Designation: G 34 – 01 (Reapproved 2007)

Standard Test Method for

Exfoliation Corrosion Susceptibility in 2XXX and 7XXX
Series Aluminum Alloys (EXCO Test)1
This standard is issued under the fixed designation G 34; the number immediately following the designation indicates the year of original
adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript
epsilon (e) indicates an editorial change since the last revision or reapproval.
This standard has been approved for use by agencies of the Department of Defense.

1. Scope 3. Terminology
1.1 This test method covers a procedure for constant im- 3.1 Definitions:
mersion exfoliation corrosion (EXCO) testing of high-strength 3.1.1 exfoliation—corrosion that proceeds laterally from the
2XXX and 7XXX series aluminum alloys. sites of initiation along planes parallel to the surface, generally
NOTE 1—This test method was originally developed for research and
at grain boundaries, forming corrosion products that force
development purposes; however, it is referenced, in specific material metal away from the body of the material giving rise to a
specifications, as applicable for evaluating production material (refer to layered appearance (Terminology G 15).
Section 14 on Precision and Bias).
4. Summary of Test Method
1.2 This test method applies to all wrought products such as
sheet, plate, extrusions, and forgings produced from conven- 4.1 This test method provides an accelerated exfoliation
tional ingot metallurgy process. corrosion test for 2XXX and 7XXX series aluminum alloys
1.3 This test method can be used with any form of specimen that involves the continuous immersion of test materials in a
or part that can be immersed in the test solution. solution containing 4 M sodium chloride, 0.5 M potassium
1.4 This standard does not purport to address all of the nitrate, and 0.1 M nitric acid at 25 6 3°C (77 6 5°F). The
safety concerns, if any, associated with its use. It is the susceptibility to exfoliation is determined by visual examina-
responsibility of the user of this standard to establish appro- tion, with performance ratings established by reference to
priate safety and health practices and determine the applica- standard photographs.
bility of regulatory limitations prior to use. 5. Significance and Use
2. Referenced Documents 5.1 This test method was originally developed for research
2.1 ASTM Standards: 2 and development purposes; however, it is referenced, in
D 1193 Specification for Reagent Water specific material specifications, as applicable for evaluating
E 3 Guide for Preparation of Metallographic Specimens production material (refer to Section 14 on Precision and Bias).
G 15 Terminology Relating to Corrosion and Corrosion 5.2 Use of this test method provides a useful prediction of
Testing the exfoliation corrosion behavior of these alloys in various
G 112 Guide for Conducting Exfoliation Corrosion Tests in types of outdoor service, especially in marine and industrial
Aluminum Alloys environments.4 The test solution is very corrosive and repre-
2.2 ASTM Adjuncts: sents the more severe types of environmental service, exclud-
Illustrations (Enlarged Glossy Prints)3 ing, of course, unusual chemicals not likely to be encountered
in natural environments.
5.3 The exfoliation ratings were arbitrarily chosen to illus-
trate a wide range in resistance to exfoliation in this test.
1
This test method is under the jurisdiction of ASTM Committee G01 on However, it remains to be determined whether correlations can
Corrosion of Metals and is the direct responsibility of Subcommittee G01.05 on be established between EXCO test ratings and realistic service
Laboratory Corrosion Tests.
Current edition approved May 1, 2007. Published May 2007. Originally
conditions for a given alloy. It is an ongoing activity of the
approved in 1972. Last previous edition approved in 2001 as G 34–01.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
4
contact ASTM Customer Service at [email protected]. For Annual Book of ASTM Ketcham, S. J., and Jeffrey, P. W., “Exfoliation Corrosion Testing of 7178 and
Standards volume information, refer to the standard’s Document Summary page on 7075 Aluminum Alloys” (Report of ASTM G01.05 Interlaboratory Testing Program
the ASTM website. in Cooperation with the Aluminum Association); and Sprowls, D. O., Walsh, J. D.,
3
Available from ASTM International Headquarters. Order Adjunct No. and Shumaker, M. B., “Simplified Exfoliation Testing of Aluminum Alloys,”
ADJG003402. Original adjunct produced in 1980. Localized Corrosion—Cause of Metal Failure, ASTM STP 516, ASTM, 1972.

Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.

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 G 34 – 01 (2007)
Task Group on Exfoliation Corrosion of Aluminum Alloys 9.2 The edges of sawed specimens need not be machined,
(G01.05.02.08) to maintain outdoor exposure tests for this but specimens obtained by blanking or shearing shall have
purpose. For example, it has been reported5 that samples of edges dressed by machining or filling to a depth equal to the
Al-Zn-Mg-Cu alloys rated EA or P in a 48-h EXCO test did not thickness of the specimen to remove cold-worked metal.
develop more than a slight amount of incipient exfoliation 9.3 Remove the cladding of alclad sheet by machining the
(EA) during six- to nine-year exposures to seacoast atmo- test surface; remove or mask the cladding on the back side
spheres, whereas, ED rated materials in most cases developed (non-test surface) also.
severe exfoliation within a year in the seacoast atmosphere. It 9.4 When removing test specimens from extrusions and
is anticipated that additional comparisons will become avail- forgings, take care to avoid specimen locations underneath
able as the outdoor tests are extended. flanges, ribs, etc., where the grain structure is usually variable.

6. Apparatus 10. Standardization

6.1 Any suitable glass, plastic, or similarly inert container 10.1 To provide an indication when some inadvertent de-
can be used to contain the solution and specimens during the viation from the correct test conditions occurs, it is necessary
period of test. Depending upon the shape and size of the to expose to the test at regular intervals a control specimen of
specimens, rods or racks of glass, plastic, or any inert sub- a material with known resistance. This control should exhibit
stance shall be used to support the specimen above the bottom the same degree of exfoliation each time it is included in the
of the container. The container should be fitted with a loose- test.
fitting cover to reduce evaporation. 10.2 The control may be any material of the alloy type
included in the scope of this test method, preferably one with
7. Reagents an intermediate degree of susceptibility (Fig. 1 and Fig. 2).
7.1 Purity of Reagents—The test solution shall be prepared 11. Procedure
with reagent grade sodium chloride (NaCl), potassium nitrate
11.1 Degrease the specimens with a suitable solvent.
(KNO3), and nitric acid (HNO3).
11.2 Mask the back surfaces of the specimens to minimize
7.2 Purity of Water—Distilled or deionized water shall be
corrosion of non-test areas. Protective coatings must have good
used to prepare test solution. The water purity must conform to
adherence to avoid crevice corrosion beneath the coating; also,
Specification D 1193, Type IV reagent water, except that for
they should not contain leachable ions or protective oils that
this method, the values of chloride and sodium can be
will influence the corrosion of the test surface. (See Figs. 1-6.)3
disregarded.
11.3 Use the solution in sufficient quantity to provide a
7.3 A test solution of the following composition shall be
volume-to-metal surface area ratio of 10 to 30 mL/cm2 (65 to
used:
200 mL/in.2). Include all exposed metal area in the determina-
NaCl (4.0 M)
KNO3 (0.5 M) tion of total surface area.
HNO3 (0.1 M) 11.4 Use fresh solution at the start of each test. Do not
Dissolve 234 g of NaCl, 50 g of KNO3 in water, and add 6.3 change the solution even though the pH increases during the
mL of concentrated HNO3 (70 weight %). Dilute to 1 L. This test. It is normal for the pH to increase from the initial apparent
solution has an apparent pH of 0.4. value of 0.4 to about 3 during the first several hours depending
7.4 The solution shall be maintained at a temperature of 25 upon the amount of corrosion that occurs.
6 3°C (77 6 5°F). 11.5 Immerse the specimens in the solution using rods or
racks of inert material to support the specimens above the
8. Sampling bottom of the container. Place the test surface upward in a
horizontal position to prevent loss of exfoliated metal from the
8.1 Sampling procedures are not considered applicable to
surface of the specimen. Do not concurrently immerse in the
this test method, as they are often covered by product specifi-
same container alloys containing less than 0.25 % copper with
cations. It is assumed that the test specimens are removed from
those containing greater amounts of copper.
representative samples of materials.
11.6 The following maximum periods of exposure are
9. Test Specimens recommended for testing the alloy types indicated:
2XXX Series 96 h
9.1 Specimens may be of any practical size or shape. 7XXX Series 48 h
Nevertheless, for the results to be of most significance a
specimen size of at least 50 by 100 mm (2 by 4 in.), or the The length of time to develop exfoliation in material of a
equivalent, is recommended. given alloy and temper may vary with the mill product form,
with some materials developing severe exfoliation in much
shorter periods than those listed. Therefore, inspect test speci-
5
Sprowls, D. O., Summerson, T. J., and Loftin, F. E., “Exfoliation Corrosion mens in place and rate in accordance with Section 12 at periods
Testing of 7075 and 7178 Aluminum Alloys—Interim Report on Atmospheric such as 5, 24, 48, and 72 h, and discontinue the exposure of a
Exposure Tests” (Report of ASTM G01.05.02 Interlaboratory Testing Program in specimen when it has developed the most severe exfoliation
Cooperation with the Aluminum Association); and Lifka, B. W. and Sprowls, D. O.,
“Relationship of Accelerated Test Methods for Exfoliation Resistance in 7XXX
rating (Fig. 6).
Series Aluminum Alloys With Exposure to a Seacoast Atmosphere,” Corrosion in 11.7 Rate the performance of test specimens in accordance
Natural Environments, ASTM STP 558, ASTM, 1974. with Section 12 immediately after discontinuation of the

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 G 34 – 01 (2007)

Undermining pitting that may form the surface give the appearance of incipient exfoliation (Keller’s Etch; 1003).
FIG. 1 Examples of Pitting Corrosion

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 G 34 – 01 (2007)

Exfoliation resulting from rapid lateral attack of selective boundaries or strata forming wedges of corrosion product that force layers of metal upward giving rise to a
layered appearance (Keller’s Etch; 1003).
FIG. 2 Four Degrees of Severity of Exfoliation Corrosion

exposure while the specimens are still wet or moist, taking into 12.2.2 P— Pitting: Discrete pits, sometimes with a tendency
account all loose products of exfoliation lying on the test for undermining and slight lifting of metal at the pit edges (Fig.
specimen or on the bottom of the container. 1).
11.8 Clean exposed test specimens, if desired, by rinsing in 12.2.3 EA through ED—Exfoliation (Figs. 1-6):
water and soaking in concentrated nitric acid after the speci- 12.2.3.1 Visible separation of the metal into layers mani-
mens have been inspected and rated. fested in various forms, such as blisters, slivers, flakes, fairly
12. Interpretation of Results continuous sheets, and sometimes granular particles resulting
from disintegration of thin layers, depending upon the grain
12.1 The following codes and classifications shall be used
morphology of the sample. Various degrees of exfoliation with
when reporting the visual rating of corroded specimens:
increasing penetration and loss of metal are illustrated in Fig.
Classification Code
No appreciable attack N
2. Additional examples of the various ratings are shown in
Pitting P Figs. 3-6.
Exfoliation EA through ED
12.2.3.2 The formation of tiny pit-blisters or the dislodge-
12.2 Descriptions of the various classifications, which are ment of an extremely thin surface layer of metal after only a
illustrated in Figs. 1-6,3 are as follows: few hours of exposure may resemble superficial exfoliation
12.2.1 N—No appreciable attack: Surface may be discol- (EA), but can in fact result from undermining pitting. If
ored or etched, but no evidence of pitting or exfoliation. continued exposure to the recommended periods in 11.6

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 G 34 – 01 (2007)

FIG. 3 Examples of Exfoliation Rating EA (Superficial): Tiny Blisters, Thin Slivers, Flakes or Powder, with only Slight Separation of
Metal

FIG. 4 Example of Exfoliation Rating EB (Moderate); Notable Layering and Penetration into the Metal

produces more corrosion but no evidence of advancing delami- rating a series of test specimens to compare them with the
nation, metallographic examination (see Guide E 3) will be photographs and captions in Figs. 1-6 rather than with each
required to determine whether the initial effect was truly other. The final rating of a specimen shall be determined by the
exfoliation (Fig. 2) or undermining pitting (Fig. 1); in the latter poorest classification observed during the exposure.
case the rating should be P. 12.3.1 When it is difficult to classify a specimen, it is
12.2.3.3 When exfoliation occurs in isolated sites, rate the advisable to place it in the category of greater susceptibility.
worst localized condition observed.
12.3 The visual ratings are intended to be finite indications NOTE 2—Enlarged glossy prints of Figs. 1-6 are available from ASTM
of the resistance to exfoliation, and care should be taken when International.3 These prints are more convenient to use and are of better

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 G 34 – 01 (2007)

FIG. 5 Examples of Exfoliation Rating EC (Severe): Penetration to a Considerable Depth into the Metal

FIG. 6 Examples of Exfoliation Rating ED (Very Severe) (Similar to EC Except for Much Greater Penetration and Loss of Metal)

quality than the reproductions in the printed standard. The user is urged to 13.1.4 A rating of the test specimens using the codes and
obtain and use these prints. classifications in Section 12, and
13. Report 13.1.5 Notation of any deviation in test procedure from that
13.1 The report should contain the following essential set forth in preceding paragraphs.
information: 13.2 Other information that may be desirable for certain
13.1.1 Alloy and temper of the material tested, types of reports includes:
13.1.2 Mill product, section thickness, and the surface 13.2.1 Size, type, and number of replicate specimens;
tested, including reference to applicable product specification, method of edge preparation, and
13.1.3 Sampling procedure if other than that specified in 13.2.2 Volume to surface ratio.
referenced product specification,

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 G 34 – 01 (2007)
14. Precision and Bias
14.1 Precision:
14.1.1 The precision of the data from this test method was
evaluated by way of an interlaboratory test program using two
non-commercial tempers of Alloy 7075 with different levels of
exfoliation corrosion susceptibility. Seven laboratories, includ-
ing experienced and inexperienced users, participated in the
round robin. The laboratories received rough machined panels,
which they finish machined, exposed according to the proce-
dure in this test method, and rated visually according to the
photographs included in this test method.
14.1.2 The raw data from laboratories is listed in Table 1
and plotted in Fig. 7. All seven laboratories rated the more
susceptible T6X material as having severe or very severe
exfoliation corrosion as designated by the ratings EC and ED.
However, for the more resistant T7X temper there was no FIG. 7 Histogram of Visual Exfoliation Ratings by Seven
Laboratories for Two Tempers of 7075 Plate Tested at the T/4
agreement as the visual ratings ranged from pitting only to very
Plane
severe exfoliation as designated by the ratings P to ED. Fig. 7
shows that there was no clustering of the ratings either, they
seem to follow a uniform distribution.
14.1.2.1 The data in Table 1 show the ratings were repeat-
able within laboratories. In each case the same rating was
obtained for both panels tested by the individual laboratory.
14.1.2.2 The reproducibility of ratings among different
laboratories is shown most clearly in Fig. 7. In addition to the
visual ratings, one of the laboratories measured the depth of
corrosion using an ultrasonic technique (the laboratories re-
ported original panel thickness) and the data showed not only
that the two tempers had different amounts of exfoliation, but
that there was good consistency within each temper as plotted
in Fig. 8. Thus the laboratory to laboratory variation in ratings
for the T7X material resulted from individual rater’s interpre-
tation of the photographs and wording used to define the visual
rating system. Samples with resistance, that is, intermediate
between highly susceptible and highly resistant samples can be FIG. 8 Histogram of Average Corrosion Depths as Measured by
the most difficult to rate visually, which is confirmed by these Ultrasonic Inspection for Two Tempers of 7075 Plate at the T/4
Plane
results. One of the reasons for this is corrosion debris that does
not result from exfoliation corrosion as discussed in Guide
G 112. highly susceptible samples, but produces a large amount of
14.1.2.3 Based on the results from this interlaboratory test laboratory-to-laboratory variaition for tempers with intermedi-
program, the visual rating system gives consistent ratings for ate levels of resistance. Experience indicates that the visual
ratings will produce more consistent results for highly resistant
TABLE 1 Visual Ratings from Interlaboratory Test of Alloy 7075
samples, such as 7075–T73X products, than it does for samples
Plate in Two Noncommercial Tempers with intermediate resistance, such as T7X tested in this
T6X T7X
interlaboratry test program.
Laboratory 14.2 Bias—The procedure in Test Method G 34 has no bias
Specimen 1 Specimen 2 Specimen 1 Specimen 2
because the exfoliation rating is defined only in terms of this
A ED ED EB EB
B EC EC ED ED
test method.
C EC EC EA EA
D EC-ED EC-ED EC EC 15. Keywords
E ED ED ED ED 15.1 exfoliation corrosion; heat treatable aluminum alloys;
F EC EC EB EB
G EC EC P P immersion corrosion test; 2XXX aluminum alloys; 7XXX alu-
minum alloys

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 G 34 – 01 (2007)
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