Course Number: ChE-302

Course Title: Chemical Engineering Laboratory-II

Experiment Number: 01
Name of the Experiment: Extraction of oil from oilcake by Soxhlet extraction

Submitted by:

Submitted to:

Mahe Rukh

Md. Nazibul Islam

Student Number: 1202036

Lecturer

Section: A2

Group Number: 02

Department of Chemical engineering

BUET

Department of Chemical Engineering

Partners Student Numbers: 1202037

Date of Performance: 28/11/15

1202038

Date of Submission: 05/12/15

1202039
1202040

Summary
Like crystallization and distillation, extraction is a separation technique commonly employed in
the laboratory to separate one or more components from a mixture. And it is also a common
practice in everyday life. When one puts a tea bag in boiling water, or wash a load of laundry,
solid/liquid extraction is performed, which refers to the removal of a component from a solid
matrix using a liquid solvent. The main objective of this experiment was to have clear conception
about the solid-liquid extraction process which is industrially known as leaching process for which
in the experiment Soxhlet extractor was used. Oil was the desired substance which was extracted
from oilcake and the extraction process was done using n-Hexane as solvent. The solid-liquid
extraction characteristics was observed in this experiment. The mechanism, performance of the
Soxhlet Extractor and the percentage of oil extracted from oil cake and the percentage recovery of
the solvent were also observed. From this experiment, the extracted oil was found 5.52 % and the
recovery of the given solvent was 68.39 %. The amount of oil extracted and recovery of solvent
are evidently low and the reasons accountable for this are explained in the discussion section.

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Introduction
Extraction is the method of selectively eliminating a compound of interest or a waste substance
from a mixture by means of a solvent. For an extraction process to be effective, the compound
must be more soluble in the solvent than in the mixture. Moreover, the solvent and mixture needs
to be immiscible. By intensive contact the agent transfers from the solid or liquid mixture into the
solvent (extract). Depending on the phases following types of extraction exist- solid - liquid
extraction, liquid -liquid extraction. The gas - liquid extraction is called absorption. The extraction
process can also be classified as single stage batch process extraction, multistage cross flow
extraction, multistage countercurrent extraction. Washing is almost same as extraction, the main
difference being one of the important is that in washing the inert material is the product to be
soluble in solvent, and the solvent used is water which is cheap and readily available.
Solid- liquid extraction or leaching is of great significance in industrial applications. One of the
main application areas of this process is food industry where it has been practiced for a long time.
Oil from soybean, corn, and rice bran cannot be separated using mechanical pressing,
consequently, leaching is used for their recovery. Oil from peanuts is also recovered by mechanical
pressing and extraction of the pressed cake to completely remove the oil. One characteristic of
solvent extracted oilseed meal is the high value of the residual protein, appropriate for further
processing into food-grade powders. Boiling tea leaves in water extracts the tannins, theobromine,
and caffeine out of the leaves and into the water. This is one daily life example of solid-liquid
extraction. This technique is also prevalent in the petrochemical refining industry. As petroleum
products are treated, impurities stay in the raw products. Using suitable solvents, the appropriate
material can be separated from the undesirable substances, and then additional extraction can be
used to separate out the various grades of hydrocarbons according to their uses, which may be as
fuels, lubricants, or as raw materials for the chemical industry. Using solid-liquid extraction
process to remove active ingredients from natural materials and to remove high quality fats from
animal corpse utilization is predominant in pharmaceutical and cosmetic industry. From
environmental standpoint, this process is applied to decontaminate soils and to recycle resources.
Basic technique of solid liquid extraction requires preparation of extraction materials (milling,
grinding, rolling, pelletizing), choice of solvent, high concentration in overflow (extract solution)
and solvent separation from overflow and underflow (wet solids). Methods that can be followed
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are- Leaching by Percolation through Stationary Solid Beds, Moving-Bed Leaching, DispersedSolid Leaching. Many other leaching devices have been established for special purposes, such as
extraction of various oilseeds, with their specific design details governed by the properties of the
solvent & of the solid to be leached. One such laboratory apparatus is Soxhlet extractor invented
in 1879 by Franz von Soxhlet. It was initially designed for the extraction of a lipid from a solid
material. Usually, Soxhlet extraction is used when the desired compound has a limited solubility in
a solvent, and the impurity is insoluble in that solvent. This method is suitable for both initial and
bulk extraction . The oilcake is placed in a thimble in an Soxlet extraction chamber, which is placed
on top of a collecting flask under a reflux condenser. A suitable solvent is taken into the flask, and
the set up is heated under reflux. When a certain level of condensed solvent has accumulated in
the thimble, it is siphoned into the flask.The chief advantage of Soxhlet extraction is that it is a
continuous process. But this process is time consuming and large volume of solvent is required to
continue this operation.
The effectiveness of this techniques is based on many operational variables such as- extraction
time, quality and quantity of solvent, temperature. The extraction temperature and time has
essential significance for oil recovery from oil cake. The higher the extraction time, the higher the
amount of oil will be extracted. High temperature ensures high extraction as it lowers viscosity of
both solvent and extract and increases solubility of extract in solvent. Short capillary path and high
percolation velocity are also required. Quantity of solvent (n-hexane) effects the solid- liquid
extraction process. when temperature and extraction time remain constant, the rate of extraction
first increases with increase in the amount of solvent and after reaching a limit increase in rate of
extraction is minimal. Again, the requirements of solvent for reducing the residual oil content of
various seeds to a particular level differ with the characteristics of seed.
Solvent selection is based on several properties: solubility of the definite compound in the solvent
should be checked. Since the solvent will be recollected in succeeding extractions; if distillation
or evaporation is used, the solvent should not foam azeotropes and the latent heat of vaporization
should not be high. The solvent should be able to wet the solid matrix and its viscosity should be
adequately low so it can flow easily. Preferably, the solvent should be nontoxic, chemical and
thermal stability, not too high boiling point, nonreactive, nonflammable, harmless to the
environment, and inexpensive for food industry no influence on smell and taste.
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For solid liquid extraction mainly benzene, hexane, carbon disulfide, trichloroethylene are used.
In the experiment, hexane was used as the solvent for oil extraction from oil cake. Hexane was
used because- it has low latent heat of vaporization, it does not react with oil cake constituents,
high recovery of this solvent can also be achieved and it is cheaper comparing to others, Solubility
of oil in hexane is higher, corrosive nature is negligible.
In leaching or solid-liquid extraction superior technical control is necessary. Also, spent solvent
must be restored and recycled. Traces of solvent may remain in the treated solids, so the toxicity
of the solvent should be considered. Solvent extraction is normally least operative on very high
molecular weight organic and very hydrophilic substances. Again, Machinery requirement per unit
production of oil is more elaborate and expensive. High moisture content decreases process
efficiency and upturns difficulty of residuals managing. These are some disadvantages of solid
liquid extraction process.

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Experimental Section
Apparatus

Total condenser

Thimble

Siphon

Round bottom flask

A hammer to grind oil cake

Electrical heater

A recycle tube

A conical flask

Weighing balance

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Experimental setup

Figure-01. A schematic diagram of the setup of the experiment

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Figure-02: A schematic diagram of the Soxhlet extractor

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Figure-03: The schematic diagram of distillation process.

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Experimental procedure
1. Measured amount of n-Hexane was taken in the flask as a solvent.
2. Some amount of oilcake was taken and grinded using hammer. Then a measured amount
of grinded oilcake was taken into a Soxhlet thimble. It is nothing but as a filter paper with
semipermeable cellulose membrane.
3. Then the flask was put on the heater and solvent was heated slowly. The condenser was
put on the top of the Soxhlet holder and cooling water was turned on. The condenser could
condense whole vapor that was entering in the chamber and so the amount of vapor that
was entering the chamber remained unaffected when it condensed back as liquid.
4. This operation continued until sufficient amount of oil was separated by siphoning.
5. After the process was completed, the flask containing n-Hexane was weighed. Increase in
weight indicated that some oil had been extracted by the solvent.
6. Distillation process was introduced by reassembling the condenser where hexane was
evaporated and was recovered in a conical flask and extracted oil remained in the round
bottom flask.

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Observed Data
Weight of empty thimble = 5.215 g
Weight of thimble with oil cake = 33.205 g
Weight of empty round bottom flask = 125.460 g
Weight of round bottom flask with n-hexane = 209.113 g
Weight of empty conical flask = 122.85 g
Weight of conical flask with n-hexane = 180.06 g
Weight of round bottom flask with oil = 127.005 g

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Calculated Data
Weight of n-hexane = 83.653 g
Weight of oil cake = 27.99 g
Weight of n-hexane recovered = 57.21 g
Weight of oil extracted = 1.545 g
Percentage of extracted oil = 5.52 %
Percentage of recovered n-hexane (solvent) = 68.39 %

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Sample calculation
Weight of empty thimble, W1 = 5.215 g
Weight of thimble with oil cake, W2 = 33.205 g
Weight of oil cake = W2-W1
=27.99 g

Weight of empty round bottom flask, W3 = 125.460 g

Weight of round bottom flask with n-hexane, W4 = 209.113 g
Weight of n-Hexane= W4-W3
= 83.653g

Weight of round bottom flask with oil, W5 = 127.005 g

Weight of oil extracted= W5-W3
= 1.545 g
Percentage of oil extracted=

weight of oil extracted from oilcake

weight of oilcake

X 100%

1.545

= 27.99 X100 %
= 5.52%

Weight of empty conical flask, W6= 122.85 g

Weight of conical flask with n-hexane, W7 = 180.06 g
Weight of n-Hexane recovered= W7-W6
= 57.21 g

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Percentage of solvent recovered =

Weight of nhexane recovered

Weight of nHexane used

X100 %

57.21

= 83.653 X100 %
= 68.39 %

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Results and discussions

Percentage of oil extracted = 5.52%
Percentage of solvent recovered = 68.39%

From the result, it is evident that amount of oil extracted and amount of solvent recovered are low.
Several reasons might be responsible for low quantity of oil extracted and n-Hexane recovered.
The reasons are enumerated below1. Grinding oilcake to fine particles is requisite in Soxhlet extraction process as it increases
surface area of particles and ensures well contact between oilcake and n-Hexane. The oil
cake was grinded in an irregular manner, so the particle size was not uniform and some of
the particles were large which might have caused low percentage of oil extraction.
2. As n-hexane is a volatile component, a small amount might have vaporized while
measuring the weight which might have caused loss of solvent.
3. Only one condenser was used to separate n-hexane. But a single condenser might not be
sufficient to condense the total amount of vapor of n-hexane. Slight amount of n-hexane
might have been lost to the atmosphere causing low recovery of solvent.
4. In this experiment, single stage extraction process was used which might have been another
reason for low percentage of oil extraction.
5. The higher the extraction time the higher the oil will be extracted. If the extraction period
was extended, higher percentage of extraction of oil could have been achieved.
6. Some solvent was not recovered due to consumption of n-hexane by oilcake. Soxhlet
thimble being a permeable cellulose filter material might have also consumed little amount
of n-hexane which caused loss of solvent.

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References
1) Foust, A. S., Wenzel, L. A., Clump, C. W., Maus, L., Andersen, L. B., Principles of Unit
Operations, 2nd edition, John Wiley and Sons, Singapore, P.15,60 (1980).
2) McCabe, W.L., Smith, J.C., Harriott, P., Unit Operations of Chemical Engineering, 5th
edition, McGraw Hill, New York, P.614-616, (1993).
3) Solvent extraction, Encyclopedia Britannica, Retrieved from
http://global.britannica.com/science/solvent-extraction [Accessed 2015/12/04]
4) Extraction of natural products, Uppsala University, Retrieved from
http://www.fkog.uu.se/course/a/biolakt/biolakt-archive/BiolAkt%2020102/StudentpresentationerHT2010%20(kopia)/BiolAktHT2010_ExtraktionNatProd_Yassir_Suzan/
Extraction%20of%20natural%20products_files/Page470.htm [Accessed 2015/12/04]

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Marking Scheme: Normal Report

Name: Mahe Rukh
Student number: 1202036
Section and marks allocated

Marks

Summary (1)
Introduction (1)
Experimental Work (1.5)
Observed Data (1)
Calculated Data (1)
Sample Calculation (1)
Graphs (1)
Results and Discussion (1)
References and Nomenclature (0.5)
Writing Quality and Style (1)
Total (10)

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