Designation: G 66 – 99 (Reapproved 2005)

Standard Test Method for

Visual Assessment of Exfoliation Corrosion Susceptibility of
5XXX Series Aluminum Alloys (ASSET Test)1
This standard is issued under the fixed designation G 66; 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.

1. Scope ceptibility to exfoliation is determined by visual examination

1.1 This test method covers a procedure for continuous using performance ratings established by reference to standard
immersion exfoliation corrosion testing of 5XXX series photographs.
aluminum-magnesium alloys containing 2.0 % or more mag- 5. Significance and Use
nesium.
1.2 This test method applies only to wrought products. 5.1 This test method provides a reliable prediction of the
1.3 The values stated in SI units are to be regarded as the exfoliation corrosion
,
behavior of Al-Mg alloys in marine
standard. The values given in parentheses are for information environments.3 4, 5 The test is useful for alloy development
only. studies and quality control of mill products such as sheet and
1.4 This standard does not purport to address all of the plate.
safety concerns, if any, associated with its use. It is the 6. Apparatus
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica- 6.1 Any suitable glass or plastic container can be used to
bility of regulatory limitations prior to use. contain the solution and specimens during the test period.
Depending upon the shape and size of the specimens, rods or
2. Referenced Documents racks of glass, plastic, or other inert substance shall be used to
2.1 ASTM Standards: 2 support the specimens above the bottom of the container. The
D 1193 Specification for Reagent Water container should be fitted with a removable cover to reduce
G 15 Terminology Relating to Corrosion and Corrosion evaporation.
Testing 7. Reagents

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3. Terminology 7.1 Purity of Reagents—Reagent grade chemicals shall be
3.1 Definitions: used in all tests.
3.1.1 exfoliation—corrosion that proceeds laterally from the 7.2 Purity of Water—Distilled or deionized water conform-
sites of initiation along planes parallel to the surface, generally ing to Specification D 1193. Type IV shall be used to prepare
at grain boundaries, forming corrosion products that force the test solution except chloride ion sodium limits can be
metal away from the body of the material, giving rise to a disregarded.
layered appearance (see Terminology G 15). 8. Test Solution
4. Summary of Test Method 8.1 Preparation of Test Solution:
4.1 Specimens are immersed for 24 h at 65 6 1°C (150 6 8.1.1 The test solution shall have the following composi-
2°F) in a solution containing ammonium chloride, ammonium tion:
nitrate, ammonium tartrate, and hydrogen peroxide. The sus- NH4Cl (1.0 M)
NH4NO3 (0.25 M)
(NH4)2C4H4O6 (0.01 M)

1
This test method is under the jurisdiction of ASTM Committee G01 on
3
Corrosion of Metals and is the direct responsibility of Subcommittee G01.05 on Aluminum Association Technical Report T1,“ Exfoliation Corrosion Testing of
Laboratory Corrosion Tests. This method was developed by a joint task group with Aluminum Alloys 5086 and 5456”.
4
The Aluminum Assoc., Inc. Sprowls, D. O., Walsh, J. D. and Shumaker, M. B., “Simplified Exfoliation
Current edition approved May 1, 2005. Published May 2005. Originally Testing of Aluminum Alloys”, Localized Corrosion—Cause of Metal Failure, ASTM
approved in 1980. Last previous edition approved in 1999 as G 66 – 99. STP 516, ASTM, 1972, pp 38–65.
2 5
For referenced ASTM standards, visit the ASTM website, [Link], or Summerson T. J., Interim Report, Aluminum Association Task Group on
contact ASTM Customer Service at service@[Link]. For Annual Book of ASTM Exfoliation and Stress Corrosion Cracking of Aluminum Alloys for Boat Stock;
Standards volume information, refer to the standard’s Document Summary page on Proceedings Tri-Service Corrosion Military Equipment Conference, October 29–31,
the ASTM website. 1974; Technical Report AFML-TR-75-42, Vol. II, p. 193–221, February 1, 1975.

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 G 66 – 99 (2005)
H2O2 (0.09 M) anhydrous calcium sulfate).6

8.1.2 Dissolve 53.5 g ammonium chloride (NH4Cl), 20.0 g 12.2 Use fresh solution at the start of each test.
ammonium nitrate (NH4NO3), 1.8 g ammonium tartrate 12.3 Immerse the specimens vertically with the top edge of
((NH4)2C4H4O6), and 10 mL of 30 % stock solution hydrogen the specimens at least 25 mm (1 in.) below the surface of the
peroxide (H2O2) in a small amount of water. After dissolving, solution and the bottom edge at least 25 mm above the bottom
mix the components together thoroughly and adjust the final of the container.
dilution to 1 L. 12.4 Immerse the specimens in the test solution continu-
ously for 24 h.
NOTE 1—If a stock solution of the above chemicals is to be stored, the 12.5 Rinse the specimens gently in running tap water
hydrogen peroxide should not be added until the solution is heated for the immediately after removal from the solution, then soak in

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test. concentrated nitric acid at room temperature until they appear
8.2 The solution will have a typical pH of 5.2 to 5.4. clean, again rinse in water, and air dry.
8.3 The solution shall be used in sufficient quantity to 12.5.1 Air-blast drying is to be avoided in order to prevent
provide a volume-to-exposed specimen surface area ratio of at mechanical removal of exfoliated metal.
least 100 L/m2 (65 mL/in.2). 13. Rating of Specimens
8.4 The temperature of the solution shall be maintained at
13.1 The following codes and classifications shall be used
65 6 1°C (150 6 2°F).
for reporting the visual appearance of corroded specimens.
Code Classification
9. Sampling N No appreciable attack
9.1 The procedure for sampling mill products is covered in P Pitting
E Exfoliation
product specifications, or otherwise, and is considered outside
the scope of this standard. 13.2 Descriptions of the various classifications, which are
illustrated in Figs. 1 and 2, are as follows:7
10. Test Specimen 13.2.1 N (no appreciable attack)—Surface may be etched or
discolored.
10.1 While this test method can be used with any form of 13.2.2 P (Pitting)—Includes discrete pitting or pit-
specimen or part that can be immersed in the test solution, it is blistering. In the latter case, attack results in a slight undercut-
preferred that specimens be at least 40 by 100 mm (1.5 by 4.0 ting of the surface. Pitting or pit-blistering is to be expected
in.) with the metal working direction in the 40-mm (1.5-in.) and may occur in varying degrees of severity, as shown in Fig.
dimension. 1; it should not be construed as exfoliation.
10.2 The specimens should be sawed or machined to mini- 13.2.3 E (Exfoliation)—Visible lifting of the surface. A
mize introducing residual stresses in edges during preparation range of exfoliation can occur in varying degrees of severity, as
of the specimens (sheared edges are allowed only if the edges shown in Fig. 2.
are sufficiently dressed or filed down a distance equal to the 13.3 Ratings of different levels of pitting or exfoliation may
thickness of the specimen in order to remove metal deformed be indicated PA, PB, PC or EA, EB, EC, ED as shown in Figs.
by shearing). 1 and 2.

11. Standardization 14. Report

11.1 To provide an indication when some inadvertent de- 14.1 Report the following information:
viation from the correct test conditions occurs, it is necessary 14.1.1 Alloy and temper,
to expose to the test at regular intervals a control specimen of 14.1.2 Product of material tested, including reference to
a material of known susceptibility. This control should exhibit applicable product specification,
the same degree of exfoliation each time it is included in the 14.1.3 Sampling procedure if other than that specified in
test. referenced product specification,
11.2 The control may be any material of the Al-Mg series 14.1.4 A rating of the test specimens using the code given in
that has a well-documented susceptibility to exfoliation corro- Section 13,
sion, preferably one with an intermediate susceptibility. 14.1.5 Notation of any deviation in test procedure from that
set forth in preceding paragraphs,
12. Procedure 14.1.6 Size, type, and number of replicate specimens;
method of edge preparation, and
12.1 Degrease the specimens with a suitable solvent. After
degreasing, prepare specimens as follows: Etch 1 min in 5 %
6
by weight sodium hydroxide solution at 80°C (176°F), rinse in Drierite, (a special form of anhydrous calcium sulfate), available from W. A.
Hammond Drierite Co., 120 Dayton Ave., Xenia, OH 45385, or an equivalent drying
water, desmut 30 s in concentrated nitric acid at room tem- agent may be used. If you are aware of alternative suppliers, please provide this
perature, rinse with distilled or deionized water, air dry. information to ASTM International Headquarters. Your comments will receive
careful consideration at a meeting of the responsible technical committee 1, which
NOTE 2—If specimens are not to be immersed in the test solution you may attend.
immediately, they should be stored in a desiccator maintained at less than 7
Glossy prints of Fig. 1 and Fig. 2 are available from ASTM Headquarters.
1 % relative humidity (use fresh desiccant such as activated alumina or Order PCN ADJG0066

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 --`,,`,,`-`-`,,`,,`,`,,`--- G 66 – 99 (2005)

FIG. 1 ASSET Tested Exfoliation Resistant Specimens (N—No appreciable attack; A, B, C—Three Degrees of Pitting
and Pit-Blistering)

FIG. 2 ASSET Tested Exfoliation Susceptible Specimens (A, B, C, D—Four Degrees of Exfoliation)

14.1.7 Solution volume to specimen surface area ratio.

15. Precision and Bias
15.1 Precision:
15.1.1 The precision of the data from this test method was
evaluated by way of an interlaboratory test program using one
commercial and one non-commercial tempers of Alloy 5086
with different levels of exfoliation corrosion susceptibility. Six
laboratories, including experienced and inexperienced users,
participated in the round-robin. The laboratories received
duplicate rough cut panels of each material which they
prepared, exposed, and rated visually according to this test FIG. 3 Histogram of Visual Exfoliation Ratings by Six
method. Laboratories for Two Tempers of 5086 Plate Tested by ASSET
15.1.2 Raw data from the laboratories are listed in Table 1 (Data in Table 1)
and plotted as a histogram in Fig. 3. All six laboratories easily

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 G 66 – 99 (2005)
TABLE 1 ASSET (Test Method G 66) Round Robin Results
Material Volume/
Laboratory Specimens/ Visual
Exfoliation Area Machined
No. Container Ratings
Type (L/m2)
1 Resistant 100 Yes 2 PA
1 Resistant 100 Yes 2 PA
1 Susceptible 100 Yes 2 EC
1 Susceptible 100 Yes 2 EC

2 Resistant 83 No 1 PA
2 Resistant 83 No 1 PA
2 Susceptible 83 No 1 EC
2 Susceptible 83 No 1 EC

3 Resistant 118 Yes 2 PA

3 Resistant 118 Yes 2 PA
3 Susceptible 118 Yes 2 EC
3 Susceptible 118 Yes 2 EC

4 Resistant 159 No 1 PA
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4 Resistant 159 No 1 PA
4 Susceptible 159 No 1 ED
4 Susceptible 159 No 1 ED

5 Resistant 115 No 1 PA
5 Resistant 115 No 1 PA
5 Susceptible 115 No 1 EC
5 Susceptible 115 No 1 EC

6 Resistant 211 No 4 PB
6 Resistant 211 No 4 PB
6 Susceptible 211 No 4 ED
6 Susceptible 211 No 4 ED

differentiated between the two materials finding one resistant 15.2 Bias:
and one susceptible to exfoliation corrosion. 15.2.1 The procedure in Test Method G 66 has no bias
[Link] The data in Table 1 show the ratings were repeat- because the exfoliation rating is defined only in terms of this
able within laboratories. In each case the same rating was test method.
obtained for both panels tested by the individual laboratory.
[Link] The reproducibility of ratings among different 16. Keywords
laboratories was consistent for the resistant material with all
laboratories obtaining pitting ratings. In the case of the 16.1 aluminum alloys; 5XXX aluminum alloys; exfoliation
exfoliation susceptible material the ratings between laborato- corrosion; pitting corrosion; visual inspection
ries were within one rating category.

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