February 2011, Volume 2, No.

1
International Journal of Chemical and Environmental Engineering

Microwave Separation of Water-In-Crude Oil

Emulsions
S. Nuurul Hudaa and Abdurahman H.Nourb
Faculty of Chemical and Natural Resources Engineering
Universiti Malaysia Pahang, 26300 Kuantan, Pahang.
Corresponding author: anuurul_huda@yahoo.com, babdurahman@.ump.edu.my

Abstract
Formation of emulsions during oil production is a costly problem, both in terms of chemicals used and due to production losses. For
economic purpose, pipeline consideration and for efficient refinery operations, the produced emulsions must dewatered and necessary
to separate the water completely from the crude oils before transporting them. The objectives of this study was to study crude oil
emulsions stability using different volume ratio of water-oil and different types of crude oils as well as to examine the performance of
microwave application in demulsification of water-in-crude oil emulsions in comparison to the conventional methods. Two types of
crude oils with three volume ratios of water-oil 50-50%, 30-70% and 20-80% (w/o) were used and a type of surfactant was SDDS.
Two different microwave powers of 180 watt and 720 watt were used. This study revealed that the stability of the water-in-oil
emulsion stabilized by ionic surfactant increases as the surfactant concentration increased. Increasing the oil content of the emulsion
resulted in increased emulsion stability. In terms of demulsification, microwave heating technology can be an alternative method for
breaking water-oil emulsion. Microwave heating technology does not required chemical addition.

Key Words- Emulsion, surfactant, water-in-oil emulsion, demulsification, microwave.

1. Introduction
During oil production, crude oils are typically
produced as water in crude oil (w/o) emulsions, which are
often very stable [1]. Among the indigenous natural
surfactants contained in the crude oils, asphaltenes and
resins are known to play an important role in the
formation and stability of w/o emulsions [2, 3].
Asphaltenes are defined as the fraction of the crude oil
soluble in toluene or benzene, but precipitating in
pentane, hexane, or heptane. They are composed of
several polynuclear aromatic sheets surrounded by
hydrocarbon tails, and form particles whose molar masses
are included between 500 and 20,000g [4]. Resins are
molecules defined as being soluble in light alkanes
(pentane, hexane, or heptane), but insoluble in liquid
propane [1]. Resins are effective as dispersants of
asphaltenes in crude oil [5].
Petroleum oil is a mix of naturally organic compounds
contains primarily hydrogen, carbon and oxygen. There
are two types of petroleum which come straight out of the
ground in form of liquid. The first one is called as crude
oil and the second one is called as condensate. Crude oil
is a dark and viscous liquid and condensate is a clear and
volatile liquid. Crude oil is a mixture of a large amount of
hydrocarbons, varying amount of waxes and low content
of asphaltenes [6]. The carbon content normally is in the
range of 83-87%, and the hydrogen content ranges from
10-14% [7]. In addition, small amounts of nitrogen,
sulfur, oxygen, nickel and vanadium may be found in the
crude oils [7]. Crude oils from different regions have
different properties [8]. The physical properties that
mainly affect the behavior and Crude oil usually in black
color but it also comes in other colors like green, red or
brown but they are not uncommon. Crude oil is come into
two characteristics either it is light or heavy. Their
characteristics depend on how this crude oil is vaporizing
when it is heating, or it is added by chemical agents. It is
light if it is a volatile oil and is heavy if it is viscous.
These viscous crudes account for 25% of the
economically recoverable oil in the United States [9].
Production of heavy crudes is expected to increase
significantly in the near future as low viscosity crudes are
depleted [10]. A significant portion of the world crude oil
is produced in the form of emulsion [11].
Emulsions are thermodynamically unstable systems
because of the unfavorable contact between oil and water
phases, and so they will always break down overtime [12,
13, 14]. Convention- Emulsion is a mixture of two
immiscible substances. It is divided into two types of
emulsion either a water-in-oil emulsion or oil-in-water
emulsion. Butter and margarine are example of water-in-
oil emulsion because oil is surrounding the water droplets.
For milk and ice cream, they are example of oil-in-water
emulsion because water is surrounding the oil droplets.
Emulsion is unstable. Higher surfactant concentrations
can reduce the interfacial tension, making deformation of
the dispersed phase easier and tending to reduce droplet
sizes [15]. There are three types of emulsion instability
 which are flocculation, creaming and coalescence.
Flocculation give a meaning when the particles form
clumps, while creaming occur when the particles
concentrate towards the surface or bottom depends on
their relative density of two phases, and coalescence
means that the particle coalesce and form liquid layer.
The instability of emulsion gives some problem for
industries.
For economic purpose, pipeline consideration and for
efficient refinery operations, the produced crude oil must
dewatered and necessary to separate the water completely
from the crude oils before transporting them [11]. Several
alternative transportation methods were proposed,
including dilution with lighter crudes, injection of a water
sheath around the viscous crude [16]. In order to
dewatered of crude oil, there are some methods that use in
industry for example dewatered of crude oil emulsion by
using microwave heating, dewatered of this crude oil by
using chemical which act as surfactants (surface active
substances) that can increase the kinetic stability of
emulsion greatly, dewatered of this crude oil by using
heat which involve radiation, conduction and convection
process or dewatered of this crude oil by using electrical
energy.
A substance which is used to stabilize the emulsion is
called as emulsifier or frequently it is called as
surfactants. Emulsifiers are surface-active ingredients that
adsorb at interfaces and facilitate the production of small
droplets by lowering the interfacial tension during
homogenization [17, 18]. Emulsifiers also improve the
stability of emulsions to droplet aggregation by
generating repulsive forces between the droplets and/or
by forming interfacial membranes around the droplets that
are resistant to rupture [14, 18, 19, 20]. However, these
emulsifiers have considerably different abilities to form
and stabilize emulsions [21]. In other words, each type of
emulsifier varies in its effectiveness at producing small
oil droplets during homogenization and in its ability to
prevent droplet aggregation under various environmental
stresses such as pH, ionic strength, heating, freezing, and
drying. This emulsifier is use widely in our life. The
example of using of emulsifier is detergent (act as
emulsifier) which is use in cleaning process. This
detergent will chemically react with the water and oil, and
then it will stabilize the interface between water or oil
droplets in suspension. Surfactants are added to improve
emulsion stability by decreasing interfacial free energy
and providing a mechanical barrier to droplet coalescence
and Ostwald ripening [22]. This principle is exploited in
soap to remove grease for cleaning process. A wide
variety of emulsifiers are used in pharmacy to prepare
emulsions such as creams and lotions. Emulsifier is very
important because it is tend to promote dispersion of the
phase in which they do not dissolve very well. That is
why they are used to stabilize the emulsion. Emulsifier
can turns into water-in-oil or oil-in-water but it is depends
on the volume fraction of both phases and on the type of
emulsifier.
70
Demulsification is a process of oil and water
separation from emulsion [23]. Typical demulsification
techniques include thermal, electrical, chemical, acoustic,
or mechanical method [24]. Not all of crude oil emulsion
can break by demulsifies because the demulsification
mechanism of demulsifier is quite complicated. In
chemical demulsification process, chemical which called
as demulsifier is added to the water-in-crude oil emulsion.
The demulsifiers are surface active agents (surfactants)
and develop high surface pressure at crude-oil-water
interface [25, 26].
In this study, heating of water-in-oil emulsion with
microwave heating technology is to separate water and
oil. Microwave heating offers a faster processing because
of their volumetric heating effects. The separation of
emulsified water from crude oil has several stages, due to
gravity settling, water droplet/droplet flocculation takes
place as water droplets approach each other [27].
Therefore, the aims of this study is to study crude oil
emulsions stability using different surfactants in different
concentration, different volume ratio of water-oil of crude
oil emulsion and different type of crude oil as well as to
examine the performance of microwave application in
demulsification of water-in-crude oil emulsions in
comparison to the conventional methods.
2. Materials And Methods
Materials and Equipment
Crude oil was supplied by the Petronas refinery
Melaka which this crude oil was come from Dubai and
Kuwait oilfield. Then the UMP chemical laboratory
stored it in the open laboratory before it was used. The
microwave that was used in this study, Elba domestic
microwave oven model: EMO 808SS was combined with
thermocouple in order to measure the temperature
distribution. Type of surfactants is Sodium Dodecyl
Sulfate (SDDS) which were taken at the UMP cleaning
room. The equipments required in this study are
thermometers, stop watch, graduated cylinders, and
beakers. Thus, the next step is to set up the microwave as
shown in Figure 1.
Process Description
Emulsions (crude oil, water and surfactant mixture)
were placed at the centre of the microwave. The power
and time were set. When the heating process begin, water
molecules in the emulsion will separate itself from the
emulsion quickly when compare to stability method. In
the stability method, there were no heat supplies thus the
separation of water from the emulsion takes long
processing time. The water molecules were going down
and the emulsion will go up. This phenomena occur
because of the water density is higher than the emulsion
density.
Surfactant that was added to this process was
functioning as stabilizer. This surfactant has two parts
which is hydrophilic and hydrophobic. Hydrophilic part
will attack the water molecules and form the thin layer
 around the water droplets then decreases the water
surface tension value (the force per unit area needed to
make available surface). So that the water molecules
cannot bind with each other to separate themselves from
the emulsion then give a result as no water volume
separate from the emulsion.
In the emulsion stability, the emulsion is considered as
stable when there were no water molecules separate from
the emulsion.
Figure 1: Microwave uses in this study
Experiment and Sampling Methodology
The purpose of the experiment is to study crude oil
emulsions stability using different volume ratio of water-
oil of crude oil emulsion and different types of crude oil
and to examine the performance of microwave application
in demulsification of water-in-crude oil emulsions in
comparison to the conventional methods.
This experiment basically focuses on separation of
water-oil system with the volume ratio of 50 %, 20 % and
30 % water in emulsion which the total volume is 200
mL. The steps in experimental work are as follows:
Emulsion preparation and emulsion stability
Sample of crude oil (Kuwait crude oil) is prepared in
the volume of 100 ml in the 1000ml gradually beakers.
The surfactant is added into this sample of crude oil. This
surfactant must be added into the continuous phase which
is oil. This oil and surfactant then is agitated vigorously
using a standard blade propeller at speed 900 rpm and at
temperature range of 25 to 30 oC (room temperature) for 2
minutes. 100 ml of tab water is added into the beaker
containing of Kuwait crude oil and surfactant after 2
minutes oil and surfactant is agitated. Tab water is added
drop by drop in order to make sure that water, oil and
surfactant are mixed well. The volume ratio of this
emulsion is 50-50 % water-in-oil emulsion. After 5
minutes water, oil and surfactant are agitated, a droplet of
this emulsion is place on the filter paper to check whether
it is water in oil or oil in water emulsion. In this study, the
emulsion needed is water in oil. To prove that the
emulsion form is water in oil, the droplets of emulsion on
the filter paper not disperse in a big size on filter paper.
For oil in water emulsion, a droplet of emulsion will
71
disperse on all of the filter paper. The water in oil
emulsion then put into the 500 ml measuring cylinder.
After 30 minutes, the water volume of water recorded.
The water volume is read in 5 hours for every 30 minutes.
The water volume reading is recorded. Step 1-6 is
repeated by prepare the volume ratio of the Kuwait and
Dubai crude oil emulsion for 30-70 % and 20-80 %
water-in-oil. For every volume ratio of the emulsion, the
SDDS surfactant must be added in concentration of 0.5%,
2.5% and 4.5%. Every emulsion was prepared and water
volume observed for 3 times to get the average volume of
water separated.
Demulsification
Two types of crude oil emulsion samples were used.
They are Kuwait crude oil and Dubai crude oil. 50-50 %
and 20-80 % water-in-oil emulsion were prepared. The
emulsifying agent SDDS were used. The emulsion then
put into the 1000ml glass beaker then this beaker was
covered by aluminum foil. The hole is done on this
aluminum foil in order to put the thermocouple after the
emulsion take out from microwave. The microwave
radiation was set at the power and time setting which is
720 Watt and 3 minutes. The 1000ml glass beaker
contains the emulsion then is put into the center of Elba
domestic microwave oven model: EMO 808SS. After 3
minutes heated, 1000ml glass beaker contains the
emulsion was taken out quickly with carefully then the
thermocouple was inserted into this beaker to take the
temperature distribution. The emulsion sample then was
put into the 500ml cylinder. After 5 minutes, water
volume was read and this observation was done in 1 hour
by taking the water volume reading in every 5 minutes.
This methodology was repeated for both crude oil in
volume ratio of 50-50% and 20-80%, types of surfactants
is SDDS, 4.5% of concentration of surfactant and 2 power
use which are 720 watt and 180 watt.
3. Results And Discussion
Emulsion Stability.
The most important characteristic of a water-in-crude
oil emulsion is its stability [28]. Water in oil emulsions
made from crude oils has different classes of stability, due
to the presence of asphlatenes and resins [29]. Unstable
emulsions are those that decompose to water and oil
immediately after mixing [28]. In the case of oil-in-water
emulsion, the oil tends to move upward under gravity due
to the difference in density between the continuous phase
and the disperse phase [30]. The droplets are accumulated
at the top of the emulsion due to the creaming effect,
resulting in oiling off (formation of an oil layer on top of
the emulsion) after some time [31]. The creaming rate of
emulsion is highly dependent on the density of the
disperse and continuous phase, viscosity of the
continuous phase, droplet size and the droplet
concentration [32].
 3.2. Effect of different type of crude oil on emulsion to move and separate water from emulsion.
stability Intermolecular force between water and oil in that
The maximum amount of water separated from emulsion also is high. In order to break this
Kuwait crude oil and Dubai crude oil emulsion while intermolecular force, these molecules need some energy
applying 0.5 % concentration of SDDS was same which such as energy supply by microwave heating that will be
85 ml as shown in figure 2. discuss later. As a result, water is separate in a small
volume and makes the emulsion more stable. Small
amount of water separate from the emulsion will give a
result as stables emulsion. From the observation, at 300
90
80
minutes processing time, the maximum volume of water
separate from emulsion (Kuwait crude oil) while using
water separation(ml)

70
60 volume ratio as 50-50% is 85 ml, 30-70% is 40 ml and
50
40 Kuwait crude oil
20-80% is 0 ml (no water is separate).
30 Dubai crude oil
20
10
0 90
30 60 90 120 150 180 210 240 270 300 80
processing time (min) 50-50%(w/o)
70

water separation(ml)
30-70%(w/o)
60
Figure 2: Effect of crude oil type on emulsion stability with 50- 20-80%(w/o)
50
50% (w/o) and SDDS surfactant.
40

30
It has shown that at early processing time, water 20
separated from emulsion in Kuwait crude oil is higher 10

than Dubai crude oil and at 180 minutes, they started to 0

30 60 90 120 150 180 210 240 270 300
be same. From this observation, Kuwait is considered less processing time (min)
stable than Dubai because it tends to separate higher Figure 3: Effect of volume ratio of water on emulsion stability with
amount of water in early processing time. Dubai is 0.5% concentration of SDDS surfactant. (Kuwait crude oil)
considered as heavy crude oil than Kuwait because of
different in stability. When the water separated is less, the 90
emulsion consider as more stable. Heavy crude oil means 80
that, it is difficult break the water when these crude oil in
water separation(ml)

a water-oil emulsion form. Heavy crude oils have high
concentration of natural surfactant. Reference [28]”
described that the formation of emulsions due to the
asphaltene and resin content of the oil. Reference
[22]”also stated that the main factor affecting the stability
of the emulsion is the presence of substances like crude
oil resins, asphaltenes, and natural wax. So that, when
synthetic surfactant is added to these crude oil they
become more stable and can’t separate water in a large
quantity. From the observation, both crude which are
Kuwait and Dubai are heavy crude due to their colors
(black colors) but Dubai is heavier crude oil than Kuwait
crude oil. Dubai has higher natural surfactant quantity
than Kuwait. Stability of emulsion also can be compare in
it volume ratio of water-oil (w/o) in the emulsion.
3.3 Effect of different volume ratio on emulsion stability
Figures 3 and 4 show the effect of volume ratio of
water on emulsion stability. From the observation, when
the volume ratio of water is less, the emulsion is more
stable. The trends are same for both crude oil which are
Dubai and Kuwait. When the water quantity in the
emulsion sample is small, the viscosity of that emulsion is
high. Low viscosity implies a mobile liquid and high
viscosity denotes the materials that are resistant to flow,
such as heavy fuel oils [33]. So that the molecule’s
velocity in the emulsion is small then make it more hard
72
70
60
50
40
30 50-50% (w /o)
30-70%(w /o)
20
20-80%(w /o)
10
0
30 60 90 120 150 180 210 240 270 300
processing time (min)
Figure 4: Effect of volume ratio of water on emulsion stability with
0.5% concentration of SDDS surfactant. (Dubai crude oil)
3.4. Effect of different volume ratio and power on
demulsification process.
Figures 5, 6, 7 and 8 shown that when the volume
ratio of water is less, the emulsion will be more stable. In
this study, stability was determined by taking the volume
of water separate from the emulsion. When the initial
volume of water added to the crude oil is small, water
separate also will be in less quantity compared to the
emulsion which initially added in a large quantity at the
same total volume (water volume plus crude oil volume).
In fact, volume of water added to the crude oil will
determine it viscosity. If the volume of water added to the
crude oil is small, the emulsion will be more viscous than
high volume of water added to the crude oil. More
viscous emulsion will reduce the velocity of the
molecules in the emulsion. Otherwise, more viscous
emulsion makes the intermolecular forces between oil and
water in the emulsion tighter. So that water is difficult to
 break down this intermolecular forces and finally make type:dubai
power:720 watt
this emulsion in stable state which are volume of water 140
appear is less or in small quantity. When this viscous 120

water separation(ml)
emulsion was heated in the microwave, energy supply by 100

microwave to the molecules will help water molecules to 80 50-50%(w/o)

20-80%(w/o)
break down intermolecular force between water and oil. 60

High power using while heated the emulsion means that 40

20
energy supply to the emulsion is also high. Then high
0
energy supply will give a result as less processing time 5 10 15 20 25 30 35 40 45 50 55 60
processing time (min)
needed to make the emulsion in a stable state(constant
reading for water volume as time processing increase). Figure 6: Effect of different volume ratio of w/o on emulsion
stability with 4.5% SDDS using microwave heating (Dubai crude oil)
For Kuwait crude oil, processing time for make the stable
emulsion while using high power (720 watt) is 30 minutes
type:kuwait
and for low power (180 watt) is more than one hour. power:180 watt
80
Otherwise for Dubai crude oil, processing time for make 70

water separation(ml)
the stable emulsion while using high power (720 watt) is 60
50
20 minutes and for low power (180 watt) is 25 minutes. 40
50-50%(w/o)
From this observation, it can be conclude that high power 30 20-80%(w/o)
20
will decrease the processing time of emulsion to be in a 10
stable state and less volume ratio of water in emulsion 0
5 10 15 20 25 30 35 40 45 50 55 60
will make that emulsion more stable. From figure 5, 6, 7 processing time (min)
and 8, it can be conclude the trend is same as figure 3 and
Figure 7: Effect of different volume ratio of w/o on emulsion
4 which are when the volume ratio of water is less, the stability with 4.5% SDDS using microwave heating (Kuwait crude oil)
emulsion will be more stable but the processing time to
make the emulsion in a stable state are different. For type:dubai
figure 3 and 4, processing time to make the emulsion in a 180
power:120 watt
stable state are not constant for volume ratio of water
water separation(%v/v)

160
140
50% and 30%, and for volume ratio of water 20%, no 120
separation of water for the both Kuwait and Dubai 100
80
emulsion while for figure 5, 6, 7 and 8, processing time to 60
50-50%(w/o)
20-80%(w/o)
make the emulsion in a stable state are 30 minutes 40
20
(Kuwait emulsion), 20 minutes (Dubai emulsion) for 0
volume ratio of water 50% and 35 minutes (Kuwait 5 10 15 20 25 30 35 40 45 50 55 60

emulsion), 45 minutes for volume ratio of water 20%. The processing time (min)

different shown are because of heat supply to the Figure 8: Effect of different volume ratio of w/o on emulsion
emulsion of crude oil decrease the processing time to stability with 4.5% SDDS using microwave heating (Kuwait crude oil)
make the emulsion in a stable.
3.5. Effect of different crude oil and power on
demulsification process.
type:kuwait
power:720 watt Figure 9 and 10 was sketch from the data obtain. From
90 the observation, Dubai crude oil trend give different trend
80
with Kuwait crude oil. This trend occur because while
water separation(ml)

70 50-50% (w/o)
20-80% (w/o)
60 heating the Dubai crude oil at 720 watt, it was splash out
50
40 in the microwave then decrease it total volume from 200
30 ml to 100 ml. The impact of this phenomenon is the water
20
10 separation volume that taken will give a small value than
0
5 10 15 20 25 30 35 40 45 50 55 60
the original value. That is why water separation using
processing time (min) Dubai crude oil at 720 watt is less stable than water
separation using Dubai crude oil at 180 watt. However,
Figure 5: Effect of different volume ratio of w/o on emulsion
stability with 4.5% SDDS using microwave heating (Kuwait crude oil)
these results are not reverse from the theory which is
increase the power (heat supply to the emulsion) will
increase the maximum processing time for stable state of
crude oil emulsion. As shown in figure 10, maximum
processing time for Dubai crude oil at power 720 watt is
20 minutes and maximum processing time for Dubai
crude oil at power 180 watt is 25 minutes. The reverse
results is, at the maximum processing time, water
separation of Dubai crude oil using power at 720 watt is
130ml which is less than water separation of Dubai crude
73
 oil (170ml) using power at 180 watt . The result for ACKNOWLEDGMENT
Dubai crude oil should be like figure 9 which are for
Financial support from University Malaysia Pahang
Kuwait crude oil. For Kuwait crude oil, maximum
is gratefully appreciated.
processing time for emulsion reach at stable state at
power 720 watt is 30 minutes and maximum processing
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