Conducting Exfoliation Corrosion Tests in Aluminum Alloys: Standard Guide For
Conducting Exfoliation Corrosion Tests in Aluminum Alloys: Standard Guide For
Conducting Exfoliation Corrosion Tests in Aluminum Alloys: Standard Guide For
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
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G 112 – 92 (2003)
that will enhance the likelihood of obtaining reliable informa- tible to exfoliation, especially if the grain size is large. Often
tion, and tips and procedures to avoid pitfalls that could lead to the recrystallized surface layer on products such as extrusions,
erroneous results and conclusions. forgings, or sheet will not exfoliate, even though it corrodes
4.3 The following three areas of testing are considered: the intergranularly.
test materials starting with the “as-received” sample up through 5.4 Sample Temper—When a large sample is obtained as a
final specimen preparation, the corrosion test procedures in- stock item for use over a long time period, the extra material
cluding choice of test, inspection periods, termination point, should be stored in a stable temper and at a low enough
and rating procedures, and analyses of results and methods for temperature so that no further precipitation will occur to alter
reporting them. the starting condition of the metal. The unaged W temper of
4.4 This guide is not intended as a specific corrosion test 7XXX alloys is not stable and will continue to age harden at
procedure by which to evaluate the resistance to exfoliation of room temperature. Room temperature storage of such material
an aluminum alloy product. should be limited to a couple of months at most. Natural aging
4.5 This guide is not intended as a basis for specifications, of these alloys can be retarded almost completely by storing the
nor as a guide for material lot acceptance. material in a freezer at −40°C (−40°F) or colder. This factor is
of even more importance in determination of mechanical
5. Material properties than the investigation of corrosion resistance.
5.1 Sample Size—Most exfoliation tests do not require any
particular specimen size, but when beginning a new investiga- 6. Selection of an ASTM Test Method
tion it is best to obtain considerably more material than the
6.1 Selection of the appropriate ASTM test method(s) to use
minimum amount needed. About 50 to 100 % overage is
will depend primarily on the type of alloy and on the end use
recommended. This avoids the need of procuring a second
environment. When testing a new alloy or temper, a test
sample, that may have a different response, to complete any
method known to be applicable to the most similar commercial
confirmatory retests or extensions to a specific program.
alloy is normally selected. The user is cautioned, however, that
5.2 Sample Reproducibility—The specific location of
even small changes in alloy chemistry, or changes in process-
samples in a mill product, and the number of samples to take
ing method (for example, rapid solidification processes) can
are beyond the scope of this guide. When testing large
markedly effect resistance of an alloy and the appropriateness
production items, a typical procedure is to test at both ends
of a test method. Normally exfoliation tests are conducted on
(front and rear), and to test at the side and at the mid-width if
ingot metallurgy alloys, that tend to have the elongated grain
the product is 0.6 m (2 ft) or more in width. Thick products
structure prone to exfoliate. The known alloy applicability of
should be tested at various planes through the thickness.
the ASTM test methods are listed below. Included are some
5.2.1 In addition, some assessment should be made of the
observed instances where a test method was found to be
uniformity of a large sample, or of numerous small samples.
inappropriate, or at least produced results different than those
Typical quick check methods would be to measure electrical
observed on the initial qualification alloys.
conductivity or hardness. If the material variability has a
6.1.1 It is advisable to initially employ more than one
pattern, for example, a difference between front and rear of a
laboratory test method and determine whether they agree; or if
long extrusion, then this should be noted and the specimens
not, which method is the most discriminating. One procedure
segregated accordingly. If the variability is random, then
for doing this is to apply different fabrication procedures to the
multiple test specimens should be randomized.
metal that are known to generally affect resistance to exfolia-
5.3 Sample Microstructure—The directionality of the grain
tion and determine which of the test methods best detects
structure of aluminum alloys will markedly affect the suscep-
differences in the corresponding resistance to exfoliation.
tibility to exfoliation. When a product shape and alloy are
Fabrication variables that often affect resistance to exfoliation
being tested for the first time, it is advisable to macroetch full
are variable quench cooling rates, slow quenches being ad-
thickness by longitudinal and by transverse slices to establish
verse; and variable amounts of aging, underaged, or peak aged
the directionality and uniformity of the grain structure. Test
conditions generally being more susceptible than overaged
panels are normally positioned such that the test surface is
conditions. (1)3
parallel to the plane in the product with the most elongated
6.2 Test Method G 66 Acidified Salt Solution Exfoliation
grain structure. Complex shaped parts, such as certain extru-
Test (ASSET) is used for 5XXX alloys containing 2.0 % or
sions or die forgings, may have several categories of grain
more magnesium. The round robin qualification tests for this
structures and grain flow that do not necessarily follow the part
test method were conducted on alloys 5086 (3.5 to 4.5 % Mg)
geometry. Grain structure of such parts must be determined by
and 5456 (4.7 to 5.5 % Mg). (2) However, Test Method G 66
macroetching or from prior experience.
(ASSET) gives problem free exfoliation indications with all
5.3.1 For a given temper condition, unrecrystallized, pan-
5XXX alloys.
cake shaped grains, that are long and wide but relatively thin,
6.3 Test Method G 34 Exfoliation Corrosion (EXCO) Test is
are the most susceptible. Pancake shaped recrystallized grains,
intended for use with high strength 2XXX and 7XXX ingot
as in sheet, are the next most susceptible. This is followed by
the long, rod shaped grains found in extruded or rolled rod and
bar with a symmetrical cross section, for example, circle,
square, hex, or a rectangle with the width not more than twice 3
The boldface numbers given in parentheses refer to a list of references at the
the thickness. An equiaxed grain structure is the least suscep- end of the text.
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G 112 – 92 (2003)
metallurgy alloys, a 96 h period being prescribed for the 2XXX 6.6 Practice G 85 Annex A4 (SALT/SO2 Spray Testing) was
alloys and a 48 h period for the 7XXX alloys. developed using the same, 2XXX and 7XXX alloys as men-
6.3.1 For the 2XXX alloys, the round robin qualification tioned above for the EXCO method (7).
tests were conducted on alloys 2024 and 2124 in the T351 and 6.7 Both the methods in Annex A3 and Annex A4 of
T851 tempers. The appropriateness of the method has not been Practice G 85 result in more gelatinous corrosion products than
fully established for all other 2XXX alloys. It has been does Annex A2. This tends to increase pitting corrosion on the
reported as being too aggressive and nonrepresentative of specimens. Annex methods A2, A3, and A4 in Practice G 85
performance in outdoor atmospheres for alloys 2219, 2419 and are not equivalent, and the user should determine which
2519 in the T851 tempers (3) and for various Al-Li alloys in method best suits the alloys and applications under investiga-
both as-quenched and artificially aged tempers (1). tion.
6.3.2 For the 7XXX alloys the round robin qualification
7. Baseline Experience
tests were conducted on alloy 7075 in the T651, T7651, and
T7351 tempers and alloy 7178 in the T651 and T7651 tempers. 7.1 The best check on the appropriateness of an accelerated
Experience has shown that the EXCO method can be used for test is to determine whether the results it produces agree with
7050 and 7150 alloys in the T651, T6151, T7451, T7651, and known service experience.
T7751 tempers, but the test is somewhat more aggressive on 7.2 When there is no actual service experience, then expo-
these alloys (4). This method also was evaluated with copper sure in a severe outdoor atmosphere known to produce
free alloys such as 7021-T6 and 7146-T6, but generally an exfoliation corrosion is a useful approximation of the condi-
abbreviated exposure period of 16 to 24 h was used. tions a part will encounter in service. The most frequently used
6.3.3 Exposure of the powder metallurgy alloys 7090 and environments are seacoast sites and highly industrialized urban
7091-T6 specimens to EXCO results in rapid dissolution and locations. Selection of the particular environment to use can
powdering of the specimen, due to continuous drop of the best be based on the intended end use. If there is no prior
extremely fine grains. Four years of exposure of the same parts experience with the particular alloy being tested, then outdoor
to seacoast atmosphere resulted only in mild general corrosion tests should be started as soon as possible to establish a
and no exfoliation (5). baseline for eventual comparison.
7.3 Seacoast atmospheres are representative of the more
6.4 Annex A2 of Practice G 85 Modified ASTM Acetic Acid
extreme conditions most parts can encounter in service. How-
Salt Intermittent Spray Test, (MASTMAASIS) was developed
ever, it is noteworthy that “Seacoast Atmospheric Conditions”
using alloys 2024, 2124, 7075, and 7178. This method usually
prevail only in the immediate vicinity of the seashore. Gener-
is run in the wet bottom condition (some solution and high
ally “seacoast” conditions no longer exist after 0.4 Km (0.25
humidity always present). A dry bottom condition (no solution
mile) distance from the shoreline.
present and gradually falling humidity during the purge and
7.3.1 Significant differences have been noted in tests con-
non-spraying periods) has been recommended for 2XXX
ducted at the two beach sites at Kure Beach, NC which are
alloys.
located 25 and 250 m (80 and 800 ft) from the shoreline (8).
6.4.1 The test cabinets used to conduct the MASTMAASIS
7.3.2 A notable example of this effect is observed at the U.S.
test, and the salt fog tests subsequently described in 6.5 and
Army’s exposure sites at Fort Sherman, at the Caribbean
6.6, are produced by several suppliers. The fog delivery
entrance to the Panama Canal. The Breakwater and Coastal
systems and cabinet geometry can differ and have gradually
sites are within sight of each other and have been photographed
evolved. Consequently some cabinet to cabinet variability in
in one picture. However, the Breakwater site incurs direct
test results is inherent, due primarily to variation in spray
saltwater spray from wave action of the Caribbean Sea,
techniques and the relative humidity conditions during the
whereas the Coastal site is about 50 m (165 ft) from the shore
non-spray portions of the cycle.
and is protected from wave action by a coral reef. Depending
6.4.2 There is no record of the MASTMAASIS environ- on the season of the year and the length of exposure, corrosion
ment being unrealistically aggressive, causing exfoliation of a rates of iron and steel were two to nine times higher for the
material that did not subsequently exfoliate in the seacoast. As Breakwater site compared with the Coastal site (9).
such any occurrence of exfoliation in this test most likely 7.3.3 At least two years exposure is needed at a seacoast site
indicates susceptibility under some service conditions. The in order to be considered a significant length of exposure.
converse of this statement has not been observed. Materials with marked susceptibility to exfoliation normally
6.4.3 MASTMAASIS is not appropriate for 5XXX alloys, begin to show some evidence of it within 6 to 24 months.
because it does not always detect exfoliation susceptibility in Materials showing very mild susceptibility to exfoliation in
materials proven to be susceptible by other test methods. accelerated tests may require as long as seven to nine years of
6.4.4 MASTMAASIS has been used with some success on exposure at a seacoast site to develop a similar degree of
6XXX series alloys. However, in some cases it caused severe exfoliation (10).
intergranular corrosion that could be confused with exfoliation
corrosion unless specimens are examined metallographically. 8. Specimens
6.5 Annex A3 of Practice G 85 Seawater Acetic Acid Test 8.1 Specimen Size—There is no required specimen size or
(SWAAT) was developed using the same 5XXX, 2XXX, and shape, but it is advisable not to use too small a specimen since
7XXX alloys as mentioned above for the ASSET and EXCO visual inspection is a key interpretation method. Specimens
methods (6). should be at least 50 mm (2 in.) long and 25 mm (1 in.) or more
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G 112 – 92 (2003)
in width. This surface area permits visual interpretation as to earthward surface usually is more prone to exfoliate than the
whether any exfoliation is just protruding whiskers of metal, skyward surface. Joint Aluminum Association-ASTM groups
small flakes, or delamination of strips of metal. Typical sizes on atmospheric exfoliation testing have recommended earth-
are: 38 to 50 by 100 mm (1.5 or 2 by 4 in.) for the Test Method ward exposure to avoid washing of exfoliated surfaces by
G 34 EXCO test, and the Method G 66 ASSET test, 75 by 150 rainfall. When conditions are not known for a particular test
mm (3 by 6 in.) for the Practice G 85 Modified Salt Fog tests, site or a new material, it may be advisable to initially use
Annex A.2 (MASTMAASIS), A.3 (SWAAT) and A.4 (SALT/ duplicate panels exposing the test surface both skyward and
SO2), and 100 by 150 to 300 mm (4 by 6 to 12 in.) or larger for earthward. Single specimens can be used when the more
outdoor atmospheric tests. critical exposure position has been established.
8.2 Specimen Identification and Records—Considerable 8.6 Surface Preparation—Specimens should be degreased
material may be lost in the testing of susceptible materials, so with a suitable solvent and it is advisable to remove any mill
scribed or stenciled specimen numbers often are inadequate. scale by mechanical methods such as machining or standing,
Some sort of permanent identification should be used. One and so forth, or by appropriate etching. A frequently used etch
method for accelerated tests is to number the back side of the technique is to etch for 1 min in 5 % by weight sodium
specimen and then mask-off that area. A separate tag of a hydroxide solution at 80°C (175°F), rinse in water, desmut 30
non-corrodible, non-conducting material is another method. s in concentrated nitric acid at room temperature, rinse with
8.2.1 On-site tests frequently run for many years and may be distilled or deionized water, and air dry.
evaluated by several persons. It is important, therefore, to have
good initial records describing the original material, the speci- 9. Initiation of Specimen Exposure
mens, the test purposes, and the intended periods of exposure. 9.1 It is advisable to start short term tests, such as the 24 h
Clear records should also be maintained with descriptive ASSET test and the 48 h EXCO test, early in the day so that the
remarks or illustrative photographs for each inspection period. specimens can be given an initial inspection before the end of
8.3 Specimen Machining—Specimen edges may be sawed the work day.
or machined. If panels are obtained by shearing, the edges 9.2 Corrosion will initiate and progress sooner during the
should be dressed back by machining, sanding, or filing to a warmer months at outdoor tests that experience appreciable
depth equal to or greater than the specimen thickness. The seasonal changes in temperature and other climatic conditions.
cladding should be removed from the test surface of specimens When possible, it is best to start outdoor tests at the beginning
from alclad sheet and either removed or masked off on the back of the warmer seasons.
(non-test) surface. When machining panels for exposure of
interior planes (T/10, T/2, and so forth.) the final machining cut 10. Test Controls
should be a light one of 0.635 mm (0.025 in.) or less to avoid 10.1 It is always advisable to include control specimens
having a highly worked surface. The grain structure of such a from known materials representing both high and low resis-
worked surface may not exfoliate and instead create a mislead- tance to exfoliation. This is recommended for both accelerated
ing artifact by peeling off in one layer when the underlying and outdoor tests. Such controls verify the validity of a
structure corrodes. For very thick plate and other thick prod- particular test and permit the investigator to make some
ucts, a good procedure is to saw off most of the material and assessment of the normalcy of a particular test run. For
machine only the last 2.5 mm (0.100 in.) or so. If any cosmetic example, it cannot be concluded that a new material is resistant
differences (for example, color changes, scratches, surface to exfoliation if the susceptible control specimen did not
roughness, and so forth.) are noted on the as-machined exfoliate to the usual degree. In outdoor tests, the condition of
surfaces, they should be recorded. Subsequently the investiga- the susceptible control serves as an indicator of when a
tor should establish whether these visible differences had an significant exposure period has been accrued. Controls are
effect on initiation or development of exfoliation. especially advisable in outdoor tests that encounter variable
8.4 Specimen Framing—Guidelines for outdoor exposure of conditions in temperature, rainfall, airborne pollutants, and so
metals are given in Practice G 50. Specimens exposed outdoors forth, beyond the control of the investigator.
should preferably be held in place by inert, non-conducting
fasteners and holders. Any metallic fasteners must be galvani- 11. In-Test Inspection
cally compatible with the test specimens, or be insulated from 11.1 Periodic Inspection—Even though there usually is a
them. It is advisable to have the panels offset from the prescribed test period, it is a good practice to inspect the panels
mounting rack, regardless of the material of construction of the in-situ during the course of the exposure to note when
rack. Normal corrosion test procedures should be used to exfoliation begins and how it progresses. Care should be taken
ensure that each specimen is electrically isolated from other so as not to dislodge any exfoliated metal from specimens
specimens and from specimen holders. Ceramic, fiber, or showing appreciable corrosion. A specimen is usually removed
plastic washers are often used to mount outdoor specimens and from test when it becomes so severely exfoliated that there is
the crevice created between the washer and the test specimen a risk of the exfoliated metal falling off with continued
may hasten the onset of exfoliation. exposure.
8.5 Many outdoor exposure tests expose the principal test 11.2 EXCO specimens, that are usually exposed for 48 h,
surface skyward to incur maximum exposure to sunlight and can be inspected after 4 to 6 h (or at the end of the first working
airborne pollutants. However, experience has shown that the day) and after 24 h exposure. Salt fog (MASTMAASIS and
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G 112 – 92 (2003)
SWAAT) specimens can be inspected after periods of 3, 7, 10, together with probable clean-up efforts. Ideally atmospheric
and 14 days. If the investigator has no idea what to expect of conditions should be continuously monitored, by means such
a new alloy or temper, it is advisable to expose replicate as those covered in Practice G 92. This includes both collection
specimens that can be removed individually as significant of atmospheric data and periodic exposures of standard speci-
progress in exfoliation is noted. mens of known response.
11.3 Outdoor Tests—Specimens exposed outdoors to natu-
ral atmospheres should be examined twice per year, or more 13. Post-Test Appraisal
often, during the first two years of exposure and at least yearly 13.1 Visual inspection—The first post test appraisal should
thereafter. In regions where the climate varies seasonally, some always be a visual inspection with no cleaning done to the
investigators prefer to make the biannual inspections in early specimens. Photographs may be advisable at this stage, (see
spring and late fall rather than on a strict semiannual basis. 13.4.1). After the panels are rated in this manner, their
11.3.1 Frequently a specimen is photographed when exfo- condition may warrant cleaning by rinsing in water and then
liation is first noted, and again when appreciable changes soaking in concentrated nitric acid and rinsing (see Practice
occur. Visual inspection may not be able to establish whether G 1), but no scraping or abrasion should be done. This is
exfoliation is present on an atmospheric specimen showing followed by reappraisal and photographing as needed.
only mild surface corrosion. In such cases it may be advisable 13.2 Standard Terminology and Ranking Guides—Much of
to remove a small coupon from a corner for metallographic the interpretation of exfoliation test results is given in qualita-
examination of the cross-section to establish the type of tive descriptions of the specimens, and not in any sort of
corrosion present. Specimens should be returned to test as numerical data. It is important therefore to use accepted
quickly as possible, and care should be taken to avoid terminology to avoid confusion between the writer and reader
contamination of the test surface with materials not present at of the report. To date an attempt at such a standard is contained
the outdoor site. Time spent out of the intended atmosphere in Test Methods G 34 and G 66 that have the first three
should be recorded, along with any unintended circumstance or categories listed in Table 1.
incident.
TABLE 1 Descriptions and Ranking Codes
12. Duration or Termination of Exposure
Classification Code
12.1 In any environment, testing of individual specimens
No appreciable attack N
generally is terminated when they become so corroded that Pitting corrosion only P
further exposure is likely to result in complete loss of the Exfoliation Four degrees, EA, EB, EC, and ED
exfoliated metal, or when the material’s performance is judged in order of increasing severity.
General corrosion G
to be too poor to be of commercial interest. Intergranular corrosion IG
12.2 Accelerated Tests—Standard tests generally are con-
ducted for the recommended exposure period. If no appreciable
exfoliation is observed on a new alloy or temper, the period can NOTE 1—Test Methods G 34 and G 66 both use the same rating code,
be doubled. If this still does not produce significant exfoliation but different illustrative photographs.
it generally can be concluded that the material is not suscep- 13.2.1 Two types of corrosion often are encountered that are
tible to exfoliation in that test method. not listed in Table 1. These are general corrosion, that can
12.3 Outdoor Tests—Past experience has shown that mate- approach uniform corrosion, and intergranular corrosion with-
rials that are very prone to exfoliation in service conditions will out any presence of exfoliation. These two additional classifi-
show marked exfoliation within four years exposure at severe cations and a corresponding code are listed below the exfolia-
outdoor sites, such as seacoast and certain highly industrialized tion ratings in Table 1 for the user’s consideration.
urban areas. If test space is limited, specimens surviving this 13.2.2 Certainly there is no confusion over the first two
length of exposure at outdoor sites known to cause exfoliation, categories in the ranking code of Table 1, especially if the
can be terminated and considered “not highly susceptible.” visual rating is substantiated by metallographic examination.
However, some investigators now have programs of 20 or more Conversely, the proper classification is not always obvious for
years duration and the indication is that continued exposure specimens showing various degrees of exfoliation. Two sets of
will discriminate between materials with the “better and best” illustrative photographs have been developed for Test Method
resistance. At this time there is no established time period after G 34, but confusion still exists when the appearance of a test
which it can be concluded that exfoliation will never occur. For panel is borderline between adjacent groupings, Categories A
long life applications, the limiting maximum exposure most to B, or B to C, and C to D. Thus a rating difference of one
likely has to be agreed upon by users and producers, based on letter grade is not uncommon when a set of panels is ranked by
the life expectancy of the product. more than one rater. For the best consistency and reproducibil-
12.4 When long time outdoor tests are conducted, the ity in rating, it is recommended that glossy prints of the
investigator must realize that all outdoor environments are standard photographs be used, and that these photographs be
changeable. Most sites experience cyclic atmospheric condi- placed next to the specimens being rated.4
tions. Also these conditions may increase and decrease in
corrosiveness, often as a function of surrounding environmen-
tal factors beyond the control of the investigator. This is 4
Enlarged glossy prints of Figs. 1 through 6 in Test Method G 34 are available
highlighted by the current critical issue of acid precipitation, from ASTM headquarters. Order PCN 12-700340-22.
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G 112 – 92 (2003)
13.2.3 Much of this variability results from individual 13.6 Metallographic Examination—Unless there is clear
interpretation and judgment as to: how uniformly the surface is evidence that the specimen is definitely exfoliated, it is
exfoliated and whether attention is given to an isolated site of advisable to metallographically examine a cross-section of the
increased severity, how obvious it is that shreds or flakes of specimen for determination of the type and extent of corrosion.
metal are protruding and actual delamination occurred, and For example, an Al-Li alloy that was expected to be susceptible
how deeply exfoliation has penetrated into the specimen. Also to exfoliation did in fact delaminate, but the exfoliated layers
some raters view specimens only in-situ, while others may were still so tightly adherent that this condition could be
carefully remove them from the solution for viewing under detected only when magnified. Conversely, other specimens
more optimum lighting, or at different angles of view. such as certain 2XXX-T8 or 7XXX-T7 type alloys can corrode
13.2.4 Until better descriptors of exfoliation are developed, appreciably in the EXCO test and be covered with corrosion
it probably is best to use the coding and photographs in Test debris not readily distinguishable from genuine exfoliation.
Method G 34 as a relative ranking guide. For the most part they Metallographic examination is needed to establish whether the
have been adequate for development or characterization inherent type of corrosion is merely pitting, with perhaps minor
projects wherein the investigator primarily seeks to establish intergranular corrosion and a large quantity of residual corro-
whether the degree of susceptibility is increasing or decreasing, sion product; or actual delamination by intergranular exfolia-
tion.
or is significantly affected by process changes.
13.7 Quantitative Analysis—No satisfactory quantitative
13.3 The investigator must realize, however, that the limit of
method has as yet been established for the analysis and ranking
acceptable performance usually is established by a producer/
of degrees of exfoliation. Investigators are urged to continually
user agreement based on exfoliation test results, other design
look for improved analytical tools, especially when developing
and economic considerations, and prior service experience. new materials or new test techniques.
Such a determination is beyond the scope of this guide.
13.7.1 Relative comparison of the gross depth and extent of
13.4 Photographs—If there is any doubt as to how to rank exfoliation may be a useful method of analysis for specimens
a specimen, it probably is best to use photographs to ad- exposed simultaneously to the same test. However, current
equately describe its condition. Often this is necessary for imprecision in exfoliation test procedures has precluded at-
atmospheric specimens that do not exfoliate uniformly and to tempts to establish precise criteria.
the same degree over the entire panel. Most investigators use a 13.7.2 Attempts have been made to evaluate the extent of
photographic magnification as close as possible to 13 (that is, exfoliation in accelerated tests by mass loss, after removing the
full size) since this will minimize the possibility of exaggerat- loosely adherent metal by cleaning and scrubbing with a bristle
ing or underplaying the specimens visual appearance. Experi- brush. Such an approach may be useful, but the investigator
ence, plus the condition of the specimen, will help decide first has to establish that all exfoliation occurs uniformly over
whether to focus straight down on a specimen, or to view it at the surface and that the exfoliated metal can be readily
an angle with lighting from the side to emphasize the lamina- removed. Panels of susceptible 5XXX series alloys and low-
tions and lifting of the exfoliated metal. copper 7XXX alloys often delaminate, but the overlying metal
13.4.1 Photographs first should be taken of the specimen as does not become dislodged. Corrosion products can become
removed from the test without any chemical cleaning. Panels entrapped so that such specimens show a mass gain. A mass
from immersion or fog tests should be photographed as quickly gain does not occur uniformly enough to be used as a method
as possible, since they will continue to corrode and change in of appraisal.
appearance even though they have been removed from the test.
Frequently it is advisable to wet them slightly, being careful 14. Reporting
not to dislodge loosely adherent metal. A damp surface helps to 14.1 Most standard test methods have sections covering the
give a sharper focus to the edges of metal flakes, than is type of things that should be reported. Examples are a full
possible with a completely dry specimen. description of the material, the tests conducted, and any
13.5 Chemical Cleaning—Sometimes it is helpful to clean divergency from standard procedure, and so forth. Such re-
specimens by a brief immersion (up to about 10 min) in quirements are taken for granted in this guide, and the intent is
concentrated nitric acid to remove loose corrosion products and to comment only on suggestions of reporting techniques unique
salt deposits, while taking care to retain the adherent exfoliated to exfoliation tests.
metal. The specimens should be gently immersed into the acid 14.2 If there are a lot of specimens to be reported, the
and kept in a relatively horizontal position at all times, with the investigator should first tabulate them, describing the material
exfoliated surface upwards, so as to avoid dislodging any more variables and test results of each specimen in detail. If very
metal than is inevitable. If the cleaning operation enhances the lengthy, this could be an appendix. The investigator should
ability to rate the specimen, then it is probably worth repho- then try to group results, and compare specimens graphically
tographing. Such cleaning generally is necessary if the inves- by code or an arbitrary number system. This will assist the
tigator wants to retain the corroded specimen for display reader to group similar specimens more quickly, and to grasp
purposes. Cleaned exhibit specimens can also be shrink- the magnitude of relative differences between specimens and
wrapped in plastic, or merely wrapped in a commercial plastic specific test parameters. The investigator should also note
“cling-wrap” to help prevent loosely adherent exfoliated metal whether the performance of replicate panels was consistent, or
from being dislodged. whether there was variability in the material’s performance.
6
G 112 – 92 (2003)
14.3 If the investigator has prior knowledge of the minimum alloys; atmospheric tests; exfoliation corrosion; immersion
performance needed for a specific application, then the test tests; salt fog (spray) tests; test procedures; test problems
results should be analyzed in that manner as well, for example,
does not meet, meets, or exceeds requirements for service, and
so forth.
15. Keywords
15.1 accelerated test; 2XXX aluminum alloys; 5XXX alu-
minum alloys; 6XXX aluminum alloys; 7XXX aluminum
REFERENCES
(1) Colvin, E. L., and Murtha, S. J., “Exfoliation Corrosion Testing of (6) Ketcham, S. J., and Jeffrey, P. W., “Exfoliation Corrosion Testing of
Al-Li Alloys 2090 and 2091,” Proceedings of the Fifth International 7178 and 7075 Aluminum Alloys,” Report of ASTM G01.05 Inter-
Aluminum-Lithium Conference, Williamsburg, VA, Materials and laboratory Testing Program in Cooperation with the Aluminum Asso-
Component Engineering Publications Ltd, U.K., March 24–31, 1989, ciation.
p. 1251. (7) Ketcham, S. J., and Jankowsky, E. J., “Developing an Accelerated
(2) Sprowls, D. O., Walsh, J. D., and Shumaker, M. B., “Simplified Test: Problems and Pitfalls,” Laboratory Corrosion Tests and Stan-
Exfoliation Testing of Aluminum Alloys,” Localized Corrosion— dards ASTM STP 866, ASTM, 1985, pp. 14–23.
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