TESTING METHOD Code
Laboratory Screening Tests to Determine the
Ability of Scale Inhibitors to Prevent the
Precipitation of Calcium Carbonate, Calcium R&D/OFC/02/11
Sulfate, Barium Sulfate and Strontium Sulfate from
Solution (for Oil and Gas Production Systems)
Rev. 2 Valid day 16/1/2017 Page 1 of 9
1. Introduction:
Scale inhibitors are specialty chemicals that are added to oil and gas production systems
to delay, reduce and/or prevent scale deposition.
2. Scope:
The test methods described in this standard are static laboratory screening tests designed
to give a measure of the ability of scale inhibitors to prevent the precipitation of Calcium
Carbonate, Calcium Sulfate, Barium Sulfate and Strontium Sulfate from solution.
These test methods are recommended only for ranking the performance of different scale
inhibitors under laboratory conditions set by these methods. They are not intended to
provide actual field treating rates.
Many factors, such as reaction kinetics, fluid velocity and composition, variable
temperatures and pressures, scale adherence, and solids dispersion can significantly affect
actual scale deposition under field conditions. Detailed consideration of these parameters
is deemed to be outside the scope of this standard. However, field conditions, field brine
composition, and other variables noted above should be considered at some point in scale
inhibitor evaluation prior to final scale inhibitor selection for field use.
Tests should be conducted at various scale inhibitor concentrations in order to obtain a
better understanding of performance under laboratory conditions set by these methods.
The scale inhibitor concentration required for a field application is likely to be different
from that determined under these laboratory conditions
3. Reference:
NACE TM 0374, NACE TM 0197, ASTM D 511, ASTM D 1126
4. Definition: N/A
5. Test Method
5.1. Calcium Carbonate Precipitation Test
5.1.1. Apparatus and Solutions
A pressure-regulated source of carbon dioxide (CO2).
Water bath
Test cells (approximately 125-ml [4-oz] bottles with positive seals).
Caution: The amount of vapor space above the test solutions in Paragraph 5.2.4 will
affect the test results. To maximize the validity and reproducibility of test results, choose
test cells that vary in capacity (volume) when sealed by 5% or less.
Graduated cylinders 50 ± 0.5 ml
Graduated measuring pipettes in the following sizes: 0.1, 0.5, and 1.0 ml.
Page: 1/9
TESTING METHOD Code
Laboratory Screening Tests to Determine the
Ability of Scale Inhibitors to Prevent the
Precipitation of Calcium Carbonate, Calcium R&D/OFC/02/11
Sulfate, Barium Sulfate and Strontium Sulfate from
Solution (for Oil and Gas Production Systems)
Rev. 2 Valid day 16/1/2017 Page 2 of 9
Synthetic brines prepared with distilled water, as follows:
Calcium-containing brine: 12.15 g/L CaCl2 • 2H2O; 3.68 g/L MgCl2 • 6 H2O;
33.0 g/L NaCl.
Bicarbonate-containing brine: 7.36 g/L NaHCO3; 33.0 g/L NaCl.
Note: Very small quantities of insoluble materials may remain after the specified
reagents have completely dissolved. For consistency of results, solutions shall be filtered
through a 0.45-µm filter.
One percent by weight (1 wt %) and 0.1 wt% dilutions of the as-received scale
inhibitors to be tested, prepared with distilled water.
5.1.2. Test Procedure
The 0.1 wt% dilution shall be used for tests in which scale inhibitor loadings are less than
10 mg/L. Run duplicates of each concentration.
[Link]. Prepare duplicate blanks as follows:
a. Prepare two samples of the calcium-containing brine (50 ml each).
Determine the calcium ion concentration of the blanks before precipitation
in accordance with Paragraph 5.2.7 and divide each value by 2.
b. Prepare and handle the blanks after precipitation as described in Paragraphs
[Link] through [Link], but do not include a scale inhibitor.
[Link]. Saturate both the calcium- and bicarbonate- containing brines with CO 2
immediately before using. Accomplish saturation at room temperature by
bubbling CO2 through a fritted-glass gas dispersion tube immersed to the
bottom of the container. A rate of 250 ml/min of CO2 for 30 minutes will be
sufficient to saturate up to 1 L of each the brine simultaneously.
[Link]. Add 50 ml of bicarbonate-containing brine to the test cell and mix well. Add
50 ml of calcium-containing brine to the test cell.
[Link]. Cap the test cell immediately and agitate to mix the brines and the scale
inhibitor thoroughly. The test cells must be capped tightly to avoid loss of CO2.
[Link]. Place all test cells and blanks in a water bath at 71 ±1°C (160 ±2°F) for 24
hours.
[Link]. Remove the test cells after the 24-hour exposure and avoid agitation. Allow
the test cells to cool to 25 ±5°C (77 ±9°F) for a time not to exceed two hours.
[Link]. Determine the calcium ion concentration by procedures given in ASTM D 511,
ASTM D 1126, APHA Standard Methods for the Examination of Water and
Wastewater (Part 300), or another accepted test method. NOTE: Calcium ion
concentration values for duplicate test samples often differ by 2% or more. A
5% difference is considered unacceptable and shall be cause for rerunning the
test.
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TESTING METHOD Code
Laboratory Screening Tests to Determine the
Ability of Scale Inhibitors to Prevent the
Precipitation of Calcium Carbonate, Calcium R&D/OFC/02/11
Sulfate, Barium Sulfate and Strontium Sulfate from
Solution (for Oil and Gas Production Systems)
Rev. 2 Valid day 16/1/2017 Page 3 of 9
[Link]. Report the average of the duplicate calcium concentration values as mg/L
calcium carbonate retained in solution for each inhibitor test concentration and
the blank.
[Link]. Inhibitive effectiveness may be calculated as shown in Equation (1):
% Inhibition = (Ca - Cb) / (Cc – Cb) x 100 (1)
Where:
Ca = Ca2+ concentration in the treated sample after precipitation.
Cb = Ca2+ concentration in the blank after precipitation.
Cc = Ca2+ concentration in the blank before precipitation.
5.2. Calcium Sulfate Precipitation Test.
5.2.1. Apparatus and Solutions
[Link]. Constant-temperature water bath or forced-draft oven with the capability of
maintaining the specified temperature within ±1°C
[Link]. Clean and dust-free glass test cells (approximately 125-mL [4-oz] bottles with
positive seals)
[Link]. Synthetic brines prepared with distilled or deionized water, as follows
a) Calcium-containing brine: 7.50 g/L NaCl; 11.10 g/L CaCl2 • 2H2O
b) Sulfate-containing brine: 7.50 g/L NaCl; 10.66 g/L Na2SO4
c) Note: Very small quantities of insoluble materials may remain after the
specified reagents have completely dissolved. For consistency of results,
solutions shall be filtered through a 0.45-μm filter.
[Link]. Apparatus for reproducibly delivering 50 ±0.5 mL
[Link]. One percent by weight (1 wt%) and 0.1 wt% dilutions of the as-received scale
inhibitors to be tested, prepared with deionized water.
[Link]. Graduated measuring pipets in the following sizes: 0.1, 0.5, and 1.0 mL.
5.2.2. Test Procedure
[Link]. Pipet the desired amount of scale inhibitor into each test cell using the 1 wt%
and 0.1 wt% dilutions. The 0.1 wt% dilution shall be used for tests in which
scale inhibitor loadings are less than 10 mg/L. Run duplicates of each
concentration.
[Link]. Prepare duplicate blanks as follows:
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TESTING METHOD Code
Laboratory Screening Tests to Determine the
Ability of Scale Inhibitors to Prevent the
Precipitation of Calcium Carbonate, Calcium R&D/OFC/02/11
Sulfate, Barium Sulfate and Strontium Sulfate from
Solution (for Oil and Gas Production Systems)
Rev. 2 Valid day 16/1/2017 Page 4 of 9
a) Set aside two samples of the calciumcontaining brine (50 mL each).
Determine the calcium ion concentration of the blanks before precipitation
in accordance with Paragraph [Link] and divide each value by 2.
b) Prepare and handle the blanks after precipitation as described in Paragraphs
[Link] through [Link], but do not include a scale inhibitor
[Link]. Add 50 mL of sulfate-containing brine to the test cell and mix well. Add 50 mL
of calcium-containing brine to the test cell
[Link]. Cap the test cell immediately and agitate to mix the brines and the scale
inhibitor thoroughly.
[Link]. Place all test cells and blanks in a forced-draft oven or immerse to 75% of their
lengths in a water bath at 71 ±1°C (160 ±2°F) for 24 hours.
[Link]. Remove the test cells after the 24-hour exposure and avoid agitation. Allow the
test cells to cool to 25 ±5°C (77 ±9°F) for a time not to exceed two hours.
[Link]. Determine the calcium ion concentration by procedures given in ASTM D 511,
ASTM D 1126, APHA Standard Methods for the Examination of Water and
Wastewater (Part 300), or another accepted test method. NOTE: Calcium ion
concentration values for duplicate test samples often differ by 2% or more. A
5% difference is considered unacceptable and shall be cause for rerunning the
test
[Link]. Report the average of the duplicate calcium ion concentration values as mg/L
calcium sulfate retained in solution for each inhibitor test concentration and the
blank
[Link]. Percent inhibition may be calculated in accordance with Paragraph [Link]
5.3. Barium Sulfate and/or Strontium SulfatePrecipitation Test.
5.3.1. Test Equipment
[Link]. Constant-temperature water bath or forced-air oven capable of maintaining the
specified test temperature.
[Link]. Analytical balance capable of weighing mineral salts and other reagents to one-
hundredth of the quantity specified.
[Link]. Clean, dust-free clear and colorless glass test bottles with a capacity of 100 to
125 mL. Caps must be capable of a positive seal, i.e., they must not deform so
as to release pressure generated within the bottle under the test conditions.
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TESTING METHOD Code
Laboratory Screening Tests to Determine the
Ability of Scale Inhibitors to Prevent the
Precipitation of Calcium Carbonate, Calcium R&D/OFC/02/11
Sulfate, Barium Sulfate and Strontium Sulfate from
Solution (for Oil and Gas Production Systems)
Rev. 2 Valid day 16/1/2017 Page 5 of 9
[Link]. Flasks fitted with dispensers capable of reproducibly delivering 50.0 mL of the
preheated test solutions.
[Link]. Assorted clear, colorless glass containers for deionized/distilled water, buffer
solutions, unfiltered brines, scale inhibitor stock solutions, post-test analytical
samples, etc.
[Link]. Filter assembly(ies) capable of filtering brines using: Cellulose acetate 0.45-
μm membrane filters
[Link]. A pH meter with an appropriate probe.
[Link]. Syringes and syringe filters for withdrawing post-test analytical samples
5.3.2. Reagents
[Link]. The chemicals (mineral salts and organic buffering agents) to prepare test
solutions.
[Link]. Deionized and/or distilled water.
[Link]. Concentrated solutions of the scale inhibitors to be evaluated
5.3.3. Preparation of Test Solutions
[Link]. Choose an appropriate composite test brine, and specify the concentrations
(mg/L) for all species in the composite brine.
[Link]. Define two new component brines which, when mixed in equal volumes, result
in a composite brine with concentrations equivalent to those specified in
Paragraph [Link]. One component brine, Brine A, shall contain all of the
polyvalent cations, and the other component brine, Brine B, all of the scaling
anions. The remaining ions, e.g., Na+ and Cl-, shall be allotted such that the
ionic concentrations in the two component brines are comparable if not equal.
[Link]. Define another component brine, Brine C, which differs from Brine B only in
that NaCl is substituted for the salts containing the scaling anions. The NaCl
substitution shall result in a Brine C ionic strength equivalent to that of Brine
B.
[Link]. Caution: Some inhibitors may be incompatible with highly saline brines or
with high concentrations of specific cations. A resulting deposit may be
mistaken for BaSO4/SrSO4 and will remove inhibitor from solution. The user
of this test method may investigate inhibitor-brine incompatibility by treating
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TESTING METHOD Code
Laboratory Screening Tests to Determine the
Ability of Scale Inhibitors to Prevent the
Precipitation of Calcium Carbonate, Calcium R&D/OFC/02/11
Sulfate, Barium Sulfate and Strontium Sulfate from
Solution (for Oil and Gas Production Systems)
Rev. 2 Valid day 16/1/2017 Page 6 of 9
the theoretically nonscaling mixtures of Brine A and Brine C with the highest
concentration of the inhibitor(s) being evaluated.
[Link]. On the day of the test(4) prepare sufficient quantities of Brines A, B, and C by
weighing out and dissolving in deionized/distilled water the salts capable of
providing the required ionic concentrations. Bring the component brines to 96
±1% of the final volume.
[Link]. Mix sufficient buffer into Brine A so that the composite brine mixtures (A+B,
A+C) will have the required pH at the test temperatures. (The required quantity
of buffer should be determined in advance by mixing, at test temperature,
appropriate aliquots of Brine A and B and quickly but carefully adding buffer.)
[Link]. Filter each component brine through a cellulose acetate 0.45-μm membrane
filter.
[Link]. Transfer the component brines to labeled flasks fitted with dispensers capable
of reproducibly delivering 50.0 mL to the test bottles. Place the flasks in a
constant-temperature bath/oven set at the test temperature.
[Link]. When the component brines have reached the test temperature, bring them to
the required volume with deionized/distilled water and mix adequately. Avoid
unnecessary heat loss and minimize out-ofbath/ oven time.
[Link]. Prepare a stock solution of each scale inhibitor to be evaluated. One-percent
solutions (weight/volume) are normally suitable.
5.3.4. Test Procedure
[Link]. Ensure that both the bath/oven and the component brines have stabilized at the
test temperature.
[Link]. Dose a range of aliquots of each scale inhibitor to be evaluated into clean,
ambient-temperature test bottles. Perform all tests at least in duplicate. (The
range chosen should be wide enough to demonstrate undertreatment (scale
precipitation) and overtreatment (no precipitation) for the scale inhibitors being
evaluated).
[Link]. To each test bottle containing a dose of scale inhibitor, add 50 mL of Brine B,
swirl briefly, and add 50 mL of Brine A. Secure the cap tightly, shake the bottle
(10 up-and-down cycles), and immediately transfer the test bottle to the
constant-temperature bath/oven stabilized at the tes temperature. Procedures
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TESTING METHOD Code
Laboratory Screening Tests to Determine the
Ability of Scale Inhibitors to Prevent the
Precipitation of Calcium Carbonate, Calcium R&D/OFC/02/11
Sulfate, Barium Sulfate and Strontium Sulfate from
Solution (for Oil and Gas Production Systems)
Rev. 2 Valid day 16/1/2017 Page 7 of 9
that minimize delays that can lead to cooling of the test solution should be
adopted. Figure 1 depicts the preparation of a standard test sample and includes
some related notes.
[Link]. Prepare two or more test bottles without scale inhibitor using the procedure
outlined in Paragraph [Link]. (for test bottles containing scale inhibitor) to
serve as blanks.
[Link]. Prepare two or more test bottles without scale inhibitor as controls by adding
50 mL of Brine C, swirling briefly, and adding 50 mL of Brine A. Seal, shake,
and place in the oven/bath as described in Paragraph [Link]. Figure 2 depicts
the preparation of the control samples.
[Link]. Expose all test bottles at the test temperature for a test duration that reflects the
likely residence time of the scale inhibitor in the field application being
modeled, but test durations less than 4 hours or more than 24 hours are not
recommended.
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TESTING METHOD Code
Laboratory Screening Tests to Determine the
Ability of Scale Inhibitors to Prevent the
Precipitation of Calcium Carbonate, Calcium R&D/OFC/02/11
Sulfate, Barium Sulfate and Strontium Sulfate from
Solution (for Oil and Gas Production Systems)
Rev. 2 Valid day 16/1/2017 Page 8 of 9
[Link]. At the end of the specified test duration, remove each test bottle, in turn, from
the bath/oven and immediately take a sample for analysis. Filter each analytical
sample without delay through a 0.45-μm syringe filter into a clean bottle and
stabilize the sample in preparation for cation analysis. (If the sample analysis is
performed immediately, sample stabilization may not be necessary. It is the
user’s responsibility to establish that stabilization is not necessary).
[Link]. Analyze all samples to establish the levels of the sparingly soluble cations of
interest (barium, strontium, etc.); avoid unnecessary delay in completing the
analysis. (Analysis of the blanks establishes the “zero inhibition” concentration
of the Ba2+ and/or Sr2+ ions for the test. Analysis of the controls establishes
the maximum possible (100% inhibition) Ba2+ and Sr2+values for the test.
The concentration values obtained for Ba2+ and/or Sr2+ are required for the
calculation of test results in Section 5.3.5)
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TESTING METHOD Code
Laboratory Screening Tests to Determine the
Ability of Scale Inhibitors to Prevent the
Precipitation of Calcium Carbonate, Calcium R&D/OFC/02/11
Sulfate, Barium Sulfate and Strontium Sulfate from
Solution (for Oil and Gas Production Systems)
Rev. 2 Valid day 16/1/2017 Page 9 of 9
5.3.5. Calculation and Reporting of Test Results
[Link]. For each scale inhibitor concentration, the test results shall be calculated as
either percentage inhibition or percentage retention of soluble barium and/or
strontium cation (M2+) as shown in Equations (2) and (3)
Prepared by Reviewed by Approved and issued by
Bui Dac Trung Dao Viet Than Thai Hong Chuong
Date: …../……/2017 Date: ….../……/2017 Date: …../…../2017
Page: 9/9
