SPE 129892
Ping Zhao (SPE), A. J.Howes (SPE), Varadarajan Dwarakanath (SPE), Sophany Thach (SPE), Taimur Malik
(SPE), Adam Jackson (SPE), Oya Karazincir (SPE), Curt Campbell, and Jeff Waite (SPE), Chevron
Copyright 2010, Society of Petroleum Engineers
This paper was prepared for presentation at the 2010 SPE Improved Oil Recovery Symposium held in Tulsa, Oklahoma, USA, 24–28 April 2010.
This paper was selected for presentation by an SPE program committee following review of information contained in an abstract submitted by the author(s). Contents of the paper have not been
reviewed by the Society of Petroleum Engineers and are subject to correction by the author(s). The material does not necessarily reflect any position of the Society of Petroleum Engineers, its
officers, or members. Electronic reproduction, distribution, or storage of any part of this paper without the written consent of the Society of Petroleum Engineers is prohibited. Permission to
reproduce in print is restricted to an abstract of not more than 300 words; illustrations may not be copied. The abstract must contain conspicuous acknowledgment of SPE copyright.
Abstract
The success of chemical flooding rests heavily on the ability to deliver high-quality and repeatable surfactant in the field.
While high-quality surfactants can easily be produced at lab scale, high oil recovery can be achieved only if similar quality
product is produced at field scale. Scale-up of chemical production from batch-scale laboratory processes to field-scale
continuous production requires a comprehensive program to evaluate surfactants produced at the bench-, pilot-plant and
commercial scale to establish surfactant performance. Given the difference between batch-scale and continuous processes,
small differences in surfactant structure can result thereby inducing differences in phase behavior and consequently oil
recovery. Rigorous laboratory work is therefore required to synthesize and characterize surfactant samples in order to
understand the correlation between structures/composition and performance in oil recovery. Following laboratory synthesis,
pilot-plant studies are used to investigate process variables in order to understand their viability range and their impact on the
large-scale product. Other important concerns are: optimal operational conditions, process repeatability, supply chain
management, logistics, quality assurance/quality control, feedstock availability and dedicated procurement team. We present
a case study for a proposed light oil surfactant polymer flood where a rigorous path for scale-up of surfactants from lab to
pilot and finally field scale was evaluated via phase behavior experiments and coreflood testing. We show that phase
behavior results are well correlated with coreflood recovery. For EOR, they are superior performance criteria to traditional
specifications of physical and compositional properties for quality control. For the two-surfactant system presented herein,
272 surfactant samples, 512 formulations and 20 corefloods were conducted. The results from this large effort were utilized
to develop appropriate manufacturing and quality-control processes to ensure the delivery of high-performance surfactants
for field application.
Introduction
Many early Chemical-EOR field trials failed to produce desired results and poor performance was attributed to the failure of
chemical flooding technology. With hindsight, a contributing factor to poor performances was the failure to deliver to the
field the same quality surfactant that was used in laboratory testing. It is difficult to estimate how many field trials failed for
this reason as the problem was seldom discussed or even recognized in the literature despite its importance. Two field-test
results hinted at the problem of under-performing surfactants. At Bell Creek, the petroleum-sulfonate blends used in the pilot
contained far more polysulfonates than the products used in the laboratory design (Holm, 1982). Chromatographic separation
(Salter, 1986) clearly occurred in the field with unfortunate consequences. Highly water-soluble and fast-moving
polysulfonates broke through early causing severe emulsions in the produced fluids. The altered composition of the trailing
micellar slug probably contributed to sub-optimal performance at Bell Creek. In one of the pilots in Indonesia (Bou-Mikael
et al., 2000), post mortem analysis suggested that the synthetic sulfonate used in the field trial was not compositionally
identical to the laboratory product though it was not clear how much this difference affected pilot performance.
While many sub-surface uncertainties are uncontrollable, the quality of the commercial surfactants used in the field is within
our control. A comprehensive evaluation program and QA/QC criteria are needed to ensure that field surfactant meets
expected performance. To clearly understand changes in phase behavior due to compositional and molecular changes,
surfactants must be analyzed and their performance in corefloods must be evaluated at all stages of their production, from
laboratory synthesis to pilot-plant and finally commercial-plant manufacturing. The scale-up from batch synthesis in the
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Evaluation and Manufacturing Quality Control of Chemicals for Surfactant
Flooding
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laboratory to a continuous process in the pilot plant is particularly fraught with difficulties. Pilot-plant conditions must be
carefully evaluated to understand their impacts at each processing step (e.g. alkylation, and sulfonation for alkyl aryl
sulfonates). The variation in the feedstock and its availability can further complicate issues, especially at the commercial
scale. Finally, blending, transportation and storage of the final commercial product may impact surfactant performance as
well.
Background
A multi-year effort was devoted to develop a surfactant formulation for a light oil chemical flood pilot. This intensive
program includes surfactant and polymer screening, development and laboratory testing of high performance formulations for
the field pilot, and scale up of surfactant manufacturing from bench scale to the pilot-plant- and commercial scale.
From the surfactant screening program for the light oil pilot, a two-surfactant system (AAS, an alkyl aryl sulfonate and OS,
an olefin sulfonate, both manufactured by Chevron Oronite) emerges as the most promising formulation for the proposed
pilot (Zhao, 2008). The addition of a second surfactant (OS) offers significant advantages: 1) OS boosts the performance of
AAS, the single surfactant used in the first pilot; 2) a two-surfactant system adds flexibility in optimizing its EOR
performance with light oil crude; 3) a two-surfactant system allows small adjustments in the final commercial-scale blends to
compensate for possible variations in commercial quality of either surfactant.
Certain changes in the operating conditions at the pilot-plant or commercial-plant scale can have a large impact on the
product conversion (activity), isomeric distribution, byproducts, etc. These changes can significantly impact surfactant phase
behavior and coreflood performance as will be seen later. To define the optimal operating conditions in the plant, over two
hundred surfactants (batch and plant samples) and over five hundred formulations were painstakingly tested in phasebehavior experiments and twenty corefloods. This intensive program, which includes several pilot-plant and commercial
scale runs, was undertaken to ensure that commercial-scale surfactants can be made reproducibly and meet the specifications
and performance of the benchmark samples used in laboratory process design.
Materials and Methods
Phase behavior procedures were similar to those described by Levitt and Jackson, 2006. In a borosilicate glass pipette, two
ml of oil were mixed with 2 ml of surfactant solution in brine at different salinities. The pipettes were then sealed and placed
in an oven at reservoir temperature and allowed to mix and equilibrate. The oil-microemulsion and microemulsion-water
interfaces were recorded for use in calculating the solubilization ratios of oil and water. In all phase-behavior experiments,
the total surfactant concentration was 2 wt% and the ratio of the two surfactants was 3 to 1. The co-solvent concentration was
set at 3 wt%. The most promising formulations from the phase behavior experiments are further tested in core flood
experiments and their performance measured against a target oil recovery.
Briarhill sandstone was used as surrogate for reservoir rock as it had similar permeability and cation exchange capacity to the
reservoir rock. Cores were assembled and potted in epoxy with taps to measure differential pressure internally and across the
core. Cores were initially saturated with synthetic reservoir brine at reservoir. Following the brine flood the cores were
flooded with crude oil at a relatively high pressure gradient until a water cut of 2% or less was observed. The cores were
aged at reservoir temperature then water-flooded at a low pressure gradient (1 psi/ft) which translates to a flow rate of
approximately 1-5 ft/day. The effluent fluid samples and pressure drops were observed until there was no oil in the effluent
and the pressure drop across the core stabilized. Finally, the cores were flooded with the surfactant. The surfactant slugs used
in all the corefloods contained an AMPS co-polymer produced by SNF.
Surfactant Manufacturing and Scale-up
Developing commercially viable multi-component surfactant systems for an EOR field trial is challenging and requires a
logically staged process to meet the desired performance criteria. For the light oil project, the surfactant acceptance
workflow used for each stage is illustrated in Figure 1. This paper will cover each of the stages: (1) surfactant development,
(2) scale up of surfactant production, (3) formulation blending, and (4) on-site delivery and evaluation. Successful
completion of these stages can lead to a valuable EOR field trial that generates the data necessary to evaluate the long-term
viability of full field expansion.
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Physical properties and chemical composition are typically used in surfactant industry to ensure that product meets
specifications. Unfortunately, the phase behavior and physical properties of surfactants are sensitive to often small
compositional and isomeric variations (Salter, S.J., 1983), which are not easily quantified to the desired precision by routine
analyses. Phase behavior and core-floods provide the ultimate assurance of surfactant quality and performance. In this work,
we found that seemingly small, unsuspected changes in surfactant composition caused by variations in synthesis steps, plant
operating conditions and feedstock can lead to significant changes in surfactant performance in Chemical EOR. A
comprehensive program has been developed to ensure high and reproducible performance for the commercial surfactant.
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In addition to selecting the appropriate surfactant(s) for a specific reservoir, EOR performance criteria must be clearly
defined. The performance tests for this project were the commonly used techniques: phase behavior, corefloods, and
reservoir simulations. The surfactant formulation performance screening criteria at Stage 1 (Figure 1) were: optimal salinity
(S*), optimum solubilization ratio (SP), equilibration time into fluid middle phases, microemulsion viscosity and core flood
oil recovery.
With the desired surfactant chemistries and performance criteria defined, the next step is to prepare laboratory samples of the
surfactants using varying conditions to determine the performance sensitivity to surfactants with varying molecular
properties. This allows one to understand the relationship between surfactant structure and performance. Simultaneously the
raw materials, intermediates, and surfactants were characterized using standard analytical techniques and in some cases new
analytical methods. For choosing the raw materials used in surfactant synthesis, a procurement team is helpful to understand
the availability and quality of raw materials in the market place. Typical process conditions that are varied include reaction
temperatures, pressures, catalyst type and loading, raw material charge molar ratios, flow rates, and reactor type (e.g., fixed
bed, batch or continuous). In these studies, it is important to select process variables and ranges that make sense from a
commercial feasibility perspective even though this work is still at the laboratory synthesis stage. Working with
commercially unreasonable conditions and/or raw materials can lead to unattainable scale-up of the surfactant synthesis from
the laboratory to full plant scale manufacturing.
The molecular properties of all raw materials, intermediates, and surfactants were probed using the following analytical
techniques (Greay and Chan, 1990 and Varadaraj et. al. 1990): nuclear magnetic resonance spectroscopy, (Carbon and Proton
NMR), infrared (IR) and mass spectroscopy (MS), gas chromatography (GC), supercritical fluid chromatography (SFC) and
high performance liquid chromatography (HPLC). Molecular properties such as the chain length (Kadam, 2006) aromatic
ring isomers (Hsieh and Shah, 1977), aromatic ring size (Zhigang et.al. 2006), and alkyl chain attachment (Borchardt, 1987)
are known to affect interfacial surfactant properties such as surface tension, critical micelle concentration, surface adsorption,
and cloud point. Other surfactant properties that are important include pH, metals content, water content, molecular weight,
activity and physical properties such as viscosity, density, flashpoint, sediment, color, and appearance.
For each laboratory surfactant sample the analytical, molecular and physical properties were recorded along with the
corresponding performance. Included with the individual surfactant performance was performance testing results of
combinations of the primary surfactant, co-surfactant, and co-solvent at various treat rates. As illustrated in Figure 1, Stage 1
is an iterative process in which alky aryl sulfonate and olefin sulfonate samples were prepared, their analytical, physical, and
molecular properties measured and then their performance determined. The performance and analytical results are then
evaluated and changes in molecular properties are considered for additional surfactant syntheses. This process may take
several iterations until acceptable performance is achieved and a surfactant or formulation is deemed acceptable.
Once a sufficient amount of performance and analytical data has been generated, the performance results along with the
analytical data were statistically analyzed to derive structure performance information and identify and quantify the critical
surfactant properties that correlate to acceptable performance of the multi-component formulation. Using the results from
statistical analysis, additional laboratory samples were prepared using narrower process condition ranges to understand how
small changes in the critical surfactant properties affect performance. In addition, surfactant syntheses were repeated to
determine surfactant preparation repeatability. These results provided the basis for defining the acceptable ranges of
surfactant properties critical to acceptable performance.
Once a formulation, or set of formulations, has been identified, it is prudent to run storage stability studies to identify any
possible surfactant degradation upon storage. For this project, we ran separate storage stability studies for each component of
the formulation and the entire formulation itself. If any component or the whole formulation is not stable for at least several
months, it may not be suitable for storage and shipment to a reservoir for EOR and alternative formulations may need to be
developed. As the surfactant development progresses through Stage 1 and even into Stage 2, environmental compliance
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Stage 1: Surfactant Development
The first step in the development of a surfactant system for any reservoir is to determine the surfactant, co-solvent, and, if
necessary, co-surfactant chemistries necessary to achieve acceptable enhanced oil recovery performance. Historically, EOR
surfactant chemistries have included various alky aryl sulfonates, olefin sulfonates, and alcohol ether sulfates. The selection
of the appropriate chemistry depends on specific reservoir properties: temperature, pressure, oil properties, rock
characteristics, reservoir brine composition, etc. For the light oil project the primary surfactant chosen was an alkyl aryl
sulfonate (AAS). A co-surfactant olefin sulfonate (OS) was selected based on the use of olefin sulfonates with high wax
crude oils by Zhao et. al. (2008). Common co-solvent chemistries include alcohols and glycol ethers and for the light oil
project, the co-solvent chosen was based upon previous work for light oil reservoirs and high wax content crude oils by
Dwarakanath et. al. (2008).
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issues such as EPA registration, pre-manufacturing notification (PMN), and, if necessary, toxicological testing must be
addressed. It is of little value to develop a surfactant that cannot be used outside the laboratory.
Listed in Table 1 are various samples of AAS synthesized in the laboratory under selected conditions to explore the impact of
physical, compositional and molecular properties on performance. To compare their performance, various AAS samples were
systematically tested in formulations containing the same benchmark OS. Similarly, all new OS lab- and pilot-plant samples
were tested with the benchmark AAS. In all, 272 lab- and pilot-plant surfactant samples were tested in 512 different
formulations.
Figures 3 and 4 summarize the results of phase-behavior evaluations in which 91 AAS lab samples were tested with
benchmark OS surfactant. Only 5 formulations met both the optimal salinity and solubilization ratio requirements. The
physical, analytical and molecular properties of the AAS samples, especially those with good performances, are carefully
correlated to synthesis conditions and feedstock. Often minor changes in certain molecular components of the AAS led to
surprisingly large shifts in either S* or SP*, or both (Figure 4). This evaluation process led to the conclusion that the best
route to boost the performance of the formulation was to modify the properties of the OS.
Once a formulation, or set of formulations, is established, it is prudent to run storage stability studies to identify possible
sample degradation. If any part of the formulation, or the whole formulation, is not stable for months at a time, it may not be
suitable for storage and shipment to a field for EOR. Alternative formulations may need to be developed or the components
in the formulation may need to be stored separately until the time of the field trial.
Stage 2: Scale-up of Surfactant Production
In our experience, meeting the performance criteria during scale-up of the surfactant manufacturing process from the
laboratory to the plant is the most difficult stage of chemical surfactant development for EOR performance. Traditionally,
the next step following laboratory preparations is to use pilot plant facilities to prepare materials. Pilot plants must be
carefully chosen such that they provide process information that can be scaled to a full scale plant. For sulfonate chemistries,
Roberts describes the optimization of linear alkyl benzene sulfonation using falling film sulfonation reactors (Roberts, 2003)
and various sulfonation technologies for linear alkylbezene, primary alcohols, ethoxylated alcohols, and alpha olefins
(Roberts, 1998). These articles explain the complexities of these chemistries and outline guidelines to be successful in
scaling up sulfonation processes.
For the light oil project, statistically designed pilot plant studies were used to determine the impact of larger scale processing
conditions on the alkyl aryl sulfonate and olefin sulfonate surfactant molecular properties followed by performance testing.
Not uncommonly, pilot plant produced surfactants had different analytical properties compared to the laboratory prepared
materials which required additional pilot plant studies and further performance testing such that this stage is also an iterative
process as in Stage 1 and exemplifies why Stage 2 is the most difficult stage of an EOR project. A thorough discussion of the
results at Stage 2 is required to determine how best to proceed. If a decline in performance is unacceptable, one may need to
re-examine the entire pilot plant process. For example, there may be a need to examine pilot plant data to determine if any
operational upsets occurred, identify any key differences in raw materials used, and examine more closely samples from the
pilot plant. Some off-line processing of material may be required as well. Ultimately, additional pilot plant runs may be
required to generate acceptable performing material with altered process conditions.
Once acceptable pilot plant material is generated, additional storage stability studies were conducted to determine if there is
any degradation in performance upon storage under nominal storage conditions. Next, document and clearly define all
process conditions and product specifications with tolerance ranges. The conditions and specifications are then used in a
plant trial in a commercial facility.
For this project, small plant trials in commercial facilities were initially conducted to gain experience with process operations
and determine the range of surfactant properties that can be generated. Like the initial lab work, samples were analyzed and
performance tested using phase behavior. Figure 5 shows the poor performance of the initial pilot sample. These results
were used to enhance the performance of future plant trial materials. Figure 6 show a comparison of the initial pilot sample,
the improved pilot sample and the benchmark sample. All of these samples were also core flooded.
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Phase-Behavior Performance— The formulations developed for this project (AAS + OS + Co-Solvent) must meet or exceed
two main performance criteria: 1) The optimal salinity (S*) should be between 0.7-1.1 wt% of Na2CO3. 2) The optimum
solubilization parameter (SP*) should be greater than 8. These criteria applied to all laboratory (batch) samples, pilot-plant
and commercial-plant samples used in phase-behavior experiments. Figure 2 shows the phase behavior of AAS and OS
surfactant samples used as benchmark: 1) Optimal salinity, S* = 0.75 wt%. 2) Optimum solubilization parameter, SP= 9.
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Coreflood Performance—All corefloods used the following sequence of slugs:
•
•
•
0.15 PV surfactant slug at optimal salinity
0.10 PV of polymer chase (with 1.5 wt% co-solvent)
More than 1.0 PV of polymer chase in synthetic reservoir brine.
Once an acceptable pilot plant material was generated for the pilot, storage stability studies were conducted to monitor any
long term performance degradation. The next task was to document and clearly define all process conditions and product
specifications with tolerance ranges. The conditions and specifications are then used in a plant trial in a commercial facility.
Small plant trials in commercial facilities were initially conducted to gain experience with process operations and determine
the range of surfactant properties that can be generated. Like the pilot plant work, samples were analyzed and performance
tested. The results obtained were used to enhance the performance of future plant trial materials. Finally, storage stability
studies were conducted on the plant trial materials to monitor any long term product degradation. Figure 8 shows the phase
behavior of AAS and OS surfactant 2009 Plant Trial samples which were stored at 40°C for 115 days. The S* is about 1.10
wt% of Na2CO3 and the optimum solubilization parameter (SP) is greater than 8. Both of these results meet the requirement
for acceptable behavior.
Stage 3: Formulation Blending
Stage 3 of the surfactant development flow sheet involves blending the primary surfactant, co-surfactant, and co-solvent to
produce the EOR formulation. Before shipment of the final blend to the reservoir, surfactant samples are blended in the
laboratory and performance tested. During the performance the treat rates of each surfactant can be varied to determine the
optimal blend. As illustrated in Stage 3 of Figure 1, this process is iterative and may require discussions if the final
formulation performance is less than satisfactory. Once a final formulation is agreed upon, a large scale blend is conducted
and the material is ready for delivery to the reservoir.
Stage 4: Delivery and On-Site Evaluation
The final step of the surfactant development flow sheet is to transport the surfactant formulation from a blending facility to
the reservoir. It is imperative that one work with a supply chain and logistics team to ensure product integrity. A partial list
of issues includes: mode of transport, type of containers, cross contamination, reliability of shipping companies, best shipping
routes, environmental concerns, customs issues, and ultimately the capability of the reservoir facilities to receive, handle,
sample, and weigh material. For this pilot, we have minimized many of these issues by shipping the blended formulation in
sealed ISO containers and selected a reliable and safe delivery route to avoid any timing disruptions. Once on-site there will
be some analysis and performance testing of each ISO container prior to injection to assure product integrity. As illustrated
in Stage 4 of Figure 1, depending on these test results a decision may need to be made about whether or not to accept certain
ISO containers or the entire shipment. These decisions are critical as they ultimately impact the quality of the EOR field trial
results.
Full Field Expansion
If the light oil pilot is successful, manufacturing sufficient materials for a full field expansion is non-trivial. For the current
formulation, there are insufficient raw materials currently available in the global market place to produce the amount of
surfactant required for full field implementation. Dedicated commercial facilities would likely need to be built to supply the
current formulation to the reservoir. However, modifications to surfactant chemistry, treat rates, and new and improved EOR
technologies may make full field expansion more attainable. Research in this area is currently in progress.
Conclusions
Too often in the past, chemical EOR was deployed in field trials based entirely on the laboratory performance of surfactants
often synthesized in small batches in the laboratory. Even today, some field trials still use surfactants whose “full
commerciality” remains to be demonstrated. This work showed that:
•
Small compositional or molecular changes that are difficult to quantify via usual chemical or instrumental analyses
can often lead to large performance differences.
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The pressure drop in the experiments was kept below 1 psi/ft at a rate of 1 ft/day. Figure 7 shows oil recovery for three
corefloods corresponding to the benchmark formulation, the formulation using initial pilot-plant samples of AAS and OS and
the final formulation using improved pilot-plant samples of these surfactants. Coreflood results are also summarized in Table
2. As expected, the improved formulation with good phase behavior also performed better in coreflood. These results
indicate excellent correlation between phase behavior results and coreflood recovery. They also further illustrate the
importance of phase behavior testing and establishment of such benchmarks for surfactant performance.
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SPE 129892
•
•
•
•
•
•
•
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•
Phase-behavior performance (minimally S* and SP*) and corefloods are the most sensitive and thus the most
reliable criteria for surfactant performance in the field.
A two-surfactant formulation gives the flexibility to optimize the performance with adjustment for one of the
products in the blend. This flexibility is very useful at the commercial scale where sub-par performance of
individual component can be expected.
To ensure delivery of high-performance and repeatable surfactant product in the field, a comprehensive, timeconsuming but necessary program for commercial surfactant manufacturing must be developed
One must establish surfactant performance criteria which are germane to field performance; traditional physical and
chemical specifications alone are not sufficient to ensure expected performance.
Important synthesis variables at the small-batch scale in the lab must be understood and correlated to physical
analytical and molecular properties of the final product.
Pilot plants must be used at key manufacturing steps of surfactants and a viable range of process variables should be
explored to understand their impact on surfactant properties and performance.
Blending, transportation, logistics for field delivery and storage must be carefully evaluated and a detailed QA/QC
plan developed ahead of time to ensure that the field surfactant-blend performs as well as the small-scale product
used in design.
Full-field expansion requires raw-material quantities that may even exceed the global market capacity. The
availability of feedstock required must be evaluated before field trial.
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# Samples
S*
SP*
Oil Recovery
Soc
Table2. Coreflood Summary
Benchmark
2009
0.7
1.0
9
8
96%
92%
1.5%±2%
3.3%±2%
Comments
Lab samples
Lab samples
Large-scale lab samples
Field batch
Lab batches
2008
1.3
5.5
71%
10.6%±2%
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15
27
5
1
91
Table1. Summary of AAS Laboratory Syntheses
Analytical criteria met
Phase Behavior Criteria
Met
1
3
5
4
1
0
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Figure 1: Surfactant Acceptance Workflow
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Figure 3: Comparison of Optimal Salinity for Benchmark and 91AAS Laboratory samples
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Figure 2: Phase Behavior of Benchmark Sample: S* ~ 0.75 wt%; SP* > 8
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Figure 5: Example of Initial Pilot-Plant Sample with Unacceptable S* (>> 0.75%) and SP* (< 8)
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Figure 4: Comparison of Solubilization Ratio for Benchmark and 91 CS 2000 Laboratory samples
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Figure 7: Comparison of Cumulative Oil Recovery Initial, Improved Pilot-Plant Samples vs. Benchmark Samples
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Figure 6: Comparison of Phase Behavior of Initial, Improved Pilot-Plants Samples with Benchmark Samples,
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Figure 8: Storage Stability of 2009 Plant Trial Sample
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