glycerol layer. The alkali-catalyzed
transesterification of vegetable oils, is known to proceed much faster than the acid-
catalyzed transesterification. (Rashid, 2008)

EXPERIMENTAL
Laboratory Set-Up
Mixture
(Oil+Methanol+NaOH)
Methyl
esters
Methanol
Hot Plate
with NaOH
Glycerol
Figure 4.9. Transesterification of Guyabano Seed Oil
A. Determination of Type of Catalyst for Transesterification
Basis for Variation: In a study conducted by Rashid et, al. (2008), the best
performing base catalyst are potassium hydroxide (KOH) and sodium hydroxide
(NaOH). Hence the researchers will use potassium hydroxide (KOH) and sodium
hydroxide (NaOH) as catalysts for the experimentation.
EXPERIMENTAL
Material Apparatus
Beakers
Guyabano Seed Oil
Hotplate
Sodium Hydroxide, Potassium Hydroxide
Thermometer
Methanol
Aluminum Foil
Objective
To determine the best base catalyst to use for the transesterification of guyabano
seed oil
Hypothesis
The best catalyst for the transesterification of guyabano seed oil is sodium
hydroxide (NaOH)
Procedure
1. In a beaker, place 90 grams of methanol, 2.2 grams of NaOH. Stir the mixture
until the NaOH is dissolved
2. Add 126.2 grams of oil in the beaker, stir, and cover with foil
3. Place the beakers on a hotplate set at 60°C for 120 mins
4. Let the mixture stand to settle the 2 phases obtained
5. Repeat procedure for KOH.

EXPERIMENTAL
Data and Results
Table 4.18 Determination of Catalyst for Transesterification
Mass Mass of Mass of Mass of Mass of

Type of
Trial of Oil Methanol Catalyst Glycero Methyl Observation
Catalyst
(g) (g) (g) l (g) Ester (g)
The mixture exists

1 126.2 75 KOH 1.5 78.6 45.0 in 2 phases. One
lighter yellow
methyl ester top
phase and one
darker yellow
2 126.2 75 NaOH 1.5 98.8 36.8 glycerol bottom
phase
Analysis
It was observed that the highest yield of glycerol is obtained by using sodium
hydroxide as catalyst for the transesterification of guyabano seed oil. The potassium
hydroxide, on the other hand, yielded more methyl ester than the desired glycerol.
The amount of methanol to be used in the transesterification process follows the

molar ratio of 1:6 or 1 mole of oil per 6 moles of methanol (Rashid, 2008). This means
that there is a need to determine the molecular mass of the oil, however, guyabano

EXPERIMENTAL
seed oil is a mixture of various fatty acids (Elagbar, 2016). Thus, the average molecular
mass of guyabano seed oil shall be computed.
The fatty acid profile of guyabano seed oil is presented in Table 4.18
Table 4.19 Fatty Acid Profile of Guyabano Seed Oil
Molecular Mass %
Fatty Acid Type of Fatty Acid
(g/mol) Composition
Palmitic Acid Saturated 256.43 18.98

Stearic Acid Saturated 284.48 5.28
Oleic Acid Monounsaturated 282.46 40.94
Palmitoleic Acid Monounsaturated 254.41 1.76
Linoleic Acid Polyunsaturated 280.45 33.02
Source: Rashid, 2008
The average molecular mass can be computed using a formula in the literature
“Elementary Principles of Chemical Processes” by Felder and Rousseau. The formula is
as follows:
𝐴𝑣𝑒𝑟𝑎𝑔𝑒 𝑀𝑜𝑙𝑒𝑐𝑢𝑙𝑎𝑟 𝑀𝑎𝑠𝑠 = 𝑥1 𝑀1 + 𝑥2 𝑀2 + ⋯ + 𝑥𝑛 𝑀𝑛
where: 𝑥 = the mole fraction of fatty acid

𝑀 = the molecular mass of the fatty acid

EXPERIMENTAL
The % composition is converted to mole fraction using a mass basis (100g) and
converting each mass of fatty acids to moles. The mole fraction is calculated as the
number of moles of a fatty acid divided by the total moles present. (Felder, 2000) The
calculation is as follows:
𝑚𝑎𝑠𝑠 𝑜𝑓𝑓𝑎𝑡𝑡𝑦 𝑎𝑐𝑖𝑑
𝑛𝑜. 𝑜𝑓 𝑚𝑜𝑙𝑒𝑠 =
𝑚𝑜𝑙𝑒𝑐𝑢𝑙𝑎𝑟 𝑚𝑎𝑠𝑠 𝑜𝑓 𝑓𝑎𝑡𝑡𝑦 𝑎𝑐𝑖𝑑
18.98𝑔
𝑛𝑜. 𝑜𝑓 𝑚𝑜𝑙𝑒𝑠 =
256.43𝑔
𝑚𝑜𝑙
𝑛𝑜. 𝑜𝑓 𝑚𝑜𝑙𝑒𝑠 = 𝟎. 𝟎𝟕𝟒𝟎

The mole fraction is calculated as follows:
𝑛𝑜. 𝑜𝑓 𝑚𝑜𝑙𝑒𝑠 𝑜𝑓 𝑓𝑎𝑡𝑡𝑦 𝑎𝑐𝑖𝑑

𝑥1 =
𝑡𝑜𝑡𝑎𝑙 𝑛𝑜. 𝑜𝑓 𝑚𝑜𝑙𝑒𝑠
0.0740
𝑥1 =
0.362
𝑥1 = 𝟎. 𝟐𝟎𝟒𝟒
Table 4.20 Composition of Fatty Acids of Guyabano Seed Oil
Mass of Fatty Molecular

Fatty Acid No. of moles Mole Fraction
Acid (g) Mass (g/mol)
Palmitic Acid 18.98 256.43 0.0740 0.2044

Stearic Acid 5.28 284.48 0.0185 0.0511
Oleic Acid 40.94 282.46 0.1449 0.4003
Palmitoleic Acid 1.76 254.41 0.0069 0.0191
Linoleic Acid 33.02 280.45 0.1177 0.3251

EXPERIMENTAL
Consequently, the average molecular mass is calculated as:

𝑔 𝑔 𝑔
𝐴𝑣𝑒𝑟𝑎𝑔𝑒 𝑀𝑊 = (0.2044) (256.43 ) + (0.0511) (284.48 ) + (0.4003) (282.46 )
𝑚𝑜𝑙 𝑚𝑜𝑙 𝑚𝑜𝑙
𝑔 𝑔
+ (0.0191) (254.41 ) + (0.3251) (280.45 )
𝑚𝑜𝑙 𝑚𝑜𝑙
𝒈
𝐴𝑣𝑒𝑟𝑎𝑔𝑒 𝑀𝑊 = 𝟐𝟕𝟔. 𝟎𝟓𝟑𝟓
𝒎𝒐𝒍
Conclusion
The best catalyst to use is sodium hydroxide as is yielded the most amount of the
desired glycerol
B. Determination of Catalyst Loading for Transesterification
Basis for Variation: In a study conducted by Rashid et, al. (2008), the
concluded best catalyst loading is 1% by mass. Hence, the researchers will use
the loadings 0.5%, 1.0%, 1.5%, 2.0%, and 2.5%
Material Apparatus
Beakers
Guyabano Seed Oil
Hotplate
Sodium Hydroxide
Thermometer
Methanol
Aluminum Foil
Objective

EXPERIMENTAL
To determine the optimal catalyst loading for transesterification
Hypothesis
The optimal catalyst loading is 1% of the total mass of the reacting mixture
Procedure
1. In a beaker, place 75g of methanol and 1g of NaOH. Stir the mixture.

2. Add 126.2 grams of guyabano seed oil and cover with foil
3. Place the beakers on a hot plate set to 60C for 120 mins
4. Let the mixture stand to separate the 2 phases formed
5. Repeat the procedure for catalyst loading of 2.2, 3.2, 4.4, and 5.4g
Data and Results
Table 4.21 Determination of Catalyst Loading for Transesterification
Mass of Mass of Mass of Mass of

Mass of
Trial Methanol Catalyst Glycerol Methyl Observation
Oil (g)
(g) (g) (g) Ester (g)
Most of the guyabano

1 126.2 90 1.2 11.4 198.4
seed oil did non react
Some of the
2 126.2 90 2.2 32.2 180.2 guyabano seed oil
did not react
A homogenous
3 126.2 90 3.2 91.8 122.6
phase was obtained

EXPERIMENTAL
A homogenous
4 126.2 90 4.4 94.0 120.2
phase was obtained
A homogenous
5 126.2 90 5.4 94.2 119.4
phase was obtained
Analysis
It was observed that the highest yield of glycerol is obtained using the 5 th trial
with a catalyst loading of 2.5%. However, it was also observed that the deviation of the
glycerol yield from that of the 4th trial at 2.0% catalyst loading is low. Hence, the
researcher’s chose the 4th trial as the optimum catalyst loading for the transesterification
of guyabano seed oil.
The amount of catalyst to be used is called the catalyst loading and it is

dependent on the total mass of the transesterification reaction mixture. Thus, the
catalyst loading is calculated as follows:
𝑚𝑎𝑠𝑠 𝑜𝑓 𝑐𝑎𝑡𝑎𝑙𝑦𝑠𝑡
𝐶𝑎𝑡𝑎𝑙𝑦𝑠𝑡 𝐿𝑜𝑎𝑑𝑖𝑛𝑔 (%𝑚𝑎𝑠𝑠) = × 100%
𝑚𝑎𝑠𝑠 𝑜𝑓 𝑚𝑒𝑡ℎ𝑎𝑛𝑜𝑙 + 𝑚𝑎𝑠𝑠 𝑜𝑓 𝑜𝑖𝑙
𝑚𝑎𝑠𝑠 𝑜𝑓 𝑐𝑎𝑡𝑎𝑙𝑦𝑠𝑡
1% = × 100%
90𝑔 + 126.2𝑔
𝑚𝑎𝑠𝑠 𝑜𝑓 𝑐𝑎𝑡𝑎𝑙𝑦𝑠𝑡 = 2.162𝑔 ≈ 𝟐. 𝟐𝒈
Conclusion

EXPERIMENTAL
The best catalyst loading is 2.0% mass as it yielded the most amount of the
desired glycerol
C. Determination of the Optimal Molar Ratio of Oil to Methanol
concluded optimal ratio of oil to methanol is 1 mole of oil per 6 moles of
methanol. Hence, the researchers will use the ratios 1:3, 1:6, and 1:9 for the
experimentation.
Material Apparatus
Beakers
Guyabano Seed Oil
Hotplate
Sodium Hydroxide
Thermometer
Methanol
Aluminum Foil
Objective
To determine the optimal ratio molar ratio of oil to methanol
Hypothesis
The optimal ratio to use is 1 mole of oil to 6 moles of methanol
Procedure
1. In a beaker, place 75g of methanol and 4.4g of NaOH. Stir the mixture.
2. Add 126.2 grams of guyabano seed oil, stir, and cover with foil
3. Place the beaker on a hot plate set to 60C for 120 mins

EXPERIMENTAL
4. Let the mixture stand to separate the 2 formed

5. Repeat procedure for amounts 90, and 135g of methanol
Data and Results
Table 4.22 Determination of the Optimal Molar Ratio of Oil to Methanol
Molar
Ratio of
Trial of Oil Methanol Catalyst Glycerol Methyl Observation
Oil to
(g) (g) (g) (g) Ester (g)
Methanol
A homogenous
1 126.2 45 4.4 1:3 44.8 165.8 phase was
observed
A homogenous
2 126.2 90 4.4 1:6 95.6 118.8 phase was
observed
A homogenous
3 126.2 135 4.4 1:9 97.8 115.6 phase was
observed
Analysis
It was observed that the highest yield of glycerol is obtained using the 3 rd trial
with an oil to methanol molar ratio of 1:9. However, it was also observed that the

EXPERIMENTAL
deviation of the yield of glycerol of the 3rd trial to the second is very low or further
increasing the ratio is insignificant to the yield.
The amount of methanol to be used is determined by using stoichiometry. Thus,

the methanol to be reacted is calculated as follows:
𝑚𝑎𝑠𝑠 𝑜𝑓 𝑜𝑖𝑙 6 𝑚𝑜𝑙 𝑚𝑒𝑡ℎ𝑎𝑛𝑜𝑙

𝑚𝑎𝑠𝑠 𝑜𝑓 𝑚𝑒𝑡ℎ𝑎𝑛𝑜𝑙 (𝑔) = × × 𝑚𝑜𝑙𝑎𝑟 𝑚𝑎𝑠𝑠 𝑜𝑓 𝑚𝑒𝑡ℎ𝑎𝑛𝑜𝑙
𝑚𝑜𝑙𝑎𝑟 𝑚𝑎𝑠𝑠 𝑜𝑓 𝑜𝑖𝑙 1 𝑚𝑜𝑙 𝑜𝑖𝑙
126.2𝑔 6 𝑚𝑜𝑙 𝑚𝑒𝑡ℎ𝑎𝑛𝑜𝑙 𝑔

𝑚𝑎𝑠𝑠 𝑜𝑓 𝑚𝑒𝑡ℎ𝑎𝑛𝑜𝑙 (𝑔) = 𝑔 × × 32.042
276.0535 1 𝑚𝑜𝑙 𝑜𝑖𝑙 𝑚𝑜𝑙
𝑚𝑜𝑙
𝑚𝑎𝑠𝑠 𝑜𝑓 𝑚𝑒𝑡ℎ𝑎𝑛𝑜𝑙 (𝑔) = 87.89𝑔 ≈ 𝟗𝟎𝒈 𝒎𝒆𝒕𝒉𝒂𝒏𝒐𝒍
Conclusion
The molar ratio of oil to methanol is 1:6 as is yielded the optimal amount of the
desired glycerol
D. Determination of the Optimal Temperature for Transesterification
concluded optimal temperature for transesterification is 60 degrees Celsius.
Hence, the researchers will use the ratios 45, 60, and 75 degrees Celsius for the
experimentation.
Material Apparatus

EXPERIMENTAL
Beakers
Guyabano Seed Oil
Hotplate
Sodium Hydroxide
Thermometer
Methanol
Aluminum Foil
Objective
To determine the best temperature for the transesterification of guyabano seed

oil
Hypothesis
The higher the temperature, the better the yield of the desired glycerol product
Procedure
1. Prepare 3 sets of methanol, on a beaker, weighing 90 grams each

2. Dissolve 4.4 grams of sodium hydroxide on each beaker respectively
3. Add 126.2 grams of guyabano seed oil on each beaker and cover with aluminum
foil to prevent methanol from evaporating
4. Place the three beakers on a hot plate set to 45 degrees Celsius for 120 mins
5. After the reaction, let the mixture cool and separate the glycerol phase from the
methyl ester phase by decantation.
6. Weigh the glycerol product and methyl ester and tabulate the data
7. Repeat the process for temperatures 60 and 75 degrees Celsius
Data and Results
Table 4.23 Determination of the Optimal Temperature for Transesterification

EXPERIMENTAL
Tempera
ture of
Trial of Oil Methanol Catalyst Glycerol Methyl Observation
Reaction
(g) (g) (g) (g) Ester (g)
(°C)
A homogenous
1 126.2 90 4.4 45 88.2 172.8 phase was
observed
A homogenous
2 126.2 90 4.4 60 94.2 119.6 phase was
observed
Rapid boiling
3 126.2 90 4.4 75 37.2 45.2 ang vaporization
was observed
Analysis
It was observed that the highest yield of glycerol is obtained using the 2nd trial
with a reaction temperature of 60°C. In contrast, the 1st trial had a lower yield than the
2nd trial. It was also observed that the 3rd trial’s temperature remained at around 65°C,
even with the hotplate set at 75°C. This is due to the boiling point of methanol (64.7°C)
being lower to the set temperature. Rapid boiling and vaporization of methanol was also
observed resulting to a lower yield since methanol is a reagent to the reaction.
Conclusion
The optimal temperature of transesterification is 60°C
D. Determination of the Optimal Time for Transesterification

EXPERIMENTAL
concluded optimal time for transesterification is 120 minutes. Hence, the
researchers will use the times 60, 120, and 180 minutes for the experimentation.
Material Apparatus
Beakers
Guyabano Seed Oil
Hotplate
Sodium Hydroxide
Thermometer
Methanol
Aluminum Foil
Objective
To determine the optimal time of reaction for the transesterification of guyabano

seed oil
Hypothesis
The longer the time, the better the yield of the desired glycerol product
Procedure
1. In a beaker, place 90g of methanol and 4.4g of NaOH. Stir the mixture.
2. Add 126.2 grams of guyabano seed oil, stir, and cover with foil
3. Place the beaker on a hot plate set to 60C for 60 minutes
4. Let the mixture stand to separate the 2 phases formed
5. Repeat the procedures for times 120 and 180 minutes
Data and Results
Table 4.24 Determination of Optimal Time for Transesterification

EXPERIMENTAL
Mass Mass of Mass of Time of Mass of Mass of

Trial of Oil Methanol Catalyst Reaction Glycerol Methyl Observation
(g) (g) (g) (°C) (g) Ester (g)
A homogenous
1 126.2 90 4.4 60 84.6 174.2 phase was
observed
A homogenous
2 126.2 90 4.4 120 96.6 111.6 phase was
observed
A homogenous
3 126.2 90 4.4 180 97.4 112.6 phase was
observed
Analysis
It was observed that the highest yield of glycerol is obtained using the 3rd trial
with a reaction time of 180 minutes. However, the increase of the glycerol yield upon
increasing the reaction time from 120 to 180 minutes is not very significant. In contrast,
the 1st trial had a lower yield than the 2nd trial. Thus the researchers concluded that the
2nd trial is the optimal reaction time for transesterification at 120 minutes
Conclusion
The optimal reaction time for the transesterification of guyabano seed oil is 120
minutes
VII. Hydrogenolysis
Hydrogenolysis (dehydration followed by hydrogenation) is a chemical reaction

whereby a carbon–carbon or carbon–heteroatom single bond is cleaved or undergoes
lysis (breakdown) by hydrogen. Hydrogenolysis of biomass-derived glycerol is an
alternative route to sustainable production of propylene glycol (Wang, S., et.al, 2007).

EXPERIMENTAL
Previous research shows that hydrogenolysis of glycerol to propane diols proceed via
dehydration of glycerol to acetol on acid catalysts and consecutive hydrogenation over
metal catalysts (Balaraju, M., et.al, 2008). Catalyst plays a vital role in the
hydrogenolysis of the glycerol reaction (Meher, L.C., et.al, 2009).
Laboratory Set-Up
Condenser
Glycerol
Oil Bath
Reaction Mechanism:

EXPERIMENTAL
C3H8O3 C3H6O2 C3H8O2

-H2O -H2
From transesterification process, 96.6g of glycerol will be used for dehydration

process. The theoretical amount of acetol to be produced is computed as follows:
𝑀𝑎𝑠𝑠 𝑜𝑓 𝐺𝑙𝑦𝑐𝑒𝑟𝑜𝑙 1 𝑚𝑜𝑙 𝐺𝑙𝑦𝑐𝑒𝑟𝑜𝑙

𝑇ℎ𝑒𝑜𝑟𝑒𝑡𝑖𝑐𝑎𝑙 𝑃𝑟𝑜𝑝𝑦𝑙𝑒𝑛𝑒 𝐺𝑙𝑦𝑐𝑜𝑙 = 𝑥 𝑥 𝑀𝑊 𝑜𝑓 𝑃𝐺
𝑀𝑊 𝑜𝑓 𝐺𝑙𝑦𝑐𝑒𝑟𝑜𝑙 1 𝑚𝑜𝑙 𝑃𝐺
96.6𝑔 1 𝑚𝑜𝑙 𝐺𝑙𝑦𝑐𝑒𝑟𝑜𝑙 𝑔

𝑇ℎ𝑒𝑜𝑟𝑒𝑡𝑖𝑐𝑎𝑙 𝑃𝐺 = 𝑔 𝑥 𝑥 76.09 𝑃𝐺
92.11 𝐺𝑙𝑦𝑐𝑒𝑟𝑜𝑙 1 𝑚𝑜𝑙 𝑃𝐺 𝑚𝑜𝑙
𝑚𝑜𝑙
𝑇ℎ𝑒𝑜𝑟𝑒𝑡𝑖𝑐𝑎𝑙 𝐴𝑐𝑒𝑡𝑜𝑙 = 79.80𝑔 𝑜𝑓 𝑃𝐺
From hydrogenolysis process, 96.6g of glycerol will be used for the process.

EXPERIMENTAL
A. Determination of Optimum Temperature in Hydrogenolysis
Basis of Constant Parameters and Variation
From the study conducted by Dasari, M.A., et. al in 2004, the optimum
parameters are presented in the table below which will be used for the experiment.
Parameter Amount/Value
Temperature 240 °C
Catalyst Copper
Catalyst (w/w %) 5%
Additionally, in a study by Suppes, G. (2006), the hydrogenolysis was done at a

temperature of 240 °C having copper as one of the best metal catalyst in the process.
Material Apparatus
Analytical balance Hot Plate
Glycerol, Copper
Thermometer Beaker
Objective
To determine the temperature that would yield the highest amount of propylene
Glycol.
Hypothesis
The longer the reaction time, the higher the amount of propylene glycol to be
recovered. Thus, 6 hours would yield higher amount of propylene glycol.

EXPERIMENTAL
Procedure
1. Place 96.6g of glycerol in a beaker then add 5% (w/w) catalyst with respect to the
solution.
2. React each mixture at 200°C for 4 hours
3. Repeat the procedure for temperatures 220, 240, 260, 280°C
Data and Results
Table 4.25 Results for the Variation of Temperature in Hydrogenolysis
Trial Mass of Type of Time Temperature Mass of Percent

Glycerol Catalyst (hours) (°C) Propylene Yield
(g) Glycol (g) (%)
1 96.6 Cu 4 200 50.8 66.76
2 96.6 Cu 4 220 58.4 76.75
3 96.6 Cu 4 240 67.6 88.84
4 96.6 Cu 4 260 68.2 89.63
5 96.6 Cu 4 280 68.6 90.16
Analysis
It can be observed that further increasing the temperature also increases the
percentage yield of propylene glycol. However, choosing the highest reaction time is
uneconomical especially with a minimal difference, thus, 3 hours is chosen with a
percentage yield of 88.84% propylene glycol.
Conclusion
The best reaction temperature to be used for the conversion of glycerol to propylene
glycol is 240°C with a percentage yield of 88.84% propylene glycol.
B. Determination of Optimum Catalyst Loading

EXPERIMENTAL
Temperature 240 °C
Catalyst Copper
Catalyst (w/w %) 5%

Material Apparatus
Glycerol, Copper
Thermometer Beaker
Objective
To determine the catalyst loading that would yield the highest amount of
propylene Glycol.
Hypothesis
5% catalyst loading would yield the highest amount of propylene glycol
Procedure
1. Place 96.6g of glycerol in a beaker then add 5% (w/w) catalyst with respect to
the solution.

EXPERIMENTAL
2. React the mixture at 240°C for 4 hours

3. Repeat the procedure for 3, 4, 5, 6, 7%
Data and Results
Table 4.25 Results for the Variation of Time in Hydrogenation
Trial Mass of Catalyst Mass of Temperature Mass of Percent

Glycerol Loading Catalyst (°C) Propylene Yield
(g) (%) (g) Glycol (g) (%)
1 96.6 3 3.0 240 48.2 63.35
2 96.6 4 4.0 240 59.2 77.80
3 96.6 5 5.0 240 65.4 85.95
4 96.6 6 5.8 240 69.0 90.68
5 96.6 7 6.8 240 69.2 90.94
Analysis
It can be observed that further increasing the catalyst loading also increases the
percentage yield of propylene glycol. However, choosing the highest reaction time is
uneconomical especially with a minimal difference, thus, 6% catalyst loadinng is chosen
with a percentage yield of 90.68% propylene glycol.
Conclusion
The best catalyst laoding to be used for the conversion of glycerol to propylene
glycol is 6% with a percentage yield of 90.68% propylene glycol.
C. Determination of Optimum Time in Hydrogenolysis
EXPERIMENTAL
Temperature 240 °C
Catalyst Copper
Catalyst (w/w %) 5%

In the study conducted by Dasari, M.A., et. al in 2004, the time used for the
hydrogenation process is 4 hours. Thus, the researchers will vary the reaction time from
1 hours to 5 hours with an interval of 1 hour.
Material Apparatus
Glycerol, Copper
Thermometer Beaker
Objective
To determine the reaction time that would yield the highest amount of propylene
Glycol.
Hypothesis
The optimum time for hydrogenolysis is 4 hours
Procedure
1. Place 96.6g of glycerol in a beaker then add 6% (w/w) catalyst with respect to the
solution.
2. React the mixture at 240°C for 2 hours
EXPERIMENTAL
3. Repeat the procedure for 3, 4, 5, 6 hours
Data and Results
Table 4.25 Results for the Variation of Time in Hydrogenation
Trial Mass of Catalyst Time Temperature Mass of Percent

Glycerol Loading (hours) (°C) Propylene Yield
(g) (%) Glycol (g) (%)
1 96.6 6 2 240 38.2 50.20
2 96.6 6 3 240 56.2 73.86
3 96.6 6 4 240 70.0 92.00
4 96.6 6 5 240 70.6 92.78
5 96.6 6 6 240 70.8 93.05
Analysis
It can be observed that further increasing the time also increases the percentage
yield of propylene glycol. However, choosing the highest reaction time is uneconomical
especially with a minimal difference thus 4 hours is chosen with a percentage yield of
92.00% propylene glycol.
Conclusion
The best reaction time to be used for the conversion of glycerol to propylene glycol
is 4 hours with a percentage yield of 90.00% propylene glycol.

EXPERIMENTAL
Dehulling Seed coat
Seed Kernels
Drying
Dried Kernels
Size Reduction
Isopropanol Ground Kernels
Solvent Extraction
Filtration Cake
Miscella
Distillation
Methanol, NaOH Oil
Transesterification
Glycerol + methyl-ester
Decantation Methyl
ester
Glycerol
Dehydration
Acetol
Hydrogenation
PROPYLENE GLYCOL
EXPERIMENTAL

Experimental Sept9

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PAMANTASAN NG LUNGSOD NG MAYNILA

University of the City of Manila

Hydrogenolysis of Glycerol Derived from Guyabano (Annona muricata) Seeds for

OBJECTIVES OF THE EXPERIMENTAL STUDY

Table 4.1 Standard and Exiting Properties

To determine the parameters that will produce the highest conversion of

To identify the equivalent unit operation and equipment of each laboratory

Hydrogenolysis of Glycerol Derived from Guyabano (Annona muricata) Seeds for

The experimental method of the study focused on performing the process in a

I. Preparation and Conditioning of Raw Material

II. Conversion Process

1. Solvent Extraction of Ground Seed Kernel

III. Testing Procedures

1. Oil and moisture content of the Guyabano seeds

Hydrogenolysis of Glycerol Derived from Guyabano (Annona muricata) Seeds for

RAW MATERIAL, REAGENTS AND APPARATUS

Figure 4.1. Collection of Raw Material

Table 4.2 Composition of Guyabano Seed

Hydrogenolysis of Glycerol Derived from Guyabano (Annona muricata) Seeds for

Table 4.3. Reagents and their Corresponding Properties

Reagent Process Chemical Structure Function Properties

Boiling point: 82.6 °C

Boiling point: 64.7 °C

Hydrogenolysis of Glycerol Derived from Guyabano (Annona muricata) Seeds for

The laboratory apparatus with their corresponding description are presented in

Table 4.4. List of Laboratory Apparatus

Laboratory Apparatus Description

Used to dehull the guyabano seeds

Container used for measuring,

A digital instrument that is used to

Used for drying the guyabano seed

Hydrogenolysis of Glycerol Derived from Guyabano (Annona muricata) Seeds for

Used to reduce the particle size of

Electrically-powered device used for

Used to stir chemicals and liquids

Used to measure temperature

A piece of porous paper used for

Hydrogenolysis of Glycerol Derived from Guyabano (Annona muricata) Seeds for

Used to on/off the distillation set-up

Used to maintain or adjust the

Used to supply cooling water to the

Used for liquefying recovered solvent

Hydrogenolysis of Glycerol Derived from Guyabano (Annona muricata) Seeds for

Used to measure, mix, and store

Used to measure the amount of time

Used to store liquids and reagents

Used to transfer small volume of

Hydrogenolysis of Glycerol Derived from Guyabano (Annona muricata) Seeds for

PREPARATION AND CONDITIONING OF RAW MATERIAL

I. Dehulling of Guyabano Seeds

Guyabano Seeds Guyabano Kernels

Determination of Mass Ratio of Guyabano Seed and Seed Kernel

Materials and Apparatus

Hydrogenolysis of Glycerol Derived from Guyabano (Annona muricata) Seeds for

The seed kernels and seeds have a definite mass ratio.

1. Weigh 500 g of guyabano seeds.

Figure 4.3 Guyabano Seed-Kernel Mass Ratio Determination

Hydrogenolysis of Glycerol Derived from Guyabano (Annona muricata) Seeds for

Data and Results

Table 4.5 Determination of Guyabano Seed-Kernel Mass Ratio

Trial Mass of Seeds (g) Mass of Kernel (g) Ratio (S:K)

386.2 + 387.4 + 384.4 + 390.2 + 383.8

Hydrogenolysis of Glycerol Derived from Guyabano (Annona muricata) Seeds for