Republic of

Republic of Iraq
Iraq
Ministry of
Ministry of Higher
Higher Education
Education and
and Scientific
Scientific Research
Research ‫جمهورية العراق‬
‫العراق‬ ‫جمهورية‬
Kerbala University
University ‫والبحث العلمي‬
‫العلمي‬ ‫العالي والبحث‬
‫وزارة التعليم العالي‬
Kerbala
‫جامعة كربالء‬
‫كربالء‬ ‫جامعة‬
Engineering faculty
Engineering faculty
‫كلية الهندسة‬
‫الهندسة‬ ‫كلية‬
Petroleum Department
Petroleum Department
‫هندسة النفط‬
‫النفط‬ ‫هندسة‬

‫رحيم‬
‫ناصررحيم‬
‫عليناصر‬ ‫علي‬
‫الدراسة‬ – ‫الثالثة‬ ‫المرحلة‬
‫المرحلة الثالثة – الدراسة‬
‫الصباحية‬
‫الصباحية‬

‫المشرف‬
‫ تحسين حميد خليف‬.‫د‬.‫م‬.‫ا‬
‫ حوراء عادل‬.‫أ‬
Thursday, August 28 2021
Thursday, November 04 2021

Soxhlet Extraction Unit

Reservoir Engineering Lab.

1
 Topics

 Introduction
 Objective and Aim
 Method
 Tools and Apparatus
 Types
 Procedure
 Calculations
 Discussion
 References

2
Introduction
Soxhlet distillation extraction removes liquid phases (oil and brine) from core
samples by virtue of a solvent vaporization and condensation process. The
cleanliness of the sample is determined from the color of the solvent once it
has permeated from the samples and condensed. The samples are placed in
[1]
the extractor and cleaned by refluxing solvent.
The solvent in this closed system is externally heated and vaporized
continuously in a flask, flow through the samples in the extraction tube,
condenses at the top of the assembly. The condensate falls back into the
sample chamber. When the latter is full, the dirty solvent returns to the flask
via a siphoning reflux sidearm located at the base of the sample chamber.
Due to the difference in boiling point temperatures, only the solvent
evaporates while the oil finds itself trapped in the flask. The apparatus
consists of a distillation/extraction glassware unit and a heating mantle with
thermostatic controller. The first comprises a boiling flask, soxhlet extractor
and condenser. Flexible plastic tubing connects the condenser to the water
cooling unit. The assembly is supported by a clamp screwed to a vertical rod,
[2]
itself fixed to the heating mantle.

Objective and Aim

The Main objective of this experiment is to clean the obtained core plug from
hydrocarbons plug from hydrocarbons and to calculate the porosity of the
[3]
core.

3
Method
A Soxhlet extraction apparatus is the most common method for dleaning
sample, and is routinely used by most laboratories. A toluene is brought to a
slow boil in a Pyrex flask, its vapors move upwards and the core becomes
engulfed in the toluene vapors (at approximately 110°C). Eventual water
within the core sample in ghe thimble will be vaporized. The toluene and
water vapors enter the inner chamber of the condenser, the cold water
circulating about the inner chamber condenses both vapors to immiscible
liquids.
Recondensed toluene together with liquid water falls from the base of the
condenser onto the core sample in the thimble; the toluene soaks the core
sample and dissolves any oil with which it come into contact. When the liquid
level within the Soxhlet tube
reaches the top of the siphon
tube arrangement, the liquids
within the Soxhlet tube are
automatically emptied by a
siphon effect and flow into
the boiling flask. The toluene is
then ready to start another cycle.
A complete extraction may take
several days to several weeks in
the case of low API gravity
crude or presence of heavy
residual hydrocarbon deposit
within the core.
Low permeability rock
may also require a long
[4]
extraction time.

4
Tools and Apparatus [5]

The Soxhlet extractor (Soxhlet, 1879) was originally designed for the extraction of a lipid from
a solid material but is used extensively in core analysis to remove water and oil from core
samples. A schematic of a Soxhlet extractor assembly is shown in Fig 1. The principal
components are:

1. A round bottomed flask or extraction pot filled with solvent.

2. A stirrer bar or anti-bumping granules.
3. A side arm (Distillation Path).
4. A Soxhlet thimble containing the core samples.
5. A siphon arm inlet.
6. A siphon arm outlet.
7. A reduction adaptor.
8. A condenser unit which can circulated with chilled water via ports 9 and 10.
11. Extraction Solid

10

7
9

4 3

11

5
Procedure[5]
1. Remove the sample from the oil and carefully blot dry an excess oil.
2. Place the sample inside the Wathman thimble and quickly weight the sample
and thimble using the analytical balance.
3. Leave the sample in the thimble.
4. Reassemble the apparatus as, tighten the ground joint fitting but don't apply
sealing or lubricant.
5. Turn on the water supply to begin circulation in the condenser.
6. Turn on the heater and adjust the rate of the boiling so that the reflex from the
condenser is a few drops of solvents (toluene) per second.
7. Allow the extraction to continue for several hours with a minimum of 7 cycles
or until the thimble content dissolved oil stain and is close to original color.
8. Monitor the toluene level during the extraction to ensure that the sample
remains completely submerged in addition.
9. When the extraction is complete the solvent will be clean or water white
depending on the color of oil removed.
 Read the volume of the water collected in the water trap, if any. Note: In many
cases the sample have been prepared using oil only to saturate the core sample,
therefore the absence of water does not mean an invalid test.
 Rectum the thimble containing the sample to the instructor, who will place
them in the drying oven at (105 - 120) degree centigrade.
 The instructor will advise when to return to collect the dried sample
(sometimes will be the next day).
 Place the dried sample in desiccators for a few hours prior to weighting to
ensure that they are completely dried.
 Place the thimble containing the sample in the analytical balance, measure the
weight of the thimble and dried core sample and record the result.
 Remove the sample and then weight the empty thimble, record the results or no
note if there are any grains of the sample remaining in the thimble in the space
provide.

6
Calculations

7
Discussion
Q1. By this process, we notice that the system is closed, what is the
purpose of that? why we choose the system to be closed?
Ans.
As we deal with vapor that it cycles many times during days or weeks, it
makes sense that the system to be closed so non if it can flush out of the
system. And then it saves the amount of Methanol which if the system is
open, then it requires much of Methanol required in every single cycle.
Q2. Why should we put the system at a specific boiling point?
Ans.
Every single type of fluid has its own boiling point which if we didn’t
make the temperature at its value, then the vaporization wouldn’t happen,
the fluid would burn immediately or it would have evaporated faster
depending on the type of fluid and make a explosion.
Q3. Why we choose a conical shape for condenser?
Ans.
To collect and transport vapor.
Q4. What are the advantages of Soxhlet extraction?
Ans.
 simple and clear design,
 production process continuity,
 ease of visual monitoring of the process,
 a low flow of solvent and the possibility of its reuse after stripping and
distillation.

8
Q4. Why Methanol is used in Soxhlet extraction?
Ans.
We required more volume of different solvents when we attempt by polarity
series. Instead of doing this, directly we can extract the material using
methanol as solvent. After concentration, the crude will be fractioned using
solvents with increasing polarity.

9
References

[1]. McPhee, C., Reed, J.& Zubizarrete, I., 201. Core Analysis. s.I.: Elsevier.
[2]. Park, A., 1985, Coring, Part 2 – Core barrel types and uses World Oil, v. 200.
[3]. Bradburn , F. R., Cheatham, C. A., 1988, Improved core recovery in laminated sand shale
sequences: Journal of petroleum Technology, v. 40.
[4]. American Petroleum Institute (API), 1960, RP 40 recommended practices for core analysis
procedures.
[5]. Core Preparation

10