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Designation NACE TM0169/ G31 – 12a Item No. 21200

Standard Guide for

Laboratory Immersion Corrosion Testing of Metals1
This standard is issued under the fixed designation TM0169/G31; the number immediately following the designation indicates the year of original
adoption or, in the case of revision, the year of last revision.

1. Scope G1 Practice for Preparing, Cleaning, and Evaluating Corro-

1.1 This guide covers and describes the factors that influ- sion Test Specimens
ence laboratory immersion corrosion tests, particularly mass G28 Test Methods for Detecting Susceptibility to Inter-
loss tests. These factors include apparatus, sampling, test granular Corrosion in Wrought, Nickel-Rich, Chromium-
specimen, test conditions (test solution composition, tempera- Bearing Alloys
ture, gas sparging, fluid motion, solution volume, method of G34 Test Method for Exfoliation Corrosion Susceptibility
supporting test specimens, duration of test), methods of clean- in 2XXX and 7XXX Series Aluminum Alloys (EXCO
ing test specimens, interpretation of results, and calculation of Test)
corrosion rates. This guide also emphasizes the importance of G46 Guide for Examination and Evaluation of Pitting
recording all pertinent data and provides a checklist for Corrosion
reporting test data. G48 Test Methods for Pitting and Crevice Corrosion Resis-
1.2 The specific evaluation of localized attack, environmen- tance of Stainless Steels and Related Alloys by Use of
tally assisted cracking, and effects of solution flow are not Ferric Chloride Solution
within the scope of this guide. G66 Test Method for Visual Assessment of Exfoliation
1.3 This guide is intended to be used by those designing Corrosion Susceptibility of 5XXX Series Aluminum Al-
laboratory immersion tests who may not be familiar with all of loys (ASSET Test)
the variables to consider and the pitfalls that could be encoun- G67 Test Method for Determining the Susceptibility to
tered when designing and conducting this kind of testing. It Intergranular Corrosion of 5XXX Series Aluminum Alloys
should be used as a reference to ensure that the test will allow by Mass Loss After Exposure to Nitric Acid (NAMLT
generation of data relevant to the application with the mini- Test)
mum of interferences. G71 Guide for Conducting and Evaluating Galvanic Corro-
1.4 The values stated in SI units are to be regarded as the sion Tests in Electrolytes
standard. The values given in parentheses are for information G78 Guide for Crevice Corrosion Testing of Iron-Base and
only. Nickel-Base Stainless Alloys in Seawater and Other
1.5 This standard does not purport to address all of the Chloride-Containing Aqueous Environments
safety concerns, if any, associated with its use. It is the G82 Guide for Development and Use of a Galvanic Series
responsibility of the user of this standard to establish appro- for Predicting Galvanic Corrosion Performance
priate safety and health practices and determine the applica- G107 Guide for Formats for Collection and Compilation of
bility of regulatory limitations prior to use. Corrosion Data for Metals for Computerized Database
Input
2. Referenced Documents G108 Test Method for Electrochemical Reactivation (EPR)
2.1 ASTM Standards:2 for Detecting Sensitization of AISI Type 304 and 304L
A262 Practices for Detecting Susceptibility to Intergranular Stainless Steels
Attack in Austenitic Stainless Steels G110 Practice for Evaluating Intergranular Corrosion Re-
D1193 Specification for Reagent Water sistance of Heat Treatable Aluminum Alloys by Immersion
E8 Test Methods for Tension Testing of Metallic Materials in Sodium Chloride + Hydrogen Peroxide Solution
E300 Practice for Sampling Industrial Chemicals G112 Guide for Conducting Exfoliation Corrosion Tests in
Aluminum Alloys
G116 Practice for Conducting Wire-on-Bolt Test for Atmo-
1
This guide is under the jurisdiction of NACE/ASTM Committee J01, Joint
spheric Galvanic Corrosion
Committee on Corrosion, and is the direct responsibility of Subcommittee J01.01, G135 Guide for Computerized Exchange of Corrosion Data
Working Group on Laboratory Immersion Tests. for Metals
Current edition approved July 1, 2012. Published October 2012. Originally G170 Guide for Evaluating and Qualifying Oilfield and
approved in 1972. Last previous ASTM edition approved in 2012 as G31–12. NACE
edition originally approved in 1969. Last previous NACE edition approved in 2000 Refinery Corrosion Inhibitors in the Laboratory
as TM0169-2000. DOI: 10.1520/G0031-12A. G184 Practice for Evaluating and Qualifying Oil Field and
2
For referenced ASTM standards, visit the ASTM Web site, www.astm.org, or Refinery Corrosion Inhibitors Using Rotating Cage
contact ASTM Customer Service at [email protected]. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on
G185 Practice for Evaluating and Qualifying Oil Field and
the ASTM Web site. For NACE standards, visit the NACE Web site, www.nace.org, Refinery Corrosion Inhibitors Using the Rotating Cylinder
or contact NACE FirstService at [email protected]. Electrode

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NACE TM0169/G31 – 12a

2.2 NACE/ASTM Standards:2 general use, except for material qualification tests where
G193 Terminology and Acronyms Relating to Corrosion standardization is required. One purpose for this guide is to
2.3 NACE International Standards:2 promote better correlation of results in the future and the
SP0690 Standard Format for Collection and Compilation of reduction of conflicting reports through a more detailed record-
Data for Computerized Material Corrosion Resistance ing of meaningful factors and conditions.
Database Input 4.3 In designing any corrosion test, consideration should be
2.4 International Organization for Standardization (ISO) given to the various factors discussed in this guide, because
Standards:3 these factors have been found to affect the results obtained.
ISO 3651-1 Austenitic Stainless Steels – Determination of
resistance to intergranular corrosion of stainless steels – 5. Factors Affecting Corrosion Behavior
Part I: Austenitic and ferritic-austenitic (duplex) stainless 5.1 The methods and procedures described herein represent
steels – Corrosion test in nitric acid medium by measure- the best current practices for conducting laboratory immersion
ment of loss in mass (Huey test) corrosion tests as developed by corrosion specialists in the
ISO 3651-2 Determination of resistance to intergranular process industries. For proper interpretation of the results
corrosion of stainless steels – Part 2: Ferritic, austenitic obtained, the specific influence of one or more of the following
and ferritic-austenitic (duplex) stainless steels – corrosion variables should be considered.
test in media containing sulfuric acid
5.1.1 Metal specimens immersed in a specific hot liquid
ISO 6509 Corrosion of metals and alloys – Determination
may not corrode at the same rate or in the same manner as in
of dezincification resistance of brass
equipment where the metal acts as a heat transfer medium in
ISO 8407 Corrosion of metals and alloys – Removal of
heating or cooling the liquid. If the influence of heat transfer
corrosion products from corrosion test specimens
effects is specifically of interest, specialized procedures (in
ISO 8993 Anodized aluminum and aluminum alloys –
which the corrosion specimen serves as a heat transfer agent)
Rating system for the evaluation of pitting corrosion –
shall be employed.
Chart method
5.1.2 In laboratory immersion tests, the motion of the
ISO 8994 Anodized aluminum and aluminum alloys –
environment relative to the specimens will normally be pro-
Rating system for the evaluation of pitting corrosion –
vided by convection currents, gas sparging, or boiling. If the
Grid method
specific effects of fluid flow are to be studied, special tech-
ISO 9400 Nickel-based alloys – Determination of resistance
niques shall be employed to create and control the relative
to intergranular corrosion
motion between the environment and the test specimens. This
ISO 11463 Corrosion of metals and alloys – Evaluation of
may be accomplished by either moving the environment as
pitting corrosion
through a tube or mechanical stirrer or by moving the speci-
ISO 11845 Corrosion of metals and alloys – General prin-
mens as by rotation.
ciples for corrosion testing
5.1.3 The behavior of certain metals and alloys may be
ISO 11846 Corrosion of metals and alloys – Determination
profoundly influenced by the presence of dissolved oxygen. If
of resistance to intergranular corrosion of solution heat-
this is a factor to be considered in a specific test, the solution
treatable aluminum alloys
should be air saturated at 1 atm or de-aerated, as appropriate.
ISO 11881 Corrosion of metals and alloys – Exfoliation
corrosion testing of aluminum alloys 5.1.4 In some cases, the rate of corrosion may be governed
by other minor constituents in the solution, in which case they
3. Terminology will have to be continually or intermittently replenished by
changing the solution in the test.
3.1 For definitions of terms used in this guide, see NACE/
ASTM Terminology G193. 5.1.5 Corrosion products may have undesirable effects on a
chemical product. The amount of possible contamination can
4. Significance and Use sometimes be estimated from the loss in mass of the specimen
or from the changes in the chemical composition of the test
4.1 Corrosion testing by its very nature precludes complete
environment. This is discussed in more detail in 9.8.3.
standardization. This standard, rather than a standardized
procedure, is presented as a guide so that some of the pitfalls 5.1.6 Corrosion products from the specimen may influence
of such testing may be avoided. the corrosion rate of the metal itself or of different metals
4.2 Experience has shown that all metals and alloys do not exposed at the same time. For example, the accumulation of
respond alike to the many factors that affect corrosion and that cupric ions in the testing of copper alloys in intermediate
accelerated corrosion tests give indicative results only, or may strengths of sulfuric acid will accelerate the corrosion of
even be entirely misleading. It is impractical to propose an copper alloys, as compared to the rates that would be obtained
inflexible standard laboratory corrosion testing procedure for if the corrosion products were continually removed. It may be
necessary to expose only alloys of the same general type in the
same testing apparatus unless it is known that no interactions
3
will occur.
Available from International Organization for Standardization (ISO), 1, ch. de
la Voie-Creuse, Case postale 56, CH-1211, Geneva 20, Switzerland, http:// 5.1.7 Specimen corrosion testing is frequently designed to
www.iso.ch. investigate general corrosion only. There are a number of other

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NACE TM0169/G31 – 12a

forms of corrosion of which one shall be aware in the design the presence of environmentally assisted cracking. This usually
and interpretation of corrosion tests. occurs with no significant loss in mass of the test specimen,
5.1.7.1 Galvanic corrosion may be investigated by special although certain refractory metals are an exception to these
devices that couple one specimen to another in electrical observations. Generally, if cracking is observed on the speci-
contact. The behavior of the specimens in this galvanic couple men, it can be taken as positive indication of susceptibility,
is compared with that of insulated specimens exposed on the whereas failure to exhibit this phenomenon means that it did
same holder. It should be observed, however, that galvanic not occur under the duration and specific conditions of the test.
corrosion can be greatly affected by the area ratios of the Separate and special techniques are employed for the specific
respective metals, the separation between the metals, and the evaluation of the susceptibility of metals and alloys to envi-
conductivity of the electrolyte. The coupling of corrosion ronmentally assisted cracking. Multiple standards from many
specimens then yields only qualitative results, as a particular different organizations are available to describe stress-
specimen reflects only the relationship between these two corrosion cracking tests.
metals at the particular area ratio involved. Galvanic corrosion 5.2 The use of welded specimens is sometimes desirable,
testing is further discussed in ASTM Guide G71, ASTM Guide because some welds may be cathodic or anodic to the parent
G82, and ASTM Practice G116. metal and may affect the corrosion rate.
5.1.7.2 Crevice corrosion or concentration cell corrosion 5.2.1 The heat-affected zone is also of importance but
may occur where the metal surface is partially blocked from should be studied separately because welds on test specimens
the corroding liquid as under a spacer or supporting hook. It is may not adequately reproduce heat input or size effects of
necessary to evaluate this localized corrosion separately from full-size vessels.
the overall mass loss. Crevice corrosion testing is further 5.2.2 Corrosion of a welded specimen is normally localized
discussed in ASTM Test Methods G48 and ASTM Guide G78. and not representative of the entire surface and therefore
5.1.7.3 Selective corrosion at the grain boundaries (for separate thickness losses should be determined in the weld
example, intergranular corrosion of sensitized austenitic stain- metal, heat-affected zone, and base metal.
less steels) will not be readily observable in mass loss 5.2.3 A complete discussion of corrosion testing of welded
measurements unless the attack is severe enough to cause grain specimens or the effect of heat treatment on the corrosion
dropping, and often requires microscopic examination of the resistance of a metal is not within the scope of this guide.
specimens after exposure. This type of corrosion may also However, important factors to be considered include the
result in loss of strength or ductility of materials. Such losses welding technique to be used, the filler metal chemistry, and
can be evaluated by mechanical property determinations before whether the weld will be ground smooth, cleaned, passivated,
and after exposure to the test environment. Testing for selective or left as-welded.
corrosion is further discussed in ASTM Practices A262, ASTM 5.3 Cast and wrought alloys considered equivalent often
Test Methods G28, G34, G66, G67, G108, G110, and ASTM have somewhat different chemical composition and metallur-
Guide G112 and ISO 3651-1, ISO 3651-2, ISO 9400, gical structure, resulting in different corrosion resistances in
ISO 11846, and ISO 11881. identical service conditions. Therefore, caution should be used
in selecting representative test materials.
5.1.7.4 Dealloying or “parting” corrosion is a condition in
5.4 Additional discussion of testing considerations is con-
which one constituent is selectively removed from an alloy, as
tained in ISO 11845.
in the dezincification of brass or the graphitization of cast iron.
Close attention and a more sophisticated evaluation than a 6. Apparatus
simple mass loss measurement are required to detect this 6.1 A typical testing apparatus consists of a kettle or flask of
phenomenon. Dealloying testing is further discussed in suitable size (usually 500 to 5,000 mL), a reflux condenser with
ISO 6509. or without an atmospheric seal, a sparger for controlling
5.1.7.5 Certain metals and alloys are subject to a highly atmosphere or aeration, a thermometer port, a temperature-
localized type of attack called pitting corrosion. This cannot be regulating device, a heating device (mantle, hot plate, or bath),
evaluated by mass loss alone. Pitting is a statistical phenom- and a test specimen support system. If agitation is required, the
enon and the incidence of pitting may be directly related to the apparatus can be modified to accept a suitable stirring mecha-
area of metal exposed. For example, a small specimen is not as nism such as a magnetic stirrer. A typical flask setup for this
prone to exhibit pitting as a large one and it is possible to miss test is shown in Fig. 1.
the phenomenon altogether in the corrosion testing of certain 6.2 These components can be modified to fit the needs of a
alloys, such as the AISI Type 300 series stainless steels in particular investigation. The chosen apparatus is limited only
chloride-containing environments. Pitting testing is further by the judgment and ingenuity of the investigator.
discussed in ASTM Guide G46, ASTM Test Methods G48, and 6.2.1 A glass reaction kettle can be used when configuration
ISO 8993, ISO 8994, and ISO 11463. and size of test specimens do not permit entry through the
5.1.7.6 Most metals and alloys are subject to environmen- narrow neck of a flask. For solutions corrosive to glass, suitable
tally assisted cracking under some circumstances. This crack- metallic or plastic kettles may be employed.
ing occurs under conditions of applied or residual tensile stress, 6.2.2 In some cases, a wide-mouth jar with a suitable
and it may or may not be visible to the unaided eye or upon closure may be sufficient for simple, ambient-temperature
casual inspection. A metallographic examination may confirm immersion tests.

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NACE TM0169/G31 – 12a

should be investigated and reported. If the reason for the

disparity cannot be found, retesting should be considered.
8.1.1 If the effects of corrosion are to be determined by
changes in mechanical properties, untested duplicate speci-
mens should be preserved in a noncorrosive environment at the
same temperature as the test environment, or at ambient
temperature, or at both, for comparison with the corroded
specimens. The mechanical property commonly used for com-
parison is the tensile strength. Measurement of percent elon-
gation is a useful index of embrittlement. The procedures for
determining these values are shown in detail in ASTM Test
Methods E8.
8.2 The size and shape of corrosion test specimens vary
with the purpose of the test, nature of the materials, and test
apparatus. A rectangular or circular test specimen is preferred
for laboratory corrosion testing. Its size and dimensions are
typically determined by the test vessel being used and the
volume of the test solution available. A ratio of surface
area-to-solution mass smaller than in 9.8.2 and a ratio of edge
area to total area of less than 20% are desirable. These ratios
can be achieved through the use of specimens of minimum
thickness, although thin specimens such as shims of some
materials produced by heavy machining or cold rolling may
have different corrosion rates from material not subjected to
NOTE 1—A = thermometer port, B = flask, C = specimens hung on
these processes. Masking may also be used to achieve the
supporting device, D = air inlet, E = heating mantle, F = liquid interface, desired area ratios but may cause crevice corrosion problems.
G = opening in flask for additional apparatus that may be required, and 8.2.1 If circular specimens are used, they should be cut from
H = reflux condenser. sheet or plate, not bar stock, to minimize the exposed end grain
FIG. 1 Typical Resin Flask (unless the intent is to test or evaluate bar stock). A circular
specimen of about 38 mm (1.5 in) diameter is a convenient
shape for laboratory corrosion tests. With a thickness of
6.2.3 Open-beaker tests should not be used for long-term approximately 3 mm (0.125 in) and an 8 mm (5⁄16 in) or 11
testing because of evaporation and contamination. If beakers mm (7⁄16 in) diameter hole for mounting, these specimens will
are used, cover plates or watch glasses should be placed over readily pass through a 45/50 ground-glass joint of a distillation
the openings. kettle. Bar stock may contain long stringers near the center that
6.2.4 In more complex tests, provisions might be needed for can lead to corrosion behavior at the center of disk specimens
continuous flow or replenishment of the corrosive liquid, while cut from bar, which is not representative of the performance of
simultaneously maintaining a controlled atmosphere. the bulk alloy. This behavior can cause problems in interpreting
performance.
7. Sampling 8.2.2 Typically, rectangular test specimens 20 mm by 50
7.1 Statistical Sampling—Statistical techniques for deter- mm (0.75 in by 2.0 in) with a thickness of 1.6 mm to 4.8 mm
mining sample size, selecting materials for test, etc., should be (0.063 in to 0.19 in), with or without a hole, are preferred.
used. Alternative dimensions may be more suitable for testing of
7.2 Corrosion Products—The bulk sampling of products is liquid/vapor interface conditions.
outside the scope of this guide. 8.2.3 All specimens should be measured carefully to permit
accurate calculation of the exposed areas. A geometric area
8. Test Specimen calculation accurate to 61% is usually adequate.
8.1 At least duplicate test specimens should be exposed in 8.3 More uniform results can be expected if a uniform layer
each test. In laboratory immersion tests, corrosion rates of of metal is removed from the specimens to eliminate variations
duplicate specimens are usually within 610% of each other in condition of the original metallic surface. This can be done
when the attack is uniform. If the rates exceed this variance, by chemical treatment (pickling), electrolytic removal, or by
retesting should be considered. Occasional exceptions, in grinding with a coarse abrasive paper or cloth such as No. 50,
which a large difference is observed, can occur under condi- using care not to work harden the surface. Abrasive materials
tions of borderline passivity of metals or alloys that depend on may be picked up in the surface if the metal is soft, and may
a passive film for their resistance to corrosion. When large lead to pitting if not removed. At least 0.0025 mm (0.0001 in)
disparities in measured corrosion rates occur, rather than or 0.016 to 0.023 mg/mm2 (5 to 10 mg/in2 ) should be
reporting an average corrosion rate, the reason for the disparity removed. (If clad alloy specimens are to be used, special

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NACE TM0169/G31 – 12a

attention shall be given to ensure that excessive metal is not 8.6.3 The relative location of test specimens in the test
removed.) After final preparation of the specimen surface, the apparatus should be recorded prior to testing to permit test
specimens should be stored in a desiccator until exposure if specimen identification in the event the identification mark is
they are not used immediately. Materials that form passive corroded away.
films may give different results if exposed after different rest 8.7 Test specimens may be scrubbed with a bleach-free
times following polishing. In special cases (for example, for scouring powder followed by thorough rinsing in water and in
aluminum and certain copper alloys), a minimum of 24 h a suitable solvent (such as acetone, methanol, or a mixture of
storage in a desiccator is recommended. The choice of a 50% methanol and 50% diethylether), and air dried. For
specific surface treatment shall be considered on the basis of relatively soft metals such as aluminum, magnesium, and
the alloy to be tested and the reasons for testing. A commercial copper, scrubbing with abrasive powder is not always needed
surface may sometimes yield the most significant results. Too and can mar the surface of the test specimen.
much surface preparation may remove segregated elements, 8.7.1 Proper ultrasonic procedures are an acceptable alter-
surface contamination, and so forth, and therefore not be nate.
representative of the application. 8.7.2 The use of towels for drying may introduce an error
through contamination of the specimens with grease or lint.
8.3.1 Final surface treatment of the specimens should in-
8.7.3 Test specimens should be handled with gloves, twee-
clude finishing with No. 120 abrasive paper or cloth or the zers, or tongs to avoid contamination of the surface after
equivalent, unless the surface is to be used in the mill-finished cleaning.
condition. This resurfacing may cause some surface work 8.8 The mass of dried test specimens should be determined
hardening, to an extent that will be determined by the vigor of on an analytical balance to an accuracy of 1 mg or better. If
the surfacing operation, but is not ordinarily significant. The cleaning deposits (for example, scouring powder) remain or
surface finish to be encountered in service may be more lack of complete dryness is suspected, then recleaning and
appropriate for some testing. drying should be performed until a constant mass is attained.
8.3.1.1 Specimens of different alloy compositions should
never be ground on the same cloth. 9. Test Conditions
8.3.1.2 Wet grinding should be used on alloys that work 9.1 Selection of the conditions for a laboratory corrosion
harden readily, such as austenitic stainless steels. test shall be determined by the purpose of the test.
8.4 Sheared edges should be removed unless the purpose of 9.1.1 If the test is to be a guide for the selection of a material
the test is to study effects of the shearing operation or unless for a particular purpose, the limits of the controlling factors in
the effect of the deformation resulting from shearing is known service shall be determined. These factors include oxygen
concentration, temperature, rate of flow, pH value, composi-
to have no effect on corrosion. A sheared edge can be removed
tion, and other important characteristics of the solution.
before testing by wet grinding to a distance from the sheared
9.2 An effort should be made to duplicate all pertinent
edge equal to the thickness of the specimen. It may be desirable
service conditions in the corrosion test.
to test a surface representative of the material and metallurgical
9.3 Test conditions should be controlled throughout the test
conditions used in practice.
in order to ensure reproducible results.
8.5 As-laser-cut edges should be removed unless the pur- 9.4 Composition of Solution:
pose of the test is to study effects of the laser-cutting process. 9.4.1 Test solutions should be prepared accurately from
The effects of laser cutting can be removed from an edge chemicals conforming to the laboratory-grade standards, such
before testing by sanding or wet grinding to a distance from the as those of the Committee on Analytical Reagents of the
cut edge equal to 125 µm (0.005 in). American Chemical Society,4 and using reagent water (ASTM
8.6 The specimen may be stamped with an appropriate Specification D1193, Type IV or better), except in those cases
identifying mark. If metallic contamination of the stamped area in which naturally occurring solutions or those taken directly
may influence the corrosion behavior, chemical cleaning shall from plant processes are used.
be employed to remove any traces of foreign particles from the 9.4.2 The composition of the test solution should be accu-
surface of the coupon (for example, by immersion of stainless rately controlled and should be described as completely and
steel coupons in dilute nitric acid following stamping with steel precisely as possible when the results are reported.
dies). 9.4.3 Minor constituents should be included because they
8.6.1 The stamp, besides identifying the specimen, intro- often affect corrosion rates.
9.4.4 Chemical content should be reported as percentage by
duces stresses and cold work in the specimen that could be
mass of the solutions. Molarity and normality are also helpful
responsible for localized corrosion or stress-corrosion crack-
ing, or both.
8.6.2 Environmentally assisted cracking at the identifying 4
Reagent Chemicals, American Chemical Society Specifications, American
mark is a positive indication of susceptibility to such corrosion. Chemical Society, Washington, DC. For suggestions on the testing of reagents not
However, the absence of cracking should not be interpreted as listed by the American Chemical Society, see Analar Standards for Laboratory
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
indicating resistance. Additional types of tests should be and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
performed to specifically study the effects of stress. MD.

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NACE TM0169/G31 – 12a

in defining the concentration of chemicals in some test solu- 9.6 Gas Sparging of Solution:
tions. Solution density and pH should also be reported. 9.6.1 Most tests related to process equipment should be run
9.4.5 An environmental sampling plan should be devised. with the natural atmosphere inherent in the process, such as the
The test solution components of interest should be determined vapors of the boiling liquid or a controlled gas atmosphere.
before the test begins to avoid costs associated with measuring 9.6.2 If gas sparging or a controlled gas flow is employed,
components not of interest and to ensure that all components of the specimens should not be located in the direct air or gas
interest are measured before the test begins. Such a plan may stream from the sparger. Extraneous effects can be encountered
follow the guidance of ASTM Practice E300. When compo- if the air or gas stream impinges on the specimens. Gas
nents of interest in the solution are expected to change over spargers that create small bubbles are usually preferred to open
time, the composition of the test solution should be checked by tubes.
analysis before and after testing to determine the extent of NOTE 1—Assuming that all other factors are equivalent, the ratio of the
change in composition. It may be useful to analyze samples of gas flow rate to the total solution volume and the average gas bubble
the test solution during the test as well. In many cases, only diameter may be useful measures of sparging efficiency.
certain components of the test solution will be of interest, for
example those components that affect corrosiveness such as 9.6.3 If complete exclusion of dissolved oxygen is neces-
pH. It may be of interest to measure soluble corrosion products sary, specific techniques are required, such as prior heating of
such as metal ion content as a method of determining the the test solution and sparging with an inert gas (usually
amount of corrosion that has occurred. nitrogen). A liquid atmospheric seal (that is, vapor lock, similar
in function to a sink drain trap) is appropriate for use on the test
9.4.6 Evaporation losses may be controlled by a constant
vessel to prevent further contamination.
level device or by frequent addition of appropriate solution to
9.6.4 If a high oxygen concentration of the test solution is
maintain the original volume within 61%. The use of a reflux
desired, one method of achieving this is by sparging with pure
condenser ordinarily precludes the necessity of adding to the
oxygen. For lower concentrations of oxygen in the solution, the
original solution.
solution may be sparged with a mixture of oxygen with air or
9.4.7 In some cases, composition of the test solution may an inert gas. The saturation concentration of oxygen in a
change as a result of catalytic decomposition, by reaction with solution is proportional to the partial pressure of oxygen in the
the test specimen, or through the buildup of corrosion products gas mixture that is used for sparging. Care should be exercised
in the solution. These changes should be determined, if when sparging with oxygen or oxygen-enriched gas, since
possible. When required, the exhausted constituents should be many materials have enhanced flammability in gas enriched
added or a fresh solution provided during the course of the test. with oxygen.
9.4.8 If several different metals are exposed in the same 9.6.5 Other atmospheres may also be used as required to
volume of test solution, the corrosion products from one metal simulate a specific service. Sparging the gas into the test
may affect the rate of attack on another metal. For example, solution allows the gas composition to approach saturation if
copper corrosion products can reduce corrosion of stainless the sparging is continued for sufficient time. However, other
steel and titanium but can accelerate corrosion of aluminum. techniques may also be employed or required to achieve
9.5 Temperature of Solution: saturation specific concentration.
9.5.1 Temperature of the test solution is typically controlled 9.7 Test Solution Flow:
to within 61°C or 62°F. In tests where the temperature is 9.7.1 The effect of fluid flow is not usually determined in
significantly above ambient (for example, >10°C or 18°F) normal laboratory tests, although specific tests have been
some method of stirring is usually desirable to avoid tempera- designed for this purpose. Controlled-flow tests are outside the
ture gradients in the solution. Magnetic stirring or gas sparging scope of this guide. ASTM Guide G170, ASTM Practice G184,
is usually sufficient to minimize temperature gradients. and ASTM Practice G185 provide useful information regarding
9.5.2 If no specific temperature, such as boiling point, is testing under flowing conditions.
required or if a temperature range is to be investigated, the 9.7.2 In tests conducted below the boiling point, thermal
selected temperatures used in the test, and their respective convection may be an adequate source of liquid agitation.
duration, should be selected to match the application being 9.7.3 In test solutions with viscosities above 100 cp, supple-
investigated. mental controlled stirring with a magnetic stirrer is recom-
9.5.3 For tests that are intended to simulate systems that are mended.
at ambient temperature, the tests should be conducted at the 9.7.4 Gas sparging can effectively agitate the test solution
highest temperature anticipated for stagnant storage in summer and prevent stagnation and the development of unwanted
months. This temperature may be as high as from 40 to 45°C concentration gradients during the test. Gas sparging should
(104 to 113°F) in some areas. not be used in solutions that are prone to foaming.
9.5.4 Tests at the boiling point of the solution should be 9.8 Volume of Test Solution:
conducted with minimum possible heat input, and inert mate- 9.8.1 The volume of the test solution should be large enough
rial boiling chips should be used to minimize excessive to avoid any appreciable change in the test solution’s corro-
bumping, turbulence, and bubble impingement. The use of a siveness through either exhaustion of corrosive constituents or
reflux condenser is strongly recommended when tests are accumulation of corrosion products that might affect further
conducted at the boiling point. corrosion.

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9.8.2 For tests up to 30 days in duration, the preferred 9.10.4 The planned-interval test is an excellent procedure
minimum ratio of test solution volume to test specimen surface for evaluating the effect of time on corrosion of the metal and
area is 0.20 mL/mm2 (130 mL/in2 ). also on the corrosiveness of the environment in laboratory
9.8.3 When the test objective is to determine the effect of a tests. If the environment may change over time, short-duration
metal or alloy on the characteristics of the test solution (for exposures should be conducted at both the beginning and the
example, to determine the effects of metals on dyes), it is end of a longer exposure to ensure that the effects of environ-
desirable to reproduce the ratio of solution volume to exposed mental changes can be separated from the effects of exposure
metal surface that exists in practice. The actual time of contact time. Other procedures that require the removal of solid
of the metal with the solution should also be reproduced as corrosion products between exposure periods do not accurately
closely as possible to assure that the effects are simulated. measure the normal changes of corrosion with time unless this
9.9 Method of Supporting Specimens: simulates the operating conditions. For example, in laboratory
9.9.1 The supporting device and container should not be tests simulating flow through systems (for example, vapor
affected by or cause contamination of the test solution. condensers), long-term tests that do not involve regular chang-
9.9.2 The method of supporting test specimens varies with ing of the test solution may seriously underestimate the plant
the test apparatus used but should be designed to hold the condition corrosiveness by allowing corrosion products to
specimens securely enough to avoid rubbing against other saturate the test solution and create films that do not occur in
specimens, to insulate the test specimens from each other service. Electrochemical techniques such as polarization resis-
electrically, and to insulate the test specimens from any tance, linear polarization, electrochemical impedance spectros-
metallic container or supporting device used within the test copy, electrical resistance probes, and electrochemical noise
apparatus. The more tightly a specimen is held the more likely measurement often allow determination of the effects of time
it is to suffer crevice corrosion. Therefore it is usually found on corrosion behavior.
that a gentle support with a minimum area in contact with the 9.10.5 If anticipated corrosion rates are moderate or low, the
support device is best. The use of a small-diameter cylindrical following equation gives a suggested test duration:
hook through a larger-diameter hole in the specimen is most Duration of test ~h!
often effective. 5 50/corrosion rate ~mm/y! or 2000/corrosion rate ~mpy! (1)
9.9.3 The shape and form of the test specimen support 9.10.5.1 Example—When the corrosion rate is 0.25 mm/y
should assure free contact of the test specimen with the test (10 mpy), the test should run for at least 200 h.
solution, the liquid line, or the vapor phase, as shown in Fig. 1.
If clad alloys are exposed, special procedures are required to 9.10.5.2 This method of estimating test duration is useful
ensure that only the cladding is exposed, unless the purpose is only as an aid in deciding, after a test has been completed,
to test the ability of the cladding to protect cut edges in the test whether it is desirable to repeat the test for a longer period.
solution. Common testing periods are 24 to 240 h (1 to 10 days).
9.9.4 Some common supports are glass or ceramic rods, 9.10.5.3 This equation for test duration is acceptable for
glass cradles, glass hooks, fluorocarbon plastic strings, and general corrosion rates only. Localized attack, for example,
various insulated or coated metallic supports. pitting, environmentally assisted cracking, crevice attack, etc.,
9.10 Duration of Test: normally have an initiation period before attack begins.
9.10.1 The duration of any test should be determined by the 9.10.6 In some cases, it may be necessary to know the
nature and purpose of the test. degree of contamination caused by the products of corrosion.
9.10.2 Materials that experience severe corrosion generally This can be accomplished by analysis of the solution after
do not need lengthy tests to obtain accurate corrosion rates. corrosion has occurred. The corrosion rate can be calculated
However, there are cases in which this assumption is not valid. from the concentration of the matrix metal found in the
For example, lead exposed to sulfuric acid corrodes at an solution and it can be compared to that determined from the
extremely high rate at first, while building a protective film; mass loss of the specimens. However, some of the corrosion
then the rate decreases considerably so that further corrosion is products usually adhere to the specimen as a scale and the
negligible. This phenomenon of forming a protective film is corrosion rate calculated from the metal content in the solution
observed with many corrosion-resistant materials. Short tests is not always correct. Corrosion rates based on post-test
on such materials could indicate a high corrosion rate and be solution analyses may, in some cases, significantly underesti-
misleading. mate the actual specimen corrosion rate.
9.10.3 Short-time tests also can give misleading results on
alloys that form passive films, such as stainless steels. With 10. Cleaning Specimens after Test
borderline conditions, a prolonged test may be needed to 10.1 Before specimens are cleaned, their appearance should
permit breakdown of the passive film and subsequent more be observed and recorded. Location of deposits, variations in
rapid attack. Consequently, tests run for long periods are types of deposits, or variations in corrosion products are
considerably more realistic than those conducted for short extremely important in evaluating localized corrosion, such as
durations. On the other hand, corrosion should not proceed to pitting and concentration cell attack. Photographic documen-
the point where the original specimen size or the exposed area tation of the test specimens, before and after testing, may assist
is drastically reduced or where the metal is perforated. in the evaluation of test results.

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NACE TM0169/G31 – 12a

10.2 Cleaning specimens after the test is a vital step in the or extrapolated to millimetres per year, thousandths of an inch
corrosion test procedure and if not done properly, can cause per year, or any other arbitrary period because rarely, if ever, is
misleading results. Methods for chemical cleaning after testing the time of initiation or rate of propagation of pits uniform.
of specific metals and alloys are described in ASTM Practice 11.2.2 The size, shape, and distribution of pits should be
G1 and ISO 8407. noted. A distinction should be made between those occurring
10.2.1 Generally, the cleaning procedure should remove all underneath the supporting devices (in crevices) and those on
corrosion products from test specimens with a minimum the surfaces that were freely exposed to the test solution (see
removal of sound metal. ASTM Guide G46).
10.2.2 Set rules cannot be applied to specimen cleaning, 11.2.3 General corrosion rates calculated from mass loss on
because procedures vary, depending on the type of metal being materials that exhibit localized pitting or crevice corrosion may
cleaned and on the degree of adherence of corrosion products. seriously underestimate the rate of corrosion penetration that is
10.3 Cleaning methods can be divided into three general occurring. In these cases, mass loss rates may not be appro-
categories: mechanical, chemical, and electrolytic. priate for predicting performance. Localized corrosion penetra-
10.3.1 Mechanical cleaning includes scrubbing, scraping, tion does not usually proceed in a linear mode with exposure
brushing, mechanical shocking, media blasting, and ultrasonic time so that penetration rates for localized corrosion cannot be
procedures. Scrubbing with a bristle brush (preferably nonme- determined from a single time exposure.
tallic) and mild abrasive is the most popular of these methods. 11.3 If the material being tested is suspected of being
The others are used principally as a supplement to remove subject to dealloying forms of corrosion such as dezincification
heavily encrusted corrosion products before scrubbing. Care or to intergranular attack, a cross section of the specimen
should be used to avoid the removal of sound metal. should be microscopically examined for evidence of such
10.3.2 Chemical cleaning implies the removal of material attack.
from the surface of the test specimen by dissolution in an 11.4 The specimen may be subjected to simple bending tests
appropriate chemical solution. Solvents such as acetone and to determine whether any embrittlement attack has occurred.
alcohol are used to remove oil, grease, or resin and are usually 11.5 It may be desirable to perform quantitative mechanical
applied prior to other methods of cleaning. Chemicals are tests to compare the exposed test specimens with uncorroded
chosen for application to a specific material. specimens reserved for this purpose, as described in 8.1.1.
10.3.3 Electrolytic cleaning should be preceded by scrub-
bing to remove loosely adhering corrosion products. 12. Calculating Corrosion Rates
10.3.3.1 Precautions shall be taken to ensure good electrical
12.1 The calculation of corrosion penetration rates from
contact with the test specimen, to avoid contamination of the
mass loss data implies that the mass loss is distributed
cleaning solution with easily reducible metal ions, and to
uniformly over the surface area. Localized corrosion such as
ensure that inhibitor decomposition has not occurred.
pitting, crevice corrosion, intergranular corrosion, weld decay,
10.4 Whatever treatment is used to clean test specimens
etc., generally results in much greater penetration with the
after a corrosion test, its effect in removing metal should be
same mass loss as general corrosion. Pitting rates should not be
determined and the mass loss should be corrected accordingly.
based on a single test interval because pitting usually has an
An unexposed control specimen should be weighed before and
induction time for initiation. In cases in which localized
after exposure to the cleaning procedure to establish this mass
corrosion has been observed, the following notation is recom-
loss (see also ASTM Practice G1 and ISO 8407). Careful
mended: “Localized corrosion (indicate type if known) was
observation is needed to ensure that pitting does not occur
observed. The calculated penetration rate from mass loss
during cleaning.
measurements does not represent the actual maximum penetra-
10.4.1 Following removal of all scale, the specimen should
tion and may underestimate it significantly.”
be treated as discussed in 8.8.
12.2 The use of corrosion rates implies that the material has
11. Interpretation of Results not been internally attacked as by dezincification or intergranu-
11.1 After corroded test specimens have been cleaned, their lar corrosion.
masses should be measured with an accuracy corresponding to 12.3 Internal attack may be expressed as a corrosion rate, if
that of the original mass measurements. The mass loss during desired. However, the calculations should not be based on mass
the test period can be used as the principal measure of loss, which is usually small, but on microsections that show
corrosion. If all corrosion products cannot be removed, the depth of attack.
mass loss should be reported but the observation made that 12.4 Assuming that localized or internal corrosion is not
some corrosion products were not removed. present or is recorded separately in the report, the average
11.2 Following cleaning and mass loss determination, a corrosion rate can be calculated for flat prismatic geometries by
careful inspection of all specimen surfaces (that is, under low the following equation:
magnification) for the presence of localized attack should be Corrosion rate 5 ~K 3 W!/~A 3 T 3 D! (2)
conducted. If pits are observed, they should be evaluated
following the guidance of ASTM Guide G46. where:
11.2.1 Pit depths should be reported in millimetres or K = a constant (see below),
T = time of exposure in hours to the nearest 0.01 h,
thousandths of an inch for the test period and not interpolated

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NACE TM0169/G31 – 12a

A = area in cm2 to the nearest 0.01 cm2, 13.1.9 Testing dates and duration of each test.
W = mass loss in g, to nearest 1 mg (corrected for any loss 13.1.10 Chemical composition, trade name, producing mill,
during cleaning (see 10.4)), and and the UNS number (or material designation) of metals.
D = density in g/cm3, (see Appendix X1 of ASTM Practice 13.1.11 Form and metallurgical conditions of test specimens
G1). including weld details if relevant.
12.4.1 Many different units are used to express corrosion 13.1.12 Exact size, shape, and area of specimens.
rates. Using the above units for T, A, W, and D, the corrosion 13.1.13 Method used to prepare test specimens for expo-
rate may be calculated in a variety of units with the following sure.
appropriate value of K: 13.1.14 Number of test specimens of each material tested,
Constant (K) in Corrosion and whether specimens were tested separately or which speci-
Corrosion Rate Units Desired Rate Equation mens were tested in the same container.
mils per year (mpy) 3.45 3 106
inches per year (ipy) 3.45 3 103
13.1.15 Method used to clean specimens after exposure and
inches per month (ipm) 2.87 3 102 the extent of any error expected by this treatment.
13.1.16 Initial and final masses and actual mass losses for
millimetres per year (mm/y) 8.76 3 104
micrometres per year (µm/y) 8.76 3 107
each test specimen.
picometres per second (pm/s) 2.78 3 106 13.1.17 Appearance of each test specimen during and after
exposure, and the evaluation of attack, if other than general
grams per square metre per hour (g/m2·h) 1.00 3 104 3 DA
milligrams per square decimetre per day (mdd) 2.40 3 106 3 DA
corrosion, such as cracking, crevices, exfoliation, or pitting
micrograms per square metre 2.78 3 106 3 DA corrosion. Microscopic or photographic documentation may be
per second (µg/m2·s) of assistance.
A
Density is not needed to calculate the corrosion rate in these units. The density 13.1.18 Corrosion rates for each test specimen.
in the constant K cancels out the density in the corrosion rate equation.
13.1.19 Number and depths of pits or crevices.
12.4.2 These constants may also be used to convert corro- 13.1.20 Extent of other types of localized corrosion (that is,
sion rates from one set of units to another. To convert a intergranular attack, dealloying).
corrosion rate in units X to a rate of units Y, multiply by KY/KX, 13.1.21 Minor occurrences or deviations from the proposed
for example: test program.
15 mpy 5 15 3 [~2.78 3 10 6!/~~3.45 3 106!#pm/s 13.2 In cases in which replicate measurements of corrosion
rates have been made, the report should include the average,
5 12.1 pm/s (3) standard deviation, and coefficient of variation (that is, the
12.5 The average corrosion rate for cylindrical specimens standard deviation divided by the average expressed as a
such as wires can be calculated from the following equations: percent) for each set of conditions.
Corrosion rate 5 ~w 3 d!/~4 3 m 3 t! (4) 13.3 Any computerized reporting or transfer of data should
follow the guidelines of NACE SP0690 and ASTM Guides
or, when m/w > 50 G107 and G135.
Corrosion rate 5 1000 3 d [1 – w/ ~1,000 3 m!#0.5 / 2t (5)
14. Keywords
when corrosion rate is in mm/year,
14.1 accelerated; corrosion rate; immersion; laboratory;
where: mass loss; metals; pitting
w = mass loss in mg,
m = specimen mass in g,
d = specimen diameter in mm, and
t = exposure time in years.
13. Report
13.1 The following is a recommended guide for reporting:
13.1.1 Name of laboratory and operator conducting the
tests.
13.1.2 Corrosive media and concentration (including any
changes during test).
13.1.3 Volume of test solution and any solution added or
removed during test.
13.1.4 Temperature (maximum, minimum, average).
13.1.5 Gas sparging or controlled-atmosphere composition
(describe conditions or technique).
13.1.6 Agitation (describe conditions or technique).
13.1.7 Type of apparatus used for test.
13.1.8 Location of test specimen within test apparatus
(liquid, vapor, interface) and support method.

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NACE TM0169/G31 – 12a

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