CANADIAN HEAVY
OIL ASSOCIATION
SPE/PS-CIM/CHOA 97748
PS2005-334
Characterisation and Emulsion Behaviour of Athabasca Extra-Heavy-Oil Produced
by SAGD
C. Noik and C. Dalmazzone, IFP, and C. Goulay and P. Glenat, Total
Copyright 2005, SPE/PS-CIM/CHOA International Thermal Operations and Heavy Oil Symposium
This paper was prepared for presentation at the 2005 SPE International Thermal Operations
and Heavy Oil Symposium held in Calgary, Alberta, Canada, 1–3 November 2005.
This paper was selected for presentation by an SPE/PS-CIM/CHOA Program Committee
following review of information contained in a proposal submitted by the author(s). Contents of
the paper, as presented, have not been reviewed by the Society of Petroleum Engineers,
Petroleum Society–Canadian Institute of Mining, Metallurgy & Petroleum, or the Canadian
Heavy Oil Association and are subject to correction by the author(s). The material, as
presented, does not necessarily reflect any position of the SPE/PS-CIM/CHOA, its officers, or
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Abstract
The production of extra heavy oil (or bitumen)
through the SAGD method (Steam Assisted Gravity Drainage)
requires the generation and injection into the reservoir of a
great quantity of steam. A typical value of the steam/oil ratio
is around 3, which means that a 100,000 bopd development
requires the injection of 300,000 bcwepd (barrels of cold water
equivalent per day) of steam, and that a corresponding
quantity of hot water will be co- produced with the oil. The
production of extra heavy oil containing many active
components with the tendency to form an emulsion combined
with the high water-cut ratio (above 80%) leads to a phase
separation process with specific issues. This study considers
an extra heavy oil field produced in SAGD in Athabasca.
The objective of the study was firstly to characterise
the produced fluids and then to analyse their tendency to form
an emulsion under controlled hydrodynamic conditions. An
innovative technique - Differential Scanning Calorimeter
(DSC) - was used to characterise the emulsion. This method is
able to define the water-in-oil or reverse emulsion nature and
to quantify the water amount without sample dilution. DSC
analysis combined with microscopy and image analysis
treatments was used to determine the droplet size distribution.
Reconstituted emulsions were then formed using a "Dispersion
Rig" set-up that allows the simultaneous pumping of crude oil
and water through a calibrated restriction in the pipe. The
amount of energy dissipated to the fluids systems can be
quantified due to the strict control of the hydrodynamic
conditions. Consequently a relationship between granulometry
distribution of the emulsion and the fixed energy or pressure
drop can be established. The main experimental parameters
investigated were the oil dilution and water-cut ratios.
It is concluded that there is a residual emulsion in
extra heavy oil which has a very small average droplet size
whatever the temperature and solvent dilution ratio. This small
droplet size results in a difficult oil/water separation which is
only possible either by addition of large quantities of additives
at high temperature and with long residence time and probably
by applying an electrostatic field.
Introduction
Albertan oil sand deposits contain an estimated 1.7 trillion
barrels of oil of which 300 billion barrels are believed to be
recoverable by surface mining or insitu developments. One of
the insitu technologies which is used in several Athabascan
developments is Steam Assisted Gravity Drainage (SAGD),
this extraction technique injects steam continually adding
energy and heating the reservoir. This injection produces a
steam chamber within the reservoir enabling Extra Heavy Oil
to be produced together with hot water back to surface via a
production well.
SAGD requires substantial quantities of steam. A typical
steam/oil ratio is in the order of 3 barrels of water equivalent
of steam per barrel of bitumen produced. This steam is then co
produced in a multiphase mixture with the bitumen. This
multiphase mixture must be separated to provide a dehydrated
oil stream which may be transported for further downstream
processing or upgraded on site. This water and oil mixture
contains active components that promote emulsion formation.
This tendency to form emulsions coupled to the produced
fluids high water cut makes separation difficult to achieve. So
that that this separation system can be adequately specified it
is essential that the emulsion is characterized. This paper sets
out the techniques used to characterise an Athabascan oil field
emulsion, the equipment used to form the emulsion in the
laboratory and then discusses the results of this
characterisation.
This paper sets out a methodology used to characterize and
study the behaviour of emulsion produced from an Athabascan
SAGD development.
Materials and Techniques
Produced fluids sample
Crude Oil: The two samples received were taken at two
different dates (2003 and 2004) but at the same sampling point
2 SPE/PS-CIM/CHOA 97748
on same wells, at the gas boot outlet, before any diluent and
additive injections. Each container received in laboratory
initially contained an oil phase (17% volume) and a free water
phase at 83% volume.
Diluent, additives: Operational diluent was used having a
specific gravity of 0.858 and the following composition: 51%
saturates, 47% aromatics and 1-2% resins. The tested additives
are those used on field and are one demulsifier and one reverse
demulsifier.
Field conditions/laboratory conditions
On field at the well-head crude oil effluent is produced with a
volume ratio of 80 % water and 20% oil. After the well-head,
the diluent is injected in-line at 15% in volume versus the total
flow rate. Under laboratory conditions and for all experiments,
when the oil samples are diluted, the dilution is expressed by
the ratio of diluent versus the total concentration of the fluids
produced (water, diluent and oil) in order to be identical to
operational condition. Taking into account the transport
conditions, the diluent percentage could be also expressed
versus anhydrous oil only. So at 15% diluent ratio in
operational condition corresponds to 59% diluent ratio in
transport condition.
Additive concentration is also directly calculated versus the
total amount of oil, water and diluent, without taking account
of the percentage of active matter.
Emulsion characterisation techniques
DSC: Differential scanning calorimeter (DSC) and
microscopy coupled with image analysis are the main
analytical methods used for emulsion characterisation 1,2.
DSC is based on the measurement of heat exchanges between
a sample and a reference as a function of time or temperature.
The peak area of the recorded signal (generally called a
"thermogram") is related to the heat flow generated or
absorbed by the sample. The sample is cooled at a constant
scanning rate (1 to 5°C/min) until the water droplets in the
emulsion crystallise. The crystallisation temperature is
correlated to the droplet sizes and decreases with them: the
smaller the volume of the droplets, the lower the temperature
of crystallisation.
The re-heating of the sample after crystallisation allows the
study of melting, the temperature of which is independent of
the aqueous solution state i.e. emulsified or free. The analysis
of the melting thermogram can give very useful information
about the water content of the emulsion and the salt
concentration. It is noteworthy that it is possible, from a single
DSC test performed on an emulsion sample without dilution,
to obtain information about:
-The emulsion type: simple (W/O or O/W), or multiple
(W/O/W or O/W/O)
-The amount of water and its state: bound, dispersed or in bulk
-The compositions (water salinity) of the dispersed and bulk
phases
-The mean diameter of the droplets and the polydispersity of
the emulsion
Droplet sizes: To complete the analysis, droplets size and
polydispersity values are determined by optical microscopy
coupled with image analysis. The droplet size distribution was
determined considering both the number and volume of
droplets. The results can be expressed with the following
diameters:
- D10 is the arithmetic average diameter of the number-based
drop size distribution
- D43 is the arithmetic average diameter of the volume-based
drop size distribution
- D50,n and D50,v.
D50,n represents the diameter below which 50% of the
droplets number is found. D50,v is the equivalent diameter
expressed in volume that is to say the average diameter below
which 50% of the total volume of the droplet population is
found. The two values are quite different when the droplet size
distribution is broad and/or bimodal.
Viscosity: Instrument used for viscosity measurements is
the Haake Rotovisco RV20, which is a concentric cylinder
rotary viscometer. For flow curves determination, shear rate is
fixed and shear stress is measured under cone-plane
rotor/stator configuration at controlled temperature. Viscosity
is determined in the shear rate range between 0.1 to 100 s-1.
Emulsion formation set-up
A specific apparatus "Dispersion Rig" was developed in order
to reconstitute water-in-crude oil emulsions in more realistic
conditions than in the laboratory that means under controlled
pressure and temperature. Detailed description of the set-up is
presented in reference 3,4. The objective is to simulate the flow
of crude oil and brine through the choke-valve by pumping
both fluids through a calibrated orifice that represents a model
choke-valve. The turbulent flow created downstream from the
orifice leads to a dispersion of water droplets in the oil phase,
i.e. emulsion formation. A programmable controller allowing a
perfect synchronisation of both piston pumps pilots the
simultaneous injection of both fluids. A maximum volume of
500 ml of each phase can be pumped at a fixed flow rate into
the supply tubes. The third pump is a metering pump which
injects additives on line just after emulsion formation. The
fluid pressure is measured at two locations, upstream and
downstream from the orifice. This allows the measurement of
the permanent pressure drop ∆Pperm induced by the orifice. The
produced water/oil mixture is collected in a separator that is
mounted above the orifice. The entire equipment is placed
inside a cupboard and can be heated up to a maximum
temperature of 80°C. The maximum pressure is 150 bar in the
piston pumps and 50 bar in the separator.
Results
Characterisation of produced fluids
Water sample analysis: The composition of the free water
phase was analysed and presented an equivalent total salinity
around 2.1 -2.4 g/l. The water phase is very turbid containing
fine particles in suspension and some hydrocarbons.
Crude oil sample characteristics: The DSC thermograms
of the two oil samples are presented in Figure 1.
Results indicated without doubt that the two oil samples are
water-in-oil emulsions. The main difference between the
samples is due to the difference in the droplet size distribution.
-The thermogram of the oil sample 2004 presented one major
crystallisation peak, characteristic of a fine emulsion, at -45°C
SPE/PS-CIM/CHOA 97748
and a series of small peaks between -35 and -20°C,
characteristic of the presence of larger droplets and free water.
-The thermogram of oil sample 2003 presented two major
peaks of emulsified water at -45°C (fine droplets) and -35°C
(larger droplets). A quite large peak characteristic of free
water was also observed at around -18°C. For the two samples
the crystallisation peak at -45°C indicated the presence of the
same fine droplet population.
The determination of the melting energy of the initial water
sample (300J/g) allowed us to calculate the water content of
each emulsified sample from the corresponding melting
energy of each sample (116J/g for oil sample 2004). It appears
that the two oil samples contained the same amount of 38 to
40% in weight of water.
Figure 1 : DSC of oil samples 2003 and 2004
fine droplets
free water
larger droplets
Melting peak
Microscopy observations on oil sample 2003 indicated the
presence of one fine droplet population. Bigger droplets have
certainly been split off during spreading on the microscopy
glass plate. The image analysis treatment indicates a droplet
diameter D50,v around 11µm and a D50,n less than 1 µm with
the average diameter D10 of 1.1 µm (Figure 2). This very fine
droplet population corresponds to the crystallisation peak at -
45°C in the thermogram.
Figure 2 : Droplet size distribution of oil sample 2003
N u m b er an d vo lu m e d ro p let siz e d istrib u tio n
100
90
80
70
60
% 50
40
30
20
10
0
1 10
Diam e te r ( µm )
Oil sample thermal stability: According to the previous
analysis results, the two oil samples 2003 and 2004 received
are water-in-oil emulsions containing 38-40 % water. In order
to evaluate the stability of these emulsions, temperature and
additive concentration were fixed in the experiments according
to the operational conditions on field i.e. 120°C and 250 ppm
respectively.
3
The thermal stability of the oil sample 2003 without any
diluent addition and any additive was analysed using DSC
technique. The apparatus used (HP -DSCVII- Setaram)
permits to work under pressure condition. The sample is put in
a pressurised cell and several thermal cycles are fixed:
- Cooling phase at 1°C/min from 25°C to -45°C for the
emulsion characterisation
- Heating phase till 120°C
- Ageing step at 120°C during 25 min
- Cooling phase (emulsion characterisation step)
The overall steps have been repeated several times on the
same sample and experiments were performed at 5 bar and 10
bar. Figure 3 illustrates the results for experiments at 5 bar. No
major effect of pressure was noticed. It is clearly shown that
the temperature cycles permit to destabilise the emulsion in the
sample. Free water appearance (indicated by sharp shape
peaks from -28°C to -20°C) is related to coalescence of bigger
water droplets corresponding to the decrease of the second
peak area (peak at -32°C). But the residual emulsion (peak at -
45°C) corresponding to smallest droplet size (<1µm) was still
present even after 5 ageing periods i.e 2 hours at 120°C.
Through bottle tests experiments, a total destabilisation of this
residual emulsion is obtained only in presence of 15% diluent
and 500ppm additive at 80°C.
Figure 3 : Tests on HPmicro DSCVII: destabilisation tests at
120°C- oil sample 2003 (without any diluent addition)
In itia l sam p le
0.32 S tep n °1
S tep s n°2 - 3
S tep s n°4 - 5
0.28
0.24
0.2
0.16
0.12
0.08
F lu x (m W /m g)
0.04
-40 -36 -32 -28 -24 -20 -16
T em perature (°C )
Oil sample analysis: For compositional analysis and further
work on emulsion formation, anhydrous oil was prepared by
Number
cu mulated Nber
centrifugation at 10 000 rpm at room temperature in presence
Volume of 15% diluent but without any additive. The composition of
cu mulated Vol.
the anhydrous oil phase obtained was determined using the
classical SARA method analysis. The results slightly over-
estimated due to the diluent addition are: Asphaltenes 6.5%,
Saturates 29%, Aromatics 48%, Resins 16.5%.
100
Rheological study
Measurements conditions: Measurements were performed on
the oil samples 2003 and 2004 which are both, according to
DSC analysis under an emulsion form containing around 38-
40% water. The oil sample is diluted under gentle mixing and
then analysed. Several dilution ratios and temperatures were
4 SPE/PS-CIM/CHOA 97748

tested. For the systems studied, no phase separation appeared

during measurement. Figure 5: viscosity versus T°C - Oil sample 2003
For better understanding, the relation between dilution
percentage expressed in the two ways versus the volume of Oil sample 2003 - viscosity versus T°C
total fluids (operational condition) or the volume of anhydrous 600
oil (transport condition) is explained in the following Table 1. Dilution
4,5%
500
Table 1: % dilution

viscosity (mPa.s)
400
operational condition 4.5% 8.5% 12% 15% 8,5%
transport condition 28% 44% 53% 59% 300

200
Due to the high viscosity of the oil sample, great variations on 12%
the viscosity values were measured. Even if a strict 100
measurement procedure was adopted, some sliding effects
0
were observed. For example, we presented in Figure 4 the 20 30 40 50 60 70 80 90
variation of the viscosity versus shear rate for oil sample 2003 Te mpe rature °C
at 4.5% dilution ratio and 80°C, for 3 tests performed on the
sample. Whatever the conditions, viscosity decrease with shear Figure 6: Viscosity variation versus 1/T(K) - Oil sample 2003
rate indicates that the oil samples 2003 and 2004 have a shear-
thinning behaviour. For all the results in the following part, for Oil sample 2003 - Log (viscosity) versus 1/ T
reproducibility and to facilitate the comparison, the 10000
represented viscosity value is the measured value at 100s-1
5,2005x
shear rate. y (4,5%) = 9E-05e

1000
Figure 4 : Viscosity curves examples: oil sample 2003-4.5%diluent
viscosity

3,4604x
- T 80°C y (8,5%) = 0,0046e

100
oil sample 2003 - 4,5% diluent - 80°C y (12%) = 0,4457e
1,7468x
400

10
viscosity (mPa.s)

350 2,8 2,9 3 3,1 3,2 3,3

1/Te mpe rature (°K -1)

300
250
200
10 shear rate (s-1)
Temperature effect: The viscosity variation versus
temperature is presented for oil sample 2003 at three dilution
ratios (4.5- 8.5 - 12 %) in Figure 5 and 6, respectively.
Whatever the dilution ratio, the oil viscosity decreased with
temperature according to an exponential law 5. The
representation in log scale of the viscosity versus the inverse
of temperature expressed in Kelvin degrees indicated that the
Dilution ratio effect: The viscosity measurements are
represented in Figure 7 versus the dilution ratio at the three
studied temperatures for oil sample 2003. The viscosity value
decreases with the percentage of dilution following an
exponential law:
Viscosity = B exp α . (Vs/Vt)
100
with B constant at a fixed temperature, α dilution factor and
Vs/Vt the dilution ratio expressed in volume of diluent Vs
versus the total volume Vt. α is a dilution factor depending on
temperature with a variation according to the Arrhenius law 6.
Figure 7: Oil sample 2003 - viscosity versus % dilution
oil sample 2003 - viscosity / % dilution
400

law variation is in accordance with the classic Arrehenius law. 350

-0,2104x
y 60°C = 931,7e
The following relation could be established: 300
viscosity (mPa.s)

-0,3317x
Viscosity = A exp – ( Ea/kT) y 40°C= 6566,1e
250
with A depending on dilution rate, k Boltzman constant and
200
Ea "Activation energy".
150

100 -0,1718x
y 80°C= 485,1e
50

0
4 6 8 10 12 14
% dilution
SPE/PS-CIM/CHOA 97748 5

Emulsion formation behaviour
Emulsions are formed under controlled hydrodynamic
conditions at a fixed temperature using the Dispersion Rig set-
up. Two series of experiments were performed at 80°C with
dehydrated oil sample 2004 prepared with different diluent
ratios.
Tests I: effect of oil viscosity: experiments with flow rate
variation at a constant water-cut of 80% and with oil at
different dilution ratios - 15% - 12% - 10%
Tests II: effect of water-cut: experiments with flow rate
variation at different water-cuts - 40% - 60% with the same oil
phase at a dilution ratio of 15%.
For all experiments, the water phase is the filtered produced
water. After formation step, fluids are collected. The amount
of water in the emulsion phase is measured by DSC and
droplet size distribution determined by microscopy and image
analysis.
Flow conditions: Oil and water are simultaneously injected
through an orifice and after flow restriction droplets are
formed. The flow regime downstream the orifice becomes
locally turbulent even at low Reynolds number.
The "orifice Reynolds number Reo" is significantly high in
comparison with Reynolds number in the pipe Rep as shown
by the following relation Rep = β .Reo with β = Do/Dp
where Uo is the average fluid velocity in the orifice and Ldis is
the length of the zone in which most of the kinetic energy is
dissipated. For a turbulent flow in a circular pipe, the general
relationship currently used to define this length is: Ldis = 2.Dp.
A suitable relation was obtained between the measured
pressure drop and the calculated value from equation (2) .
Oil viscosity effect: For these tests, the oil phase was prepared
with different percentages of diluent. The oil phase viscosity
and density were measured at 80°C (Table 2).
Table 2: oil sample 2004 - % diluent
% Diluent 10% 12% 15%
Density (kg/m3, 20°C) 980 970 950
Viscosity (mPa.s, 80°C) 62 48 45
Relation Flow rate – water in the formed emulsion: The water
amount measured by DSC in the emulsion phase was
expressed in percentage of water versus the total amount of
water and oil not included diluent in order to facilitate the
comparison between experiments and with the operational
water-cut of 80%. Variation of water volume included in
emulsion phase versus the flow rate is presented in Figure 8.
Figure 8 : %water in the emulsion versus flow rate - 80°C -Diluent
effect
T 80°C - WC 80% - O il + % d ilu e n t - % Wate r in e mu lsio n

(diameter ratio between the orifice diameter Do and the pipe 35

diameter Dp). Reynolds number values calculated according to

% water (water/water +oil without diluent)

30
equation (1).
Re = 4. ρ . Q / Π. µ D [1] 25

with Q total flow rate, D tube or orifice diameter (Dp = 4.8mm, 20

Do = 0.6 mm), ρ density (ρ=1000 kg/m3) and µ viscosity (50
cP – 80°C) of the continuous phase. Reynolds number values 15

1 5 % d ilu e n t
at the orifice varies between 236 and 1416 for a flow rate of 20 10 1 2 % d ilu e n t
and 120 l/h, respectively. These values mean that the flow can 1 0 % d ilu e n t

be considered as laminar upstream the orifice and as turbulent 5

in the orifice, according to the literature which considers that 0

flow in orifices becomes turbulent at Reynolds numbers as low 0 20 40 60 80 100 120 140
flow r a te (l/h)
as 300.
The permanent pressure drop ∆P of flow through an orifice is
given by equation (2): Whatever the flow conditions at this water-cut of 80%, a free
⎛ 1 ⎞
( )
1 1 water phase co-exists with an emulsion phase. At this high
∆Pperm = ρU 2p ⎜⎜ 4 − 1⎟⎟ 1 − β 2 water-cut, a total emulsification does not proceed. The flow
⎝β
2
c0 2 ⎠ [2] rate or dissipated energy increase induces the formation of
where c0 is the orifice coefficient, ρ the fluid density, Up the emulsion and the total water amount in the oil phase increases
average pipe velocity and β the ratio between orifice and tube as illustrated in Figure 8. A sudden increase in the amount of
incorporated water is noticed between 60l/h and 80l/h and then
diameter. In the experiment β is equal to 0.125 and the chosen
a plateau value appears.
density is 1000 kg/m3 as the two fluids have very close density
When dissipated energy exceeds the threshold value of 1.8 107
values. In literature co is an experimental coefficient with
W/Kg (60l/h), the oil phase reaches a saturation in water
values varying between 0.6 and 0.8.
content. This saturation level is slightly dependent on the oil
The permanent pressure drop is caused by the dissipation of
dilution ratio or oil viscosity in the studied % range. At the
kinetic energy due to turbulence. Under the assumption of
15% dilution ratio, the maximum of emulsified water in the oil
homogeneous isotropic turbulence, the average amount of
phase is around 30% which is quite similar to the 40% of
energy that is being dissipated per time and mass unit can be
emulsified water measured in the initial oil samples 2003 and
estimated by equation (3):
2004.
∆Pperm U o 1 ⎛ 1 ⎞⎛ 1 ⎞
ε≈ = U 3p ⎜⎜ 4 − 1⎟⎟⎜⎜ 2 − 1⎟⎟ [3]
ρL dis 2c 02 L dis ⎝β ⎠⎝ β ⎠
6 SPE/PS-CIM/CHOA 97748

Relation Flow rate - water droplet sizes in formed emulsion emulsified amount of water drastically increases. The energy
For each test, the droplet size distribution was determined and limit increases with the water-cut. At 40% water-cut the flow
the volume or number diameter D50,v or D50,n of the droplet rate limit is above 20l/h and at 40l/h the water is totally
population are calculated. The experiments at different flow emulsified, no free water appears. At 60% water-cut, the
rates clearly indicated that the droplet size decreases as energy or flow rate limit is not clearly identified and the oil
dissipated energy increases (Figure 9). tends to incorporate all the water for flow rates above 100l/h.
A minimum diameter value is rapidly measured and the two At 80% water-cut, a water saturation appears for flow rates
D50 values tend to meet because the droplet size distribution above 60l/h and a free water phase is still observed.
becomes less polydisperse. Whatever the oil dilution ratio, all
the emulsions formed above the energy threshold value of 1.8 Figure 11: % water in emulsion versus flow rate - 80°C -
107 W/Kg (60l/h) were very fine with an average diameter D10 water-cut effect
close to 2µm. As indicated on the DSC thermograms in Figure T 8 0 C - W C v a r ia b le - O il + 1 5 % D ilu e n t - % w a te r in e m u ls io n
10, the droplet distribution of reconstituted emulsion is close 60
to that determined in the oil samples. Moreover, similarity

% water (water / water+oil without diluent)

with DSC and microscopy analysis on this reconstituted 50

emulsion confirmed that the fine peak observed in the oil

40
sample 2004 thermogram at -45°C during crystallisation
corresponds to a fine droplet population. 30

Figure 9: droplet size variation D50,v versus flow rate- 80°C - 20

Diluent effect
WC 80%
10
T ° 8 0 C - W C 8 0 % - O il + % d ilu e n t - D r o p le t s iz e D 5 0 ,v WC 60%
2 0 ,0 0 WC 40%
0
1 8 ,0 0
0 20 40 60 80 100 120 140
1 6 ,0 0 flow ra te (l/h)
Droplet size D50,v (µm)

1 4 ,0 0

1 2 ,0 0
1 5 % d i lu e n t
1 2 % d i lu e n t
Relation Flow rate - water droplet sizes in formed emulsion
1 0 ,0 0
1 0 % d i lu e n t The diameter variation (D50,v) versus flow rate is presented in
8 ,0 0
Figure 12. As previously observed, the droplet size decreases
6 ,0 0

4 ,0 0
as flow rate increases in relation with the dissipated energy
2 ,0 0
increase. Above the energy barrier, where the oil phase tends
0 ,0 0
to be saturated with water, droplets have about the same size
0 20 40 60 80 100 120 140 (D10 around 2 µm) whatever the studied water-cut.
F lo w r a t e ( l/h )

Figure 12 : Droplet size variation D50,v versus flow rate- 80°C-

Figure 10 : DSC of reconstituted emulsion and oil sample water-cut effect
2004
T 80C - WC variable - Oil + 15 % diluent - Droplet size D50,v
20
depart2004_2.000 20,00
R econstituted em ulsion O ilm anip8.000
sam ple 2004
O il + 15% diluent – Q = 120l/h 18,00

16,00
droplet size D50,v (µm)

10

14,00
WC 80%
12,00
WC 60%
Heat Flow (mW)

0 10,00 WC 40%

8,00

6,00
-10
4,00

2,00

0,00
-20
-120 -100 -80 -60 -40 -20 0 20 40 0 20 40 60 80 100 120 140
Exo Up Tem perature (°C) Universal V2.5H TA Instrum ents
Flow rate (l/h)

Discussion on emulsion formation- comparison with other

Water-cut effect: In these tests, the oil phase was diluted crude: The crude oil behavior through experiments performed
with 15% diluent and only the water-cut varied. Experiments on the same Dispersion Rig set-up was compared between the
were performed at several flow rates. studied heavy oil and a paraffinic oil.
Relation flow rate - water in formed emulsion The composition and main characteristics of the two oils
Water amount incorporated in the emulsion phase versus the presented in Table 3 underline their main differences: amount
flow rate is presented in Figure 11. An important water-cut of polar components and viscosity.
effect is noticed on emulsion formation. As previously "Dispersion Rig" experiments are performed within the same
observed, an energy threshold value exists above which the conditions except temperature.
SPE/PS-CIM/CHOA 97748 7

This droplet distribution is close to that determined in the

crude samples of the heavy oil, both 2003 and 2004 samples.
Table 3 : Characteristics extra heavy oil - paraffinic oil The reconstituted emulsion formed in the Dispersion rig
extra heavy oil Paraffinic oil experiments is representative of the residual emulsion that
Composition %: (+15% diluent) existed in the crude oil sample. This small droplet size is a
Saturated 29 58 sign of emulsion stability and of further difficulty for oil/water
Aromatics 48 34 phase separation.
Resins 16.5 7
Asphaltens 6.5 <1 Conclusions
Density (kg/m3) 950 850
Viscosity (mPa.s) 45 -(80°C) 10 (25°C) • Analytical results indicated that the two oil samples
received are water-in-oil emulsions containing around
For water-cut 40% and 60%, the variation of the amount of 38% to 40% water with an average droplet diameter D10
water incorporated in the formed emulsion versus the of 1,1 µm.
dissipated energy is shown in Figure 13 for the two oil/water • Crude oil presents classic viscosity behaviour: viscosity
systems. decreases with increasing temperature and dilution: The
Arrhenius law is verified for viscosity evolution with
Figure 13 : Oil behaviour comparison temperature. Viscosity decreases with increasing dilution
ratio according to an exponential law.
C o m p ariso n - W C 40% - 60% • Reconstituted emulsion formed during Dispersion Rig
P araffin ic o il - 25°C-10 m P a / H eavy o il - 80°C- 50 m P a experiments at high mixing energy (or high flow rate)
70
presented a droplet distribution similar to that of the
%w ater/ w ater+ oil w ith o ut d ilu e

60 residual emulsion from the initial crude oil samples. The

emulsion formed have an average droplet diameter D10
50
varying in the experimental conditions between 1,5µm
40 and 3 µm. This small droplet size is a sign of emulsion
30
stability and of further difficulty for oil/water phase
Heavy O il - W C 60%
separation.
20 Heavy O il - W C 40%

10 P araffinic O il -W C 40% Acknowledgments

0
0 5
En e r g y W /K g - E+0 7
The two oil/water systems exhibit identical behaviour on the
following points:
- The more the energy is dissipated in the liquid phases, the
more the oil tends to form "fine" water-in-oil emulsions
- Whatever the water-cut, a threshold energy exists above
which the oil/water system tends to be totally emulsified
- At 40% water-cut, above the energy limit, we observe no free
water as both oils are completely emulsified.
The noticed behaviour differences are: The threshold energy
value is higher for extra heavy oil compared to paraffinic oil
particularly at 60% water-cut where the energy limit seems
above 1.5 108 W/Kg (120l/h).
The main differences between the two oils are from the the
droplets size distribution of the emulsion formed. Even if both
oils tends to form "fine" emulsions with an average droplet
size decreasing with the fixed energy or flow rate the variation
domain is different for both oils:
-Paraffinic oil presented a bi-modal distribution 4 whatever the
flow conditions with a bigger droplet distribution above 10µm
and a finest droplet population with an average diameter D10
varying between 5µm up to 3µm.
-Extra heavy oil presented a mono-modal distribution with an
average diameter D10 varying between 3µm up to 1,5 µm.
P araffinic O il -W C 60% The authors wish to thank Total and IFP for granting
10 15 permission for publication this paper. Delvas S., Podesta-
Foley L., Mouret A. and Thoral P. are thanked for their useful
help for performing all the experiments.
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