SPE 105534

Case Studies of Emulsion Behavior at Reservoir Conditions

Sunil Kokal, SPE, and Mohammed Al-Dokhi, Saudi Aramco
Copyright 2007, Society of Petroleum Engineers
This paper was prepared for presentation at the 15th SPE Middle East Oil & Gas Show and
Conference held in Bahrain International Exhibition Centre, Kingdom of Bahrain, 1114 March
2007.
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Abstract
Most emulsion studies are conducted with depressurized
crude/water samples. Can emulsions form in the reservoir at
high pressures and high temperatures? The answer to this
question is generally anecdotal. This paper provides a unique
method and new data from emulsion studies at high pressures
and high temperatures. Two case studies will be presented
where emulsions were suspected to be the cause of production
challenges in several wells. The experiments were conducted
in a special visual PVT cell with the capability of observing
emulsion phase behavior at reservoir conditions. The effects of
several variables on emulsion behavior were investigated
including shear, pressure, temperature, watercuts, and
asphaltene precipitation tendency of the crude.
The first case study is in a field that produces tight
emulsions. The results of this study indicate that emulsions
can form at reservoir conditions, with mixing, especially if the
crude has a propensity to precipitate asphaltenes. The new
data suggests that emulsion behavior is closely linked to the
presence of fine solids through in-situ dynamic precipitation
of organic (asphaltenes) and inorganic salts (scales) as well as
fines migration in the reservoir. In the second case study, a
series of emulsion tests were performed on bottomhole and
wellhead samples from several wells. The results suggests that
the emulsions are relatively loose at bottomhole conditions but
become progressively tighter with a reduction in pressure and
temperature. The tightness of the emulsions was linked to fine
solids that stabilize them. These include primarily calcite and
sulfur-rich heavy hydrocarbons like asphaltenes, with trace
amounts of silicates (clays and/or fine grained silica), iron-rich
precipitates and barite.

Introduction
Produced crude oil is generally commingled with water which
can cause a number of challenges during oil production. Some
of this water can form an emulsion with the crude oil.
Emulsions are difficult to treat and cause a number of
operational problems such as tripping of separation equipment
in gas-oil separating plants (GOSP), productivity decline in
wells, production of off-spec crude oil, and creating high
pressure drops in flow lines. Emulsions have to be treated to
remove the dispersed water and associated inorganic salts to
meet crude specification for transportation, storage and export
and to reduce corrosion and catalyst poisoning in downstream
processing facilities.
Emulsions can be encountered in almost all phases of oil
production and processing (Fig. 1): inside the reservoirs, well
bores and well heads, wet crude handling facilities,
transportation through pipelines, crude storage and during
petroleum processing. The question that has received some
debate is the formation and nature of emulsions inside the
reservoir, and in the wellbores at bottomhole conditions. In
other words, can emulsions form inside the reservoir? This
paper provides a novel method and new data from emulsion
studies at high pressures and high temperatures. Two case
studies are presented where emulsions were suspected to be
the cause of production challenges in several wells. The
experiments were conducted in a special visual PVT cell with
the capability of observing emulsion phase behavior at
reservoir conditions. The effects of several variables on
emulsion behavior were investigated including shear, pressure,
temperature, watercuts, and asphaltene precipitation tendency
of the crude.
There is very little work reported on petroleum emulsion
behavior at high pressures and temperatures (HPHT), i.e., at
reservoir conditions1-2. The bulk of the reported work has been
conducted with depressurized emulsion samples3-6. One of the
challenges in conducting HPHT work with emulsions has been
the availability (or lack of) equipment for handling them. This
paper describes a method which uses a PVT (pressurevolume-temperature) cell to study emulsion behavior at HPHT
conditions.
Experimental Setup
A state-of-the-art PVT apparatus was used to investigate the
behavior of emulsions under live HPHT conditions7. It is a
high pressure, high temperature apparatus and consists of a

variable volume, visual PVT cell that is retrofitted with fiber

optic light transmission probes to observe the behavior of
fluids concurrently with fluid volumetric data. A schematic of
the apparatus is shown in Fig. 2. The apparatus consists of a
laser power source, a fiber optic bundle that carries the laser
light into the PVT cell, the actual PVT cell containing the
crude at pressure and temperature, another fiber optic bundle
that carries the transmitted laser light from the PVT cell, and a
power meter that measures the amount of light received. The
PVT cell is mounted inside a temperature-controlled oven and
has an effective volume of 110 cc. The PVT cell is a
windowed cell that permits visual observation of the fluids
inside the cell. A variable-volume displacement pump controls
the volume and pressure of the fluid inside the cell. The PVT
cell also has a specially designed magnetically coupled
impeller mixer that provides powerful mixing and maintains
equilibrium in the fluid system. The PVT cell is designed for
operation at pressures up to 10,000 psi and temperatures up to
360oF.
The apparatus was designed for detecting the onset of
asphaltene precipitation from crude oils7. Example plots of
precipitating and non-precipitating fluids are shown in Fig. 3.
For the non-precipitating fluid the laser power (as measured
by the power meter) increases monotonically (almost linearly)
as the pressure is dropped down to the bubble point. At this
point the evolving gas bubbles scatter light and the
transmittance drops sharply. For the precipitating fluid, the
laser power drops before the bubble point. The point at which
the curve deviates from the straight line corresponds to the
onset of asphaltene precipitation. This drop in laser power is
related to the precipitation of solids that scatter light and cause
the power of the transmitted light to deviate from the expected
linear curve. The point determines the onset pressure for solids
precipitation.
The sample was first transferred from the single-phase
bottomhole sampler (see section below) into a titanium
floating-piston cylinder maintained at reservoir conditions. A
typical experiment was conducted by transferring a small
amount of emulsion or oil sample (~40 cc) from the titanium
cylinder (at reservoir conditions) into the PVT cell. The PVT
cell was maintained at reservoir temperature and a specified
pressure. The fluid sample was visually observed in the cell.
The procedures followed during the experiments are described
under the individual case studies.
Sampling.
The samples used in this study were single-phase (liquid)
bottomhole samples collected using special single-phase
samplers. The procedures for collecting these samples are
described elsewhere8. The samples were maintained in single
phase conditions and transferred into titanium floating piston
cylinders. The samples were then transferred into the PVT
apparatus, also maintained at HPHT conditions. It is important
to note that the collected sample never split into two-phases
(gas-liquid) during sampling, handling, transferring and
experimenting. This is important for such studies as it has

SPE 105534

been illustrated that asphaltene precipitation during handling

can impact the results.
Case Study I
A few wells in a Saudi Arabian field (Field-A) have shown
production related challenges that were thought to be affected
by asphaltene precipitation and emulsion blocks2. These
challenges were specially pronounced after the wells became
wet. This study was initiated with the objective of finding the
causes of production related challenges in these wells and
finding effective ways to mitigate the problem. Several
potential causes were investigated including the precipitation
of asphaltenes, emulsion blocking, mixing of hydrocarbons
from a deeper reservoir, inorganic scale precipitation, aquifer
brine and injected water compatibility, regional geology
including rock quality, drilling fluid damage, and distance of
wells from the Gas Oil Separation Plant (GOSP). These were
described in an earlier SPE paper2.
This section presents the extensive experimental work
done to understand the emulsion behavior at reservoir
conditions.
Emulsions Experiments at Reservoir Conditions. To
investigate the formation of emulsions at reservoir conditions
several tests were designed and conducted in the PVT
apparatus described earlier. This is the first time such
experiments have been conducted to our knowledge. The first
step was to conduct an asphaltene precipitation onset
experiment.
Fig. 4 shows the asphaltene precipitation onset results for
Well-1. Several cycles were repeated (depressurization
followed by repressurization) and precipitation was observed
in each of the cycles. There is some evidence of asphaltene
redissolution as the fluid is pressurized. These experiments
show that the precipitation tendency is not strong and may be
kinetically controlled (time-dependent). It was also observed
that once precipitation starts, the precipitated asphaltenes
aggravated the situation and caused further precipitation. For
dry wells, contact with water aggravated the precipitation of
asphaltenes.
At the end of the pressurization experiment the laser power
output was ~3 W. The pressure was then stabilized at 3000
psi @ 210oF. Reservoir brine was then added very slowly
from the bottom of the cell at a rate to avoid any mixing of oil
and water. The brine formed a clear phase at the bottom of the
cell. After the brine was added the laser output was recorded
and is plotted in Fig. 5. After a few minutes the oil and water
mixture in the cell was mixed very slowly using the stirrer.
The laser power dropped immediately as the water formed
droplets that came in the path of the laser light. This reduction
in laser power is attributed to light absorbance as well as light
scattering by water droplets. The stirrer was stopped and the
oil-water mixture left to stand for a few minutes. The laser
power increased slowly as the water droplets settled down at
the bottom of the cell. Free water was observed as water
droplets coalesced at the bottom of the cell. The mixer was
started slowly again and the same cycle was observed. After a

SPE 105534

few minutes the mixer was started at high speed (for a few
seconds) to mix the oil and water thoroughly. The mixture was
then allowed to stand and observed visually (through the PVT
cell) as well as through the laser light. The settling time was
increased. Visually no oil-water separation was observed. The
laser output increased beyond the values at the beginning of
the experiment. An explanation for this observation is as
follows: during stirring the water mixes with the oil and forms
an emulsion (water-in-oil). The emulsion is formed and
stabilized by the fine asphaltene particles that were present in
the crude oil. The asphaltene-stabilized water droplets descend
to the bottom of the cell and away from the path of the laser
light. As finer water droplets descend, they carry the
asphaltenes, and hence the laser light output increases. No free
water was seen at the bottom of the PVT cell indicating the
formation of a tight emulsion. Once the laser light output had
stabilized, the oil-water mixture was mixed again thoroughly
by starting the stirrer for a few seconds. The mixture was
allowed to stand overnight. A similar behavior was observed:
no oil-water separation and no free water at the bottom of the
cell. The mixing had caused the formation of a very tight
emulsion.
After 20 hours, 100 ppm of demulsifier was injected to
enhance oil-water separation. The demulsifier was mixed
using the stirrer. The laser-light response was dramatic. It
went down during mixing and then rapidly increased upon
standing. There was still no free water seen at the bottom of
the cell. Another 100 ppm of demulsifier was added and the
mixture was allowed to stand. Within minutes the tight
emulsion was broken and water droplets were seen coalescing
at the bottom of the cell. After a few minutes, the water had
separated completely.
These experiments clearly showed that tight emulsions
were formed at reservoir conditions that were difficult to
break. High concentration of demulsifier (200 ppm) was
needed to break the emulsions completely. The foregoing
experiments show that small amounts of asphaltene
precipitation (minor by itself) may help in the stabilization of
emulsion upon water encroachment. Furthermore, this action
may be aggravated when the rock quality is tighter resulting in
high pore velocities causing more shear, and small rock pore
throat sizes, causing the blocking by emulsions to be more
effective.
Extensive investigations2 carried out with the samples
suggests that emulsion behavior is closely linked to the
presence of fine solids through in-situ dynamic precipitation
of organic (asphaltenes) and inorganic salts (scales) as well as
fines migration in the reservoir. These are described in
Reference 2.
Case Study II
Another field has been facing emulsion challenges after the
wells started to produce water9. It has three operating offshore
GOSPs and one onshore GOSP to process the crude. The wet
crude forms a very tight, complex emulsion that settles down
in the processing equipment. An investigative study9
diagnosed the problem related to emulsions, which was

brought under control by the installation of demulsifier dosing

pumps. It is now confirmed that the emulsions at the wellhead
(before demulsifier injection) are tight. When, how and where
do the emulsions become tight? Are they tight at bottomhole
conditions? The tightness of the emulsion has affected the
flow assurance and deliverability of these wells. This study
was initiated to determine the characteristics of pressurized
emulsions and investigate the causes of emulsion problems in
the field.
A series of emulsion tests were conducted at surface and
reservoir conditions. The section below describes emulsion
experiments at reservoir conditions. Depressurized emulsion
experiments were described in an earlier SPE paper9.
Emulsions Experiments at Reservoir Conditions. A singlephase sample was collected from a producing well in the field.
The sample was first transferred from the single-phase
bottomhole sampler into a titanium floating-piston cylinder
maintained at reservoir conditions. It contained oil and water
when heated to reservoir temperature.
Oil was transferred at from the top of the cylinder into the
PVT cell. A simple asphaltene precipitation depressurization
test was conducted at a reservoir temperature of 170oF. The
results are shown in Fig 6 and indicate that there was no
precipitation observed during depressurization. Several other
cycles were repeated and not precipitation was observed at
reservoir conditions.
Water was then slowly transferred from the bottom of the
cylinder to constitute a 25% watercut sample in the PVT cell.
Several emulsion experiments were conducted at different
temperature and pressures. The brine formed a clear phase at
the bottom of the cell. The oil and water mixture in the cell
was mixed very slowly using the stirrer. The mixing was
conducted in three steps of low, medium and high shear by
controlling the speed of the mixer inside the PVT cell as
follows:
o Low Shear: The fluid sample (oil+water) was mixed
using a mixer in the PVT cell. The amount of mixing was
limited to a quarter turn for the mixing knob (~200 rpm)
for 10 seconds.
o Medium Shear: The fluid sample (oil+water) was mixed
using a mixer in the PVT cell. The amount of mixing was
limited to a half turn for the mixing knob (~400 rpm) for
10 seconds.
o High Shear: The fluid sample (oil+water) was mixed
using a mixer in the PVT cell. The amount of mixing was
limited to a quarter turn for the mixing knob (~600 rpm)
for 10 seconds.
After low-shear mixing the stirrer was stopped and the oilwater mixture left to stand for a few minutes. The photographs
of the cell during the experiment are shown in Figs. 7-8. Free
water was observed as water droplets coalesced at the bottom
of the cell. The mixer was started at a slightly higher speed
(designated as medium shear). The mixture was then allowed
to stand and observed visually (through the PVT cell). The
settling time was increased. Visually some oil-water

SPE 105534

separation was observed (Figs. 7-8). During the third cycle the
mixer was started at a higher speed (high shear case).
The fluids were then observed visually after mixing to
monitor the oil-water separation and the formation and
stability of emulsions. The observations are described in the
table below:
Expt.
No
Shear

T
(F)
165

P
(psi)
3000

Low
Shear

165

3000

Medium
Shear

165

3000

High
Shear

165

3000

Low
Shear

130

1800

Low
Shear

85

888

Observations
Very fast separation. No
emulsions observed at reservoir
condition.
Fast emulsion break and water
separated partially within one
hour, small rag layer was formed.
Slower emulsion break and water
separated partially within two
hours, small rag layer was formed.
Slower emulsion break and water
separated partially within eight
hours, rag layer was formed.
Slower emulsion break and water
separated partially within 24
hours, rag/interfacial layer was
formed.
Slowest emulsion break and water
separated partially within 24
hours. Tight emulsion with a
prominent rag layer was formed in
the middle.

The results clearly indicate that the emulsions were not stable
(separated into oil and water) at bottomhole, reservoir
conditions. With mixing and a reduction in pressures and
temperatures (wellhead conditions), the emulsions became
progressively tighter. This indicates that emulsions are being
stabilized during the production process from the bottomhole
to the wellhead. By the time the emulsions have reached the
wellhead, emulsions have become relatively tight.
The tightness of the emulsions was linked to fine solids
that stabilize them. These include primarily calcite and sulfurrich heavy hydrocarbons like asphaltenes, with trace amounts
of silicates (clays and/or fine grained silica), iron-rich
precipitates and barite.
Conclusions
The following conclusions are based on this work:
A novel method has been presented to observe and
understand the characteristics of emulsions in a high
pressure and high temperature environment.
Emulsions are generally not formed inside the reservoir
before discovery. Their formation is linked with mixing
and/or changes in pressure, temperature and presence of
fine solids.

Crudes that have a tendency to precipitate asphaltenes are

likely to form tight(er) emulsions.

Acknowledgments
The authors would like to acknowledge the help of several
individuals in this study: Hydrocarbon Phase Behavior unit
employees for sampling and handling of samples, and
Reservoir Engineering Department engineers for working
closely on the studies.
References
1. Kokal, S.L. and Alvarez, C., Reducing Pressure Drop in
Offshore Pipelines by Controlling the Viscosities of
Pressurized Emulsions SPE 81511 paper presented at the
6th Middle East Oil Show, Bahrain, March (2003).
2. Kokal, S.L. et al. Productivity Decline in Oil Wells
Related to Asphaltene Precipitation and Emulsion
Blocks SPE 87088 published in Reservoir Engineering
and Evaluation, November (2003).
3. Kokal, S.L.: Crude Oil Emulsions Chapter in SPE
Petroleum
Engineering
Handbook,
General
Engineering, SPE (2006).
4. Schramm, L., Emulsions: Fundamentals and
Applications in the Petroleum Industry, Advances in
Chemistry Series No. 231, Washington, DC (1992).
5. Kilpatrick, P.K. and Spiecker, P.M., Asphaltene
Emulsions, in Encyclopedic Handbook of Emulsion
Technology, Sjoblom J. (Ed.) Dekker (2001)
6. Yarranton, H.W., Hussein, H., Masliyah, J.H., "Water-inHydrocarbon Emulsions Stabilized by Asphaltenes at
Low Concentrations," J. Colloid Interface Sci., 228,
(2000), 52-63.
7. Hammami, A., Chang-Yen, D., Nighswander, J.A., and
Strange, E., An Experimental Study of the Effect of
Paraffinic Solvents on the Onset and Bulk Precipitation of
Asphaltenes, Fuel Science & Tech.. Int., Vol 13(9), pp
1167-1184 (1995).
8. Williams, J and Kokal, S.L.: Reservoir Fluid Sampling
Chapter in SPE Petroleum Engineering Handbook,
General Engineering, SPE (2006).
9. Kokal, S.L., Al-Yousif, A., Meeranpillai, N.S., and AlAwaisi, M., Very Thick Crude Emulsions: A Field Case
Study of a Unique Crude Production Problem SPE
71467 paper presented at the SPE ATCE, New Orleans,
October (2001).

SPE 105534

Separator

Surface samples
Gas
Oil

PVT Cell

Water

Light
Detector

Emulsion
Grains

Laser Light
Source

Oil
Flow
Water-in-oil
emulsion

Oil-in-water
emulsion

Figure 2: Cross-section of the PVT Cell with

Laser Light Source and Detector

Figure 1: Photograph of the HP/HT PVT Apparatus

Source Fiber
Optics Bundle

PVT Cell

10
o

T = 210 F

detector
Detector Fiber
Optics Bundle

Laser Power
( W)

T = Constant
No precipitation

Laser Power (W)

Laser
Light
Source

8
6
4
Bubble Point

Precipitation
Bubble Point

0
0
Pressure

Figure 3: Schematic of the principle of operation

of the asphaltene precipitation cell

1500

Run 1 (Depressurization)
Run 2 (Depressurization)
Run 3 (Pressurization)
Run 4 (Depressurization)

3000

4500

6000

Pressure (psia)

Figure 4: Asphaltene precipitation experiment:

Well-1, Field-A

SPE 105534

2.5

10

T = 170 F

Very
Slow
Mixing

6
Brine
added

Stirrer on
few secs
Very
Slow
Mixing

100 ppm
Demulsifier
Stirrer
on few
secs

100 ppm
Demulsifier

Laser Power (W)

Laser Power (W)

T = 210 F
P = 3000 psi

2.0
1.5
1.0

Bubble Point

0.5
0.0

0
1

10

100

1000

10000

1500

Figure 5: Emulsion experiment: Well-1, Field-A

t=0s

t = 60 s

t = 600 s

t = 60 s

t = 900 s

t = 3600 s

t = 120 s

t = 1800 s

t = 2700 s

6000

t = 900 s

t = 1800 s

T = 165oF, P = 3000 psia - High shear

t = 1800 s

t = 60 s

t = 1200 s

t = 3600 s

t = 36000 s

T = 130oF, P = 1800 psia - Low shear

T = 165oF, P = 3000 psia - Low shear

t = 60 s

4500

Figure 6: Asphaltene precipitation experiment:

Well-1, Field-B

T = 165oF, P = 3000 psia - No shear

t=0s

3000

Pressure (psia)

Time (mins)

t = 3600 s

t = 60 s

t = 3600 s

t = 36000 s

t = 2 days

T = 165oF, P = 3000 psia - Medium shear

T = 85oF, P = 900 psia - Low shear

Figure 7: Photographs during emulsion

experiment with Field B reservoir fluids

Figure 8: Photographs during emulsion

experiment with Field B reservoir fluids