OTC-29683-MS

Improved Protocol for Scale Inhibitor Evaluation: A Meaningful Step on

Scale Management

Katia Regina Silva Alves da Rosa, Rosane Alves Fontes, Francisca Ferreira do Rosário, Tiago Cavalvante Freitas,
Mônica de Oliveira Penna, Bruno Barbosa Castro, Mário Germino Ferreira da Silva, Giselle Maria Lopes Leite da
Silva, Jussara Mello Silva, and Mariana Rocha Figueiredo, Petróleo Brasileiro S. A. – PETROBRAS

Copyright 2019, Offshore Technology Conference

This paper was prepared for presentation at the Offshore Technology Conference Brasil held in Rio de Janeiro, Brazil, 29–31 October 2019.

This paper was selected for presentation by an OTC program committee following review of information contained in an abstract submitted by the author(s). Contents of
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Abstract
Scale occurrence can cause oil and gas production loss with high economic impacts. Currently, the use
of chemicals is one of the key strategies for scale management. A laboratory tests protocol is essential to
qualify and guarantee chemical effectiveness in the field. The objective of this work is to present a protocol
that includes improvements in the procedures to evaluate scale inhibitors and allows wide application to
several production scenarios. The protocol is an improvement based on published international technical
standards and the literature. These adjustments of the experimental procedures enabled the representation
of a wide range of scaling scenarios from reservoir to topside facilities. An efficient application of
scale inhibitor includes the definition of the ionic composition of aqueous fluids as well as the pressure
and temperature conditions of the target scenario. To perform the laboratory tests, synthetic waters are
prepared to represent the water production scenario, including pH. The tests are performed using synthetic
produced water, including evaluation of fluids compatibility (one or two phase experiment), thermal stability
and static and dynamic performance (DSL-dynamic scale loop). The proposed test protocol allows the
qualification of scale inhibitors to the production scenario considered, reducing the associated uncertainties
of upscaling from laboratory to field. The availability of the company's protocols makes it possible
to achieve greater accuracy in the recommendation of commercial scale inhibitors, allowing a better
cost-benefit with the optimization of the effective minimum concentrations. In addition, this availability
encourages the development of new generation inhibitors for challenging scenarios with high scaling
potential. The improved protocol is designed to represent critical salt precipitation scenarios, similar to those
found in the Brazilian Pre-salt (high salinity, high temperature, high saturation ratio, high CO2 content), and
has been successfully applied in the screening and qualification of scale inhibitors.

Introduction
Generally carbonate and sulfate scale, formed under natural depletion or water injection support, can occur
in the production system from the reservoir to the topside facilities impacting on well productivity. Scale
control has become a challenging task as the oil industry tends to go for deeper water with complex
2 OTC-29683-MS

completion wells which may produce from harsh environmental conditions (high salinity, high temperature,
high saturation ratio, high CO2 content). Scale management has become a power tool to assure that the oil
loss due to precipitation along the oil production process is avoided and costs associated to its prevention
and remediation treatments are minimized (1).
The most important factor for the success of this approach is that flow assurance strategies are considered
in the field planning as the appropriate technology to be adopted. The most practical and economical method
to prevent the scale problem is to use chemical scale inhibitors. Scale inhibitors prevent deposition of
inorganic or organic material and the formation of scale. These chemicals act on the thermodynamic stability
of the nuclei maturation, causing the dissolution of nucleated precipitates and/or interfering in the crystal
increase process, resulting in the blockage of the growth sites (2, 3).
The appropriate laboratory procedures for the determination of scale inhibitor performance will define
a successful scale management. Inhibitor performance in terms of the minimum inhibitor concentration
(MIC) or the threshold concentration required to prevent scale is one of the most important aspects for
scale efectiviness control. Another aspect that must be considered is the available facilities for the adequate
placement of the inhibitors.
Scale prevention must be carried out in function of the potential assessment, seeking the application
of technological solutions more appropriate to the production scenarios evaluated. The alternative of
bottomhole chemical injection requires the application of injection systems capable of ensuring the
continuous and controlled dosing of chemical products like scale inhibitors. (4)
Oscillatory behavior can take place in an injection system due to natural fluctuations of the production
tubing pressure. The effects of such variations may be important on the system capability to deliver a fairly
constant flow rate at the productions stream, leading to inappropriate chemical dosage. Column separation
may increase flow rate variations amplitudes, especially at low frequencies, as in scale inhibitor case. (4)
The laboratory test protocols must adopt by the oil and gas industry are very quite similar and are based
upon static “bulk” inhibition performance tests and dynamic inhibitor performance tests (DSL-dynamic
scale loop or tube blocking)(5).
However, methods that are more agile have been developed to assess and investigate the circumstances
that result in scale formation, as well as to evaluate the efficiency of formulations inhibiting this process.
Techniques that take in count the surface (heterogeneous nucleation), can be applied to assess and investigate
the scale formation and to evaluate the efficiency of formulations to inhibiting them (6 - 11). Among them are
particularly promising methods that use Quartz Crystal Microbalance (QCM).
The methods like the QCM can been used to scale potential evaluation or to inhibitors performance,
by measuring particulates deposition, such as calcium carbonate, onto the microbalance sensor with high
accurance sensitivity. The immediate and sensitive response of QCM to the formation of deposits on its
metallic surface enables monitoring the scaling process from its initial stage (nucleation) until the growth
phase on a surface (12, 13).
Thus, the technique of QCM is an alternative for the development of methods that takes in count the
heterogenic nucleation, besides promoted a response faster compared with usual inhibitor performance
methods. However, the QCM technique has some limitations. One of these is about the application
temperature, because, normally is up to 70°C, but it depends on equipment, sensor and fluid(12).
The quartz crystal transducer is a wafer coated with a metal such as gold. A high frequency current is
applied. A frequency shift occurs as precipitation on the quartz crystal wafer and growth happens. The
microbalance can measure precipitation with nanogram sensitivity. The quartz wafer can be used to model
a clean system, or it can be prepared with a deposit of the scale under study to provide a measurement
of growth on an existing substrate. The profile versus time can be evaluated using graphical or statistical
techniques to determine the time where control loss occurred (12).
OTC-29683-MS 3

Scale testing under high surface shear flow conditions, and selection of effective inhibitors, is of
increasing importance in oilfield production. It has long been recognised that the force generated by the
movement of fluid across a metal surface, the wall shear stress, is a key parameter in determining the
performance of chemical inhibitors in an oilfield production system. It is also known that deposits of
inorganic scale are commonly found in areas experiencing high shear stress and turbulence such as flow
restrictions, valves and submersible pumps(14).
Therefore, understanding how scaling processes are affected by elevated shear conditions and having
appropriate laboratory techniques to evaluate inhibitor performance under these conditions is of critical
importance. This is particularly the case as the use of inflow control devices (ICDs) and inflow control valves
(ICVs) in well completions becomes more common. Elevated shear stress and turbulence influence scale
nucleation, surface growth and adhesion processes and so the development and understanding of suitable
methods allowing testing under more field representative flow regimes is vital. Although there is increasing
recognition of these issues, there have until recently been limited reports regarding the development of
test methodologies for the assessment of scale formation under high shear, turbulent flow conditions. Most
of these methods focus on comparing laminar and turbulent flow regimes, and provide good evidence for
the increased risk of scale formation under turbulent flow, but do not achieve the very high shear stresses
experienced in real field situations. Reported approaches include stirring, rotating cylinder methods, and
modified dynamic tube-blocking apparatus. More recently, alternative techniques have been reported in the
literature and used to advance the understanding of scaling under more field representative, high shear and
turbulent environments. Jet Impingement (JI) is an alternative technique that is more suitable for simulating
pipeline flow under moderate to high shear conditions in the laboratory. It involves a high velocity jet of
fluid from a small-bore nozzle being directed at a flat metal coupon. Its advantages include the fact that
shear stresses across the coupon surface as the fluid flows radially outwards can be readily calculated, and
that different coupon materials can be examined. The shear stress generated can be easily controlled by
altering the nozzle diameter and/or the flow rate, and it is possible to achieve very high values that are
representative of those expected in the field, which other techniques are unable to reach (14).
Despite the importance of hydrodynamic representation in laboratory tests for scale inhibitors, this
technique (JI) is still not widespread. The present work proposes an improvement test protocol for
evaluation of scale inhibitors. Based on conventional methodologies, aiming at a better representation of the
production scenarios, including high scenarios (HT, HP, HS) like pre-salt Brazilian Pre-salt oilfields. This
protocol emphasizes the importance on the mimic synthetic brine preparation in the laboratory, chemical
compatibility and inhibition efficiency (static and dynamic performance test).

Protocol for Scale Inhibitor Evaluation

Preparation of synthetic waters
To perform laboratory tests it is necessary to prepare synthetic water compositions with similar to the
produced waters defined for each scenario to be evaluated.
In the preparation of the water(s) to be used it should be taken into account that, if it has potential for
scale, precipitation may occur prior to the tests, impairing the correct evaluation of the inhibitors. Therefore,
it is recommended to prepare two synthetic brines (cation brine and anion brine), keeping similar salinity
and pH.
The cationic and anionic solutions used in the study must be pre-filtered with 0.45 μm cellulose acetate
membrane.
In order to reach the target pH value in the synthetic brine, the pH of the cation brine should be adjusted
with HCl, or NaOH solution. The anion brine pH should be adjust with gaseous CO2, if necessary, to reach
specified pH value after mixing with cation brine. The tolerance of ± 0,3 é aceptable.
4 OTC-29683-MS

The increase/decrease of the pH value is associated to an increase/decrease of the CO32- ion concentrations
in the brine phase, and it has a strong effect on the CaCO3 scale formation. Even if the solubility of the
CaCO3 in the brine phase would be independent of the pH value, some CaCO3 can be generated in the brine
phase (due to an increase of the CO32- concentrations at higher pH values). Thus, the driving force for a
CaCO3 precipitation from the brine can become extremely strong (15).

Compatibility Test
“Considering the diversity of flow assurance issues that is likely to be managed during the development of
the Brazilian Pre-salt areas, one of the challenges highlighted: chemical product compatibility. A feasible
tactic to combat all the flow assurance problems is subsea injection of chemical addictives. Dedicated
umbilical lines and topside facilities for each chemical can be very expensive, or technically unfeasible,
depending on the well completion and pipeline layout. Besides, there are uncertainties regarding the
prediction of the flow assurance problems, which can lead to an unexpected requirement for a specific
chemical. Combo products, which combine one or more chemical functionalities, have been sought as a
reasonable solution to reduce the number of injection lines or manage with an underestimated injection
system. Chemical compatibility is not an issue restricted to combo injection, but it is essential for any
sort of simultaneous injection. The effectiveness of a particular chemical a ddictive can be affected by the
presence of an incompatible chemical injected simultaneously through a separated umbilical. Compatibility
evaluation has been performed as an approval test to certificate the chemical addictives to be used in the
Brazilian Pre-salt areas” (16).
The behavior of the inhibitor compatibility in the presence of synthetic water (brine) should be evaluated,
considering the inhibitor reactions with calcium ion on a representative pH. In this assay a turbidity or
precipitation formation is assessed visually and/or with the aid of a turbidimeter when the inhibitor is added
to the representative brine of the study. Additionally pH measurements and image recording is are made.
The anion brine has its precipitating ions (bicarbonate and sulfate) suppressed from the composition and
replaced with NaCl in the chemical compatibility tests. So, the brine will have similar ionic strength in
comparison with the original produced water.
The cation brine and anion brine should have pH adjusted. So the final pH reaches the specified value
in the reported composition, with a tolerance of ± 0.3.
Note 1 - The ionic strength of a solution as a function of the total ion concentration is given by:

At where:
I = ionic strength;
c = concentration;
z = ion charge.
Therefore, for the ionic strength to remain the same, divalent anions must be replaced by the quadruple
of monovalent anion moles. That is, 17.43 g of K2SO4 should be replaced with 17.53 g of NaCl.
In this test the scale inhibitor is added in different amounts to the anion brine. So that, the mixture with
cation brine will result final concentrations as indicated below:
– Surface facilities (Topside): 0 (blank), 10, 25, 50, 100, 250, 500, 1,000, 2,000 and 5,000 mg / L.
– Subsurface facilities (Subsea): 0 (blank), 100, 250, 500, 1,000, 2,500, 5,000, 10,000, 20,000, 50,000,
100,000, 200,000 and 300,000 mg / L.
Immediately after the mixing of synthetic waters, pH, turbidity, should be measured as well as the
appearance of the solution (clear, cloudy or precipitate).
OTC-29683-MS 5

The measurements are performed as quickly as possible, the solutions are returned to the oven, and the
test will continue to be runned. Additional measurements will at 1, 2 and 24 hours, after initial mixing will
be performed.
The scale inhibitor is considered compatible when the solution remains clear (NTU ≤ 10). The presence
of turbidity and / or precipitation indicates scale inhibitor maximum dosage limitation.
Procedure for temperatures above 90 °C. Due to high temperature, the cation and anion brines must be
conditioned at a temperature of 90 °C prior to mixing. The flasks are then returned to the heater for heating
to the test temperature.
During the test, immediately (90 °C) and after 1, 2 and 24 hours of initial mixing, the image is recorded
and visually classified based on the appearance of the solution (clear, cloudy or precipitate).
The scale inhibitor is considered compatible when the solution remains clear. The presence of turbidity
and / or precipitation indicates scale inhibitor maximum dosage limitation.
Procedure for squeeze treatment application. The inhibitor is added in different volumes to a 2% KCl
solution (mass/volume), prepared with purified water Milliq®, in order to give final concentrations of
100,000 and 200,000 ppmv of inhibitor. These two solutions are called 10% v / v inhibitor solution and
20% v/v inhibitor solution.
Compatibility tests consist of mixing each of the inhibitor solutions with synthetic water without the
precipitating anions (bicarbonate and sulfate) in different ratios (scale inhibitor: synthetic water): 10:90,
50:50 and 90:10.
Additionally, the test should be repeated with synthetic water without precipitating anions (bicarbonate
and sulfate) added with calcium up to 20,000 mg / L.
The test result will be based on visual evaluation and image recording. The turbidity and pH
measurements will not be performed.
Scale Inhibitor and other injected chemicals. Due to the injection of other chemicals (H2S scavenger,
corrosion inhibitors, demulsifiers, hydrate inhibitors, biocides, paraffin inhibitors, etc.) into the production
system a possible interaction/incompatibility between these chemicals and the scale inhibitor must be
investigated.
Scale Inhibitor × Chemical. In this test, chemicals are mixed in different ratios (90:10, 50:50 and 10:90
v/v). After mixing, observations are made in relation to the visual aspect, in order to verify possible
incompatibilities (formation of precipitates or turbidity of the solution) or miscibility between them at pre-
defined temperatures. The observation time adopted, in most cases, are immediate mixing, and after 1, 2
and 24 hours. The temperature simulates the condition at the chemicals injection points.
The Figure 1 shows examples of different results of compatibility between scale inhibitor and ethanol
during the compatibility test. In this example, scale inhibitor A is total compatible and the scale inhibitor
B forms precipitation.
6 OTC-29683-MS

Figure 1—Compatibility between scale inhibitor and ethanol during the compatibility
test, scale inhibitor A is total compatible and the scale inhibitor B forms precipitation.

Scale Inhibitor × Chemical × Synthetic Water. In this test, the inhibitor is added in different amounts
to the anion brine. The inhibitor and cation brine mixture define the final concentrations similar to the
concentrations at the dosage point (Topside or Subsea).
To the synthetic water, also, the other chemical under test is added. In general, its content is already
known. A blank test is performed, that is, without addition of inhibitor.
Immediately after the mixing of synthetic waters, pH, turbidity, image registration and visually
classifying the appearance of the solution (clear, cloudy or precipitate) should be measured.
The measurements must be done as quickly as possible. After the test sample must be returned to the oven.
The measurements are repeated for 1, 2 and 24 hours test, after initial mixing. The temperature simulates
the condition at the chemicals injection points
An example of compatibility between scale inhibitor and brine additived with H2S scavenger during the
compatibility test, it is showed in the Figure 2.
OTC-29683-MS 7

Figure 2—Compatibility between scale inhibitor and brine additived with H2S scavenger during the compatibility test.

Note 1 – If the test temperature is above 90 °C, the test shall be monitored by visual inspection (clear,
cloudy or precipitate) and image recording.
Note 2 – Chemicals, water based, should be dosed into the water of anions prior to mixing with the water
of cations.
Note 3 - If the chemical is in organic solvent, the compatibility tests are conducted in a biphasic system
containing 80% synthetic water and 20% oil. Typically, the oil used is oil representative of the field under
study.

Static Efficiency Test

The static efficiency test is used in the evaluation of chemicals aiming determination of inhibition efficiency,
specifically to avoid sulfate salts (generally BaSO4 and SrSO4) precipitation.
In this methodology, based on NACE Standards (17, 18), the synthetic waters (cation and anion brines) are
preheated and then mixed. The tests are conducted in the absence (blank test) and presence of the scale
inhibitor at the temperature of interest for the predetermined time of 1h and 24h.
The monitoring of the test is carried out by evaluating the concentration of the precipitating cations (Ba2+
and Sr2+) remaining in solution. To do this, the following procedure is performed:
– The vial containing the solution resulting from the test is removed from the oven and a small aliquot
(~ 1 ml) of the sample is withdrawn from the resulting solution without homogenization with a
disposable syringe (without a needle), thus avoiding collection of possible supernatant precipitates.
– A filter of 0.45 μm is used to filter the sample collected in a collection bottle.
– At room temperature, an aliquot of this sample, collected and filtered, is diluted in acidified distilled
water. Considering the appropriate dilution factor, the concentration of the precipitating cation
(Ba2+ and/or Sr2+) in solution is determined by the Inductively Coupled Plasma Optical Emission
Spectrometry (ICP-OES) analytical technique.
This assay is carried out in triplicate and the mean values obtained in the determination of the cations
(Ba2+ and/or Sr2+) remaining in solution allow the calculation of the efficiency percentage of the inhibitor.
8 OTC-29683-MS

At where:
Ca = concentration (mg.L-1) of the cation in solution after the test in question (with inhibitor);
Cb = concentration (mg.L-1) of the cation in solution in the blank (without inhibitor);
Co = concentration (mg.L-1) of the resulting cation in synthetic water.
The scale inhibitor is considered efficient when it achieves at least 90% efficiency in the 1-hour test. As
an example, the results are expressed graphically according to Figure 3.

Figure 3—Static efficiency test to evaluate scale inhibitor in differents concentrations.

Dynamic Efficient Test

The dynamic efficiency test, based on NACE 31105 (19), is used in the evaluation of chemicals aiming
inhibition efficiency determination, mainly in relation to the precipitation of calcium carbonate salts
(CaCO3), but due to the temperature limitation in the static test, this procedure is also used for the evaluation
of the inhibition of the deposition of sulfate salts (BaSO4 and SrSO4) at temperatures above 90°C.
The equipment (Figure 4) used to evaluate a dynamic scale inhibitor is called DSL (Dynamic Scale Loop)
or TBT (Tube Blocking Test) (20-22).

Figure 4—Schematic of dynamic tube blocking equipment (TBT) (22).

OTC-29683-MS 9

This equipment is basically composed of two HPLC pumps capable of pumping synthetic waters (cation
and anion brines), as described above, at the set pressures. The fluids will pass through streamers where they
will be heated and finally mixed before passing through the capillary. The pressure differential between the
inlet and the capillary outlet is monitored and recorded. A noticeable increase in the pressure differential
after reaching the steady state indicates the precipitation and the consequent end of the test.
In order to standardize the tests, the following parameters were pre-defined: total flow = 10mL/min;
capillary length = 1 meter; internal diameter of the capillary = 0.5 mm; and blank end-of-test pressure
differential = 4 psi.
Note 4 – These parameters can be changed by the customer, who must define them in the information
of the qualification scenario.
Before starting the tests it is important to condition the equipment. For this it is necessary to pump distilled
water in the same one generating a base line for the experiment. With the water being pumped the pressure
and the temperature of the fluid must be adjusted until they are stabilized.
A blank test (synthetic water without addition of any product) should be performed prior to the start of
the inhibitor tests. The time taken for it to generate the end-of-test pressure differential must be monitored.
It is recommended to carry out at least two blank tests, and these should not present a time difference greater
than 10% (in relation to time) to each other.
The pH of the synthetic cation water should be adjusted with HCl or NaOH and the pH of the synthetic
anion water should be adjusted with the use of gaseous CO2 so that after mixing the pH reaches the specified
value in the reported composition.
The scale inhibitor should be applied to the synthetic water containing the precipitating anions.
For an inhibitor concentration to be approved, it must prevent the pressure differential from reaching 0.5
psi from the baseline. The test time is at least three times the blank or for one hour, whichever is greater.
As an example, the results are expressed graphically according to Figure 5.

Figure 5—Dynamic efficiency test to evaluate scale inhibitor in differents concentrations.

The capillary should undergo a cleaning procedure immediately after each test, even if precipitation is
not noticed in the previous test. This procedure aims to remove remnants of the previously used inhibitor
and precipitates which, while not causing capillary obstruction may be precipitation kinetics enhancers for
subsequent testing.
10 OTC-29683-MS

This cleaning can be carried out with acids (in case of precipitation of carbonates) or alkaline (in case
of precipitation of BaSO4/SrSO4) followed by distilled water, in order to guarantee the total withdrawal of
cleaning fluids from the system.
Note 5 – The presence of other chemicals such as H2S scavenger may alter the performance of the scale
inhibitor. If desired, the efficiency of the scale inhibitor should also be determined in the presence of these
chemicals.

Final Remarks
The availability of the company's protocols makes it possible to achieve greater accuracy in the
recommendation of commercial scale inhibitors, allowing a better cost-benefit. Therefore, to obtain
consistent results from different laboratories, the testing procedures used must be agreeded upon and adheret
to.
The recommendations based on these laboratory protocols have been applied to assure that the oil loss
due to precipitation along the oil production process is avoided and costs associated to its prevention and
remediation treatments are minimized.
The procedures must mimic field conditions as close as possible in order to derive both a true ranking
and determine appropriate MIC values. There are already studies in the literature that cite the definition of
MIC under conditions closer to field reality, such as studies in the presence of solids of different chemical
natures, or even in different hydrodynamics. However, a general procedure is being shared in this work
that contemplates critical scenarios found in the Brazilian Pre-Salt (high salinity, high temperature, high
saturation rate, high CO2 content).
Besides the appropriate MIC values an other important issue is the scale inhibitor compatibility either
with brine or with other chemicals applied simultaneously or in combination.
The improved protocol also encourages the technology solutions development new generation inhibitors
development for challenging scenarios with high scaling potential in cooperation with research institutions
and industry.

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