ASTM D4048 - 19a

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This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles

for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

Designation: D4048 − 19a

Standard Test Method for


Detection of Copper Corrosion from Lubricating Grease1
This standard is issued under the fixed designation D4048; 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.
This standard has been approved for use by agencies of the U.S. Department of Defense.

1. Scope* 3. Terminology
1.1 This test method covers the detection of the corrosive- 3.1 Definitions—See Terminology D4175.
ness to copper of lubricating grease. 3.2 copper corrosion, n—effect of a chemical attack on
1.2 The values stated in SI units are to be regarded as copper metal by a lubricant causing various levels of tarnishing
standard. The values given in parentheses after SI units are and change in appearance.
provided for information only and are not considered standard. 3.2.1 Discussion—Acidic and other aggressive species, of-
1.3 This standard does not purport to address all of the ten sulfur-based, in a lubricant can attack copper or copper
safety concerns, if any, associated with its use. It is the alloys present in bearings or other lubricated surfaces. The
responsibility of the user of this standard to establish appro- presence of this antagonistic interaction is often apparent in a
priate safety, health, and environmental practices and deter- well-defined series of color changes.
mine the applicability of regulatory limitations prior to use. 3.3 lubricant, n—any material interposed between two sur-
For specific warning statements, see Sections 7, 8, and 10. faces that reduces the friction or wear between them.
1.4 This international standard was developed in accor- 3.4 lubricating grease, n—a semi-fluid to solid product of a
dance with internationally recognized principles on standard- dispersion of a thickener in a liquid lubricant.
ization established in the Decision on Principles for the 3.4.1 Discussion—The dispersion of the thickener forms a
Development of International Standards, Guides and Recom- two-phase system and immobilizes the liquid lubricant by
mendations issued by the World Trade Organization Technical surface tension and other physical forces. Other ingredients are
Barriers to Trade (TBT) Committee. commonly included to impart special properties.
2. Referenced Documents 4. Summary of Test Method
2.1 ASTM Standards:2 4.1 A prepared copper strip is totally immersed in a sample
D97 Test Method for Pour Point of Petroleum Products of grease and heated in an oven or liquid bath at a specified
D130 Test Method for Corrosiveness to Copper from Petro- temperature for a definite period of time. Commonly used
leum Products by Copper Strip Test conditions are 100 °C 6 1 °C (212 °F 6 2 °F) for 24 h 6
D2500 Test Method for Cloud Point of Petroleum Products 5 min. At the end of this heating period, the strip is removed,
and Liquid Fuels washed, and compared with the Copper Strip Corrosion Stan-
D4175 Terminology Relating to Petroleum Products, Liquid dard.
Fuels, and Lubricants
2.2 ASTM Adjuncts: 5. Significance and Use
Copper Strip Corrosion Standard3 5.1 This test method measures the tendency of lubricating
grease to corrode copper under specific static conditions. It
may be of some value in predicting possible chemical attack on
1
This test method is under the jurisdiction of ASTM Committee D02 on lubricated parts, such as bearings that contain copper or copper
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of
Subcommittee D02.G0.01 on Chemical and General Laboratory Tests.
alloys. Such corrosion, for example, can cause premature
Current edition approved July 1, 2019. Published September 2019. Originally bearing failures. However, no correlations with actual field
published in 1981. Last previous edition approved in 2019 as D4048 – 19. DOI: service, most of which are under dynamic conditions, have
10.1520/D4048-19A. been established. It does not measure either the ability of the
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM lubricant to inhibit copper corrosion caused by factors other
Standards volume information, refer to the standard’s Document Summary page on than the lubricant itself nor does it measure the stability of the
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the ASTM website.


3
grease in the presence of copper.
Available from ASTM International Headquarters. Order Adjunct No.
ADJD0130. Originally produced in 1973. NOTE 1—Because this test method requires the ability to determine

*A Summary of Changes section appears at the end of this standard


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D4048 − 19a
subtle differences in color of copper strips, persons with certain types of 7. Reagents and Materials
color blindness may find it difficult to accurately compare a test strip to the
Copper Strip Corrosion Standard. 7.1 Acetone—American Chemical Society Reagent-Grade
acetone is suitable. (Warning—Extremely flammable. Harm-
6. Apparatus ful if inhaled. Vapors may cause flash fires.)
7.2 Copper Strips—Use strips 12.5 mm 6 2 mm (1⁄2 in. 6
6.1 Test Containers—Containers with a minimum width of
⁄ in.) wide, 1.5 mm to 3.0 mm (1⁄16 in. to 1⁄8 in.) thick, cut
1 16
24 mm and at least 85 mm tall (sufficient depth to allow the
75 mm 6 5 mm (3 in. 6 1⁄4 in.) long from smooth-surfaced,
complete insertion of the copper test strip), made of glass or
hard-temper, cold-finished copper of 99.9+ % purity; electrical
other inert material. bus bar stock is generally suitable. (See Appendix X1 on
6.2 Test Container Covers—Any small porcelain or glazed Optional Useful Equipment in Test Method D130.) The strips
silica crucibles or crucible covers or watch glasses or vented may be used repeatedly but should be discarded when the
corks that lightly cover the test containers, allowing pressure surfaces become deformed on handling.
equalization between the inside and outside of the containers, 7.3 Polishing Materials—Silicon carbide grit paper of vary-
yet minimizing exposure of the inside of the containers to ing degrees of fineness, including 65 µm (220 grit CAMI-grade
foreign vapors present in the oven will also be satisfactory. or P220 FEPA-grade) paper or cloth, also a supply of 105 µm
(120 grit to 150 grit CAMI-grade or P120 to P150 FEPA-
6.3 Oven—A circulating air oven or liquid bath capable of
grade) silicon carbide grain and absorbent cotton (cotton
maintaining a temperature of 100 °C 6 1 °C (212 °F 6 2 °F)
wool).
or other desired temperatures with the same precision.
7.4 Wash Solvent—Volatile, sulfur-free hydrocarbon solvent
6.4 Polishing Vise—For holding the copper strip firmly may be used provided that it shows no tarnish at all when tested
without marring the edges while polishing. Any convenient at 50 °C 6 1 °C (or 122 °F 6 2 °F). Knock test-grade
type of holder (see Appendix X1 on Optional Useful Equip- isooctane (Warning—see 8.1.2) or American Chemical Soci-
ment in Test Method D130) may be used, provided that the ety Reagent-Grade n-heptane (Warning—see 7.1) are suitable
strip is held tightly and that the surface of the strip being solvents. Because of possible toxic effects, the use of benzene
polished is supported above the surface of the holder. should be avoided.
6.5 Viewing Test Tubes—Flat glass test tubes may be used to
8. Preparation of Strip
protect corroded strips for close inspection or storage. (See
Appendix X1 on Optional Useful Equipment in Test Method 8.1 Mechanical Cleaning of Strips:
D130.) 8.1.1 Surface Preparation—Remove all surface blemishes
from all six sides of the strip with silicon carbide paper of such
6.6 Copper Strip Corrosion Standard—Consists of repro- degrees of fineness as are needed to accomplish the desired
ductions in color of typical strips representing degrees of results efficiently (see Note 2). Finish with 65 µm (220 grit
tarnish and corrosion, the reproductions being encased in CAMI-grade or P220 FEPA-grade) silicon carbide paper or
plastic in the form of a plaque. cloth, removing all marks that may have been made by other
6.6.1 Keep the plastic-encased printed Copper Strip Corro- grades of paper used previously. Immerse the strip in wash
sion Standard protected from light to avoid the possibility of solvent (Warning—see 7.1.) from which it can be withdrawn
fading. Inspect for fading by comparing two different plaques, immediately for final polishing or in which it can be stored for
one of which has been carefully protected from light (new). future use.
Observe both sets in diffused daylight (or equivalent), first NOTE 2—Only final preparation (8.1.2) is necessary for commercially
from a point directly above and then from an angle of purchased pre-polished strips. Statistical evaluation involving pre-
approximately 45°. If any evidence of fading is observed, polished copper strips has been performed using gasoline sample types
particularly at the left end of the plaque, it is suggested that the (see Test Method D130). The recommendation for grease is based on this
evaluation, as well as additional data generated by Subcommittee
one that is the more faded with respect to the other be D02.G0.01 and the technical judgment of its members.
discarded.
8.1.1.1 As a practical manual procedure for surface
6.6.1.1 Alternatively, place a 20 mm (3⁄4 in.) opaque strip
preparation, place a sheet of the paper on a flat surface, moisten
(masking tape) across the top of the colored portion of the it with wash solvent, and rub the strip against the paper with a
plaque when initially purchased. At intervals, remove the rotary motion, protecting the strip from contact with the fingers
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opaque strip and observe. If there is any evidence of fading of or by wearing impervious gloves (see Note 3). Alternatively,
the exposed portion, it is suggested that the standard be the surface of the strip may be prepared by use of motor-driven
replaced. machines using appropriate grades of dry paper or cloth.
6.6.1.2 These plaques are full-color productions of typical
NOTE 3—Disposable polyethylene is one type of glove that has been
strips. They have been printed on photolithographed strips and found to be satisfactory. However, any type of glove that is impervious to
are encased in plastic for protection. Directions for their use are the reagents and materials used in this test method, while preventing
given on the reverse side of each plaque. fingers from contacting the strip directly, may also be used.
6.6.2 If the surface of the plastic cover shows excessive 8.1.2 Final Polishing—Remove strip from the wash solvent.
scratching, it is suggested that the plaque be replaced. Holding it in the fingers protected with the ashless filter paper,

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D4048 − 19a
polish first the ends and then the sides with the 105 µm (120 quantitative filter paper by blotting and not by wiping, and
grit to 150 grit CAMI-grade or P120 to P150 FEPA-grade) inspect, in diffused daylight (or equivalent), for evidence of
silicon carbide grains picked up from a clean glass plate with tarnishing or corrosion by comparison with the Copper Strip
a pad of cotton (cotton wool) moistened with a drop of wash Corrosion Standard. Hold both the test strip and the standard
solvent. Wipe vigorously with fresh pads of cotton (cotton strip plaque in such a manner that light reflected from them at
wool) and subsequently handle only when wearing impervious an angle of approximately 45° will be observed.
gloves (see Note 3) or with stainless steel forceps; do not touch NOTE 5—It has been suggested that a very light grease may be blotted
with naked fingers. Clamp the strip in a vise, and polish the off the strip with filter paper or a laboratory wiper. Heavier greases may
main surfaces with silicon-carbide grains on absorbent cotton. require wiping or removal with a plastic, rubber, or stainless steel spatula.
Rub in the direction of the long axis of the strip, carrying the However the grease is removed from the strip, exercise care not to disturb
stroke beyond the end of the strip before reversing the the tarnish or corrosion on the strip.
direction. Clean all metal dust from the strip before reversing 9.6.2 In handling the test strip during the inspection and
the direction. Clean all metal dust from the strip by rubbing comparison, the danger of marking or staining can be avoided
vigorously with clean pads of absorbent cotton until a fresh pad if it is inserted in a flat tube (see Appendix X1 on Optional
remains unsoiled. When the strip is clean, immediately im- Useful Equipment in Test Method D130), which can be
merse it in the prepared sample. (Warning—Forceps can stoppered with absorbent cotton.
scratch copper, affecting the results.)
8.1.2.1 It is important to polish the whole surface of the strip 10. Interpretation
uniformly to obtain a uniformly stained strip. If the edges show 10.1 Interpret the corrosiveness of the sample according to
wear (surface elliptical), they will likely show more corrosion how the appearance of the test strip agrees with one of the
than the center. The use of a vise will facilitate uniform strips of the Copper Strip Corrosion Standard.
polishing. 10.1.1 When a strip is in the obvious transition state
between that indicated by any two adjacent standard strips,
9. Procedure judge the sample by the more tarnished standard strip. Should
9.1 Place sufficient amount of grease sample into the bottom a strip appear to have a darker orange color than standard strip
of a clean test container (see 6.1) to bring the depth of the 1b, consider the observed strip as still belonging in this
grease to about 80 mm (3.2 in.). Tap the grease down into the Classification 1b; however, if any evidence of red color is
container carefully. Smooth the top to give a relatively flat noticed, the observed strip belongs in Classification 2.
surface. Wipe excess grease off the container walls. 10.1.2 A claret red 2a strip can be mistaken for a 3a strip, if
the brassy underlay of the 3a strip is completely masked by a
NOTE 4—The use of a syringe to prepare a grease sample with minimal magenta overtone. To distinguish between them, immerse the
entrained air and then to transfer it to the test container has been found to strip in acetone (Warning—see 7.1). A 2a strip will appear as
be helpful in reducing the amount of air trapped in the sample during
filling. A syringe with a wide nozzle and a diameter just less than that of a 1b strip, while a 3a strip will not change.
the test container may be most helpful in this regard. This may reduce the
potential risk of breaking fragile test containers during the action of
TABLE 1 Copper Strip Classifications
tapping it to remove air from the grease sample.
Classification Designation DescriptionA
9.2 To prevent touching the strip with fingers, wear imper-
Freshly Polished
vious gloves (see Note 3) or use stainless steel forceps; and StripB
insert cleaned copper strip into the grease until it touches the 1 Slight tarnish a. Light orange, almost the same
as a freshly polished strip
bottom of the tube and is completely immersed and covered by ... b. Dark orange
at least 5 mm (0.2 in.) of grease. 2 Moderate a. Claret red
tarnish
9.3 Cover the container(s) loosely with a beaker, crucible, ... b. Lavender
watch glass, or vented cork (see 6.2). ... c. Multicolored with lavender, blue
or silver, or both, overlaid on
9.4 Place the container(s) in an oven or liquid bath so that claret red
they are supported approximately vertical. Regulate the oven ... d. Silvery
... e. Brassy or gold
or liquid bath to maintain a specified temperature for a 3 Dark tarnish a. Magenta overcase on brassy
specified period of time. Commonly used conditions are strip
100 °C 6 1 °C (212 °F 6 2 °F) for 24 h 6 5 min. ... b. Multicolored with red and green
showing (peacock) but no gray
9.5 At the end of the test period, remove the containers(s) 4 Corrosion a. Transparent black, dark gray, or
brown with peacock green barely
from the oven or liquid bath and allow them to cool to room showing
temperature. ... b. Graphite or lusterless black
... c. Glossy or jet black
9.6 Strip Examination: A
The Copper Strip Corrosion Standard is a colored reproduction of strips
9.6.1 Wearing impervious gloves (see Note 3), or using characteristic of these descriptions.
stainless steel forceps, remove the strip from the grease, and B
The freshly polished strip is included in the series only as an indication of the
carefully remove excess grease clinging to the strip. Take care appearance of a properly polished strip before a test run; it is not possible to
duplicate this appearance after a test, even with a completely noncorrosive
not to disturb the tarnish on the strip, and immediately immerse sample.
it in wash solvent. Withdraw the strip at once, dry with
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D4048 − 19a
10.1.3 To distinguish a 2c strip from a 3b strip, place it in a 12.1.1 Repeatability can be judged by the fact that 96 % of
20 mm by 150 mm test tube, and bring it to a temperature of duplicate results obtained in the normal simultaneous proce-
315 °C to 370 °C (600 °F to 700 °F) in 4 min to 6 min using a dure by twelve laboratories with six samples were in agreement
hot plate. Adjust the temperature by observing an ASTM (see Note 6).
high-temperature distillation thermometer inserted in a second 12.1.2 Reproducibility may be judged by the fact that twelve
test tube lying on the hot plate. A 2c strip will assume the color laboratories matched consensus within a numerical classifica-
of a 2d strip and successive stages of tarnish, while a 3b strip tion (1, 2, 3, 4) 92 % of the time and within a numerical and
will take on the appearance of a 4a strip.
descriptive classification (a, b, c, d) 69 % of the time with five
10.1.4 Repeat the test if blemishes due to fingerprints or due
samples showing good or poor protection against copper
to spots from any water droplets or entrained air that may have
corrosion. A sample (Grease F) with somewhat marginal
touched the test strip during the test period or from other
unknown causes are observed. If blemishes on the strip are still corrosion protection properties found agreement between labo-
observed, the rating for the more tarnished portion of the strip ratories only 50 % of the time by either numerical or numerical
should be applied to the whole strip. and descriptive classification.
10.1.5 Repeat the test also if the sharp edges along the flat NOTE 6—Actual data on which this precision statement is based can be
faces of the strip appear to be in a classification higher than the found in Appendix X1. Test conditions were 100 °C, 24 h.
greater portion of the strip; in this case, it is likely that the
edges were burnished during polishing. 12.2 Bias—The procedure in Test Method D4048 has no
bias because the rating of copper corrosion is defined only in
11. Report terms of this test method.
11.1 Report the corrosiveness in accordance with one of the
classifications and descriptions in Table 1. State the duration of 13. Keywords
the test and the test temperature. 13.1 copper corrosion; copper strip; copper tarnish; lubri-
4 cating grease
12. Precision and Bias
12.1 Due to the nature of the results, the precision of this
test method was not obtained in accordance with RR:D02-
1007.

4
Supporting data have been filed at ASTM International Headquarters and may
be obtained by requesting Research Report RR:D02-1187. Contact ASTM Customer
Service at service@astm.org.

APPENDIX

(Nonmandatory Information)

X1. PRECISION STATEMENT DATA

Grease A B C D E F
Run No. 1 2 1 2 1 2 1 2 1 2 1 2
1 2c 2c 1a 1a 1b 1b 1a 1a 4a 4a 2c 2c
2 1a 1a 1a 1a 1b 1b 1a 1a 4a 4a 1b 1b
3 1a 1a 1a 1a 1b 1a 1a 1a 4a 4a 1b 1b
4 1a 1a 1b 1b 1b 1b 1b 1b 3b 3b 2c 2c
5 1a 1a 1a 2 2 2 2 2 4 4 3 3
6 1a 1a 1a 1a 1a 1a 1a 1a 4b 4b 4a 4a
7 1a 1a 1b 1b 1b 1b 1a 1a 4a 4a 3a 3b
8 1a 1a 1a 1a 1a 1a 1a 1a 4a 4a 1b 1b
9 1a 1a 1a 1a 1a 1a 1a 1a 4a 4a 1b 1b
10 1a 1a 1a 1a 1a 1a 1a 1a 4b 4b 1b 1b
11 2c 1b 1a 1b 1b 1b 1a 1a 4a 4a 2c 2c
12 1a 1a 1a 1a 1a 1a 1a 1a 4b 4b 1b 1b

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D4048 − 19a
SUMMARY OF CHANGES

Subcommittee D02.G0 has identified the location of selected changes to this standard since the last issue
(D4048 – 19) that may impact the use of this standard. (Approved July 1, 2019.)

(1) Added new Note 2. (2) Revised subsection 6.6.1.2.

Subcommittee D02.G0 has identified the location of selected changes to this standard since the last issue
(D4048 – 16ɛ1) that may impact the use of this standard. (Approved June 1, 2019.)

(1) Revised 6.1, 6.2, 9.1, Note 4, and 9.3 – 9.5.

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