Astm G184-06 PDF
Astm G184-06 PDF
1. Scope 3. Terminology
1.1 This practice covers a generally accepted procedure to 3.1 The terminology used throughout shall be in accordance
use the rotating cage (RC) for evaluating corrosion inhibitors with Terminologies G 15 and D 4410 and Guide G 170.
for oil field and refinery applications.
1.2 The values stated in SI units are to be regarded as the 4. Summary of Practice
standard. The values given in parentheses are for information 4.1 This practice provides a method of evaluating corrosion
only. inhibitor efficiency in a RC apparatus. The method uses a
1.3 This standard does not purport to address all of the well-defined rotating specimen setup and mass loss measure-
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safety concerns, if any, associated with its use. It is the ments to determine corrosion rates in a laboratory apparatus.
responsibility of the user of this standard to establish appro- Measurements are made at a number of rotation rates to
priate safety and health practices and determine the applica- evaluate the inhibitor performance under increasingly severe
bility of regulatory limitations prior to use. hydrodynamic conditions.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
efficiencies. The minimum solution volume to metal surface through the vessel, tubing, and joints shall be avoided.
area is not less than 14 cm (11). 8.3 The appropriate composition of gases is determined by
6.4 Open-beaker tests should not be used because of evapo- the composition of gases in the field for which the inhibitor is
ration and contamination. Open-beaker test must not be con- evaluated. (Warning—Hydrogen sulfide (H2S) and carbon
ducted when H2S (hydrogen sulfide) is used. In some tests, dioxide (CO2) are corrosive gases.) (Warning—H2S is poison-
provisions might be needed for continuous flow or replenish- ous and should not be released into the atmosphere.) The
ment of the corrosive liquid, while simultaneously maintaining appropriate composition of gas can be obtained by mixing H2S
a controlled atmosphere. and CO2 streams from the standard laboratory gas supply.
6.5 For experiments above atmospheric pressure, a high- Nitrogen or other inert gases can be used as a diluent to obtain
temperature, high-pressure rotating cage (HTHPRC) system the required composition of corrosive gases. Alternatively, gas
and a vessel that can withstand high pressure without leakage mixtures of the required compositions can be purchased from
shall be used. suppliers of industrial gases. The concentrations of impurities,
6.6 The suggested components can be modified, simplified, particularly oxygen, shall be kept as low as possible with
or made more sophisticated to fit the needs of a particular guidelines of below 5 ppb and preferably under 1 ppb oxygen
investigation. in solution.
8.4 The solution pH before and after testing shall be
7. Materials measured, recorded and reported. The solution pH should be
monitored regularly (at least once a day) during the test.
7.1 Methods for preparing specimens for tests and for 8.5 Inhibitor concentrations should be measured and re-
removing specimens after the test are described in Practice G 1. ported in % mass/volume or parts per million (ppm). The
Standard laboratory glassware should be used for weighing and method of injecting the inhibitor into the test solution should
measuring reagent volumes. reflect the actual field application. Water-soluble inhibitors
7.2 The coupons shall be made of the material (such as may be injected neat (as-received) into the test solution
carbon steel) for which the inhibitor is being evaluated. The (aqueous phase). To avoid the errors associated with handling
coupon should have the same metallographic structure as that small volumes of solution, an inhibitor stock solution may be
used in the service components. The coupons should be ground prepared by diluting the as-received chemical in an appropriate
to a specified surface finish (such as 150-grit). The grinding solvent. The type of solvent and the concentration of the stock
should produce a reproducible surface finish, with no rust solution depend on the characteristics of the inhibitor and on
deposits, pits, or deep scratches. All sharp edges on the coupon the specified test conditions.
should be ground. All loose dirt particles should be removed. 8.6 Oil-soluble, water-dispersible inhibitor solutions are
7.3 The coupons are rinsed with distilled water, degreased prepared by the following partition method. The required
by immersing in acetone (or any suitable alcohol), ultrasoni- amounts of oil and brine are placed in the partitioning vessel
cally cleaned for 1 min, and dried. The surface of the (usually a separation funnel). The relative volumes of oil and
specimens should not be touched with bare hands. The speci- aqueous phases should reflect the ratios of water and oil in the
mens are weighed to the nearest 0.1 mg, the dimensions are field for which the inhibitor is evaluated. If samples from the
measured to the nearest 0.1 mm, and the surface areas are field are not available, heptane, kerosine, or any suitable
calculated. hydrocarbon may be used. The corrosion inhibitor is added to
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appropriate). Position the liquid inlet and outlet so that none of pressure at which the experiment is planned. For example, if
them is protruding into the solution. the experiment is planned at 250 psi (1724 kPa), test the system
9.5 Initially all other ports of the experimental vessel, at about 400 psi (2759 kPa). This testing is required to ensure
except the inlet and outlet ports are closed. The inlet tube the safety of the personnel and the equipment and also to detect
should have a Y-joint, where one end is attached to the any leak.
experimental vessel. Attach the other two ends to the prepara- 10.1.2 After pressurizing the autoclave to the preset value,
tion vessel and to an inert gas, such as argon or nitrogen close the inlet and outlet valves.
cylinder. 10.1.2.1 After 30 min, test the autoclave for any leaks.
9.6 Pass the inert gas to expel oxygen from the experimental 10.1.2.2 If any leak is found, tighten the autoclave head
vessel. screws and recheck for any further leak.
10.1.2.3 If there is still any pressure loss, then the system is
9.7 After 15 min, stop the gas flow, and close the passage faulty. Stop the experiment, and have the autoclave inspected
between the experimental vessel and the gas cylinder. and repaired.
9.8 Open the passage between the experimental and prepa- 10.1.2.4 If the pressure holds constant for more than 30 min,
ration vessels, and pump the gas-saturated brine, which may or release the pressure by opening the outlet. Once the pressure
may not contain inhibitor prepared as per 8.4 or 8.5, into the gage shows that the pressure has been released, close the outlet
experimental vessel. valve.
9.9 Close the passage between the experimental and prepa- 10.2 Follow the steps as in the atmospheric pressure experi-
ration vessels. Maintain the experimental vessel with the heater ments (see 9.2-9.11) to charge the autoclave.
or the water bath at the required temperature. 10.3 For high-temperature, high-pressure experiments using
9.10 The additional gas inlet on top of the vessel should a premixed gas composition, pressurize the autoclave using the
allow keeping the gas mixture blanket on top of the solution, specified gas composition, and depressurize to approximately
which is required when the experiment is planned for a longer 0.2 bars above atmospheric pressure.
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REFERENCES
(1) Papavinasam, S., “Corrosion Inhibitors,”Uhlig’s Corrosion Handbook, Inhibitor Selection,” Materials Performance, Vol 39, Issue 8, August
Revie, R. Winston, ed., 2nd edition, John Wiley & Sons, Inc., 2000, p. 2000, pp. 58-60.
1089, and “Evaluation and Selection of Corrosion Inhibitors,” p. 1169. (9) V. Jovancicevic, Ramachandran, and Ahn, Y. S., “Using Reaction
(2) Papavinasam, S., Revie, R. W., Attard, M., Demoz, A., and Michae- Engineering to Compare Corrosion Inhibitor Performance in Labora-
lian, K., “Comparison of Laboratory Methodologies to Evaluate tory and Field Experiments,” NACE Corrosion Conference, Paper No.
Corrosion Inhibitors for Oil and Gas Pipelines,” Corrosion, NACE, 1027, Houston, TX, 2001.
Vol 59, No. 10, October 2003, pp. 897-912. (10) Papavinasam, S., Revie, R. W., Attard, M., and Bojes, J., “Rotating
(3) Schmitt, G. A., Bruckhoff, W., Faessler, K., and Blummel, G., “Flow Cage—A Compact Laboratory Methodology for Simultaneously
Loop versus Rotating Probes—Experimental Results and Service Evaluating Corrosion Inhibition and Drag Reducing Properties of
Applications,” NACE Corrosion Conference, Paper No. 23, Houston, Chemicals,” NACE Corrosion Conference, Paper No. 2495, Houston,
TX, 1990. TX, 2002.
(4) Stegmann, D. W., Hausler, R. H., Cruz, C. I., and Sutanto, H., (11) Papavinasam, S., Doiron, A., and Revie, R. W., “Effect of Rotating
“Laboratory Studies on Flow Induced Localized Corrosion in CO2/ Cage Geometry on Flow Pattern and Corrosion Rate,” NACE
H2S Environments: I. Development of Test Methodology,” NACE Corrosion Conference, Paper No. 3333, Houston, TX, 2003.
Corrosion Conference, Paper No. 5, Houston, TX, 1990.
(12) Deslouis, C., Belghazi, A., AI-Janabi, Y. T., Plagemann, P., and
(5) Hausler, R. H., Stegmann, D. W., Cruz, C. I., and Tjandroso, D.,
Schmitt, G., “Quantifying Local Wall Shear Stresses in the Rotated
“Laboratory Studies on Flow Induced Localized Corrosion in CO2/
Cage,” NACE Corrosion Conference, Paper No. 4727, Houston, TX,
H2S Environments: II. Parametric Study on the Effects of H2S,
2004.
Condensate, Metallurgy, and Flowrate,” NACE Corrosion Conference,
Paper No. 6, Houston, TX, 1990. (13) Papavinasam, S., Revie, R. W., Attard, M., Demoz, A., and Michae-
(6) Hausler, R. H., Stegmann, D. W., Cruz, C. I., and Tjandroso, D., lian, K., “Comparison of Laboraotry Methodologies to Evaluate
“Laboratory Studies on Flow Induced Localized Corrosion in CO2/ Corrosion Inhibitors for Oil and Gas Pipelines,” Corrosion, NACE,
H2S Environments: III. Chemical Corrosion Inhibition,” NACE Cor- Vol 59, No. 10, 2003, p. 897.
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rosion Conference, Paper No. 7, Houston, TX, 1990. (14) Crolet, J. L., and Bonis, M. R., “How to Pressurize Autoclaves for
(7) Schmitt, G. A., Bruckhoff, W., Faessler, K., and Blummel, G., “Flow Corrosion Testing under Carbon Dioxide and Hydrogen Sulfide
Loop versus Rotating Probes—Experimental Results and Service Pressure,” Corrosion, NACE, Vol 56, 2000, p. 167.
Applications,” Materials Performance, February 1991, p. 85. (15) Hausler, R. H., “Methodology for Charging Autoclaves at High
(8) Papavinasam, S., Revie, R. W., Attard, M. A., H. Sun, Demoz, Donini, Pressures and Temperatures with Acid Gases,” Corrosion, NACE,
J. C., Michaelian, K. H., “Laboratory Methodologies for Corrosion Vol 54, 1988, p. 641.
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