ASTM D3340-98(2003)

Standard Test Method for Lithium and Sodium in Lubricating Greases by Flame Photometer

SIGNIFICANCE AND USE
Lubricating greases can contain the lithium soap of hydroxy stearic acid or the sodium soap of various fatty acids as thickeners. The determination of total lithium or total sodium is a measure of the amount of thickener in the grease.
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 % and accepted SI units. The values given in parentheses are for information only.

General Information

• Status: Historical
• Publication Date: 09-May-2003
• ICS: 75.100 - Lubricants, industrial oils and related products
• Technical Committee: D02 - Petroleum Products, Liquid Fuels, and Lubricants
• Drafting Committee: D02.03 - Elemental Analysis

Relations

• Replaces: ASTM D3340-98 - Standard Test Method for Lithium and Sodium in Lubricating Greases by Flame Photometer
• Effective Date: 10-May-2003
• Replaced By: ASTM D3340-07 - Standard Test Method for Lithium and Sodium in Lubricating Greases by Flame Photometer (Withdrawn 2013)
• Effective Date: 01-Dec-2007
• Referred By: ASTM D7303-23 - Standard Test Method for Determination of Metals in Lubricating Greases by Inductively Coupled Plasma Atomic Emission Spectrometry
• Effective Date: 10-May-2003
• Referred By: ASTM D7455-19 - Standard Practice for Sample Preparation of Petroleum and Lubricant Products for Elemental Analysis
• Effective Date: 10-May-2003
• Referred By: ASTM D7578-20 - Standard Guide for Calibration Requirements for Elemental Analysis of Petroleum Products and Lubricants
• Effective Date: 10-May-2003
• Referred By: ASTM D7740-20 - Standard Practice for Optimization, Calibration, and Validation of Atomic Absorption Spectrometry for Metal Analysis of Petroleum Products and Lubricants
• Effective Date: 10-May-2003

Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
An American National Standard
Designation:D3340–98 (Reapproved 2003)
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 tee onAnalytical Reagents of theAmerican Chemical Society,
where such specifications are available. Other grades may be
1.1 Thistestmethodcoversdeterminationofthelithiumand
used, provided it is first ascertained that the reagent is of
sodium content of lubricating greases by means of a flame
sufficiently high purity to permit its use without lessening the
photometer.
accuracy of the determination.
1.2 This standard does not purport to address all of the
6.2 Purity of Water—Unless otherwise indicated, references
safety concerns, if any, associated with its use. It is the
to water shall be understood to mean reagent water as defined
responsibility of the user of this standard to establish appro-
by Type II of Specification D 1193.
priate safety and health practices and determine the applica-
6.3 Lithium Sulfate, Stock Solution—1.188 g of lithium
bility of regulatory limitations prior to use.
sulfate dried to constant weight at 180°C (356°F), is dissolved
1.3 The preferred units are mass % and accepted SI units.
in water and made up to 1 L. This will contain 150 mg/L
The values given in parentheses are for information only.
lithium.
2. Referenced Documents
6.4 Sodium Sulfate, Stock Solution—0.1544 g of sodium
sulfate, dried to constant weight at 105°C (221°F), is dissolved
2.1 ASTM Standards:
inwaterandmadeupto1L.Thiswillcontain50mg/Lsodium.
D 1193 Specification for Reagent Water
6.5 Sulfuric Acid (rel. den. 1.84)—Concentrated sulfuric
3. Summary of Test Method
acid (H SO ).
2 4
3.1 The sulfated ash of the grease is extracted with water
7. Sampling
and the lithium and sodium content of the resulting solution is
7.1 A homogeneous sample shall be obtained to ensure
determined by means of a suitable flame photometer.
quantitative analytical results.
4. Significance and Use
8. Procedure
4.1 Lubricating greases can contain the lithium soap of
8.1 Weigh to the nearest 1 mg approximately1gofthe
hydroxy stearic acid or the sodium soap of various fatty acids
grease into a platinum dish or crucible. Heat the dish until the
as thickeners. The determination of total lithium or total
sample can be ignited with a flame. Maintain at such a
sodium is a measure of the amount of thickener in the grease.
temperature that the sample burns at a uniform and moderate
5. Apparatus
rate, leaving only ash and carbon when the burning ceases.
8.2 Cool the dish and completely moisten the residue by the
5.1 Flame Photometer, suitably equipped to determine
dropwise addition of concentrated sulfuric acid. Heat the dish
lithiumandsodiumoverarangefrom0to15mg/Llithiumand
at a low temperature, taking care to avoid spattering of the
from 0 to 5 mg/L sodium.
contents, and continue heating until fumes are no longer
6. Reagents
evolved. Place the dish in a furnace at 550 6 25°C (1022 6
45°F) and continue heating until the oxidation of the carbon is
6.1 Purity of Reagents—Reagent grade chemicals shall be
practically complete.
used in all tests. Unless otherwise indicated, it is intended that
all reagents shall conform to the specifications of the Commit-
1 3
This test method is under the jurisdiction of ASTM Committee D02 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 on Elemental Analysis. listed by the American Chemical Society, see Analar Standards for Laboratory
Current edition approved May 10, 2003. Published July 2003. Originally Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
approved in 1974. Last previous edition approved in 1998 as D 3340–98. 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.
D3340–98 (2003)
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 0.007 0.039
M
...