Question 1: Definition of fluid saturation

Saturation is the measure of the fluid volume present in the pore volume of a
porous medium. By definition, the saturation of a fluid is the ratio of the fluid
volume to the pore volume or the rock.

Hence,

considering the fluids typically present in a reservoir

rock:
This property is expressed mathematically by the
following relationship:

fluid saturation:

total volume of the fluid

pore volume

The average saturation of each reservoir fluid is calculated from the following
equations:

volume of oil
pore volume

volume of gas
,S
pore volume

volume of water
,S
pore volume

,S

: oil saturation

: gas saturation

: water saturation

All the saturation values based on pore volume and not on the gross reservoir
volume. The saturation of each individual phase ranges between zero to 100
percent. By definition, the sum of the saturation is 100% and can be verified with
this equation:

+S

+ S

= 1.0

The fluids in most reservoirs are believed to have reached a state of

equilibrium and, therefore, will have become separated according to their density,
i.e., oil overlain by gas and underlain by water. In addition to the bottom (or edge)
water, there will be connate water distributed throughout the oil and gas zones. The
water in these zone will have been reduced to some irreducible minimum. The
forces retaining the water in the oil and gas zones are referred to as capillary forces
because they are important only in pore spaces of capillary size.

Connate (interstitial) water saturation S wc is important primarily because it

reduces the amount of space available between oil and gas. It is generally not
uniformly distributed throughout the reservoir but varies with permeability,
lithology, and height above the free water table.

Another particular phase

saturation of interest is called the critical saturation and it is associated with each
reservoir fluid.

Where Si and Vi, I = w,o,g and are the saturations and volumes of water, oil,
and gas. The sum of saturation of each fluid phase is equal to unity since the pore
space is completely filled with fluids (or at least the effective pore volume). Because
the fluids and their saturations in the pore space may vary from point to point and
pore to pore, the values of saturation are meaningful only for samples large enough
for the porous medium to be considered a continuum.
It is important to consider the saturation change occurring in the core from
in-situ to surface conditions. 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. 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.
These Figure presents saturation values at different stages of core extraction
showing how important the change in saturation can be.

Example of Saturation Changes Occurring in the Core from In-situ to

Surface Conditions

QUESTION 2: Compare all methods to determine the fluid saturation

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. Centrifuge Flushing
A centrifuge which has been fitted with a special head sprays warm solvent onto the
sample. The centrifugal force then moves the solvent through the sample. The used
solvent can be collected and recycled.
3. Gas Driven Solvent Extraction
The sample is placed in a pressurized atmosphere of solvent containing dissolved
gas. The solvent fills the pores of sample. When the pressure is decreased, the gas
comes out of solution, expands, and drives fluids out of the rock pore space. This
process can be repeated as many times as necessary.
4. Soxhlet Extraction
A Soxhlet extraction apparatus is the most common method for cleaning sample,
and is routinely used by most laboratories. As shown in Figure 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 110C). Eventual water within the
core sample in the 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
extraction time.
Electric or gas heaters are used to vaporize the solvent. The hot vapors meet the
samples in the thimble and dissolve the oil and water. Vapors are condensed and
cover the sample until over- flown back to the solvent flask. The extraction process
continues for several hours and is terminated when no more oil remains in the
samples. This is recognized when the condensing vapors remain clean because no
oils is left in the cores to be dissolved. After the extraction, samples are dried in an
electric oven. Sometimes vacuum may also be applied to the oven. 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 extraction time. The dried samples are
kept in a desiccator sealed with grease and has some moisture absorbents at its
bottom.
5. Dean-Stark Distillation-Extraction
The Dean-Stark distillation provides 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 samples. In this method, the water and
solvent are vaporized, recondensed in a cooled tube in the top of the apparatus and
the water is collected in a calibrated chamber (Figure b). The solvent overflows and
drips back over the samples. The oil removed from the samples remains 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.

Figure: Schematic diagram of Soxhlet (a) and Dean- Stark (b) apparatus
6. Vacuum Distillation
The oil and water content of cores may be determined by this method. As shown in
Figure c, a sample is placed within a leak proof vacuum system and heated to a
maximum temperature of 230C. Liquids within the sample are vaporized and
passed through a condensing column that is cooled by liquid nitrogen.

Figure C: Vacuum distillation Apparatus.

Summary of method
The direct-injection method is effective, but slow. The method of flushing by using
centrifuge is limited to plug-sized samples. 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 here
is that it is not suitable for poorly consolidated samples or chalky limestone. The
distillation in a Soxhlet apparatus is slow, but is gentle on the samples. 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 and frequently used for poorly consolidated cores since the process
does not damage the sample. The oil and water values are measured directly and
dependently of each other.
In each of these methods, the number of cycles or amount of solvent which must be
used depends on the nature of the hydrocarbons being removed and the solvent
used. Often, more than one solvent must be used to clean a sample. The solvents
selected must not react with the minerals in the core. The commonly used solvents
are:
Acetone, Benzene, Carbon-tetrachloride, Chloroform, Methylene Dichloride,
Toluene, Trichloro Ethylene, Xylene and etc
Toluene and benzene are most frequently used to remove oil and methanol and
water is used to remove salt from interstitial or filtrate water. The cleaning
procedures used are specifically important in special core analysis tests, as the
cleaning itself may change wettabilitys.
The core sample is dried for the purpose of removing connate water from the pores,
or to remove solvents used in cleaning the cores. When hydratable minerals are
present, the drying procedure is critical since interstitial water must be removed
without mineral alteration. Drying is commonly performed in a regular oven or a
vacuum oven at temperatures between 50C to 105C. If problems with clay are
expected, drying the samples at 60C and 40 % relative humidity will not damage
the samples.

Question 3: Assume that you have been asked to carry out an experiment
to determine the fluid saturation in core sample. Choose one method and
describe in details the procedure, expected data and calculations,
equations involved and summary of your experiment
Saturation determination: The Dean-Stark distillation

Objective:
-

The objective of the experiment is to determine the oil, water and gas saturation
of a core sample.

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.

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 distillation-extraction 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 vapor will move upward and the rock sample becomes
immerse in the toluene vapors that begin to extract the oil and water present in the
rock sample. Then the rising vapor 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.

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 distillationextraction 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

Theory:
Fluid saturation can be determined by a few methods which includes injection of
solvent, centrifuges flushing, gas driven solvent extraction and Dean-stark
distillation-extraction. The Dean-stark Distillation-extraction method of determining

fluids saturation depends upon the distillation of water fraction and solvent
extraction of oil fraction from sample. The Dean-Stark 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 chloroforms over the plug
samples. In this method, water and solvent are vaporized, re-condensed in a cooled
tube in on the top of apparatus and water is collected in calibrated chamber. The
solvent overflows and drips back over the samples. The oil removed from the
samples remains 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.

The Dean and Stark procedure can be used to measure water content of a
diverse range of samples, and has been extensively used in industrial laboratories
to measure water in petroleum oils. The oil content is calculated from weight
difference and therefore it is important that no sand grains be lost from the core
during the analysis, as this would result in erroneously high calculated residual oil
saturation.
The principle of operation is straightforward. When the core to be analyzed is
weighed, the resulting measurement will consist of the weight of the sand grains, as
well as the oil and water present in the pore space. The sample is then placed
within a tear in the apparatus, and this unit is suspended above a flask containing a
solvent such as toluene. Whatever the solvent, it must have a boiling point higher
than water and be both immiscible with and lighter than water. The dripping solvent
mixes with oil from the sample, and both the solvent and oil are returned to the
solvent flask. The process continues until the sample is raised to the boiling point of
water. When it does, the water vaporizes, rises in the condensing tube until it is
condensed, and falls back into the calibrated tube. Because it is heavier than the
solvent, it collects at the bottom of the tube, where its volume can be measured.
When successive readings indicate no additional water recovery has occurred, we
know all water has been removed from the sample, and the water volume is
recorded for further calculations

Apparatus:
-

Dean-stark apparatus

Rock sample(core plug)

Solvent

Procedure:

1) Weigh a clean, dry thimble. Use tongs to handle the thimble.

2) Place the cylindrical core plug inside the thimble, 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 105C to 120C),
until the sample weight does not change. The dried sample should be stored in a
desiccater.
8) Obtain the weight of the thimble and the dry core.
9) Calculate the loss in weight W L, 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.

Data and calculations:

Sample No:
Porosity, :

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

Where D and L are diameter and length of the core

sample, respectively

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 105 C to 120C), 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.

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

References
a) Ahmed, Tarek : Reservoir Engineering Handbook-Ch.4: Fundamentals of Rock
Properties, Second Edition, Gulf Professional Publishing, 2001.
b) Amyx, James : Petroleum Reservoir Engineering-Ch.2: Fundamental Properties of
Fluid Permeated Rocks, 1960
c) Dean-Stark apparatus . (2013, March 15). Retrieved May 19, 2013, from DeanStark apparatus: http://en.wikipedia.org/wiki/Dean-Stark_apparatus 2.
d) O.Torsaeter,

M.

A.

Laboratory Workbook
Engineering

(2000,

August).

Experimental

Reservoir

Engineering

. Retrieved May 19, 2013, from Experimental Reservoir

Laboratory

http://www.ipt.ntnu.no/~oletor/kompendium4015.pdf 3.
e) http://www.ipt.ntnu.no/~oletor/kompendium4015.pdf

Workbook:

Appendix

Modified Dean and Stark Extraction apparatus for determining Toluene insoluble in
phosphorus