Designation: G67 − 13

Standard Test Method for

Determining the Susceptibility to Intergranular Corrosion of
5XXX Series Aluminum Alloys by Mass Loss After Exposure
to Nitric Acid (NAMLT Test)1
This standard is issued under the fixed designation G67; 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 (´) indicates an editorial change since the last revision or reapproval.

1. Scope 4. Significance and Use

1.1 This test method describes a procedure for constant 4.1 This test method provides a quantitative measure of the
immersion intergranular corrosion testing of 5XXX series susceptibility to intergranular corrosion of Al-Mg and Al-
aluminum alloys. Mg-Mn alloys. The nitric acid dissolves a second phase, an
aluminum-magnesium intermetallic compound (βAl-Mg), in
1.2 This test method is applicable only to wrought products. preference to the solid solution of magnesium in the aluminum
1.3 This test method covers type of specimen, specimen matrix. When this compound is precipitated in a relatively
preparation, test environment, and method of exposure. continuous network along grain boundaries, the effect of the
preferential attack is to corrode around the grains, causing
1.4 The values stated in SI units are to be regarded as the
them to fall away from the specimens. Such dropping out of the
standard. The values given in parentheses are for information
grains causes relatively large mass losses of the order of 25 to
only.
75 mg/cm2 (160 to 480 mg/in2), whereas, samples of
1.5 This standard does not purport to address all of the intergranular-resistant materials lose only about 1 to 15 mg/
safety concerns, if any, associated with its use. It is the cm2 (10 to 100 mg/in2). When the βAl-Mg compound is
responsibility of the user of this standard to establish appro- randomly distributed, the preferential attack can result in
priate safety and health practices and determine the applica- intermediate mass losses. Metallographic examination is re-
bility of regulatory limitations prior to use. quired in such cases to establish whether or not the loss in mass
is the result of intergranular attack.
2. Referenced Documents 4.2 The precipitation of the second phase in the grain
2.1 ASTM Standards:2 boundaries also gives rise to intergranular corrosion when the
D1193 Specification for Reagent Water material is exposed to chloride-containing natural
G1 Practice for Preparing, Cleaning, and Evaluating Corro- environments, such as seacoast atmospheres or sea water. The
sion Test Specimens extent to which the alloy will be susceptible to intergranular
corrosion depends upon the degree of precipitate continuity in
3. Summary of Test Method the grain boundaries. Visible manifestations of the attack may
be in various forms such as pitting, exfoliation, or stress-
3.1 This test method consists of immersing test specimens corrosion cracking, depending upon the morphology of the
in concentrated nitric acid at 30°C (86°F) for 24 h and grain structure and the presence of sustained tensile stress.3
determining the mass loss per unit area as a measure of
susceptibility to intergranular corrosion. 5. Interferences
5.1 If all loose particles are not removed during cleaning
after exposure, the mass loss will be low relative to the amount
1
This test method is under the jurisdiction of ASTM Committee G01 on of corrosion that actually occurred.
Corrosion of Metals and is the direct responsibility of Subcommittee G01.05 on
Laboratory Corrosion Tests. This method was developed by a joint task group with 6. Apparatus
The Aluminum Association, Inc.
Current edition approved May 1, 2013. Published May 2013. Originally 6.1 Nonmetallic Container—A suitable inert, nonmetallic
approved in 1980. Last previous edition approved in 2004 as G67 – 04, which was container should be used to contain the nitric acid and
withdrawn January 2013 and reinstated May 2013. DOI: 10.1520/G0067-13.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
3
contact ASTM Customer Service at [email protected]. For Annual Book of ASTM Craig, H. L. Jr., “Nitric Acid Weight Loss Test for the H116 and H117 Tempers
Standards volume information, refer to the standard’s Document Summary page on of 5086 and 5456 Aluminum Alloys,” Localized Corrosion—Cause of Metal
the ASTM website. Failure, ASTM STP 516, ASTM, 1972, pp. 17–37.

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

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 G67 − 13
specimens during the period of the test. The use of individual 11.4 Immerse the specimens in 5 % NaOH solution at 80°C
beakers for each specimen is recommended; however, the (176°F) for 1 min followed by a water rinse, a 30-s immersion
immersion of multiple specimens in the same container is in HNO3 (desmut), and a water rinse. Allow the specimens to
acceptable. air dry. Do not wipe dry with a cloth or paper towel.
6.1.1 The specimens should be situated in the container so 11.5 Weigh the specimens to no more than 61.0 mg,
that none of the major surfaces is in total contact with the walls preferably 0.1 mg.
of the container. Also, specimens should be isolated electrically
from one another. A recommended method of positioning the 11.6 Immerse the specimens in the test solution for 24 h.
specimens is to incline them so that the edges rest on the 11.7 Remove the specimens, and rinse with water while
bottom and side wall of the container. brushing with a stiff plastic bristle brush, for example, a
6.1.2 The container should have a loose fitting cover to toothbrush, to remove all adhering particles. Allow to air dry.
reduce evaporation and to confine any fumes evolved by the 11.8 Weigh the specimens and determine mass losses to no
acid. more than 61.0 mg, preferably 0.1 mg. Reclean to obtain a
constant weight in accordance with Practice G1.
7. Reagents
11.9 Calculate the mass losses per unit area and express as
7.1 Purity of Reagents—The nitric acid (HNO3) test solu- mg/cm2 to the nearest whole number.
tion shall be reagent grade and have a specific gravity within
the range of 1.4134 to 1.4218 (70 to 72 weight %). The sodium NOTE 1—Optional—To ascertain the morphology of corrosion, the
hydroxide (NaOH) solution used for etching and the HNO3 (70 specimen can be cross-sectioned, polished, and examined metallographi-
cally after the mass loss determination.
to 72 weight %) used for desmutting shall also be reagent
grade. 12. Report
7.2 Purity of Water—Use water conforming to Specification 12.1 The report should contain the following information:
D1193 Type IV to prepare the NaOH solution and for rinsing 12.1.1 Alloy identification,
purposes. 12.1.2 Product and temper of material,
12.1.3 Sampling procedure particularly with respect to lo-
8. Test Solution cation in the product and the original material thickness,
8.1 Use sufficient test solution to fully immerse the speci- 12.1.4 Mass loss per unit area,
mens and constitute a volume to specimen surface area ratio of 12.1.5 Any deviation in test procedure from that set forth in
at least 30 L/m2 (19 mL/in2). preceding paragraphs,
12.1.6 Solution volume to specimen surface area ratio,
8.2 Maintain the test solution temperature at 30 6 0.1°C (86 12.1.7 Specimen dimensions, and
6 0.2°F). 12.1.8 Number of specimens tested in each container.

9. Sampling 13. Precision and Bias

9.1 The specific location of samples in a mill product, the 13.1 Statement on Precision:
number of samples that should be tested, and so forth, are 13.1.1 Reproducibility of the mass loss results decreases
outside the scope of this standard. with increased susceptibility to intergranular attack. Data on
the precision of test results obtained by this test method derived
10. Test Specimens from interlaboratory tests of 5086 and 5456 alloys are shown in
ASTM STP 516.3 The standard deviations for test results
10.1 Prepare specimens with dimensions 50 mm by 6 mm (2 among six different laboratories ranged from 0.2 to 3.9 mg/cm2
in. by 0.25 in.) by product thickness. The 50-mm dimension for resistant materials with mean mass losses ranging from 1 to
shall be parallel to the longitudinal direction of the product. 8 mg/cm2 and from 5.5 to 6.6 mg/cm2 for susceptible materials
10.2 If the thickness of the product is greater than 25 mm (1 with mean losses ranging from 30 to 44 mg/cm2 (see Footnote
in.), reduce it by one half or to 25 mm, whichever is less, while 4). The coefficient of variation is 0.3 6 0.1.
retaining one original as-fabricated surface. All sawn surfaces 13.1.2 The repeatability/variation within a laboratory is
shall be machined to the final dimensions. about 0.05 coefficient of variation.
10.3 Take a minimum of two specimens from each sample. 13.1.3 To provide an indication when some inadvertent
deviation from the correct test condition occurs, it is necessary
11. Procedure to expose to the test at regular intervals a control specimen of
a material with known resistance. This control should exhibit
11.1 Smooth all edges with a fine file or fine emery paper the same degree of mass loss each time it is included in the test.
(320). 13.1.4 The control may be any material of the alloy type
11.2 Identification of specimens can be achieved by either included in the scope of this test method, preferably one with
scribing or stamping. Confine identification of specimens to an an intermediate degree of susceptibility.
as-fabricated surface. 13.2 Bias—The procedure in this test method has no bias
11.3 Measure all three dimensions to the nearest 0.02 mm because the value of mass loss due to intergranular corrosion is
(0.001 in.), and calculate the total surface area. defined only in terms of this test method.

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 G67 − 13
14. Keywords
14.1 5xxx aluminum alloys; aluminum alloys; grain bound-
ary sensitization; intercrystalline corrosion; intergranular cor-
rosion; mass loss; nitric acid; pitting corrosion

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