UNIVERSITI TEKNOLOGI MARA

FAKULTI KEJURUTERAAN KIMIA

RESERVOIR ENGINEERING LAB
( CGE 617 )
NAME & STUDENT NO

MOHAMMAD FAIZUAN BIN ISMAIL (2013252638)

EXPERIMENT
DATE PERFORMED
SEMESTER
PROGRAMME/ CODE
GROUP

:
:
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:
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CLEANSING AND SATURATION DETERMINATION

Checked by:

26 MARCH 2015
4
EH243
EH2434A

Question 1 : Definition of fluid saturation .

Geologist noted that the rock pore are filled with water at first and then the water was
displaced by the hydrocarbon present . The hydrocarbon moved to displaced the water to
some minimum residual saturation . Therefore more than one fluid is normally present in the
reservoir .
Fluid saturation can define as the measure of the gross void space in the reservoir rock that is
occupied by a fluid . The fluid can be water, gas, or oil . Therefore saturation of any given
fluid in the pore space is the ratio of the volume of that fluid to the pore space volume not
gross reservoir volume .

Question 2 : Compare all method to determine the fluid saturation .

2.1 : DIRECT INJECTION OF SOLVENT
The solvent is injected into the sample in a continuous process. The sample is held in a rubber
sleeve thus forcing the flow to be uniaxial .

2.2 : CENTRIFUGE FLUSHING

A centrifuge has been fitted with special head sprays warm solvent onto the sample. This
method produce centrifuge force then move the solvent through the sample . The used solvent
can be recollect and recycled .

2.3 : GAS DRIVEN SOLVENT EXTRACTION

The sample is placed in a pressurized atmosphere of solvent containing dissolved gas . The
solvent fills the pore sample . When the pressure is decrease, the gas come out of solution,
expends, and drives fluids out of the rock pore space . This process can be repeated as many
times as necessary .

2.4 : SOXHLET EXTRACTION

This method is commonly used for cleaning sample , and is routinely by most laboratories.
But 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 cause long extraction time .
Toluene is brought to a slow boil in a pyrex flask. Its vapour moved upwards and the core
become engulfed in the toluene vapour ( around 110 oC ) . Eventual water within the core
sample in the thimble will be vapourized. The toluene and water vapour enter the inner
chamber of the condenser, the cold water circulating about the inner chamber condenses both
vapour to immiscible liquids . The toluene soak the core sample and dissolve any oil which
come into contact . When the liquid level in soxhlet tube reach top of the siphon tube
arrangement , the liquid within the soxhlet tube are automatically emptied by a siphon effect
and flow into the boiling flask. The toluene is the ready to start another cycle .

2.5 DEAN-STARK DISTILLATION-EXTRACTION

The Dean Stark distillation provide a direct determination of water content. The oil and
water area extracted by dripping a solvent, usually toluene or a mixture of acetone and
chloroform, over the plug sample. In this method, the water and the solvent are vaporized,
recondensed in a cooled tube in the top of apparatus and the water is collected in a calibrated
chamber. The solvent overflow and drops back over the samples. The oil removed from the
sample remain in solution in the solvent. Oil content is calculated by the difference between
the weight of water recovered and the total weight loss after extraction and drying .

2.6 VACUUM DISTILLATION

A sample is placed within a leakproof vacuum system and heated to a maximum temperature
of 230 0C. Liquids within the sample are vaporized and passed through a condensing column
that is cooled by liquid nitrogen .

CONCLUSION
Based on the data above, we can conclude that all the method above can be used to determine
the water saturation. The direct-injection method is effective, but slow. The method of
flushing by using centrifuge is limited to plug-sized sample. The samples also must have
sufficient mechanical strength to withstand the stress imposed by centrifuging . However, the
procedure is fast . The gas driven-extraction method is slow . The disadvantage is that it is not
suitable for poorly consolidated sample or chalky limestone. The distillation in a soxhlet
apparatus is slow, but give less stress on the sample. The procedure is simple and very
accurate water content determination can be made. Vacuum distillation is often used for full
diameter cores because the process is relatively rapid. Vacuum distillation is also can be used
for poorly consolidated core since the process does not damage the sample. The oil and water
values are measured directly and dependently of each other.

Question 3 : Chose one method and Describe the experiment.

1.0 SUMMARY
The objectives of this saturation determination experiment are to study the procedures in
cleaning of the core samples from residual fluids and to define and determine the oil and gas
saturation of a core sample using the Dean-stark distillation-extraction method. But due to
technical and laboratory problem, we were unable to conduct this experiment. However, we
managed to do some research and finding about saturation determination, procedure in
cleaning of the core samples from residual fluids and about the Dean-stark distillationextraction method in order to achieve the understanding and objectives of this experiment
without conducting the experiment.
We suppose to heat the hydrocarbon solvent which is toluene to its boiling point which is 110
C. Its vapour will move upward and the rock sample becomes immerse in the toluene
vapours that begin to extract the oil and water present in the rock sample. Then the rising
vapour will be condense in condenser and collected in the graduated tube.

Since toluene is completely miscible with the extracted oil, the condensed liquid in the
graduated tube will consist of two liquid phases which are water and mixed hydrocarbon
phase containing toluene and oil from the rock sample. Due to higher density, the water phase
will settles at the bottom of the graduated tube while the solvent overflow and drips back over
the rocks sample. This process should be continuing until no more water is collect in the
receiving tube.

2.0 INTRODUCTION
When the core arrives in the laboratory, plugs are usually drilled 20 to 30 cm apart
throughout the reservoir interval. All these plugs are analyzed with respect to porosity,
permeability saturation and lithology. Fluid saturation can be determined by a few methods
which include injection of solvent, centrifuges flushing, gas driven solvent extraction and
Dean-stark distillation-extraction.
The Dean-stark distillation-extraction is appropriate for plug samples and for rotary sidewall
cores. This method of determination fluids saturation depends upon the distillation of water
fraction and solvent extraction of oil fraction from the sample. Besides, this method provides
a direct determination of water content. The oil and water are extracted by dripping a solvent,
usually toluene or a mixture of acetone and chloroform aver the plug samples. In this method,
water and solvent are vaporized, re-condensed in cooled tube in on the top of apparatus and
water is collected in calibrated chamber.
The set up basically consist of a longneck round-bottom flask that contains a suitable
hydrocarbon solvent such as toluene, a heating element or electric heater to boil the solvent, a
condenser and a graduated tube receiver to measure the volume of extracted fluids.

3.0 OBJECTIVES
1. To study the procedure in cleaning of the core samples from residual fluids.
2. To define and determine the oil and gas and water saturation of a core sample using
Dean-stark distillation - extraction method.

4.0 THEORY
Fluid saturation is defined as the ratio of the volume of fluid in a given core sample to the
pore volume of the sample.
S w=

Vw
VP

S 0=

V0
VP

Sg =

Vg
VP

S w + So + S g=1
where Vw, Vo, Vg and Vp are water, oil, gas and pore volumes respectively. Meanwhile Sw,
So and Sg are water, oil and gas saturations. Fluid saturation may be reported either as a
fraction of total porosity or as a fraction of effective porosity. Since fluid in pore spaces that
are not interconnected can not be produced from a well, the saturations are more meaningful
if expressed on the basis of effective porosity. The weight of water collected from the sample
is calculated from the volume of water by the relationship:
W w = w V w
where w is water density in g/cm3. The weight of oil removed from the core may be
computed as the weight of liquid less weight of water:
W o =W LW w

where

WL

is the weight of liquids removed from the core sample in gram. Oil volume

may then be calculated as Wo/o. Pore volume Vp is determined by a porosity measurement.

Oil, gas and water saturation may be calculated by equation above.

5.0 APPARATUS
1. Dean-stark apparatus
2. Rock sample(core plug)
3. Solvent

6.0 PROCEDURE
1. Weigh a clean, dry thimble. Use tongs to handle the thimble.
2. Place the cylindrical core plug inside the thimble, and then quickly weigh the thimble and
sample.
3. Fill the extraction flask two-thirds full with toluene. Place the thimble with sample into the
long neck flask.
4. Tighten the ground joint fittings, but do not apply any lubricant for creating tighter joints.
Start circulating cold water in the condenser.
5. Turn on the heating jacket or plate and adjust the rate of boiling so that the reflux from the
condenser is a few drops of solvent per second. The water circulation rate should be adjusted
so that excessive cooling does not prevent the condenser solvent from reaching the core
sample.
6. Continue the extraction until the solvent is clear. Change solvent if necessary.
7. Read the volume of collected water in the graduated tube. Turn off the heater and cooling
water and place the sample into the oven (from 105

to 120

), until the sample

weight does not change. The dried sample should be stored in desiccators.
8. Obtain the weight of the thimble and the dry core.
9. Calculate the loss in weight WL, of the core sample due to the removal of oil and water.
10. Measure the density of a separate sample of the oil.
11. Calculate the oil, water and gas saturations after the pore volume Vp of the sample is
determined (O.Torsaeter, 2000).

7.0 RESULTS
Porosity, : 11.5 %
Worg

Wdry

g/cm

g/cm

Vw

Wo

Vo

Vp

cm3

cm3

cm3

So

Sw

Sg

31.98

31.44

1.00

0.80

0.34

0.20

0.25

0.132

0.410

0.562

0.026

Where
Worg: Weight of original saturated sample
Wdry: Weight of desaturated and dry sample

Calculation
WL = Worg - Wdry
= 31.984g 31.441 g = 0.543 g
weight of water -0.343 g
Wo = WL - Ww
= 0.543g - 0.343g
=0.200 g
Vb =

(D/2)2 L

(1.5 / 2)2 (3.0)

= 5.3 cm3
Vw = Ww / w
= 0.343 /1.0
= 0.343 cm3
Vo= Wo / o
= 0.2 / 0.8
= 0.25 cm3
Volume of pore
Assume Porosity =11.5%
Vp =

Vb

= (11.5 / 100 )( 5.3)

= 0.6095 cm3

Where D and L are diameter and length of the core sample, respectively.
Diameter of core plug sample 1.5 cm
Length of core plug sample 3.0 cm

Saturation
Sw = V w / V p
= 0.343 / 0.6095
= 0.5628
So = V o / V p
= 0.250 / 0.6095
= 0.4102

Sg + Sw + So = 1
Sg = 1-Sw-So
= 1- 0.5628 0.4104
= 0.0268
8.0 DISCUSSION
The main objective of this experiment is to determine the oil, water and gas saturation of a
core sample. Saturation is the measure of how much porosity of porous medium been
occupied by fluid. Fluid saturation is defined as the ratio of the volume of fluid in a given
core sample to the pore volume of the sample.

The experiment need to be carried in such orders as first weighed a clean, dry thimble and
then place the cylindrical core plug inside the thimble, and then quickly weigh the thimble
and sample. Next filled the extraction flask two-thirds full with toluene and placed the
thimble with sample into the long neck flask. After that, start circulating cold water in the
condenser Turn on the heating jacket or plate and adjust the rate of boiling so that the
reflux from the condenser is a few drops of solvent per second. Continued the extraction until
the solvent is clear. By the time it finish, Turn off the heater and cooling water and place
the sample into the oven (from 1050C to 1200C), until the sample weight does not change
meanwhile the dried sample should be stored in a desiccators. Then, the weight of the thimble
and the dry core is obtained in order to calculate the loss in weight WL, of the core sample
due to the removal of oil and water. Measure the density of a separate sample of the oil and
last calculate the oil and water saturation.
However, due to unavoidable technical problems we are unable to carry out this experiment
thoroughly. For the information, as we know it is important to consider the saturation change
occurring in the core from in-situ to surface conditions. Such as the condition, suppose a core

is being recovered while drilling a well with water-based drilling mud. Water from the
drilling mud will enter the rock expulsing oil. The result as the core is lifted, the reduction in
pressure will cause the oil to release gas and this will expand expulsing oil and water out of
the rock.

9.0 CONCLUSION
The main objective of this experiment is to determine the oil, water and gas saturation of a
core sample using the Dean-stark distillation. Through this experiment we can also study the
procedures in cleaning of the core samples from residual fluids. But due to technical and
laboratory problem, we were unable to conduct this experiment. Saturation is the important
parameter that we should know to estimate how much fluids occupied in the pore space. The
fluids are oil, water or gas. As we know it is important to consider the saturation change
occurring in the core from in-situ to surface conditions. Such as the condition, suppose a core
is being recovered while drilling a well with water-based drilling mud. Water from the
drilling mud will enter the rock expulsing oil. The result as the core is lifted, the reduction in
pressure will cause the oil to release gas and this will expand expulsing oil and water out of
the rock.

10.0 REFERENCES
1. Dean-Stark apparatus. (2013, March 15). Retrieved May 19, 2013, from Dean-Stark
apparatus: http://en.wikipedia.org/wiki/Dean-Stark_apparatus
2. O.Torsaeter, M. A. (2000, August). Experimental Reservoir Engineering Laboratory
Workbook. Retrieved May 19, 2013, from Experimental Reservoir Engineering
Laboratory Workbook: http://www.ipt.ntnu.no/~oletor/kompendium4015.pdf
3. http://www.ipt.ntnu.no/~oletor/kompendium4015.pdf

11.0 APPENDICES

Figure 1: Modified Dean and Stark Extraction apparatus for determining Toluene insoluble in
phosphorus (Dean-Stark apparatus, 2013).

Figure 2: Dean-Stark apparatus (Dean-Stark apparatus, 2013)

1: Stirrer bar/anti-bumping granules

2: Still pot
3: Fractionating column
4: Thermometer/Boiling point temperature
5: Condenser
6: Cooling water in
7: Cooling water out
8: Burette
9: Tap
10: Collection vessel