Summative Practical

Biodiesels Synthesis and Analysis

Stage 2 Chemistry - SACE: 904243R
Name: Gia Giao Bao Nguyen
Summative Practical
Biodiesels Synthesis and Analysis
Stage 2 Chemistry - SACE: 904243R
Name: Gia Giao Bao Nguyen
Introduction
What is Biodiesel?
Biodiesel in particular, or biofuel in general, is a type of renewable energy, having properties
equivalent to diesel fuel. However, instead of being produced from petroleum, Biodiesel is derived from
vegetable oils or animal fats or even waste cooking oil (Biodiesel.org, 2020). The process used to
convert these oils to Biodiesel is called transesterification, which is described clearly below. While oil
directly from the agricultural industry is the greatest potential source, it is not produced commercially
simply because it is too expensive to produce raw oil. It is as well too costly to compete with fossil fuel,
after the expense of converting it to biodiesel has been added on (Afdc.energy.gov, 2020). Waste
vegetable oil can also be freely sourced or processed for a small price, assuming the waste oil has to be
processed to eliminate impurities before conversion to biodiesel. Biodiesel produced from waste
vegetable oil can eventually compete with fossil diesel as a result.
Benefits of Biodiesel
Biodiesel has many environmental properties (Biodidel.com, 2020). The main benefit of
biodiesel is that the fuel produces no net output of carbon in the form of carbon dioxide (CO 2), which
causes air pollution in particular, and environmental pollution in general. Technically, CO 2, which is one
of the greenhouse gases, emits infra-red radiation which causes the warmup of the Earth and lead to
greenhouse effect. Therefore, increased emission of greenhouse gases, in particular CO 2, enhances
greenhouse effect, in which it absorbs more radiation and gets the Earth getting warmer.
Biodiesel Production
Almost all biodiesel is produced using base catalysed transesterification as it is the most
economical process requiring only low temperature and pressure (Afdc.energy.gov, 2020). The
transesterification process is the reaction of a triglyceride (fat/oil) with an alcohol to form esters and
glycerol. A triglyceride has a glycerine molecule as its base with 3 long chain fatty acids attached. The
characteristics of the fat are determined by the nature of the fatty acids attached to the glycerine. The
nature of fatty acids can in turn affects the characteristics of biodiesel. During the esterification process
(Afdc.energy.gov, 2020), the triglyceride is reacted with alcohol in the presence of a catalyst, usually a
strong alkaline like potassium hydroxide which has been found to be more suitable for the methyl ester
biodiesel production. The alcohol reacts with the fatty acids to form the mono-alkyl ester, or biodiesel
and crude glycerol. In most production, methanol is the alcohol used (methanol produces methyl esters)
and is base catalysed by potassium hydroxide.
The figure below shows a chemical process for methyl ester biodiesel. The reaction between the
fat or oil and the alcohol is a reversible reaction and so the alcohol must be added in excess to drive the
reaction towards the right and ensure complete conversion.

Figure 1. Chemical process of methyl ester biodiesel (Available at: http://www.esru.strath.ac.uk/)

Materials (as provided)

Reagents
Chemical Form Quantity
Summative Practical
Biodiesels Synthesis and Analysis
Stage 2 Chemistry - SACE: 904243R
Name: Gia Giao Bao Nguyen
catalyst solution 5% w/v 7.5g *do not exceed
KOH in methanol this amount
oil Liquid 50g
beads Solid 2-3
Distilled water liquid 150mL

 Additional equipment  Boiling points of Reactants/Products

Apparatus Size Number Oil Olive oil
quick-fit apparatus for 1 Biodiesel formed assorted
reflux and distillation Glycerol
separating funnel 1 Methanol 25mL
measuring cylinder 25mL 1 Water 0-2000C
thermometer 0-2000C 1 KOH 50mL
conical flask 50mL 1
beakers 100mL 2

Method
Reflux
As per task sheet, this process is conducted (figure 1) to achieve the
transesterification reaction of olive oil with methanol catalysed with potassium
hydroxide, provided with a heating mantle, adjustable jack, a volumetric flask
and a condenser. Methanol and the catalyst are added in the volumetric flask,
in the amounts established for each experiment. The olive oil with the solution
is heated to 700C, which is the temperature established for the reaction. The
mixture is vigorously refluxed and as a result, biodiesel is produced as the
obtained fatty acid methyl ester (FAME) yield at 50 minutes of reaction time.
The transesterification product was allowed to stand in a separating funnel for
glycerol separation.
Separation
As per task sheet, this separation process is made to purify out the ester
(biodiesel) that formed from the reflux process. It is observed that there are two layers in the conical
flask (figure 2); the top layer with an olive colour is ester which takes up the most, and the thin layer in
the bottom is the glycerol which has a brownish colour. The liquids in the flask is then poured in the
separator and it keeps forming 2 layers with two totally different colours. The glycerol is always
forming in the bottom due to its gravity of 1.26 which is slightly denser than water, hence being easily
separated out. Distilled water is added in between each separation to ensure there is a minimum glycerol
left in the ester. This is explained that glycerol is highly soluble in water due to the hydrogen-bonding
between hydrogen in glycerol with water molecules. In addition, the ester is only slightly water-soluble
since it doesn’t engage in hydrogen bonding and is therefore intermediate in boiling points between the
alkane

Safety hazards/ Ethical risks

Hazard Precaution
Flame Tying long hair up;
Moving away any fire-catch items;
Hygiene Washing hands with soap, or Wearing gloves on;
Safety/Glass Wearing aprons and goggles to protect the body and the eyes;
Hot water/equipment Working carefully to prevent spilling the water on others and
getting burnt;
Summative Practical
Biodiesels Synthesis and Analysis
Stage 2 Chemistry - SACE: 904243R
Name: Gia Giao Bao Nguyen
Disinfection Disinfecting the aprons and googles, or any supplies that have
been used during the experiment.

Results
Enthalpy of Combustion of Olive Oil Calculation
Qwater =mwater ×C water × Δ T =100 × 4.18× 9.4=3934.84 J
mbiofuel 0.24 −4
n biofuel = = ≈ 8.203 × 10 mol
−1
M biofuel 292.56
Δ H =4789.69 kJ . mol
Qwater 3934.84 −1
∆ H= = =4789694.8 J . mol =4789.69 kJ .m
nbiofuel 0.24
292.56
Table 1. This table shows the obtained data of our group. The final result of the enthalpy of combustion
of olive oil with 3 wash is shown in the left column, while the calculation is worked out in the right one.

crude 1 wash 3 wash

mass of fuel used (g) 0.41 0.35 0.27
M biofuel (g.mol-1) 292.56 292.56 292.56
n used (mol) 0.00140 0.00120 0.00082
change in temperature (0C) 10 10 10
mass of water (g) 100 100 100
Enthalpy of Combustion (kJ.mol-1) 2982.64 3493.94 4529.19
Table 2. This table illustrates the obtained data of olive oil as it is crude, washed once and washed three
times.

2020 Class data

Group Enthalpy of combustion (kJ . mol−1 )
1 −2264.6
2 −4149.13
3 −3795.2
4 −4789.69
Table 3. This table shows the obtained results of enthalpies of combustion of olive oil with 3 wash from
other groups in year 12 conducted in Norwood Morialta High School.
Combustion step
How close the flame to the can
Enthalpy = Q/n
Qwater=mcT=100x4.18x
Nfuels=m/M

Analysis of Result

According to table 1, the enthalpy of combustion of olive oil after 3 wash is collected to be
−1
Δ H =4789.69 kJ . mol . Apparently, it is very accurate when compared to the data of the 3-wash fuel
from table 2 which is Δ H =4529.19 kJ . mol−1 . In addition, it is observed that the more time fuel is
washed the higher enthalpy of combustion is. This is due to the fact that crude oil reacts in an
Summative Practical
Biodiesels Synthesis and Analysis
Stage 2 Chemistry - SACE: 904243R
Name: Gia Giao Bao Nguyen
endothermic reaction with water. In this experiment, the results gathered and presented in Table 2 above
articulates the mass of fuel used in the experiment, which reduces after consecutive washes. After
washing the crude oil for two times, the mass reduced from 0.41 grams to 0.35grams, and finally 0.27
grams (see table 2). In this regard, it’s quite evident that part of the crude oil’s weight was washed off.
Since the biofuel used is a compound or rather, a substance containing elements and atoms, it has a
molecular weight of 292.56 g/mol, which remains constant for the compound even after washing.
With the relative molecular mass remaining constant for the biofuel, then the number of moles n
is directly proportional to them mass of the biofuel, as the mass reduces, number of moles used reduces
respectively. During the experiment, temperature remained constant at 10 degrees Celsius. The mass of
water used was 100 grams, which remained constant after washing the biofuel (see table 2). As seen in
table 2 above, enthalpy of fuel combustion in crude oil is 2982.64 kJ/mol, and 3493.94 kJ/mol after
washing the first time, and 4529.19 kJ/mol after the final wash. Table 1 above portrays the enthalpies of
combustion of olive oil calculated using the collected data. The enthalpy of olive oil combustion by
calculation is ΔH = 4789.69 kJ/mol. As evident in Table 3, each class group had a different enthalpy of
olive oil combustion. The difference in the outcome must have been from a difference in the mass of
water, which of biofuel used. Also, the mass lost after washing for each group was different. As a result,
the enthalpies for the reaction of crude oil turned different for each group. Coconut Oil has smaller
enthalpy change of combustion as compared to both canola oil and olive oil. On the other hand, canola
oil has higher enthalpy of combustion than olive oil (see Table 4 & 5 below).
CANOLA OIL
crude 1 wash 3 wash
0.39 0.32 0.25
294.58 294.58 294.58
0.00132 0.00109 0.00085

10 10 10
100 100 100

3157.27 3847.92 4925.34

Table 4: Portrays the enthalpy of combustion of canola oil

COCONUT OIL
crude 1 wash 3 wash
mass of fuel used
(g) 0.47 0.40 0.28
M Biofuel (g.mol-1) 237.92 237.92 237.92
n used (moles) 0.00198 0.00168 0.00118
Change in
temperature (°C) 10 10 10
Mass of water (g) 100 100 100

Enthalpy of 2115.93 2486.22 3551.74

Combustion
(kJ.mol-1)

Table 5: Shows the enthalpy of combustion of coconut oil

Summative Practical
Biodiesels Synthesis and Analysis
Stage 2 Chemistry - SACE: 904243R
Name: Gia Giao Bao Nguyen

Class Data Comparison

6000
Enthalpy of Olive Oil Combustion

5000

4000

3000

2000

1000

0
Group 1 Group 2 Group 3 Group 4
Graph 1: 2020 Class Data Comparison

Discussion

According to (), Trans esterification is a base catalysed process that can be used for the
manufacture and production of biofuels. As per the studies of (), in the production of biofuels from oil, a
reaction is that fatty acids in the used cooking oil are esterified into fatty acid methyl esters FAME and
the remainder bound in triglycerides are trans esterified to methanol, also producing FAME. The acid
process is used for esterification, but it does not adequately promote trans esterification at decent
reaction rates, while the base-catalyzed process does; however, it is inadvisable to use the base first
because the high free fatty acid content of used oil produces a large amount of soap as a byproduct,
which both consumes potential feedstock and gives you a colossal pain in the ass later in the process.
(), claims that Trans esterification is relatively easy to do and many people do it at home.
However, I personally am leery of homebrew biodiesel because few home brewers go through the effort
necessary to make sure their biodiesel has a low enough soap content to not damage engines in the long
run. The third way that used oil can produce fuel for bio cars is through hydrogenation. Basically,
straight oil is input into a catalytic hydrogenation reactor, which totally hydrogenates the oil: all fatty
acids lose their oxygen and become long chain paraffin’s, all glycerol’s lose their oxygen and become
propane. The result is treated as a normal refinery blend stock, albeit one that doesn't contain branched
compounds (and thus has to go through isomerization to be suitable for use as gasoline or diesel). This
type of fuel is known as hydro treated vegetable oil (HVO). Most of the time virgin oil is used, but used
oil has been put through the process as a proof of concept.
The process however will first start with some sort of biomass or biomass products. These
products are generally cellulose, starch or oil based, or a mix of several of them. These biomass products
may need to be sorted or processed to a specific purity or treated in a specific way to ready them for the
process. This could be an enzyme/acid/steam treatment process, dehydration, or grinding/mixing
process. The treated material would them be fed through a transformation process. The common
transformation processes would be: anaerobic digestion, fermentation, pyrolysis, gasification,
palletisation, or oil extraction/crushing. Each of these methods have a preferred feed stock and will
result with various energy and waste products.
Diesels will run on straight vegetable oil (SVO) if it is heated sufficiently to be liquid. As it is
likely to congeal at ambient temperature, it will clog your entire fuel system if this happens. You must
Summative Practical
Biodiesels Synthesis and Analysis
Stage 2 Chemistry - SACE: 904243R
Name: Gia Giao Bao Nguyen
have a diesel tank, start and end every journey on diesel. After starting, you must heat the SVO to a
liquid state, switch fuels for the majority of the journey, and switch back to diesel near the end in time to
completely purge the fuel system of SVO. Failure to do so will lead to a very expensive repair or
scrapping of the vehicle. The Tran esterification process is very dangerous in a home situation, you are
combining oil, alcohol, lye, and fire (to heat it to drive the reaction). If anything goes wrong you have
the risks of a major fire, explosion, or severe chemical burns.

Conclusion
In conclusion, it is quite clear that biofuels can be prepared from crude oil, olive oil, and coconut
oil among any other oil. As demonstrated by the experiment, the preparation of biofuel can be easily
done using both the reflux and separation methods to form biofuels from crude oil. The primary
objective of this experiment was to prepare biofuels from crude oil. The experiment has compared how
other types of oil behave and combust to prepare the biofuels. The experiment was finished successfully
and all guidelines and lab precautions were adhered to. Based on the results of this experiment, it is
evident that biofuel can be produced and synthesized using reflux and separation methods.

Reference list
1. ‘Biodisel Basics.’ BioDiesel. Available at:
https://www.biodiesel.org/what-is-biodiesel/biodiesel-basics
2. ‘Biodiesel Fuel Basics.’ US Department of Energy, Alternative Fuels Data Centre. Available at:
https://afdc.energy.gov/fuels/biodiesel_basics.html
3. ‘Biodiesel Benefits.’ Pacific Biodiesel. Available at: https://www.biodiesel.com/biodiesel-
benefits/
4. ‘Biodiesel Production and Distribution.’ US Department of Energy, Alternative Fuels Data
Centre. Available at: https://afdc.energy.gov/fuels/biodiesel_production.html
5. Jun 23, 2017. ‘Glycerol.’ Biology Dictionary. Available at:
https://biologydictionary.net/glycerol/#:~:text=Glycerol%20is%20easily%20soluble%20in,will
%20sink%20to%20the%20bottom.
6.