ABSTRACT

The amount of oil in oilseeds is the amount of oil extracted from the seeds and is expressed as
a percentage. This analysis is carried out by removing all impurities from the oilseeds.
Oilseeds contain high levels of oil, protein, carbohydrates, minerals, and vitamins. Oilseed
crops such as soybean, sunflower, rapeseed, peanut, sesame, safflower date, olive, and
coconut are available in abundance for crude oil production. This experiment, it was aimed to
determine the oil properties of hazelnuts for quality determination. The experiment consisted
of two stages. Extraction was done in the first stage and distillation was done in the second
stage. In the first stage, an experimental setup was established by weighing 7.1609 g of
hazelnuts and an empty distillation flask as 128.4128 g. The solvent petroleum ether has a
volume of 375 mL. The heating process was chosen according to the boiling point of
petroleum ether. That is, the system was heated at 50-60 °C. Since the system was not ideal,
the time started to be recorded after the first 2-3 siphon movements. It was timed 17 times in
total. Tap water is connected to the system for the condenser part. The system in this first
stage is the batch system and the flow is co-current. A new setup has been set up for the
second stage. Obtained oil and petroleum ether are separated from each other by reheating and
condensing at this stage. Then, the sample bottle was kept in an oven for a while, and a small
amount of remaining ether was removed. Finally, the sample taken out of the oven was
allowed to cool and the sample was weighed. The amount of distillation flask weighed is
130.8912 g. Laboratory conditions were measured as 21.7 °C and 1 atm. When calculations
are made for this experiment, the oil percentage is 34.6100%. When the percentage of oil
found for 7.1609 g hazelnuts is multiplied, 2.4783 g hazelnut oil is obtained. For the error
percentage in the experiment, the reference theoretical oil percentage was taken as 60.8000%
and the error percentage was found as 43.0800 % as a result of the necessary calculations.

i
 TABLE OF CONTENTS
ABSTRACT................................................................................................................................i

1. THEORY............................................................................................................................1

1.1. Solid-Liquid Extraction.............................................................................................1

1.1.1. Soxhlet Extractor................................................................................................1

1.2. Vapor Pressure (P°)...................................................................................................2

1.3. Petroleum Ether.........................................................................................................3

1.4. Vegetable Oils.............................................................................................................3

2. PROCEDURE....................................................................................................................4

2.1. First Stage of the Experiment.......................................................................................4

2.2. Second Stage of the Experiment..................................................................................4

3. EXPERIMENTAL DATA................................................................................................5

4. CALCULATION...............................................................................................................6

5. DISCUSSION AND RESULTS........................................................................................7

6. CONCLUSION..................................................................................................................8

7. RECOMMENDATIONS..................................................................................................8

8. REFERENCES...................................................................................................................9

ii
LIST OF FIGURES

Figure 1: Soxhlet Device............................................................................................................2

Figure 2: Distillation Stage.........................................................................................................6
Figure 3: Hazelnut Oil…………………………………………………………………………6

iii
LIST OF TABLES

Table 1: Measured Siphon Numbers and Times.........................................................................6

Table 2: Experimental Data........................................................................................................7
Table 3: Oil Values (grams)........................................................................................................7

iv
 1. THEORY

1.1. Solid-Liquid Extraction

In chemical engineering and in industry, solvents are used to remove soluble components (in
the used solvent) from the solid material in a solid-liquid extraction. Making tea or coffee is a
daily life example for a solid-liquid extraction process. Coffee or tea particles are the
extracted materials, while water is used as the solvent. The component of the transition is the
coffee or tea's zest. In terms of extraction rate, the size of the solid is significant. Using
smaller size particles helps in speeding up the extraction process because as a particle's
surface area grows, the contact area with the solvent also increases. Another crucial factor for
extraction is temperature. Despite higher yields at higher temperatures, care should be taken
to prevent the degradation of the used raw material(s). Also, the desired ingredient must
dissolve in the extraction solvent of choice. [1]

There are several techniques for solid-liquid extraction. However, since the 1890s, the Soxhlet
Apparatus method has been the primary extraction technique.

1.1.1. Soxhlet Extractor

A Soxhlet extractor is a piece of lab equipment used for continuous batch solid/liquid
extraction that was created in 1879 by Franz von Soxhlet. [2] The solid component needs to
be dissolved in the liquid solvent in a certain quantity before the Soxhlet extraction may
proceed. If the solids are insoluble in the solvent, Soxhlet extraction cannot be performed. In
extraction, only pure organic solvents or their combinations are used. At the solvent's boiling
point, the solid components must be thermally stable. [1]

1
 Figure 1: Soxhlet Device
The Soxhlet apparatus consists of a balloon flash which contains the solvent, a medium-flow
liquid flow pipe (siphon), a cooled condenser, and a heating system, as it can be seen from the
setup in Figure 1.

This technique uses a porous bag to contain the powdered/grinded sample, which is then put
within the Soxhlet equipment’s thimble chamber. To stop solid particles from entering the
system with the flow, the sample is put within the device and given such further protection. A
heating source, such as a heating mantle, is used to evaporate the solvent balloon flask. The
extraction solvent used determines the heating temperature. The bottom flask's solvent
vaporizes into the condenser because of the applied heat, then falls back into the sample
thimble as it condenses in the condenser. The liquid is drained into the bottom flask as it
reaches the siphon arm, and the procedure is repeated. [2]

Soxhlet extraction offers a few alluring benefits. The new solvent is continuously in touch
with it. As a result, the products that are separated from the solid are simpler to handle. It is
also an inexpensive equipment. [3] Additionally, the Soxhlet extraction method allows for the
extraction of a high volume of material without the requirement for post-process filtering.
Unfortunately, there are several drawbacks to this approach. In the Soxhlet extraction, a large
volume of solvent is utilized, and the extraction process takes a lot of time; for example, 12
hours, 22 hours, and 24 hours are as instances of lengthy extraction periods. In this extraction
procedure, between 200 and 250 ml of solvent are typically utilized. [4] Even though it wastes
time and is bad for the environment, this approach has been around for a long time.

1.2. Vapor Pressure (P°)

2
The pressure at which a compound's vapor is in equilibrium with its completely condensed
phase is known as the vapor pressure (P°) (solid or liquid). Due to changes in molecule-
molecule interactions, vapor pressures are largely dependent on temperature and vary greatly
with various chemicals. The temperature at which the vapor pressure of a liquid equals one
atmosphere (P° = 1 atm) is known as the normal boiling point of a liquid. Vapor pressure
determines how a substance is distributed into and out of gaseous ambient phases (the
atmosphere, marsh bubble gas). [5]

1.3. Petroleum Ether

Petroleum ether is a typical laboratory solvent made up of aliphatic hydrocarbons and boiling
between 35 and 60 °C in the petroleum fraction. [6] Petroleum ether is not ether, despite its
name; the phrase is primarily used metaphorically to denote high lightness and volatility.

Petroleum ether is another term for the lightest, most volatile liquid hydrocarbon solvents that
may be purchased from providers of laboratory chemicals. Petroleum ether typically has little
aromatic material and is mostly made up of aliphatic hydrocarbons. To cut down on the
quantity of aromatic and other unsaturated hydrocarbons, it is frequently hydro-desulfurized
and might be hydrogenated. Petroleum ether often has a descriptive suffix that specifies the
boiling point range. It is therefore feasible to purchase a variety of petroleum ethers with
boiling ranges such as 30–50 °C, 40–60 °C, 50–70 °C, 60–80 °C, etc. from the top
international providers of laboratory chemicals. Petroleum ether, as opposed to petroleum
spirit, is the name given in the US to laboratory-grade aliphatic hydrocarbon solvents with
boiling ranges as high as 100-140°C. [7]

Employing a fraction with a boiling point range of more than 20 °C is not advised due to the
possibility of losing the more volatile component during recrystallization, etc., and the
resulting differing solubilizing characteristics of the higher boiling residue. [8]

1.4. Vegetable Oils

Vegetable oils are oils extracted from seeds or from other parts of fruits. Like animal fats,
vegetable fats are mixtures of triglycerides. Vegetable oils are chemically known as
triglycerides of fatty acids and consist of a combination of three fatty acids and one glycerin
molecule. Soybean oil, grape seed oil, and cocoa butter are examples of seed oils, or fats from
seeds. Olive oil, palm oil, and rice bran oil are examples of fats from other parts of fruits. In

3
common usage, vegetable oil may refer exclusively to vegetable fats which are liquid at room
temperature. Vegetable oils are usually edible. The production process of vegetable oil
involves the removal of oil from plant components, typically seeds. This can be done via
mechanical extraction using an oil mill or chemical extraction using a solvent. The extracted
oil can then be purified and, if required, refined or chemically altered. Vegetable oils are used
as an ingredient or component in many manufactured products. Vegetable oils are also used to
make biodiesel, which can be used like conventional diesel. [9]

2. PROCEDURE

The system consists of two stages. In the first stage of the experiment, the extraction process
is performed, and the distillation process is performed in the second stage.

2.1. First Stage of the Experiment

 Nuts were selected as the oil seeds to be used in the system. About 7 grams of nuts are
weighed.
 The weighed nuts are wrapped in filter paper and placed in the cartouche. The
prepared cartouche is placed in the extractor.
 The empty balloon flask is weighed. 3/4 of the 500 ml balloon flask (375 mL) is filled
with petroleum ether. The balloon flask is placed inside the heat source.
 Vaseline is applied to the attachment points of equipment.
 The extractor is first placed on top of the balloon flask. Then a condenser is placed on
top of the extractor.
 The water inlet hose is connected to the lower part of the condenser, the outlet hose is
connected to the upper part, and the water is turned on at a certain speed.
 The heater is set to 55°C degrees and the heater is started.
 The siphon time is measured until the siphon time is fixed.
 Several siphon runs are allowed to take place to extract the oil in the peanuts.

2.2. Second Stage of the Experiment

 The experimental setup is set for distillation. Vaseline is applied to the connection
points of the equipment. The condenser used in the distillation process is placed at the
top of the extractor.

4
  The experimental setup is set for distillation. Vaseline is applied to the connection
points of the equipment. The condenser used in the distillation process is placed at the
top of the extractor. Water connections are made in the condenser.
 A beaker is placed at the end of the condenser. The heater and the water valve are
opened.
 After a large part of the solvent has been removed, the heater and the water valve are
closed. Equipment connections are separated.
 The balloon flask is placed in the drying oven and left for 5 minutes. After the balloon
flask is removed from the drying oven, it is allowed to cool.
 The cooled balloon is weighed with the oil in the flask. All weigh-ins are noted.

3. EXPERIMENTAL DATA

The measured siphon time intervals are tabulated in Table 1.

Table 1: Measured Siphon Numbers and Times

Numbers of Siphon Times of Siphon (minutes)

1 15,02
2 1,31
3 1,29
4 6,14
5 2,13
6 2,11
7 5,10
8 2,05
9 4,41
10 2,35
11 2,13
12 5,06
13 2,07
14 4,48
15 2,39
16 2,05
17 3,36

5
 Figure 2: Distillation Stage Figure 3: Hazelnut Oil

4. CALCULATION

Calculations using experimental data which are shown in Table 2 and Table 3 are as follows.

Table 2: Experimental Data

Measured Weight (g)

m1: weight of the balloon flask (g) 128,4128
m2: weight of the sample (g) 7,1609
m3: weight of balloon flask + oil (g) 130,8912

m3−m1
% oil= x 100
m2

130,8912−128,4128
% oil= x 100
7,1609

% oil=34,6100

oil ∈sample=7,1609 x 0,3461=2,4784 g

Table 3: Oil Values (grams)

Theoretical oil value (g) [10] Calculated oil value (g)

60,8000 34,6100

m theoretical−mcalculated
% error=
mtheoretical

6
 60,8000−34,6100
% error= x 100
60,8000

% error=43,0800

5. DISCUSSION AND RESULTS

In this experiment, the oil content of the selected oil seed was determined by extraction and
distillation methods. This determined ratio was compared with the theoretical value.

Hazelnut was chosen as the oilseed, and the hazelnut was crushed into small pieces before
being used. This is because it increases the surface area where it will interact with the solvent.
Petroleum ether was chosen as the solvent for oilseed analysis. The reason for this is that
petroleum ether, which has a nonpolar structure, easily dissolves oil, which has a nonpolar
structure, based on the principle of like dissolves like; moreover, both are hydrocarbons).
Since the boiling temperature of petroleum ether used as a solvent in this experiment is 60°C,
55°C was chosen as the operating temperature. The reason for choosing the operating
temperature below the boiling point is that the evaporation rate increases as the temperature
increases. With the increase in the evaporation rate, the contact time of the solvent and the
hazelnut decreases, and the amount of oil transferred to the solvent decreases. Another reason
why it cannot be worked at high temperatures is to reduce the risks that may occur in the
experiment. It has been mentioned that increasing temperature increases the flow rate and
increasing the flow rate increases that of the condenser surface pressure. This pressure
increase can cause the condenser to burst. More vapor formation results in more pressure in
the glassware which increases the risk of the glassware to explode as more stress is being
applied on the glassware’s walls.

The increase in temperature and pressure in the system affects the number of siphons.
Increasing the temperature increases the evaporation rate, and this causes the siphon time to
decrease. So, the siphon fills and empties faster. The increase in the boiling point with the
increase in pressure causes the siphon time to decrease.

Since the established test setup is not an ideal system, the siphon time is not directly fixed.
After a few siphon counts, the siphon time values on the forehead give more accurate results.
In our system, the first flush time is recorded as 15.02 minutes. This is why it is farther in

7
precision and accuracy than flush times obtained later. Likewise, if the system is not ideal
(which is), it increases the calculated amount of error.

When the system for the condenser was examined, it was determined that the system was
batch and co-current. Since petroleum ether vapor and cooling water entering the condenser
are fed from the same direction, it has been determined that the system is co-current. The log
means temperature value in flow direction co-current flow is lower than counter-current flow.
It increases the low possible contact surface area of the log mean temperature and increases
the contact of oil and solvent and increases the amount of condensation. The reason why the
system is called batch is that there is no input or output to the system during the experiment.

6. CONCLUSION

In this experiment, in which the amount of oil in the hazelnut was determined, the amount of
oil was calculated as 34.6100%. Approximately 7 grams of hazelnut sample is taken, and
2.4784 grams of sample were determined as fat. When compared with the literature value, an
error rate of 43.08% was reached. The factors causing the error are discussed in the report.

7. RECOMMENDATIONS

The size of the particles shall not be big nor too fine; else more extraction time will be
needed, or the particles can escape with the siphon cycles. The water connections must be
controlled and checked as the hoes may be removed from the glassware. The flowrate of the
exiting water also must be continuously monitored to ensure a steady condensation rate –
sometimes the water supply pump’s efficiency decreases upon long operating times. A
complete evaporation of solvent must be ensured to avoid wrong readings; at the same time,
we need to ensure none of the extracted oil evaporates. The obtained mass of the extracted
liquid cannot be greater that the weight of the used nuts; else, that means we still have
unevaporated solvent with the extracted oil.

8
8. REFERENCES

[1] Şengün, D., “Extraction of Phenolic Compounds from Hazelnut Shell Waste”, July 2018,
İzmir.
[2] Kasiramar, G., “Significant Role of Soxhlet Extraction Process in Phytochemical
Research”. Researchgate.net. Retrieved November 30, 2022,
(https://www.researchgate.net/publication/332407655)
[3] Luque-Garcıa, J. L., and MD Luque De Castro. "Focused microwave-assisted Soxhlet
extraction: devices and applications." Talanta 64.3 (2004): 571-577.
[4] Subramanian, R., et al. "Double bypasses soxhlet apparatus for extraction of piperine
from Piper nigrum." Arabian journal of chemistry 9 (2016): 537-540.
[5] Persaud, N. (2005). Vapor pressure. Water Encyclopedia.
(https://doi.org/10.1002/047147844x.me411)
[6] David R. Lide, ed. (2010), “CRC Handbook of Chemistry and Physics”, (90th ed.), CRC
Press, pp. 2–60.
[7] Phenix, A., “Generic Hydrocarbon Solvents: a Guide to Nomenclature”,  WAAC
Newsletter.
[8] Vogel, A., “Practical Organic Chemistry”, Longman, 1989, pp. 397–398.
[9] (https://www.thespruceeats.com/what-is-vegetable-oil-5201006) (access date: 30.11.2022)
[10] Naturel i̇ç Findik 500g. FİSKOBİRLİK EFİT A.Ş. (n.d.). Retrieved November 30, 2022,
(https://www.findikciyiz.com/naturel-findik/naturel-findik-500g)