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APPENDIX B

Laboratory and Field Testing of


Candidate Chemical Treatments
Chemical Treatment Selection
The efficacy of a chemical treatment will depend on the particular field characteristics of the
system. Prior to field evaluations, candidate treatments are normally screened using
laboratory testing. Ultimately, laboratory testing alone cannot simulate actual operating
conditions. Thus, small scale field trials and monitoring are necessary prior to use of an
inhibitor in engineering operations.
Results of laboratory testing should also be used to identify compatibility issues. Specific
compatibility concerns include the interaction of the inhibitor with:
(1) materials within the system
(2) other oilfield chemicals
(3) health, safety and environmental considerations.

Laboratory Testing (ASTM G170, ASTM G184, and ASTM G185)


Prior to evaluating a candidate chemical treatment in the field, laboratory testing is used to
screen potential treatments such as corrosion inhibitors. Laboratory tests provide a simple,
compact, quick, and economical means to predict the behavior of a new candidate inhibitor
with respect to relevant field operations. The results of testing should predict the
performance of the treatment in terms of inhibitor efficiency and should be scalable (i.e.;
performed under various hydrodynamic conditions).
When conducting laboratory evaluations of corrosion inhibitors, it is imperative that the
system operating conditions and method of injection be defined as these parameters have a
significant influence a corrosion inhibitor’s performance. Parameters that must be defined
prior to testing include:
(1) materials
(2) hydrocarbon compositions
(3) gas compositions and partial pressures (CO2 and H2S)
(4) water/brine compositions and cut
(5) operating temperatures
(6) flow velocities
(7) inhibitor concentrations
(8) method of inhibitor injection (batch or continuous)
The efficiency of the corrosion inhibitor is generally expressed by a measure of the corrosion
rates in the un-inhibited system and after inhibitor injection. Calculation of the inhibitor
efficiency is determined using the following equation:
CR  CRinhibited
Inhibitor Efficiency (%)  100 Uninhibited [B.1]
CRuninhibited

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Where:
CRun-inhibited = corrosion rate of the un-inhibited system
CRinhibited = corrosion rate of the inhibited system

For a complete performance evaluation of a candidate inhibitor, laboratory tests should not
only assess the inhibitor efficiency but also:
(1) water/oil partitioning
(2) solubility
(3) emulsification on tendency
(4) foaming tendency
(5) thermal stability
(6) toxicity
(7) compatibility with other additives and materials.
In addition, the injection pump performance and other maintenance activities (e.g. pigging),
need to be taken into consideration for the performance evaluation.
As previously discussed, two main treatments are generally used for corrosion inhibitor
deployment. These treatments are batch treatments and continuous treatments (refer to
Section 3.2.1). When assessing batch inhibitors in the laboratory, specimens are dipped into
the inhibitor, rinsed with distilled water or a hydrocarbon solvent to remove excess product,
and placed in the corrosion test cell or autoclave. When assessing continuous inhibitors in
the laboratory, a preconditioning cell that contains the multiphase system (oil, gas, brine)
and appropriate concentration of inhibitor is used. This cell is maintained at simulated field
conditions and is continuously pumped into the corrosion test cell.
Several sophisticated laboratory tests are available to evaluate inhibitor performance. The
methodologies suggested in ASTM Standard G170 include:
(1) Rotating Cylinder Electrode (RCE)
(2) Rotating Cage (RC)
(3) Jet Impingement (JI).
In addition, bubble (kettle) tests and flow loop testing are also used to evaluate inhibitor
performance. Measurement techniques associated with each of these methodologies may
involve mass loss, electrochemical techniques, or both. It is important to note that no one
test will provide all relevant information. Rather, the methodology that best provides the
information in line with the goals of the evaluation should be selected. Each methodology is
introduced and described below.

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Rotating Cylinder Electrode (RCE)
The rotating cylinder electrode (RCE, ASTM G185) methodology allows for the measurement
of corrosion rates using both electrochemical methods, as well as mass loss. Experiments
using RCE are commonly performed in the turbulent-flow regime over a wide range of
Reynolds numbers. Hydrodynamic flow conditions using this methodology are well defined
and easily controlled. Additionally, only small amounts of solution (oil, brine, and inhibitor)
are necessary to perform the tests. Figure B.1 and B.2 show a schematic and a photograph
of the RCE system, respectively.
By increasing the electrode rotation speed, flow around the RCE can change from laminar
flow to unstable flow to a fully turbulent flow where eddies increasingly break up the regular
flow pattern. Within the fully turbulent flow regime, the RCE can be used to simulate flow
behavior by hydrodynamic analysis.
The RCE method does have some limitations which include:
(1) method is unable to account for erosive effects such as those due to the presence of
sand particles.
(2) if the electrode is not normal to all electrically isolating planes, the current and potential
distributions will not be uniform at the same time. Such non-uniformity makes
interpretation of results dependent upon application of fairly sophisticated
mathematical models.
(3) maintaining low-resistance electrical connection to the rotating electrode can be
difficult.
(4) rotating coupons require a bearing guided shaft to avoid wobble.

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1. Reference electrode
2. Gas inlet
3. Gas outlet
4. Luggin capillary
5. Platinum counter electrode
6. Rotating cylinder
8. Temperature probe
9. Water in from loop
10. pH-electrode
11. Working electrode

Figure B.1 Schematic of the RCE Setup

Figure B.2 RCE Setup

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Rotating cage (RC)
The rotating cage (RC, ASTM G184) methodology is widely used to evaluate corrosion
inhibitors under high turbulent conditions. This method simulates the worst-case scenario,
due to its extreme turbulent flow velocities especially at the grooves or gaps between
coupons. Localized corrosion rates are increased at the leading and trailing edge of the gaps
between coupons. Similar to the RCE method, the RC method is easy to conduct,
economical, and reproducible. Corrosion rates using this method are determined using
mass loss. Other advantages include the ability to test multiple coupons at once and
simulation of extreme conditions.
Similar to the RCE method, the RC method is unable to account for erosive effects such as
those due to the presence of sand particles. A schematic of the RC system is shown in
Figure B.3.

Figure B.3 Schematic of the RC Setup

Jet Impingement (JI)


The jet impingement (JI) methodology allows for the simulation of high turbulent conditions
in multiphase systems (i.e. oil, brine, and gas). More recently used in the evaluation of
corrosion inhibitors, JI also allows for the examination of flow-induced corrosion. Turbulence
associated with bends, valves, welds, threaded joints, and so forth within pipelines,
flowlines, and tubulars can be simulated using this technique. Similar to RCE and RC, JI also
requires small test solutions and is easily controlled. Figure B.4 represents a schematic of
the JI system.

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Advantages of the JI methodology includes:
(1) the fluid flow is well characterized.
(2) electrode is flat and stationary allowing for film thickness determinations using
ellipsometry.
(3) shear induced erosion corrosion can be studied.

Limitations to the JI method are:


(1) can allow entrainment of particles and/or air bubbles that may be undesirable.
(2) mass transfer characteristics are not uniform over all regions.

Figure B.4 Jet Impingement Schematic

As previously stated, partitioning tests are essential in the performance evaluation of a


candidate inhibitor. The main purpose of this test is to estimate the inhibitor dose rate
required on total fluids. To determine dose rates, it is essential that testing be conducted at
realistic water/oil ratios and that injection rates change with water cut.

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Bubble Test
The bubble test, also known as the kettle or stirred corrosion test, is used to evaluate
corrosion inhibitors under low shear conditions. A popular laboratory method for evaluating
inhibitors, the methodology allows for the measurement of corrosion rates, using both
electrochemical methods, as well as mass loss. In addition, bubble tests are also used to
evaluate partitioning and persistency characteristics of inhibitors.
Benefits of the bubble test are that they allow for the simulation of composition and
temperature conditions of the environment encountered in the field. Flow or fluid movement
is controlled by the bubbles generated through gas purging. Unlike the RCE, RC, and JI
methods, the main limitation of bubble tests are that they do not simulate flow conditions in
the field (i.e. high shear or turbulent conditions).

Flow Loop Testing


Flow loop testing allows for the simulation of flow patterns similar to those observed in the
field. Used for the evaluation of flow velocity on corrosion, erosion-corrosion, and corrosion
inhibition, flow loop testing allows for the measurement of corrosion rates using both
electrochemical methods, as well as mass loss. In addition, multiple corrosion monitoring
techniques (e.g. coupons, probes, etc.) similar to those used in the field can be utilized.
Figure B.5 shows a schematic of a flow loop system.
Flow conditions using this methodology are well characterized, accounting for such
parameters as temperature, pressure, pipe diameter, maximum flow velocities, fluid
properties, flow restrictions, pipe lengths, and multiple phases. Tested media is often
recirculated through the loop and, thus, pumps and solution reservoirs are required.
Advantages of flow loop testing include:
(1) multiple coupons and probes can be placed at various orientations, providing
information on differential shear
(2) monitoring results tend to be simple to interpret and easy to extrapolate for other
systems due to the well characterized flow conditions.
Limitations associated with flow loop testing include:
(1) tests are generally long term and run continuously
(2) associated equipment and maintenance are expensive
(3) setups require significant amounts of space
(4) there is a high potential for leaks
(5) setups require large volumes of solution.

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Figure B.5 Example Schematic of a Flow Loop Testing System

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Number of
Aqueous/ Erosive
Coupon Coupons Measuring
Methodology Oil/Gas Conditions Effects
Shape Tested at Techniques
Phase Considered
Once
Weight loss & Does not simulate
Bubble test Rectangular 2 Aqueous field flow No
electrochemical
conditions
Weight loss &
Aqueous
Rotating Cylinder electrochemical
Cylindrical 1 High turbulent No
Electrode (RCE)
Aqueous/Oil Weight loss

Aqueous or
Rotating Cage (RC) Rectangular 8 Weight loss High turbulent No
aqueous/oil
Weight loss &
Aqueous Flow induced or Shear induced
electrochemical
Jet Impingement (JI) Disc 4 high turbulent erosion
Aqueous/Oil Weight loss conditions corrosion

Aqueous or Weight loss & Simulates field


Flow Loop Testing Various Multiple Yes
aqueous/oil electrochemical flow conditions

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Field Testing
The next step in evaluating a candidate inhibitor is to perform small scale field trials utilizing
corrosion monitoring tools. The performance and effectiveness of a candidate inhibitor may
be evaluated using corrosion coupons, solution analysis for iron and inhibitor
concentrations, nondestructive testing (NDT) methods that determine wall loss, or electronic
probes. During field trials, the optimum injection levels and effect of a candidate inhibitor on
local conditions may be assessed.
When conducting field trials, it is important to select a location that accurately represents
the system of interest and that has sufficient monitoring capability. Monitoring
instrumentation should be in place to continuously record corrosion rates and production
rates during testing.
Prior to testing, a test plan should be formulated and approved by Operations. Information
addressed in the plan should include:
(1) purpose of testing
(2) basis for evaluating tests
(3) complete description of testing procedures
(4) test expectations and possible side effects
(5) measures planned to return system to “baseline” conditions prior to subsequent
inhibitor testing.
During testing, communication between operations, corrosion control, and the chemical
manufacturer is essential to ensure that all relevant data for assessing a candidate
inhibitor’s performance is obtained.
The next step is to determine field dosage rates. Initial dosage rates are commonly based off
laboratory partitioning tests. From there, dosages are gradually decreased and increased to
an optimum value, based upon field monitoring. Other factors to consider when evaluating a
candidate inhibitor include negative impact on facility operations, such as emulsion-
breaking and foaming.
Once all candidate inhibitors are tested in the field, cost-performances of each product is
determined and compared.

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