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Abstract
The potential for hydrocarbon solid formation and deposition
adversely affecting flow assurance in deepwater production
systems is a key risk factor in assessing deepwater
developments. To reduce this risk, a systematic approach to
defining and understanding the thermodynamic and
hydrodynamic factors impacting flow assurance is required.
The development of experimental and simulation techniques
to provide this information are a current focus of attention in
the reservoir fluid phase behavior community. This paper
provides a case study of the various aspects of a state of the art
laboratory and simulation assessment for a Gulf of Mexico
reservoir crude. The case study illustrates the application of a
systematic approach to characterization of the crude and the
impact of this knowledge on potential production and flow
assurance strategies.
Introduction
Deepwater exploration and development in the Gulf of
Mexico and other deepwater offshore areas around the world
have become key activities for the majority of oil and gas Figure 1: Areas of potential solids problems
exploration and production companies. Development and perforations, to the wellbore, topside surface facilities and
activities in the deepwater face significant challenges.1 Of pipelines. Viewing this in another way, Figure 2
particular concern, are the effects of produced fluid schematically demonstrates the superimposed thermodynamic
hydrocarbon solids (i.e. asphaltene, wax, and hydrate) and phase boundaries for the potential hydrocarbon solid
their potential to disrupt production due to deposition in the phenomenon. Also shown is the potential production P-T
production system. It is noted that the deposition of inorganic pathway that would obviously be dependent on the specific
solids arising from the aqueous phase (i.e. scale) also poses a hydrodynamic and heat transfer characteristics of a given
2 A.K.M. JAMALUDDIN, J. NIGHSWANDER AND N. JOSHI SPE 71546
completion and facilities system. As can be seen, the pressure the asphaltenes produced by pressure drop in a reservoir
and temperature PT pathway of the production circuit can production system are different than the asphaltenes produced
intersect one or all three elements of hydrocarbon solid by solubility criteria as defined above. The reservoir
formation, and consequently result in potential flow assurance asphaltene includes some additional components such as
problems wherever these boundaries are crossed. It is noted resins.
that crossing the thermodynamic conditions for the formation
of hydrocarbon solids does not necessarily imply that a flow Waxes are also high molecular weight, highly saturated
assurance problem will be encountered. In other words, if organic substances. The formation of wax crystals depends
hydrocarbon solids form but do not deposit, they are not a significantly on temperature change. Pressure and composition
problem. Current techniques to assess the deposition tendancy also affect their formation but not to a significant extent.8
of the hydrocarbon solids and the factors affecting the
deposition of solids are not currently well understood and are Gas hydrates are defined as the “Clathrate” inclusion
compounds. They are formed by the contact of hydrate
forming gases (primarily methane, ethane, propane, carbon
dioxide, and hydrogen sulfide) and liquid water at low
temperature (0-40oC) and high-pressure conditions9. Two
types of gas hydrates are classified in the literature and they
are Structure I and Structure II.10 Each hydrate building block
has a central cavity to encapsulate molecules of hydrate
forming gases.
During open hole Modular Formation Dynamics Testing precipitate is filtered, dried and weighed. The solvent is
(MDT), Single-Phase Multi-Chamber (SPMC) module is removed from the soluble portion of the sample, which is
normally used in collecting single-phase reservoir fluid referred to as the maltenes. The maltenes are then re-dissolved
samples for asphaltene analysis. In the SPMC module, the in pentane and are chromatographically separated into
fluid pressure is maintained above the reservoir pressure while saturates, aromatics and resins (polars) fraction by elution
the sample is retrieved to the surface by having a pre-charge from a column filled with activated alumina, using various
nitrogen cushion in the sample chamber. Thus, making the solvents and solvent mixtures. The solvents are then removed
SPMC suitable for asphaltene precipitation testing. Details of from each fraction and the amount of material weighed. The
the equipment and procedural issues surrounding these data from the three methods are combined to determine the
operations can be found in reference 11. In the MDT module amount of each component type in the original sample. Mass
other conventional chambers that are not pressure balances are calculated throughout the procedure to assure
compensated are also used to collect the reservoir fluid accurate data.
samples. In these conventional sample modules, fluid may For the case study considered in this work, the fluid
undergo phase change phenomenon, and hence, render the characterization data determined using the techniques
sample invalid for asphaltene analysis. described above are summarized in Tables 1- 3. This fluid
For the present case study, the SPMC samples were not was noteworthy as it had quite a low GOR (1037 SCF/STB)
available, and hence, a sub-sample from the one-gallon for the bubble point of 6267 psia and a relatively high stock
chamber was used. tank oil density of 0.898 g/cm3 (26oAPI). It is also noted from
the SAR(P)A analysis that the asphaltene (0.67 wt%) and wax
Fluid Compositional Characterization. Upon arrival of fluid (0.86 wt%) contents of the crude oil are quite low.
samples in the laboratory, the sample chambers are first
Table 1: Preliminary Fluid Properties
validated by determining the opening pressure. Subsequently,
a sample is chosen for study and the sample is heated to the Parameters Units Description
reservoir temperature using a custom made heating jacket. The
sample bottle is then placed into a rocking stand and agitated
for a minimum of 5 days to insure homogenization of the Reservoir Pressure - Pi psia 7393
reservoir fluid. After stabilization, a small portion of the Reservoir Temperature o
F 152
single-phase reservoir fluid is subjected to a single stage flash Flash Gas-Oil Ratio SCF/STB 1037
experiment to determine the Gas-Oil-Ratio (GOR), C36+
Bubblepoint Pressure (Pb) at Tres psia 6267
composition, density at sample pressure and temperature, and
Density of Stock-Tank Oil (STO) g/cc 0.898
stock oil density (API gravity). The flash is conducted from a
pressure slightly above the bubble point at reservoir Density of Reservoir Fluid at Pb g/cc 0.801
temperature down to ambient conditions. The resulting mass Density of Reservoir Fluid at Pi g/cc 0.819
and volumes of gas and liquid is recorded and the flashed OBM Contamination in STO % (w/w) 0.845
fluids (gas and liquid) are then analyzed using gas OBM Contamination in Reservoir Fluid % (w/w) 0.717
chromatography13. The live oil composition is then calculated
based on the measured gas and liquid compositions and GOR
values. Finally, if the samples were obtained by open-hole
sampling (as was the case in this work), the level of OBM Preliminary Screening For Solids. After completion of the
contamination in the stock tank oil needs to be determined. fluid compositional characterization, a series of screening
This is completed by a subtraction method taking into account criteria and simulation are used to evaluate the potential of the
the OBM filtrate composition and the contaminated stock tank crude oil under consideration to exhibit solid formation
oil composition14. problems. For asphaltenes in particular, the first screening test
In addition to the grouped carbon number analysis is called the De Boer plot (Figure 3a) was developed based on
provided for above, a portion of stock tank liquid is also field observations by Shell2. Using the data from the case
prepared for Saturate-Aromatic-Resin(Polars)-Asphaltene study considered here, the plot indicates that the sample under
(SAR(P)A) analysis. In this technique, a spinning band consideration would not be expected to exhibit any problems
distillation is carried out on the sample to establish two in the field. The second screening criteria is the asphaltene to
fractions. The initial boiling point fraction (up to 300oC) is resin ratio15. As can be seen in Figure 3b, this criteria also
then analyzed using a supercritical fluid chromatographic indicated that there should be no solid formation problems for
(ASTM 5186-91) method to determine saturates and aromatics the case study crude oil considered in this work. The third
content. The greater than 300oC fraction is subjected to a screening criteria used was the colloidal instability index
gravimetric analysis to determine the heptane insoluble suggested by Baker-Petrolite15. Referring to Figure 3c, it can
content (asphaltenes). This method dissolves the fraction in an be seen that according to this criteria, there is potential for
equal weight of toluene then 40 volumes of heptane are added asphaltene formation in this crude. Finally, an asphaltene
to precipitate the insoluble portion of the sample. The stability index criteria developed by Oilphase-Schlumberger is
4 A.K.M. JAMALUDDIN, J. NIGHSWANDER AND N. JOSHI SPE 71546
shown in Figure 3d. By these criteria, the case study fluid is Table 3: SARA Analysis of Stock-Tank Oil
on the border between stable and unstable with respect to
Cylinder Saturates Aromatics Resins Asphaltenes Wax
asphaltene formation. Predictive techniques for asphaltene
formation are not well developed at the current time, and it is (n-heptane
felt that the screening criteria adequately serve this purpose. Insolubles)
Based on the results presented in Figure 3a-d, it was felt that % (w/w)
there was a probability of asphaltene formation, thus justifying
further lab testing to clarify this potential. Sample 1 49.53 31.70 18.10 0.67 0.86
Preliminary screening for wax formation generally
involves consideration of the stock tank oil wax content (UOP
Procedure16), the Cross Polar Microscopy (see below) wax 12000
appearance temperature and preliminary thermodynamic Severe
modeling. If wax content is greater than 2 wt% and the 10000 Problems
measured or predicted STO wax appearance temperature is in
Undersaturation (psia)
excess of 120oF, this may indicate a significant concern. 8000
Sample 1
Table 2: Reservoir Fluid Composition
6000
Flashed Flashed Reservoir No
Components Liquid Gas Fluid
4000 Problems
% mole
Uncertain
Nitrogen 0.00 0.10 0.07 2000
Carbon Dioxide 0.00 0.14 0.10
Hydrogen Sulfide 0.00 0.00 0.00 0
Methane 0.00 84.92 60.99 0.50 0.60 0.70 0.80 0.90
Ethane 0.00 6.08 4.37
Propane 0.00 3.45 2.48 In situ density (g/cc)
I - Butane 0.00 0.76 0.54
N - Butane 0.01 1.54 1.11
I - Pentane 0.04 0.96 0.70 Figure 3a: de Boer Plot
N - Pentane 0.09 0.65 0.49
pseudo C6H14 1.65 0.74 1.00
pseudo C7+ 98.21 0.67 28.15 5.0
4.5
Total 100 100 100
Unstable
MW 293.42 20.85 97.66 4.0
Asphaltenes % (w/w)
3.5
Mole %
C7+ 98.21 0.67 28.15 3.0 Stable
C12+ 71.29 0.00 20.09
2.5
C20+ 35.80 - 10.09
2.0
Molar Mass 1.5 Sample 1
C7+ 297.27 100.31 293.90
C12+ 362.94 165.43 362.94 1.0
C20+ 515.90 - 515.90 0.5
production, it is advisable to complete experiments to quantify scope and nature of more detailed fluid behavior
the actual hydrate formation conditions. For the case study measurements. Typically, the experimental identification of
completed here, although the general criteria did not indicate the thermodynamic phase boundaries for the individual solid
significant potential for wax or hydrate problems, it was hydrocarbon elements is the first step in this process. Various
nonetheless anticipated from production profile estimations laboratory techniques such as fluorescence spectroscopy17,
that the produced fluids would exhibit quite cold temperature conductive measurements,18 acoustic resonance,19
(as low as 40oF) and hence it would be advisable to complete a gravimetric, and light-scattering technique (LST)8, 21-23 have
20
series of wax and hydrate experimental measurements. been used in determining the onset of solids formation
conditions. A general summary of the various techniques for
75.0 asphaltene formation can be found in reference 24. Reference
Reference: Baker Petrolite 8, presents techniques to define the thermodynamic conditions
of wax appearance temperature (WAT). Various literatures
65.0 present the measurements of hydrate formation conditions and
Asphaltenes + Saturates
continuously during the course of a test. For consistency, the solids and/or gas bubbles) that may occur. Visual observation
fiber optic light transmittance system referred to here is of the cell contents are also made and recorded during the
termed as the light scattering system (LSS). course of the experiment. At the end of the experiment, the
The viscosity of the reservoir fluid is measured at the PVT cell is depleted and then rinsed with toluene to measure
reservoir temperature and pressure conditions using a the amount of any residual asphaltenes that may remain in the
Cambridge SPL440 electromagnetic viscometer. The cell. The quantity obtained provides a qualitative indication of
viscometer consists of one cylindrical cell containing the fluid the percentage of total asphaltenes that may precipitate during
sample and a piston located inside the cylinder. The piston is production whereas the rest tend to flow with the oil.
moved back and forth through the fluid by imparting an High-Temperature High Pressure Filtration for Bulk
electromagnetic force on the piston. Viscosity is measured by Precipitation of Asphaltene. The high pressure high
monitoring the time for the piston to traverse the cell under a temperature filtration test is conducted to quantify the amount
known force. The reported accuracy of the viscometer is of asphaltenes that may flow at a given pressure.
±1.5% of full scale. The viscosity of stock-tank oil is Conventional theory suggests maximum amount of
measured using a capillary tube technique. The assembly of an asphaltenes are precipitated at the bubblepoint pressure24.
oil reservoir attached to a capillary tube is maintained at the Hence, to quantify the maximum amount of asphaltenes that
required temperature. Subsequently, the oil is allowed to flow may precipitate during production, filtration at bubblepoint
under gravity between two marked levels in the capillary tube. pressure is normally conducted. For the case study considered
The time taken to pass through the marked level is then here, asphaltenes were detected to be present at the reservoir
converted to viscosity. conditions and hence, an additional filtration at the reservoir
In addition to the PVT equipment, LSS, and viscosity, temperature and pressure was conducted to quantify the
high-pressure filters are also used during the asphaltene amount of asphaltene that are present in the initial reservoir
precipitation study to quantify the amount of asphaltene in the fluid.
fluid at the specified conditions. The filter assembly consists The filtration tests are conducted with a 0.22µm filter
of two plates screwed together with the hydrophobic filter paper size. To prevent flashing of the reservoir fluid as it
sandwiched between them. Details of the equipment can be passes through the filter, high-pressure helium is used to
found in reference 24. Finally, Wax Appearance Temperature maintain a backpressure on the downstream side of the filter.
(WAT) of the stock-tank oil (STO) is measured using Cross- As a result, the filtration process is very close to an isobaric
Polar Microscopy (CPM) equipment. The CPM method is transfer. After displacement of the test fluid through the filter,
based on the principal that the formation of wax crystals will the volume of filtrate is measured and the asphaltene content
rotate the plane of polarization of light passing through the on the filter paper and the filtrate is determined.
oil/wax sample. The apparatus for CPM (in serial order)
consist of a light source, an IR-filter, a polarizer, a Cross Polar Microscope (CPM) for Wax Appearance
temperature-controlled stage, an analyzer, a video camera, and Temperature of STO. The STO oil sample is homogenized at
a PC. This setup is designed to detect any rotation of the the reservoir temperature and then a drop is mounted on a
plane of polarization due to crystal formation. slide and a cover slip is placed on top of it. The slide is placed
on the stage of a microscope to visually observe the WAT
Experimental Procedure with simultaneous recording of the process using a video
Isothermal Depressurization for the Onset of Asphaltene camera. The rate of cooling of the stage is controlled at
Precipitation. Onset of asphaltene precipitation (OAP) 1.5oF/min. The slide is brought under focus for visual
measurements using the light scattering system (LSS) involves observation and the sample is cooled from an initial
charging a known volume of the test fluid at reservoir (or temperature of 150oF. The WAT is identified off-line at
specified) temperature and pressure to the JEFRI PVT cell. which the first detectable bright spots are visible.
The LSS components are then mounted across the windows of
the PVT cell. The cell contents are then homogenized at a Live and dead oil viscosity measurements for Wax
maximum mixer speed of 1400 rpm for about 30 minutes. Appearance Temperature. Prior to measuring the viscosity, a
Subsequently, a light transmittance scan is conducted to suitable size piston is selected with the proper viscosity range
establish a reference baseline. The depressurization and the electromagnetic viscometer is calibrated using a fluid
experiment is then started with simultaneous measurement of with known viscosity. A portion of the reservoir fluid is then
light transmittance power. The maximum depressurization transferred into a high-pressure high-temperature
rate used in this system is in the order of 40 psi/min. electromagnetic viscometer. The viscometer is initially
The average transmitted light power and the corresponding evacuated and its temperature is controlled at the desired
pressure are recorded every minute and the experiment is temperature. During the transfer of reservoir fluid to the
stopped after reaching a certain pre-defined lower pressure. evacuated viscometer, flashing of oil takes place, and hence,
During the depressurization run, any change in the light the viscometer system is flushed with two viscometer volumes
transmittance characteristics is a reflection of various fluid of reservoir fluid to ensure that a representative oil sample is
property and phase change phenomenon (ie. appearance of taken. Subsequent to transfer of reservoir fluid into the
SPE 71546 A SYSTEMATIC APPROACH IN DEEPWATER FLOW ASSURANCE FLUID CHARACTERIZATION 7
viscometer, the fluid system is allowed to achieve thermal and The formation and decomposition points are not the same due
pressure equilibration. Then, the viscosity reading is taken. to transient hysteresis.
For wax appearance temperature testing as considered in this
work, the temperature is then reduced while maintaining Experimental Results
pressure at the desired level. After thermal stabilization, Isothermal Depressurization for the Onset of Asphaltene
another viscosity reading is completed. This is repeated for a Precipitation. Following the procedures outlined previously,
pre-defined series of test temperatures. the reservoir fluid sample was stabilized for a period of 5 days
at reservoir temperature (152oF) and a pressure of 14,000 psig.
Isobaric Cooling for Wax Appearance Temperature of The stabilized sample was then transferred to the JEFRI PVT
Reservoir Fluid. The isobaric cooling experiments using LSS cell at these conditions and the LSS test initiated. The LSS
are conducted to measure the onset of wax appearance data for this test is provided in Figure 4. As can be seen, the
temperature (WAT) of the reservoir fluid. In these fluid light transmittance initialy increases as expected and then
experiments, a known volume of the test fluid is charged into begins to fall at approximately 13,000 psia indicating the
the PVT apparatus at the reservoir temperature and pressure formation of asphaltenes. This occurrence was surprising in
conditions. The LSS components are then mounted across the so much as the asphaltene onset occured well above reservoir
windows of the PVT cell. The cell content is then pressure of 7393 psia. Such a phenomenon could be attributed
homogenized at a maximum mixer speed of 1400 rpm for to two factors:
about 30 minutes. The fluid is then isothermally flashed and 1) The sample under consideration was not valid
equilibrated at the designed experimental pressure. because it was a sub-sample from a one-gallon
Subsequently, the formed vapor phase is displaced from the sample chamber and went through phase separation
PVT cell to ensure constant liquid composition during the during sample retrival from the wellbore.
isobaric cooling. Following gas displacement, a light 2) The sample behavior deviated from the conventional
transmittance scan is conducted to establish the reference thinking that the aggregated asphaltenes cannot exist
baseline. The isobaric cooling experiment is then started with at reservoir conditions.
simultaneous measurement of light transmittance power and Subsequently, to establish any temperature dependency on the
temperature. A maximum cooling rate of 1oF/minute is used asphaltene onset pressure, it was decided to complete an
for this system. additional asphaltene onset screening test at 130 F. This test
was completed in the same manner as described above and the
Isobaric Cooling for Hydrate Formation Temperature. A LSS data for this test are provided as Figure 5. In this case, an
small volume of the homogenized single-phase fluid is asphaltene onset pressure of 7600 psia was identified. This
transferred into JEFRI PVT cell at reservoir temperature and indicated very significant effect of temperature on the
pressure conditions. After stabilization, the system pressure is asphaltene stability for this crude oil.
reduced to the experimental pressure below the bubblepoint
pressure. This generates a gas phase. Subsequently, a 1000
sufficient amount of water is charged to the PVT cell to make
sure that the Oil System has excess free water. The system is
then equilibrated at the specified pressure. After stabilization, 800
Light Transmittance (nW)
about the sample validity, the data interpretation is in the Cross Polar Microscope (CPM) for Wax Appearance
realm of possibilities and ambiguous conclusions. Hence, no Temperature (WAT) of STO. As mentioned previously CPM
further asphaltene characterization was deemed appropriate. for determining the WAT of the stock tank oil is a general
screening parameter for potential wax formation issues. The
CPM data for the crude oil considered in this work is provide
1600 as Figure 6. As can be seen, the first crystals of wax can be
identified forming in the STO at approximately 104oF.
Light Transmittance (nW)
1200
Poap = 7600 psia
800
400
0 o
0 3000 6000 9000 12000 15000
Figure 6a: Stock-Tank Oil at 152 F
Pressure (psia)
Wax Crystal at
initiation
Figure 5: Isothermal Depressurization: Onset of
o
Asphaltene Precipitation at 130 F
of solution gas below the fluid saturation pressure and will It is noted that wax will have formed at these conditions;
show a slight increase with pressure above the saturation however, this will not affect the hydrate forming condition, as
pressure. The 1080F measurement for the reservoir fluid in
this case was attributed to the relative uncertainty of the 300
viscometry technique for WAT determination, which is
estimated to be +/- 10oF. It is noted that the viscometry 250
100.0
100
WAT = 93oF
50
10.0
Viscosity (cP)
0
0 30 60 90 120 150 180
Temperature (F)
1.0
the molecular weight of the fluid, and the measured fluid thermodynamic and hydrodynamic behavior of the reservoir
saturation pressures, WAT’s, and Hydrate formation fluid. This information is summarized in Figure 11. As can be
conditions. All tuning and predictions were completed using a seen, the pressure-temperature profile during production at
commercially available software package (PVTsim). 13000 bpd (Curve A) is at least 25oF higher than wax/hydrate
After tuning, the model was first used to predict the vapor- precipitation at any pressure. Thus, the reservoir fluid is not
liquid equilibrium curve as shown in Figure 11. However, the believed to encounter wax/hydrate deposition problems during
software did not provide a direct tuning capability for Hydrate early production. However, as the production rate decreases to
formation. The un-tuned hydrate prediction at 2000 psia was 8000 bpd after five years, the heat transfer characteristics
11oF above the measured decomposition temperature of 52oF. change as indicated by Curve B in Figure 11. The path for
Hence, the predicted curve was horizontally shifted to match curve B crosses the conditions conducive for wax and hydrate
the measured data as shown in Figure 10. Although this formation. Hence, wax and hydrate deposition problems are
approach is not strictly rigorous, it was felt that it was an expected during production at later times when production
acceptable estimation given the desired use of the predictive rates begin to decline.
model. The wax deposition phase envelope (Figure 11) was Finally, as determined during experimental measurements,
predicted after tuning the compositional model with the wax asphaltene instability could not be established with the given
appearance temperature of 103.6oF for the stock-tank oil. The uncertainties. Hence, effort to establish the asphaltene
tuned model predicted the wax appearance temperature of precipitation phase behavior was abandoned.
93oF at 2000 psia without the need for additional tuning.
It is noted that asphaltene formation modeling was not
successful or meaningful given the experimental observation
V-L-E Phase Envelope
that asphaltenes are present in a range of aggregated states
Measured Hydrate Decomposition
throughout a large range of the anticipated production Simulated Hydrate Envelope
conditions. For this reason, no asphaltene model results were Adjusted Hydrate Envelope
completed. 10000
Table 5: Hydrodynamic Calculation Assumptions
8000
Parameters Values Units
Pressure (psia)
6000
Production tubing diameter 5 inches
4000
Flow Rate 13000 - 8000 barrels per day
Tubing Insulated
2000
Completion Subsea
0
0 20 40 60 80 100
Hydrodynamic Modeling. To estimate the potential
production P-T pathways for the reservoir under Temperature (F)
consideration, a commercially available software package
(Olga) was used to simulate the hydrodynamic behavior of the Figure 10: Hydrate Phase Envelope
reservoir fluid. For the calculations, it was assumed that an
initial fluid flow rate of 13000 barrels per day would be
achieved and that this would reduce to 8000 barrels per day
after 5 years. The hydrodynamic calculations at 13000 bpd are
represented as Curve A in Figure 11 whereas that as 8000 bpd
are presented as Curve B. The input parameters for the
simulations are summarized in Table 5. The simulations here
obviously involve gross assumptions regarding the
hydrodynamic behavior of the produced fluid over time,
however they were felt to provide a reasonable bound for the
range of expected production conditions to be encountered by
the reservoir fluid.
13. Jamaluddin, A.K.M., Ye, S., Thomas, J., D’Cruz, D., Hydrocarbon Production,” paper SPE 49465 presented at
Nighswander, J.: “Experimental and Theoretical the 8th Abu Dhabi Petroleum Exhibition and Conference,
Assessment of Using Propane to Remediate Liquid Buildup Abu Dhabi, U.A.E., 11-14 October 1998.
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