OTC-28714-MS

Cold Finger Benchmarking Study for Paraffin Inhibitor Selection

Yun Peng, Shell International Exploration and Production Inc.; Abhishek Golchha, Baker Hughes a GE Company;
George Broze, Shell International Exploration and Production Inc.

Copyright 2018, Offshore Technology Conference

This paper was prepared for presentation at the Offshore Technology Conference held in Houston, Texas, USA, 30 April–3 May 2018.

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Abstract
Selection of effective paraffin inhibitors is critical for managing wax deposition risks in existing assets and
for enabling potential CAPEX savings in new developments. Cold finger (CF) testing is a common method
used for screening paraffin inhibitors (PI), but there are various kinds of in-house-developed and commercial
CF equipment used throughout the industry. Additionally, there is no standard PI testing protocol. In some
cases, there are inconsistent results between laboratories when evaluating PI performance.
To better understand the root causes of PI testing discrepancies and investigate the impact of key
parameters on test results, a benchmarking study using both in-house and commercial CF equipment was
conducted. Additionally, Shell (the Company) and BHGE (the Vendor) conducted a detailed joint exercise
to understand and benchmark the commercial CF equipment used in both of their laboratories. Finally,
the laboratory results were compared against field performance through a case study for a Gulf of Mexico
operating asset.
PI performance was found to depend upon the particular oil as well as testing conditions, test procedures,
and equipment. Good agreement in PI performance was observed between the two laboratories using the
same testing conditions with the same CF equipment and equipment specifications, under similar procedures
for a given crude oil. In this study, it was observed that shear and CF roughness can play a significant role
on PI test results. Rougher CFs tend to make certain PIs less effective under low shear conditions. Hence,
a PI chosen based on a specific set of conditions, equipment, and procedures might appreciably differ in its
performance if any of the above parameters are changed. Therefore, selecting appropriate testing parameters
is important to identify and qualify an effective PI suitable for a specific field application.
This work makes it possible to improve standardization between laboratories and helps to better
understand the limitations, uncertainties, and suitability of CF tests for predicting PI performance in the
field. It also provides insights on how to design tests and equipment to better represent PI field performance.

Introduction
Paraffin inhibition is a widely-used technology for mitigating wax deposition. Selection of a PI becomes
critical to manage wax deposition risks in both mature assets and to enable potential CAPEX savings for
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new developments using competitive scope. Wax deposition, if not controlled well, can result in adverse
events associated with significant remediation and deferment costs.
Most PI selection in the industry is conducted using CF equipment. It is almost 30 years since the
Company developed this technology. Currently, it is the most commonly used testing method for PI
screening [1–4]. However, there are various in-house developed and commercial CF equipment used
throughout the industry. In addition, there is no industrial standard for PI testing. This can lead to different
PI performance evaluations and, in worst case scenarios, inappropriate CF testing conditions may result in
the mis-selection of a PI for specific field applications.
PI selection is critical for a successful field application. An example of the PI selection process is
illustrated in Figure 1. The Company has mixed experiences in PI selection and field applications in the
past. In some cases, qualitatively good alignment of PI performance between the laboratory and field
was observed. In some other cases, there was inconsistency in testing results between the Company and
multiple chemical suppliers’ laboratories. In addition, there is a lack of validation data available to verify PI
performance in the field due to unreliable surveillance methods or missing baseline data (i.e., without PI).
There are examples of PIs deployed for a specific application without a good way to confirm that the PI is
effective; thus, a system is operated "blind". Therefore, the confidence in laboratory qualification methods
needs to be improved. At the same time, operators are continuously seeking more cost-effective PI solutions
(e.g., optimizing dosages, more cost-effective chemistries). This also requires a good understanding of PI
performance scale up from the laboratory to the field, as well as reliable surveillance methods for validation.

Figure 1—PI selection process flow chart

To address these technical gaps in PI testing and selection, the Company has recently conducted a CF
benchmarking study using different CF equipment with various oils and PIs. The Company also collaborated
with the Vendor to benchmark test results with the Vendor's commercial CF equipment made by the same
manufacturer.
The objectives of this work are to better understand effects of testing parameters on PI performance, root
causes of PI testing result discrepancies, and the limitations/validity of using CF for PI testing. For PI testing,
it is most important to apply appropriate parameters and to improve/standardize the PI selection protocol.
OTC-28714-MS 3

Testing Method and Equipment

CF tests are typically conducted at atmospheric pressure using a small volume of stock tank oil (STO) under
low shear conditions. CF can create a temperature differential as a driving force to form wax deposition.
The PI performance is determined based on how much wax (mass flux) is reduced with the PI compared
to the blank deposit(s).
The Company owns multiple in-house developed CF set-ups, each of which contains a single CF. The
overarching design is the result of a comprehensive investigation on CF equipment testing parameters
and repeatability conducted in 1998. Several modifications, including roughening the CF surface, were
made to reduce experimental uncertainties at that time. In recent years, multiple-position CF units have
gained popularity for PI screening tests, as they have the flexibility of testing multiple PIs or one PI at
different concentrations simultaneously by combining a group of CF units in one temperature control bath.
Therefore, tests are run more efficiently. Some commercial turnkey CF kits also have removable sleeves,
making deposition weight measurement much easier. To better understand the PI testing results between the
Company and the Vendor's laboratories, the Company conducted an extensive benchmarking study using a
commercial CF testing kit, which is also used by the Vendor and other chemical suppliers.
Due to the nature of CF design, CFs cannot fully simulate the flow regimes, shear conditions, and
temperature gradients of production flowlines. Appropriate testing conditions (e.g., temperature, shear, etc.)
are important to create representative wax deposits for selection of an effective PI for field applications.
Examples of typical testing conditions used in CF tests for PI selection by the Company are given in Table 1.

Table 1—The Company's CF PI Testing Condition Requirements

Other testing procedures, such as chemical rinsing to remove excess oil from deposits and analyzing
wax content of deposits, are also important to determine the PI effectiveness. After the CF test is complete,
deposit masses are determined. There are several methods to determine the deposit weights used by different
laboratories depending on the CF configuration and procedures, namely,
a. Tare the CFs and weigh the deposited CFs after tests (applicable for detachable CF)
b. Determine wax content by characterizing the deposits with high temperature gas chromatography
(HTGC, measuring concentrations of individual normal paraffins) (in-house & chemical suppliers)
c. Collect deposits by soaking deposited CFs in hot solvent, measure topped bulk deposit weights, and
determine wax amounts in deposits by interpreting deposits’ high temperature simulated distillation
(HTSD) analysis (measuring carbon number fractions) (in-house method)
d. Use clean paper towels to wipe off deposits and weigh the clean and used towel and determine the
deposit weight collected by the towel (chemical suppliers)
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e. Use a rubber tube to scrape deposits off the CF if CFs are smooth and measure deposit weight collected
by the tube (chemical suppliers)
The Company's safe operating procedures (SOP) for (c) is to (i) remove excess oil with cold methyl ethyl
ketone (MEK) rinses, (ii) remove deposit with hot solvent (i.e., toluene), (iii) evaporate the solvent and (iv)
analyze the topped deposit by HTSD to determine wax and oil masses separately. One of the objectives
of the shakedown tests of the commercial CF was to determine if a simpler method (a) could be used to
quantify the bulk deposit and determine inhibitor effectiveness. The commercial CF comes with removable
sleeves that can be weighed and tared to get deposit mass. Later, the uncertainties introduced by a simpler
method (a) have also been described, i.e., eliminating steps (ii) through (iv).

Findings and Discussion

Baseline Testing Benchmarking
The commercial CF equipment used in this study consists of multiple racks that can be used simultaneously.
It is important to understand the experimental uncertainties of baseline deposits (untreated) across
different racks and separate tests as PI effectiveness is determined by comparing treated ones to the baseline.
Repeated CF tests were conducted with three different oils (oils A and B are black oils and oil C is a
condensate) using the commercial CF equipment. Table 2 lists the experimental baseline errors of mass flux
(on both wax only and bulk deposit basis). The bulk deposit mass flux data exhibit up to ±30% uncertainty
which is mainly attributed to occluded oil content uncertainties. Whereas the "wax only" mass flux has
much lower uncertainty (~up to ±13%). This is similar to what is observed in the tests with the in-house
CF equipment.

Table 2—Commercial CF Blank Tests’ Uncertainty Range

It was also observed that procedures of post-processing deposits (e.g., drying time) are crucial in
controlling experimental errors in bulk deposit weights.
The procedures must demonstrate consistency between separate tests to achieve repeatable results. The
simpler method (a) measures bulk deposit weights and is useful for quick initial PI product screening, but
it causes higher uncertainties due to occluded oil content variation. HTSD or HTGC analysis is always
recommended to quantify wax amounts to reduce the uncertainties introduced by the occluded oil in bulk
deposits and therefore, generate a more accurate baseline for PI selection screening. If sample volume
allows, it is also preferred to run duplicates per chemical per dosage.
The Company's commercial CF is benchmarked against the Company's in-house CF as well as the
Vendor's commercial CF. All tests were conducted at the Company and Vendor's laboratories at the same
temperature conditions and test duration (16hrs) for a given oil but at specific stir rates determined for
each type of CF kit and testing oil. The Company uses HTSD analysis and HTGC analysis is used by the
OTC-28714-MS 5

Vendor to characterize deposits and determine the deposits’ wax content. The Vendor's HTGC analysis
counts only normal paraffins while the Company's HTSD analysis considers carbon number fractions up
to 108. The Company's commercial CF sleeves (15.5mm OD) are the newer design and rougher than the
Vendor's commercial CF sleeves (14mm OD). In addition, the in-house CF equipment uses sandblasted
probes (15.5mm OD), which are rougher than the commercial CF sleeves.
The wax mass flux data from these tests using the three CF kits are plotted in Figure 2. More wax is
deposited (≥ 30% in terms of mass flux as interpreted with HTSD data) with the in-house CF than the
commercial CF for all six oils tested. Qualitatively, there is good agreement between both laboratories using
the commercial CF equipment, though wax content is characterized using different methods. Although the
two methods yield different wax amounts for a given deposit, the PI effectiveness on a wax content basis
tested with both laboratories’ commercial CF is similar as demonstrated later in this article.

Figure 2—Comparison of baseline HTSD wax for six oils (Oils D, E and F are
discussed later) between the Company's in-house and commercial CF tests.

It is noticed that the commercial CF surface area towards the bottom (seen as the top in the image) is
always covered by very little deposits (up to ~15% of overall deposit height considered), as seen in Figure
3, which is not seen in the in-house CF tests. This is mainly due to the gap between the inner probe and
outer sleeve bottoms. The actual deposit area is thus ~15% less than the overall deposit height, as used in
the wax mass flux calculation. This can contribute to lower mass flux from the commercial CF as compared
to the in-house CF data. The wax mass flux offset caused by the gap may not be a concern for PI testing
which examines relative differences between the treated and untreated deposits if the gaps across different
CFs are the same and do not introduce additional experimental uncertainties.

Figure 3—Blank deposits from commercial CF test

After canceling out the ~15% less deposited area due to the gap, the remaining difference in deposition
rates between commercial and in-house CF may be attributed to other factors such as CF surface roughness,
testing bottle size, or actual CF surface temperature variation/fluctuation between the two different CF units.
The CN distribution profiles of deposits from commercial and in-house CF are slightly different, i.e., a little
6 OTC-28714-MS

bit shorter and broader with the in-house CF (an example of oil B's deposits is shown in Figure 4). This may
potentially be due to differences in geometric and/or heat transfer specifications of the two CF equipment,
which were also observed with some other oil samples that were tested.

Figure 4—Oil B deposits’ CN distribution profiles with the commercial and in-house CF tested by the Company

PI Testing benchmarking
The similarities/differences in the PI performance tested by the different laboratories were investigated. For
that purpose, both laboratories separately tested a commercial product, PI-X, for oil C (condensate). PI-X
is observed to be highly effective in both laboratories’ testing (~90% at 500ppm based on bulk deposit) on
the commercial equipment. However, the Company's test results using the in-house set-up exhibit slightly
less inhibition (79% wax basis, 76% bulk deposit basis) than the commercial equipment.
In addition, a subsea-qualified PI for oil B was in the process of being selected. The preliminary testing
with PI-X demonstrated good performance using the Company's commercial CF (90% inhibition on bulk
deposit basis).
However, when PI-X is reformulated to a subsea-qualified product (PI-Y) by the Vendor, very different
results were observed by both laboratories. The PI is not effective with the Company's commercial CF but
effective with the Vendor's commercial CF. After conducting "job shadowing" to align testing procedures
between the two laboratories, such as drying time and MEK rinsing procedures, plus further extensive joint-
exercises, we found that the testing result discrepancy is likely caused by the difference in the CF sleeve's
roughness. (The surface roughness in terms of Ra, arithmetical mean roughness value, as measured by a
profilometer is plotted in Figure 5).
OTC-28714-MS 7

Figure 5—Surface Roughness (Ra) Specifications of Different CF Kits

Figure 6 shows the testing performance comparison between the two laboratories with a given CF sleeve
type (either smooth or rough sleeve). Two deposit samples (untreated and treated) obtained from smooth
sleeves from the Vendor's test were also analyzed with the HTSD method and exhibited similar performance
(30%) as those based on HTSD analysis from the Company's test using the same sleeves (37%). On the other
hand, PI-Y tested by both laboratories does not perform (negative inhibition on both HTGC and HTSD wax
only basis) with rough sleeves. This also indicates that the test results can be reproduced by the laboratories
with the same test parameters/specifications/procedures.

Figure 6—PI-Y performance from the joint testing exercise

Additional dosage tests were conducted with both smooth and rough sleeves to study the roughness
effect. Figure 7 shows that PI-Y tested on the smooth sleeves at 500ppm and 1000ppm exhibits similar
performance as on the rough sleeves at 1500ppm and 3000ppm respectively. The PI exhibits different dosage
thresholds on two different sleeves, i.e., requiring higher dosages to perform with rough sleeves at equivalent
effectiveness level as on the smooth sleeves. It is also noted that the dosage at a given effectiveness increases
proportionally with the increase of roughness (rough sleeves are ~3 times as rough as the smooth sleeves
in terms of Ra). This correlation may also be subject to change under higher shears.
8 OTC-28714-MS

Figure 7—Roughness effect on PI-Y performance for oil B. Note wax inhibition% is determined with
deposits’ nC30+ HTGC data except that wax inhibition% for 1000ppm with smooth sleeve uses HTSD data

As mentioned earlier, there is a minor difference in the deposits’ CN distribution profiles between in-
house and commercial CF (with the rough sleeves). However, CN distribution profiles with rough and
smooth CF sleeves are the same, as shown in Figure 4. It was also observed that the treated deposits on
rough CF (both in-house and commercial) are much oilier than untreated ones whereas blank and treated
deposits with commercial smooth sleeves are both oilier (see Figure 8 where HTSD wax% in deposit= 1-
occluded oil% in deposit). This phenomenon is also subject to the occluded oil content uncertainties.

Figure 8—Wax content (characterized with HTSD) of deposits tested with different CF

We observed a similar phenomenon that PI becomes less effective on rougher surface when testing some
PIs with the in-house CF as well as on oils treated at relatively low dosages. One speculation for PI-Y
behaving differently on rough and smooth CF sleeves is how wax deposits grow on the CF surface plus the
likely competition of adhesion and cohesion forces with shears. This behavior is possibly dosage- and/or
chemistry-dependent and/or oil-specific.
Figure 9 shows that the treated CF deposits on smooth sleeves appear very patchy, indicating there
is a greater tendency of sloughing with smooth sleeves at certain dosages than rougher sleeves. It also
shows that at 2000ppm, the deposit just starts to exhibit a little bit sloughing with the rough sleeve,
indicating that the effect of roughness on PI effectiveness also depends on dosages. Such behavior gets
more pronounced under higher shears by increasing the stirring rates. However, the exact mechanism of
how surface roughness impacts PI effectiveness is not well understood. A further investigation into wax
crystal deposit structures, plus interactions between wax crystals and surfaces and between wax crystals
OTC-28714-MS 9

from the molecular perspective is needed for a better understanding of such behavior. Such studies will help
answer if the roughness affects the initial deposit build up only or the impact of roughness plays a role in
deposit build up with/without PI presence plus the effectiveness of a PI after thickness becomes larger than
the surface roughness of the pipe.

Figure 9—Deposits from PI-Y testing with smooth and rough CF sleeves

From a practical point of view, the surface roughness of pipe in production systems are orders of
magnitude higher (e.g., carbon steel's roughness ~45μm) than any of the tested CFs and the production
system may already have deposits when a PI is deployed. Therefore, it is very important to understand
the implications of roughness on PI performance, e.g., how the laboratory dosage threshold correlates to
field dosage thresholds for production with rougher pipe surfaces plus how shear, another key factor on PI
effectiveness affects the threshold.
By only looking at the wax inhibition %, tests with rough sleeves give more conservative results, i.e.,
PI-Y would not be selected/approved based on tests with rough sleeves but it may be considered from the
tests with smooth sleeves. Therefore, field validation is necessary to assess the validity of the CF testing
results. That requires reliable field data as a quantitative indicator of wax deposition with and without PI
application. Typically, field data used to quantify wax deposition includes pressure differentials across the
pipe or tubing, pigging frequency/wax return amount, intervention data (wax cutting history/frequency/
thickness measurement) and deposit profile measurement, etc. Other qualitative supporting data could be
topside monitoring of solids in Norman filters, on coupons, or in a test separator.

Field validation
To better understand how PI laboratory performance (relating to roughness impact) correlates to the field
performance, a current PI field application is benchmarked against laboratory test data. Wax deposition is
observed in the three Direct Vertical Access (DVA) wells (oil D, oil E, oil F) producing from the same field.
Continuous PI treatment (PI-C) is applied to manage wax issues and periodic wireline scraping is conducted
as needed. The three oils exhibit similar properties such as CP (103-106°F) and API gravity. However, PI-
C exhibits varying performance between the three wells. The temperatures at the injection points are above
the reservoir fluids’ CP.
The surveillance data of the three wells, such as tubing pressure differentials (dP) along with well
intervention histories, are summarized in the Table 3. There are two incidents of tubing dP increase caused
by injection system issues occurring in both well D and well E. These two events are used as baseline to
compare to the dP during continuous injection.
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Table 3—Field data summary of wells D, E, and F

Wax deposition is well controlled at well D with PI injected at ~1400ppm. The well is scraped every 2-3
years and 0.45-0.75" of wax is detected. The dP increases steadily over three years except for one incident
of injection downtime, which caused a rapid dP increase.
An improvement in reducing wax thickness/scraping frequency and tubing dP on well E when increasing
the dosage from 500-700ppm to ~1500ppm was observed as shown in Figure 10 and Table 3. The wireline
scraping tool detected wax buildup of ~0.875" over a year when injected at 500-700ppm compared to 0.5"
over three years when the PI is injected at dosages of ~1500ppm. The recent injection system issues caused
a rapid increase in dP. Once the system was restored, PI dosage was increased to ~1900ppm which seemed
to slough off some deposits and helped to reduce the dP as seen in Figure 10.

Figure 10—Plot of tubing ΔP trend, production data, and PI injection rates for well E

Well F is newer than the other two. An increase of tubing dP over six months was observed, as well as
various topside issues at well F with PI treatment at rates of 600-800ppm, e.g., ⅓ of the test separator (~12
bbls) was filled with paraffin during well ramping to a higher drawdown.
OTC-28714-MS 11

PI testing with both in-house and commercial CF (with rough sleeves) for all three oils was conducted.
The Company's standard dT (= Toil - Tcold) of 18°F is used for testing all three oils. The collected deposit
samples from wireline scraping and the topside flowline coupon are compared to CF deposits. There is a
good match of CN distribution profiles between the field deposits (via wireline scraping) and CF deposits
(as shown in Figure 11), indicating the choice of dT of 18°F represents the field conditions in this case.

Figure 11—Oil E CF and field deposits’ normalized CN distribution profiles

The testing results are shown in Table 4, where the following is observed:
– PI performance is oil-specific.
– PI-C is less effective on the in-house CF than the commercial CF for oil E as treated at 1000 and
1400ppm. Similar behavior is also observed for oil D treated at 1000ppm. This is likely due to the
roughness difference between the two CFs.
– PI-C is ineffective for oil F with both in-house and commercial CF at 1000ppm and oil F has higher
deposition rates (untreated) than the other two oils.
– Bulk deposit inhibition % is not necessarily the same/similar as wax inhibition % due to occluded
oil content variations.
12 OTC-28714-MS

Table 4—CF testing results for oils D, E, F with in-house and commercial CF equipment
OTC-28714-MS 13

Shear stresses in the field are usually several times or order of magnitude higher than CF. Shear may
improve performance and allow us to further reduce the field dosages. The goal is to get the most benefit
from a PI for de-risking and reduce OPEX of wax remediation and PI. Given the benchmarking results
between the laboratory and field (summarized in Table 5), operations is taking actions to adjust field dosages
accordingly, i.e., curtailing dosages at wells D and E and increasing dosages at well F plus conducting
detailed surveillance during PI optimization.

Table 5—CF laboratory vs field performance for oils D, E, F

Conclusions
In this work, benchmarking tests for several oils with different CF equipment were conducted. Both
laboratories reproduced PI testing results when using the same testing specifications and protocols. Use
of appropriate testing parameters and protocols for PI testing is critical for PI selection for a specific field
application. It is concluded that HTSD or HTGC analysis is important to reduce experimental uncertainty
due to occluded oil content variance and to accurately quantify PI effectiveness.
It was also found that CF surface roughness difference between different CF kits can cause discrepancy
in PI testing results, as performance of some PIs is sensitive to roughness and shear. As CFs are operated at
relatively low shears, appropriate CF roughness suitable for low shear CF tests is necessary to differentiate
PIs and better match PI field performance while ensuring repeatability. The field case benchmarking study
indicated that roughened CF can be more stringent when screening PIs. On the other hand, CF with very
low roughness (e.g., polished surface) may cause repeatability issues or give spurious high PI efficiencies.
Further field validation is needed to better understand and refine the appropriate roughness for PI tests.
CF may not be the best method to test the PIs having strong dependence on roughness and shear. To
better verify the shear impact on PI performance, other methods such as a high shear device [5–6] or flow
loop [7] can be used.
In general, CF evaluation of PI performance in the industry is recognized as qualitative. The laboratory
recommended dosage may not reflect the actual inhibition under field conditions. CF can be used for PI
screening/ranking rather than to quantitatively predict PI effectiveness in the field. The PI dosage is usually
optimized based on field experiences.
14 OTC-28714-MS

Acknowledgement
The authors would like to thank Gina Nall who conducted the experimental work, Dexter Benda, Neil Jarrett,
Miguel Araya, Norvel Taite, and Nicholas Garza, who provided field data and surveillance support, and
personnel from BHGE for testing work collaboration.

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