ASTM D3340-98
(Test Method)Standard Test Method for Lithium and Sodium in Lubricating Greases by Flame Photometer
Standard Test Method for Lithium and Sodium in Lubricating Greases by Flame Photometer
SCOPE
1.1 This test method covers determination of the lithium and sodium content of lubricating greases by means of a flame photometer.
1.2 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.
1.3 The preferred units are mass percent and accepted metric units. The values given in parentheses are for information only.
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Standards Content (Sample)
NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
An American National Standard
Designation: D 3340 – 98
Standard Test Method for
Lithium and Sodium in Lubricating Greases by Flame
Photometer
This standard is issued under the fixed designation D 3340; 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 all reagents shall conform to the specifications of the Commit-
tee on Analytical Reagents of the American Chemical Society,
1.1 This test method covers determination of the lithium and
where such specifications are available. Other grades may be
sodium content of lubricating greases by means of a flame
used, provided it is first ascertained that the reagent is of
photometer.
sufficiently high purity to permit its use without lessening the
1.2 This standard does not purport to address all of the
accuracy of the determination.
safety concerns, if any, associated with its use. It is the
6.2 Purity of Water—Unless otherwise indicated, references
responsibility of the user of this standard to establish appro-
to water shall be understood to mean reagent water as defined
priate safety and health practices and determine the applica-
by Type II of Specification D 1193.
bility of regulatory limitations prior to use.
6.3 Lithium Sulfate, Stock Solution—1.188 g of lithium
1.3 The preferred units are mass % and accepted SI units.
sulfate dried to constant weight at 180°C (356°F), is dissolved
The values given in parentheses are for information only.
in water and made up to 1 L. This will contain 150 mg/L
2. Referenced Documents lithium.
6.4 Sodium Sulfate, Stock Solution—0.1544 g of sodium
2.1 ASTM Standards:
sulfate, dried to constant weight at 105°C (221°F), is dissolved
D 1193 Specification for Reagent Water
in water and made up to 1 L. This will contain 50 mg/L sodium.
3. Summary of Test Method
6.5 Sulfuric Acid (rel. den. 1.84)—Concentrated sulfuric
acid (H SO ).
3.1 The sulfated ash of the grease is extracted with water 2 4
and the lithium and sodium content of the resulting solution is
7. Sampling
determined by means of a suitable flame photometer.
7.1 A homogeneous sample shall be obtained to ensure
4. Significance and Use
quantitative analytical results.
4.1 Lubricating greases can contain the lithium soap of
8. Procedure
hydroxy stearic acid or the sodium soap of various fatty acids
8.1 Weigh to the nearest 1 mg approximately1gofthe
as thickeners. The determination of total lithium or total
grease into a platinum dish or crucible. Heat the dish until the
sodium is a measure of the amount of thickener in the grease.
sample can be ignited with a flame. Maintain at such a
5. Apparatus
temperature that the sample burns at a uniform and moderate
rate, leaving only ash and carbon when the burning ceases.
5.1 Flame Photometer, suitably equipped to determine
8.2 Cool the dish and completely moisten the residue by the
lithium and sodium over a range from 0 to 15 mg/L lithium and
dropwise addition of concentrated sulfuric acid. Heat the dish
from 0 to 5 mg/L sodium.
at a low temperature, taking care to avoid spattering of the
6. Reagents
contents, and continue heating until fumes are no longer
evolved. Place the dish in a furnace at 550 6 25°C (1022 6
6.1 Purity of Reagents—Reagent grade chemicals shall be
45°F) and continue heating until the oxidation of the carbon is
used in all tests. Unless otherwise indicated, it is intended that
practically complete.
1 3
This test method is under the jurisdiction of ASTM Committee D-2 on Reagent Chemicals, American Chemical Society Specifications, American
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee Chemical Society, Washington, DC. For suggestions on the testing of reagents not
D02.03.0B on Spectrometric Methods. listed by the American Chemical Society, see Analar Standards for Laboratory
Current edition approved Nov. 10, 1998. Published January 1999. Originally Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
e1
published as D 3340 – 74. Last previous edition D 3340 – 90 (1995) . and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
Annual Book of ASTM Standards, Vol 11.01. MD.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
D3340–98
TABLE 1 Precision Values for Lithium and Sodium (Mass% )
Sodium, mass % 5 Y/100 W (3)
Lithium, Repeatability Reproducibility
2/5 2/5
where:
x 0.014(x) 0.075(x)
Y = sodium content of the water extract in mg/L sodium
0.01 0.002 0.011
(see 8.7), and
0.05 0.004 0.022
0.1 0.005 0.029
W = mass of the grease taken, g.
0.2 0
...
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