1656 Energy & Fuels 2006, 20, 1656-1663

Novel Organic Solids Deposition and Control Device for Live-Oils:

Design and Applications
Mohammed Zougari,* Scott Jacobs, John Ratulowski, and Ahmed Hammami
Schlumberger ReserVoir Fluid Center, Oilphase-DBR, Edmonton, Alberta, Canada T6N 1M9
George Broze, Matthew Flannery, and Artur Stankiewicz
Shell Global Solutions (US) Inc., 3333 Highway 6 South, Houston, Texas 77082
Kunal Karan
Department of Chemical Engineering, Queens UniVersity, Kingston, ON, Canada K7L 3N6
ReceiVed December 14, 2005. ReVised Manuscript ReceiVed May 1, 2006

A novel laboratory-scale flow assurance tool termed an organic solids deposition and control (OSDC)
device has been developed to assess the potential for and severity of organic solids deposition problems from
hydrocarbon fluids at realistic production and/or transportation conditions. The OSDC device is a shear cell
based on Couette-Taylor flow with a cylindrical geometry. The shear cell geometric parameters are optimized
to maximize the Reynolds number. The OSDC device mimics the typical pipeline production conditions of
temperature, pressure, composition, turbulence, shear rate, surface type, and roughness. These key parameters
can be accurately and independently controlled, allowing the deposition tests to be conducted over a wide
range of conditions. Deposition tests were performed on live waxy and asphaltenic oils. Reproducible deposits
have been generated under consistent test conditions. Wax deposition rates from OSDC are comparable to
those found in pilot-scale flow loops while using orders of magnitude less fluid.

Introduction coldfinger or cold spot configurations. One interesting variation

was a rotating disk cold spot apparatus. All flow-through
Organic solids (e.g., waxes, asphaltenes, hydrates, and dia-
systems reported in the literature were pipe loops with the
mondoids), as well as scales, are encountered in all facets of
exception of one, which was a plate and frame heat exchanger.
petroleum production and transportation. An example pressure-
Recognizing the limitations of the existing deposition tech-
temperature phase diagram depicting phase boundaries for wax,
niques, which include a lack of high-pressure adaptability, the
asphaltene, and hydrates along with the liquid-vapor phase
requirement of having a large sample volume, and the inability
envelope of typical Gulf of Mexico deepwater black oils has
to simulate intensive turbulent flow regimes, the design and de-
been recently published.1 Long offsets and cold water temper-
velopment of a novel laboratory-scale apparatus capable of mi-
atures present a challenge for subsea developments in deepwater.
micking the deposition process of wax and/or asphaltene from
This is due to the fact that some or all of the solid-fluid phase
live reservoir fluids under realistic production and transportation
boundaries may be crossed during production, leading to
conditions was undertaken. While developing a fundamental un-
precipitation and subsequent deposition of organic solids.
derstanding of the deposition process was deemed important,
Experimental techniques to assess the propensity and rate of
major emphasis was placed upon designing and testing an ex-
organic solids deposition under realistic production conditions
perimental setup that could meet the following key design
are relatively limited. A review of open literature on wax and
criteria:
asphaltene deposition revealed that a majority of the experi-
mental studies on wax deposition were carried out mainly in (1) small sample volume, to require only small quantities of
low-pressure systems; only a few mentioned asphaltene deposi- expensive bottom-hole fluids for testing;
tion. Table 1 summarizes published deposition techniques and (2) accurate temperature control, to ensure testing under well-
corresponding key findings/observations as reported in the open defined thermal conditions;
literature. Briefly, the experimental systems for wax deposition (3) high-pressure adaptability, to allow testing of fluids at
could be classified as either batch systems or flow-through reservoir conditions (up to 105 MPa);
systems. The batch systems were essentially variations of (4) broad temperature range operation (-20-200 C), to
allow simulation of seabed to reservoir temperatures;
* To whom correspondence should be addressed. (5) controlled shear at the wall, to enable scalability of
Currently with Shell Global Solutions (U.S.) Inc., 3333 Highway 6
South, Houston, TX 77082, USA. deposition results;
Currently with Shell International Exploration and Production in (6) well-defined hydrodynamics, to allow testing under flow
Houston, TX. conditions ranging from laminar to fully turbulent regimes;
Currently with Shell International Exploration and Production in
Rijswijk, The Netherlands. (7) accuracy/precision of detection techniques, to ensure
(1) Ratulowski, J.; Amin, A.; Hammami, A.; Muhammad, M.; Riding, generation of reproducible and reliable data;
M. Flow Assurance and Sub-sea Productivity: Closing the Loop with (8) ability and flexibility to test surface types and roughness,
Connectivity and Measurements. Presented at the 2004 SPE Annual
Technical Conference and Exhibition, Houston, Texas, September 26-29, to allow testing of actual pipeline materials as well as assessment
2004; SPE 90244. of new surface materials and coatings;
10.1021/ef050417w CCC: $33.50 2006 American Chemical Society
Published on Web 06/07/2006
NoVel Organic Solids Deposition and Control DeVice Energy & Fuels, Vol. 20, No. 4, 2006 1657

Table 1. Summary of Published Deposition Methods and Key Findings

deposition device
ref type description test conditions main conclusions
Wax Deposition Studies
Jessen and Howel14 flow-through pipe loop laminar/turbulent maximum deposition rate around laminar-turbulent
transition
0.75/2.0 in. diam + 5 ft long deposition controlled by molecular diffusion
kerosene/wax mixture lower deposition in plastic and coated pipe
compared to metal pipes
Cole and Jessen15 flow-through plate and frame laminar surface wettability important parameter for deposition
kerosene/wax mixture free surface energy of paraffin and surface responsible
for adsorption forces
Hunt, Jr.16 batch and cold spot cold spot surface: 0.75 in. 1.25 in., deposit held in place by surface roughness
20 gauge
flow-through pipe loop pipe loop: 1/8 in. diam composition not important for deposition
refined wax-oil mixture + crude oil
Jorda17 batch cold spot cold spot surface: 2.0 in. diam surface roughness influenced amount,
1/ in. thick distribution, wax content of the deposit
8
refined wax-refined solvent mixture heat transfer important factor influencing
deposition and surface roughness affects
heat transfer characteristics
varying surfaces material
varying surface roughness
Patton and Casad18 batch cold spot cold spot surface: 2.0 in. diam 1/8 in. thick surface roughness and coatings do not affect deposition
refined wax-refined solvent mixture + plastic coating decrease deposit amount due to
insulation effect
refined wax-kerosene mixture deposition rate increases with increasing
temp differential (Tc - Ts)
Bott and Gudmundson19 flow-through pipe loop turbulent deposit thickness quickly reaches asymptotic value
13.1 mm i.d., 15 mm o.d., heat flux and shear stress are the main
762 mm entry length + 914 mm factors influencing the asymptotic thickness
jacketed length
wax-kerosene mixture mechanism of wax deposition is determined
by cohesive property of wax particles formed
in the boundary layer
Burger et al.20 flow-through pipe loop laminar both molecular diffusion and shear dispersion
are important deposition mechanism
4.93 mm i.d., 2.9 m long; deposit contains significant amount of oil
10.2 mm i.d., 2.83 m long (83-86%)
shear rate 3.5-31 s-1;
heat flux 0.9-88 W/m 2

Sadlerochir crude oil

Newberry21 batch rotating disk dimensions not available NA
Weingarten and Euchner22 batch and diffusion cylinder cylindrical 6-chamber diffusion cell wax diffusion test provide useful wax diffusion rate
flow-through and pipe loop pipe loop 0.25 in. diam; sloughing occurs when wall shear stress
heat transfer rate 19-5800 W/m2; exceeds strength of wax deposit; this is
shear rate 12-4960 s-1 unrelated to laminar-turbulent transition
flow-through capillary tube dimensions not available none
Hartley and bin Jadid23
crude oil
Agrawal et al.24 flow-through pipe loop laminar-turbulent maximum wax deposition occurs at laminar-turbulent
transition
pipe loop: 6 mm i.d., 25 cm long
Bombay high crude
Majeed et a.l25 flow-through pipe loop laminar-developing model does not predict asymptotic time-dependent
behavior
pipe loop: 6, 9, or 12 mm diam, 1.0 m long depletion effects could be significant in laboratory
experiments
North Sea crude
Hamouda et al.26 batch high-pressure cylinder cold spot of 40 mm diam molecular diffusion is the controlling wax
coldfinger deposition mechanism
North Sea crude
Hsu and Santamaria27 flow-through high-pressure laminar-turbulent flow turbulence depresses the temperature at which
flow loop maximum deposition occurs
pipe loop: 0.5 in. i.d., 5 ft long sloughing effect generated under turbulent flow has
significant effect on deposition rates
stock tank oil and recombined live-oil wax hardness and carbon number increases with aging
time
Brown et al.28 flow-through pipe loop shear rate: 330-1330 s-1 wax deposition by shear dispersion is not significant
stock-tank oil no deposition observed for zero heat flux
need for multiphase flow data
Wu et al.29 batch cold disk in an unknown small sample size (115 mL)
agitated vessel flow regime undefined
Ibrahim et al.30 flow-through pipe loop unknown wax deposition by shear in a concentric tubes setup; the
deposit is produced in the inner tube
Asphaltene Deposition Studies
de Boer et al.31 flow-through coiled tube no details available no conclusions available
(not a loop)
Alboudwarej32 flow-through pipe loop 1.91 cm o.d., 1.57 cm i.d. tubular geometry should allow easy scalability.
Wang et al.33 flow-through coiled capillary 16-32 m long laminar flow regimes only
tube 0.51 mm i.d. rate of deposition unaffected by flow rate and capillary
tube length overthe range studied
higher deposition rate with higher molar volume
precipitants
waxes codeposit with asphaltenes above WAT
1658 Energy & Fuels, Vol. 20, No. 4, 2006 Zougari et al.

Figure 1. Schematic representation of cylindrical Couette-Taylor

device. Figure 2. Velocity profile comparison between CT and pipe flows:12
(symbols) CT flow; (line) pipe flow.
(9) ability to test sour fluids, to allow testing of a wide variety
of reservoir fluids. and Rosende et al.10 performed theoretical and experimental
analyses comparing the turbulent scalar transport process in CT
flow to that encountered in pipe flow; evidence of similarities
Design of Organic Solids Deposition and Control System between both flows has been established. Wang et al.11 investigated
the effect of shear rate on the aggregation and breakage of particles
The organic solids deposition and control (OSDC) system was
in CT and pipe flow using both a computational fluid dynamics
designed and developed to study the fundamentals of physical and
(CFD) model and some experimentation and found excellent
chemical processes governing wax and asphaltene deposition from
agreement between the two flows. Smith and Townsend12 measured
petroleum fluids under typical production and transportation condi-
the velocity profile for the CT flow which when compared to pipe
tions. The designated objectives of the OSDC cell operation include
flow using the same geometrical dimension (pipe diameter vs flow
deposit formation, qualification, composition and the determination
gap in CT flow) and flow setup produced a similar profile as
of deposition kinetics as a function of temperature, pressure, shear-
depicted in Figure 2. The results so obtained correspond to a
rate, surface roughness, and surface type.
pipeline i.d. of 0.152 m, a centerline velocity of 4.6 m/s, and a
Basic Couette-Taylor Flow and Similitude with Pipe Flow.
Reynolds number of 700 000. More importantly, Smith and
The OSDC device is based on the flow between rotating concentric
Townsend12 also showed that the CT radial and vertical velocities
cylinders, also called the Couette-Taylor (CT) system. A schematic
are very small compared to the rotational velocity and, thus, deemed
diagram of the OSDC cell is shown in Figure 1. The OSDC cell
the centrifugal forces in CT flow negligible. Similarly, Bilson and
comprises a central rotating cylinder and an outer stationary cylinder
Bremhorst13 concluded that a virtually identical scalar transport
with the process fluid occupying the annular space. Although, this
process occurs in both CT and pipe configurations, including
geometry is clearly different from that of a pipe, there exists
average and localized radial velocities and acceleration representa-
similitude between flow in a CT system and a pipe. In analogy
tive of centrifugal forces.
with the flow in pipelines, the central rotating cylinder in the CT
OSDC System Description and Characterization. The OSDC
flow acts as a pump driving the flow in a closed loop and the
system consists of the following three major components: (1) a
stationary wall acts as the pipe wall. Lathrop et al.2 and Lewis and
pressurized shear deposition cell, including a spindle, deposition
Swinney3 performed extensive experimental analyses, which led to
surface, and heat exchanger system; (2) a secondary heat exchange
the establishment of a preliminary scalability of the two flow
system, which includes a cooling/heating bath, heater system, heat
processes in terms of a torque-Reynolds number relationship.
exchanger, circulating pump, and controllable valves; (3) instru-
Dubrulle and Hersant4 and Eckhardt et al.5 characterized a global
mentation and control systems, including controllers, data acquisi-
momentum transport analogy between the two flows using the
tion, and communication interfaces.
turbulent model approach and energy dissipation as used in
Figures 3 and 4 show a graphical picture of the whole OSDC
Rayleigh-Benard theory. Maynord6 used a CT flow to model the
setup and a schematic representation of the shear deposition cell,
transport of particles (fish eggs) in an open channel and concluded
respectively. Table 2 summarizes the key features of the OSDC.
that the CT flow gave a good indication of the shear mortality of
Optimization of the OSDC Cell Configuration. One of the
eggs in high flow-rate rivers. Van der Berg et al.7 analyzed the
key criteria in designing the OSDC cell was the ability to perform
effect of surface roughness on dimensionless torque using Gross-
experiments in a fully developed turbulent flow regime, a condition
mann-Lahose theory, which reinforced the analogy between CT
difficult to achieve in existing laboratory-scale devices. The
and Rayleigh-Benard flows. Tan and Swinney,8 Lee and Lueptow,9
geometry of the OSDC cell was optimized to achieve the maximum
Reynolds number for a fixed outer cylinder radius allowing the
(2) Lathrop, D.; Fineberg, J.; Swinney, H. Transition to shear-driven
turbulence in Couette-Taylor flow. Phys. ReV. A 1992, 46 (10), 6390-
attainment of turbulent flow conditions at reasonable rotational
6405. speeds.
(3) Lewis, G.; Swinney, H. Velocity structure functions, scaling, and
transitions in high-Reynolds-number Couette-Taylor flow. Phys. ReV. E (9) Lee, S.; Lueptow, R. Mass transfer in rotating reverse Osmosis based
1999, 59 (5), 5457-5467. on Couette-Taylor flow. Presented at the 13th International Couette Taylor
(4) Dubrulle, B.; Hersant, F. Momentum transport and torque scaling in Workshop, Barcelona, Spain, July 3-5, 2003.
Couette-Taylor flow from an analogy with turbulent convection. Eur. Phys. (10) Rosende, M.; Vieira, P.; Sousa, R.; Giordano, R. L.; Giordano, R.
J. B 2002, 26, 379-386. C. Estimation of mass transfer parameters in a Taylor-Couette-Poiseuille
(5) Eckhardt, B.; Grossmann, S.; Lohse, D. Scaling of global momentum Heterogeneous reactor. Braz. J. Chem. Eng. 2004, 21 (02) 175-184.
transport in Couette-Taylor and pipe flow. Eur. Phys. J. B 2000, 18, 541- (11) Wang, L.; Vigil, R.; Fox, R. CFD simulation of shear induced
544. aggregation and breakage in turbulent Taylor-Couette flow. J. Colloid
(6) Maynord, S. Concentric Cylinder Experiments of Shear Mortality of Interface Sci. 2004, 285, 167-178.
Eggs and LarVal Fish; Environmental Report 23, Upper Mississippi River- (12) Smith, G. P.; Townsend, A. A. Turbulent Couette flow between
Illinois Waterway, 2001. concentric cylinders at large Reynolds number. J. Fluid Mech. 1982, 123,
(7) Van der Berg, H.; Doering, C.; Lohse, D.; Lathrop, D. Smooth and 187-217.
rough boundaries in turbulent Couette-Taylor flow. Phys. ReV. E 2003, 68, (13) Bilson, M.; Bremhost, K. Comparison of Turbulent Scalar Transport
445010-445014. in a Pipe and a Rotating Cylinder. Presented at the 3rd International
(8) Tan, W.; Swinney, H. Mass transport in turbulent Couette-Taylor Conference on CFD in Minerals and Process Industries, December 10-12,
flow. Phys. ReV. A 1987, 36 (3), 1374-1381. 2003.
NoVel Organic Solids Deposition and Control DeVice Energy & Fuels, Vol. 20, No. 4, 2006 1659

Table 3. Similitude between CT and Pipe Flows

parameter pipe Couette-Taylor

uDe u(ro - ri)

Reynolds Re ) Re )
number34
1 1
wall shear ) Ffru2 ) Fu1.8
stress35,36 8 8
Nusselt Nu ) AReaPrb Nu ) AReaPrb
number37,38
dimensionless6 P ) C1Re(3/2)+R1 + C2Re2+R2 G ) C1Re(3/2)+R1 + C1Re2+R2
(P, G)
1 1
friction factor4,39 ) C1 log(Rexfr) + C2 ) C1 log(Rexfr) + C2
xfr xfr
ln(Re) ln(Re)
hydrodynamic p ) 91De CT ) 3.8(ro - ri)
boundary Re Re0.8
layer40,41
Figure 3. Graphical model of the OSDC system.
be scaled up reliably to the actual field operating conditions, it is
essential that the relevant characteristics of the OSDC device be
accurately defined. For scale-up of wax and asphaltene deposition
data, in addition to the control of the three thermodynamic variables
(temperature, pressure, and composition), the hydrodynamic and
heat transfer characteristics of the system must be well defined.
Accordingly, an extensive experimental program was undertaken
to establish the thermal-hydrodynamic stability of the OSDC
system.
This paper is not intended to provide a thorough or detailed
analysis on CT flow scalability to pipe flow but rather to prove the
existence of similitude between the two flows, sufficient to endorse
the CT flow approach to model and simulate the deposition process.
A detailed and specific fluid mechanics analysis, including extensive
experimentation, is ongoing to define and parametrize the scalability
process from CT flow to pipe flow, and representative experimental
results will be published in a separate paper.
Table 3 compares key flow and heat transfer parameters for CT
flow and pipe flow processes. The observed similitude is based on
Figure 4. Schematic diagram of the OSDC deposition cell.
established correlations for momentum, heat transfer, and mass
Table 2. OSDC System Parameters and Characteristics transport; hence, the CT flow has been adapted to physically mimic
the organic solids deposition process. It is recognized that the OSDC
parameter value device is a batch system similar to a flow loop; therefore, there are
sample volume 150 cm3 concerns regarding precipitate/deposit depletion effects as well as
heat transfer and deposition area 125.4 cm2 the possible effects of remnants of hydrodynamic vortices (i.e., CT
secondary flow rate up to 50 L/min flow instabilities known to occur below the critical Reynolds
temperature rating -20-200 C number2-13). However, the testing conditions (i.e., duration and flow
pressure rating up to 103 MPa (15 000 psi)
rotational speed up to 9000 rpm
regime) can be carefully designed so as to avoid both issues or at
surface roughness any least minimize their effects.
surface type any For instance, one can conduct preliminary deposition tests for
controlled shear yes the candidate waxy fluid as a function of time (i.e., perform a
flow regime any deposition kinetic study). From the plot of the corresponding deposit
sour fluid handling yes mass vs time curve combined with high temperature gas chromato-
graph (HTGC) analytical data of the parent oil and respective
The generalized form of the Reynolds number for Couette- deposits (i.e., n-paraffin content and distribution), a critical time
Taylor flow can be written as follows:2 during which no significant depletions occur can be determined.
Similarly, the initial slope of the deposit mass vs time curve amounts
F to a deposition rate fairly representative of those encountered in
Re ) r (r - ri) ) ri(ro - ri) (1)
i o V production flow lines. Alternatively, a large oil reservoir and
circulation system can be connected to the CT cell so that the total
where (ro - ri) is the gap between the inner (rotating) cylinder and oil volume employed is several times greater than that of the CT
the outer (stationary) cylinder, is the rotational speed, and ri is cell. Meanwhile, visualization experiments can be conducted to
the radius of the rotating device. We see from eq 1 that, for fixed determine the critical rotational speed (or Reynolds number) above
and ro, the Reynolds number is maximized by the choice ri ) which no flow instabilities (vortices) are present.
ro/2, for which choice: Table 4 shows an example of actual data output from two
different pipe configurations and their Couette-Taylor equivalent
Re F systems based on the existing and/or new correlations summarized
) (r - 2ri) ) 0 (2)
ri o in Table 3. In this comparison, we matched the Reynolds number,
wall shear stress, and hydrodynamic boundary layer thickness, likely
This optimization allows the OSDC device to achieve the highest proven to be among the most important quantities affecting the
possible turbulence regime for a fixed outer diameter. This enhances deposition process, where the input parameters were based on a
the wall shear stress and provides for a wider shear rate range. dynamic viscosity ) 1 cP, a density F ) 0.85 g/cm3, fluid
Scalability of OSDC Cell Data to Pipe Flow Conditions. To temperature Tf ) 25 C, and a Prandtl number Pr ) 10. The
ensure that the data generated from the laboratory-scale device can comparison shows that both systems yield similar results provided
1660 Energy & Fuels, Vol. 20, No. 4, 2006 Zougari et al.

Table 4. OSDC vs Pipe Parameters Benchmark m3 Gas-to-oil ratio (GOR). It is important to note that the
parameter pipe-1 couette-1 pipe-2 couette-2 deposition tests were carried out at a fixed pressure, temperature
diameter/gap (m) 0.1524 0.0711 0.0889 0.0432 differential between bulk fluid and deposition wall, fluid
flow velocity 4.10 8.85 3.0 6.1 composition, and constant spindle speed. Hence, the deposition
(max) (m/s) results for each OSDC test correspond to one specific point/
production rate/ 40 000 Bpd 1200 rpm 10 000 Bpd 1355 rpm location (of similar conditions) along a production pipeline. A
rotational speed
Reynolds no. 615 000 615 000 263 567 263 567
minimum of three deposition tests (covering the temperature
wall shear stress 4.5 4.5 2.80 2.80 range and fluid residence time) would be required to mimic a
(Pa) typical deposition profile expected along production and/or
wall velocity (m/s) 0.082 0.082 0.065 0.065 transportation flow lines.
wall Reynolds no. 1240 2800 1300 1150
Re ) u/V The STO sample was also tested for wax deposition using a
boundary layer 31 34 38 37 Shell pilot-scale flow loop and a Shell coldfinger apparatus.
thickness (m) Table 5 summarizes the specifications and characteristics of
Nusselt no. 1050 880 527 564
Shell pilot-scale flow loop. The Shell coldfinger apparatus is a
15.9 mm (5/8 in.) o.d. tube approximately 7.6 cm (3 in.) long,
a careful selection of testing parameters is ensured. As illustrated
in Table 4, a CT design can be developed to closely correspond to which is closed at the bottom. Coolant is injected through a
a specified pipe configuration. Therefore, one can design the OSDC tube near the inside bottom of the finger and exits through a
cell to mimic any pressure, temperature, surface type and roughness tube at the top. The finger is immersed in 50 mL of oil in a
(through carefully designed and machined cylindrical inserts), and sample container. The test oil is mixed using a magnetic stirrer
either Reynolds number or wall shear stress but not always both. bar at speeds ranging from 50 to 200 rpm. The sample container
OSDC Thermal Characteristics. Two sets of thermal experi- is heated by a water bath. The coolant temperature, oil
ments were undertaken. The first set was to establish how accurately temperature, and stirrer speed are controlled and recorded. At
the OSDC could be maintained at constant uniform temperature. the end of the experiment, deposits are removed with a solvent.
The second set was to define the heat transfer coefficient of the
The recovered deposit-solution mixture is topped, weighed,
shear cell. The response of thermocouples placed in the test fluid
(on the primary side) and those located inside the outer cylinder and analyzed to determine the wax and oil content.43
near the inner wall surface were measured to be within (0.3 C at
any given time during isothermal test runs, confirming that uniform (14) Jessen, P. W.; Howell, J. N. Effect of Flow Rate on Paraffin
and constant temperatures of up to 200 C can be achieved and Accumulation in Plastic, Steel and Coated Pipe. Pet. Trans., AIME 1958,
maintained. Figure 5 shows the temperature profiles from the bulk 213, 80-84.
(15) Cole, R. J.; Jessen, P. W. Paraffin Deposition. Oil Gas J. 1960, 58
(38), 87-91.
(16) Hunt, E. B., Jr. Laboratory Study of Paraffin Deposition. JPT, J.
Pet. Technol. 1962, (November), 1259-1269.
(17) Jorda, R. M., Paraffin Deposition and Prevention in Oil Wells. JPT,
J. Pet. Technol. 1966, (December), 1605-1612.
(18) Patton, C. C.; Casad, B. M. Paraffin Deposition from Refined Wax-
Solvent Systems. SPE J. 1970, (March), 17-24.
(19) Bott, T. R.; Gudmundsson, J. S. Deposition of Paraffin Wax from
Kerosene in Cooled Heat Exchanger Tubes. Can. J. Chem. Eng. 1977, 55,
381-385.
(20) Burger, E. D.; Perkins, T. K.; Striegler, J. H. Studies of Wax
Deposition in the Trans Alaska Pipeline. JPT, J. Pet. Technol. 1981, (June),
1075-1086.
(21) Newberry, M. E. Chemical Effects on Crude Oil Pipeline Pressure
Problems. JPT, J. Pet. Technol. 1984, (May), 779-786.
(22) Weingarten, J. S.; Euchner, J. A. Methods for Predicting Wax
Figure 5. Temperature distribution during a heat transfer run. Precipitation and Deposition. SPE Prod. Eng. 1988, (February), 121-126.
(23) Hartley, R.; bin Jadid, M. Use of Laboratory and Field Testing to
Identify Potential Production Problems in the Troll Field. SPE Prod. Eng.
of the fluid to the coolant side at different vertical locations as a 1989, (February), 34-40.
function of time, which reveals remarkable thermal stability and (24) Agrawal, K. M.; Khan, H. U.; Surianarayanan, M.; Joshi, G. C.
control of the implemented cooling system. Wax Deposition of Bombay-High Crude under Flowing Conditions. Fuel
OSDC Pressure Stability Tests. Precipitation of asphaltenes 1990, 69 (June), 794-796.
as well as waxes can be effected by changes in fluid pressure. As (25) Majeed, A.; Bringedal, B.; Overa S. Model Calculates Wax
Deposition for N. Sea Oils. Oil Gas J. 1990, 18, 63-69.
such, the maintenance of stable pressure at a specified level during (26) Hamouda, A. A.; Viken, B. K. Wax Deposition Mechanism Under
deposition testing of high-pressure live (saturated or undersaturated) High-Pressure and in Presence of Light Hydrocarbons. Presented at the SPE
petroleum fluid is important to ensure high quality and reliable International Symposium on Oilfield Chemistry, New Orleans, LA, March
experimental data. The pressure profile during an isobaric run was 2-5,1993; SPE Paper 25189.
measured over 6 h. The OSDC cell is able to maintain a test (27) Hsu, J. J. C.; Santamaria, M. M. Wax Deposition of Waxy Live
pressure of up to 103 MPa with a maximum deviation of 0.1 MPa Crudes Under Turbulent Flow Conditions. Presented at the SPE Annual
Technical Conference and Exhibition, New Orleans, LA, September 25-
or 1 atm. 28, 1994; SPE Paper 28480.
(28) Brown, T. S.; Niesen, V. G.; Erickson, D. D. Measurement and
Case Studies Prediction of the Kinetics of Paraffin Deposition. Presented at the SPE
Annual Technical Conference and Exhibition, Houston, TX, October 3-6,
Wax Deposition Tests. Detailed OSDC wax deposition 1993; SPE Paper 26548.
(29) Wu, C.-H.; Wang, K.-S.; Shuler, P. J.; Tang, Y.; Creek, J. L.;
experiments completed for two petroleum fluids of different Carlson, R. M.; Cheung, S. Measurement of Wax Deposition in Paraffin
origins, namely Gulf of Mexico (GoM) and Thailand, have been Solutions. AIChE J. 2002, 48 (9), 2107.
reported elsewhere.42 In this study, we briefly discuss some of (30) Ibrahim, J.; Toma, P.; Ivory, J.; Korpany, G.; de Rocco, M.;
the key findings obtained for the GoM fluid. The tested samples Holloway, L. Direct Observations on Paraffin Deposition Mechanism under
Laminar and Turbulent Flow for Direct Applications to Paraffin Oil
consisted of 36 American Petroleum Institute (API) stock-tank Transportation. Presented at the 5th International Conference on Petroleum
oil (STO) and corresponding recombined live-oil with 321 m3/ Phase Behaviour and Fouling, Banff, Canada, June 14-17, 2004.
NoVel Organic Solids Deposition and Control DeVice Energy & Fuels, Vol. 20, No. 4, 2006 1661

Table 5. Shell Pilot-Scale Flow Loop Characteristics and

Specifications
storage tank volume up to 10 bbl
flow loop specifications 5.08 cm diameter
60.96 m overall jacketed length
12.19 m preheat section for precision
controlled tests
6.10 m deposition test section with
countercurrent coolant flow in jacket
1.22 m spool piece for wax deposit removal
flow conditions maximum 2000 BOPD
turbulent or laminar flow
heating and controls 16 Chromalox heaters in eight 3.05 m
(10 ft) zones
14 matched calibrated RTDs for process
measurement and control
Farex SR-Mini PID controller with 7
control zones
control oil and coolant temperatures in test
section to within +0.2 C

Figure 6 presents photographs depicting the deposit formed

only on the inside surface of the outer OSDC stationary cylinder
(i.e., deposit wall) from the GoM samples.42 The spindle surface
appears coated with only residual oil as expected. The deposit
wall and spindle surfaces were photographed before and after
being subjected to rinsing with cold dichloromethane (DCM),
which is used to remove the oil (dark) film. Evidently, the post
rinse wax deposit is essentially white (like candle wax) with a
tint of yellow indicative of slight oil entrapment in the n-paraffin
rich material. The post rinse spindle surface is virtually clean
(i.e., deposit-free). One of the remarkable features that can be Figure 6. Photographs showing GoM oil wax buildup formed on
observed from these photographs is the uniformity of the deposit OSDC deposition wall and spindle.
thickness. In other words, there is negligible variation (if any)
in deposit characteristics over the entire deposition surface. This analyzed for n-paraffin composition and entrapped oil content
qualitative evidence suggests well-controlled hydrodynamics using HTGC and simulated distillation (SIMDIST), respectively.
within the OSDC cell. The relevant analyses of the total deposit, The deposition test parameters and results so obtained are
such as composition, can be averaged without introducing any summarized in Table 6. Figure 7 shows a graphical comparison
significant error.42 of wax deposition rates measured for the same STO using the
Hot toluene (70 C) is used to dissolve the postrinse deposit OSDC, Shell pilot-scale flow loop, and Shell coldfinger. Under
(i.e., the wax deposit) under high rotational spindle speed for similar test conditions, the OSDC cell produced results that are
at least 20 min. The resulting solution is then collected and fairly representative of those obtained using the flow loop in
subjected to roto-evaporation under a fume hood to dryness (i.e., terms of deposit oil content and deposition rate. However, the
constant mass). The resulting wax is weighed and subsequently OSDC uses only a fraction (0.01%) of the oil volume (10
bbl) required for the flow loop. Meanwhile, the coldfinger
(31) de Boer, R. B.; Leerlooyer, K.; Eigner, M. R. P.; van Bergen, A.
yielded wax deposits with very high entrapped-oil contents
R. D. SPE Prod. Facil. 1995, 2, 55-61. (minimum 70%) and, in turn, the corresponding wax deposition
(32) Alboudwarej, H. Asphaltene Deposition in Flowing Systems. PhD rates are significantly lower than those generated using OSDC.
Dissertation, University of Calgary, Calgary, Alberta, Canada, 2002. These results are plausible since oil content is an inverse function
(33) Wang, J.; Buckley, J. S.; Creek, J. L. Asphaltene Deposition on
Metallic Surface. J. Dispersion Sci. Technol. 2004, 25 (3) 287-298. of wall shear stress. In the case of the coldfinger, the wall shear
(34) Bird, B.; Stewart, W.; Lightfoot, E. Transport Phenomena, second stress is significantly lower than those attained in the OSDC
ed.; John Wiley & Sons: New York, 2002. and flow loop. More importantly, only the OSDC could be used
(35) Necati, O. In Heat Transfer: A basic Approach; McGraw-Hill: New
York, 1985 to conduct wax deposition measurements for typical reservoir
(36) Wendt, F. Ing. Arch. 1933, 4, 577. fluid compositions at realistic production conditions. It is useful
(37) Reohsenow, W. M. In Handbook of Heat Transfer, third ed.; to mention that uncertainty in empirical scaling procedures often
McGraw-Hill: New York, 1998. results in conservative predictions for wax deposition. The
(38) Gardone, M.; Astarita, T.; Carlomagno, M. Infrared Heat Transfer
Measurements on a Rotating Disk. Opt. Diagn. Eng. 1996, 1 (2) 1-7. OSDC cell deposition data can be scaled on the basis of
(39) Colebrook C. F. Turbulent flow in Pipes with Particular Reference fundamental and relevant fluid mechanics parameters such as
to the Transition Region Between the Smooth and Rough Pipes Laws. J. Re, wall shear stress, thermal gradient, etc. Accordingly, the
Inst. CiVil Eng. 1939, 11, 133-156.
(40) Schlichting, H. In Boundary Layer Theory, 8th revised and enlarged modeling of the flow-line conditions results in less conservative
ed.; Springer: Berlin, 2000. estimates.1
(41) Pope, S. B. Turbulent Flows, 1st ed.; Cambridge University Press: Asphaltene Deposition Tests. Asphaltene deposition tests
Cambridge, UK, 2001.
(42) Zougari, M.; Hammami, A.; Broze, G.; Fuex, N. Live-Oils Novel
were completed for a recombined South American live-oil at
Organic Solid Deposition and Control Device: Wax Deposition Validation. the reservoir temperature and 1 MPa above the corresponding
Presented at the 14th SPE Middle East Oil & Gas Show and Conference, saturation pressure. Bottom hole fluids from the same field are
Manama, Bahrain, March 12-15, 2005; SPE 93558. known to precipitate asphaltenes upon pressure depletion at the
(43) Ratulowski, J.; Westrich, J.; Leitko, A. Thermodynamic Model For
Wax Precipitation in Live-Oil Systems. Presented at the ACS Spring reservoir temperature.44-46 Field observations indicate the
National Meeting, San Francisco, CA, March 26-30, 2000. reservoir fluid is problematic; slow asphaltene deposition has
1662 Energy & Fuels, Vol. 20, No. 4, 2006 Zougari et al.

Table 6. Wax Deposition Test Parameters and Results (Run Time ) 3 h)

Ta pressure wall shear total deposit wax deposit oil content wax deposition
oil sample (C) (MPa) Re stress (Pa) (mg) (mg) (mass %) rate (mg/(hr cm2))
STO 2.6 0.1 2.5 104 32 183.4 137.8 25 0.49
live-oil 3.3 13.8 1.3 105 19 261.1 221.1 15 0.70
a T ) bulk oil temperature - deposition wall temperature. Bulk oil temperature ) cloud point or wax appearance temperature in this study.

Table 7. Sampling Information and Measured Properties for South American Live-Oil
reservoir conditions
pressure temp single stage asphaltene saturation asphaltene onset
(MPa) (C) flash GOR (m3/m3) contenta (mass %) API pressure (MPa) pressure (MPa)
60 138 123 5.8 30 19 28
a For topped STO, asphaltene content ) 6.7 mass %.

case of wax deposition, the asphaltene deposits appear quite

uniform in thickness and texture; however, they are qualitatively
much thinner than the aforementioned wax deposits.
DCM was used to simultaneously dissolve and recover the
oil film and asphaltene deposit from the cell deposition wall.
The resulting solution was collected and subjected to roto-
evaporation under a fume hood to dryness (i.e., constant mass).
The resulting topped residue (denoted as the total deposit) is
weighed and subsequently subjected to asphaltene content using
a modified IP-143 method.47 Table 8 summarizes the deposition
test parameters and corresponding results. Note the test matrix
includes one deposition measurement (test #1) at 17 MPa above
the measured asphaltene onset pressure; thereby, no measurable
asphaltene deposition is expected. The results of this test yield
the asphaltene deposit baseline (i.e., lowest detectable deposit
mass) of the OSDC cell. The corresponding total deposit (i.e.,
topped residue of the DCM rinse solution) and total asphaltenes
(i.e., precipitated + deposited) amount to 54.5 mg and 3.7 mg,
respectively. The difference between these two quantities yields
the mass of maltenes (i.e., de-asphalted, topped residue of the
DCM rinse solution). This mass combined with the topped STO
asphaltene content (i.e., 6.7 mass %) is then used to calculate
the amount of asphaltenes precipitated from the oil phase in
the total deposit. Finally, the asphaltene deposit mass is
determined using a mass balance (i.e., total asphaltenes -
precipitated asphaltenes). For test #1, the asphaltene deposit
mass amounts to 0.1 mg, which is within the margin of error
Figure 7. Comparison of shear cell (OSDC) wax deposits to those of measurement. As such, an asphaltene deposit mass less than
obtained using flow loops (FL) and coldfinger (CF): (a) deposition 1 mg is deemed negligible.
rate, (b) entrapped oil.
Tests #2-4 were designed to evaluate the effect of wall shear
been reported in few producing wells.45-46
Table 7 summarizes stress (by varying the spindle speed) on the amount of asphaltene
the sampling information and measured/reported properties of deposit. From the results listed in Table 8, three main observa-
the recombined oil. Figure 8 shows typical photographs of the
spindle smooth surface coated with oil film and the OSDC
stationary wall covered with asphaltenelike deposit. As in the

(44) Karan, K.; Hammami, A.; Flannery, M.; Stankiewicz, A. Systematic

Evaluation of Asphaltene Instability and Control During Production of Live-
Oils: A Flow Assurance Study. Pet. Sci. Technol. 2003, 21 (3 and 4), 629-
645.
(45) Stankiewicz, A. B.; Flannery, M. D.; Fuex, N. A.; Broze, G.; Couch,
J. L.; Dubey, S. T.; Iyer, S. D.; Ratulowski, J.; Westrich, J. T. Prediction
of Asphaltene Deposition Risk in E&P Operations. In Proceedings of the
3rd International Symposium on Mechanisms and Mitigation of Fouling in
Petroleum and Natural Gas Production, AIChE 2002 Spring National
Meeting, New Orleans, LA, March 10-14, 2002; Paper 47C, pp 410-
416.
(46) Flannery, M.; Cornelisse, P.; Zougari, M.; Hammami, A. Asphaltene
precipitation and deposition under live-oil conditions in a novel experimental Figure 8. Photographs of OSDC deposition wall and spindle following
device. Presented at the 4th International Conference on Petroleum Phase the isothermal and isobaric asphaltene deposition experiment for South
Behavior and Fouling, Trondheim, Norway, June 23-26, 2003. American live-oil.
NoVel Organic Solids Deposition and Control DeVice Energy & Fuels, Vol. 20, No. 4, 2006 1663

Table 8. Asphaltene Deposition Test Parameters and Results (Run Time ) 1 h at 138 C)
spindle speed pressure Re wall shear total deposita total asphaltenesb maltenesc asphaltene asphaltene deposition
test # (Hz) (MPa) 10-4 stress (Pa) (mg) (mg) (mg) deposit (mg) rate 102 (mg/hr/cm2)
1 40 45 5.5 15.2 54.5 3.7 50.8 tracesd 0.0
2 100 20 13.7 72.4 87.0 9.5 77.5 3.9 3.1
3 60 20 8.2 30.4 132.0 13.6 118.4 5.1 4.1
4 40 20 5.5 15.2 300.0 36.5 263.5 17.6 14.0
a Total deposit ) topped DCM wall rinse solution (i.e.,maltenes + total asphaltenes). b Total asphaltenes ) deposited asphaltenes + precipitated asphaltenes.
c Maltenes ) topped de-asphalted DCM wall rinse solution. d Traces ) asphaltene mass is <1 mg.

tions are readily made: (i) measurable asphaltene deposits for production system design and chemical screening, the OSDC
formed under all three test conditions, (ii) higher wall shear can test not only export oils (low pressure) but also bottom-
stress, as expected, yields lower asphaltene deposit, and (iii) hole and pressurized fluids (sample volume 150 mL) up to
the asphaltene deposition rate is fairly low. These findings are a pressure of 103 MPa. Existing pipe flow loops or other
quite plausible and consistent with reported field observations deposition tools can only test export oils (usually stock-tank
and experience.45-46 This is, to our knowledge, the first time oils) and require barrels of oils to yield representative and
asphaltene deposits have been generated in a laboratory cell at scalable results. The OSDC generates comparable results to the
wellbore pressure, temperature, and composition under con- Shell pilot-scale pipe flow loop with significantly (orders of
trolled and well-defined shear conditions. Measurements such magnitude) less fluid volume. It enables a dramatic increase in
as those reported herein assess the true tendency of a fluid to flow assurance prediction and confidence of system selection.
deposit asphaltene, and it is anticipated that they would form The increased predictive accuracy of OSDC can minimize the
the basis of a predictive asphaltene deposition model.1,44 adoption of overly conservative system design criteria, thus
minimizing both capital and operating expenses.
Conclusions
Symbols
A novel device termed the organic solids deposition and Re ) Reynolds number
control (OSDC) cell has been designed, developed, and suc- De ) pipe hydraulic diameter
cessfully tested for the study of wax and asphaltene deposition fr ) friction factor
from petroleum fluids. The cell is based on the Couette-Taylor G ) nondimensional torque
or concentric cylinder geometry. Mathematical analysis indicated h ) cell height
that the wall shear stress in the OSDC is comparable to that ro ) radius of the Couette-Taylor cell stationary deposition surface
achieved in tubular flow-lines or pipelines. Thermal character- ri ) radius of Couette-Taylor cell spindle
ization of the OSDC system was carried out to define the level T ) torque
of temperature control attainable. Experimental results estab- ) ri/ro
Pr ) Prandtl number
lished that the axial variation in the bulk fluid temperature in
Pn ) normalized pressure
the turbulent flow regime was less than (0.1 C, whereas the u ) linear fluid velocity
variation in the deposition wall temperature was within 0.3 C. F ) fluid density
The ability of the system to operate under stable high-pressure ) fluid kinematic viscosity
conditions was also established. Upon comparing the existing ) CT friction factor
thermal-hydraulics correlations from both pipe flow and ) boundary layer thickness
Couette-Taylor flow, it was concluded that there is similitude
between both flows and, therefore, the scalability from one to Acknowledgment. The authors wish to thank Shell International
E&P, ChevronTexaco, and the DBR Group of Companies (now
the other is possible.
Schlumberger Reservoir Fluid Center SRFC) for funding this
The desired functionality of the OSDC cell was successfully project and for permission to publish the results. The authors would
demonstrated by conducting wax deposition tests on stock tank also like to acknowledge the contributions of Nick Fuex, Peter
oil as well as live-oil samples for both wax and asphaltene. Cornelisse, Vladimir Liakhovitch, and Alan Leitko of Shell Global
Unlike pipe flow loops and other existing deposition techniques Solutions; Jeff Creek, Nancy Burke, and Mietek Boduszynski of
used by the industry to generate key flow assurance input data ChevronTexaco; Larry Holloway of the Alberta Research Council;
and Terry Sopkow, Ryan Jacobsen, Rob Lundstrom, Kent Knight,
(47) Hammami, A.; Ratulowski, J. Precipitation and Deposition of Rob Fisher, Craig Borman, Abdel Kharrat, and Moin Muhammad
Asphaltenes in Production Systems: A Flow Assurance Overview. In of SRFC.
Asphaltenes, HeaVy Oils and Petroleomics; Kluwer Academic Publica-
tions: Norwell, MA, 2006; Chapter 23, in press. EF050417W