ASTM D5185-02e1

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An American National Standard
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Designation: D 5185 – 02
Standard Test Method for
Determination of Additive Elements, Wear Metals, and
Contaminants in Used Lubricating Oils and Determination of
Selected Elements in Base Oils by Inductively Coupled
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Plasma Atomic Emission Spectrometry (ICP-AES)
This standard is issued under the fixed designation D 5185; 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.
This standard has been approved for use by agencies of the Department of Defense.
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e NOTE—Equation 9 and Paragraph 8.3 were corrected editorially in November 2003.
INTRODUCTION
Costs associated with maintenance due to engine and machine wear can be significant. Therefore,
diagnostic methods for determining the condition of engines and other machinery can be important.
This test method is intended to quantify, for the purpose of equipment monitoring, the concentration
of metals in used lubricating oils. Although the precision statement was determined by analyzing a
variety of used oils this test method can, in principle, be used for the analysis of unused oils to provide
more complete elemental composition data than Test Methods D 4628, D 4927 or D 4951.
1. Scope* times the repeatability standard deviation. For calcium, sulfur,
and zinc, the low limits represent the lowest concentrations
1.1 This test method covers the determination of additive
tested in the interlaboratory study.
elements, wear metals, and contaminants in used lubricating
1.7 The values stated in SI (metric) units are to be regarded
oils by inductively coupled plasma atomic emission spectrom-
as the standard. The inch-pound units given in parentheses are
etry (ICP-AES). The specific elements are listed in Table 1.
for information only.
1.2 This test method covers the determination of selected
1.8 This standard does not purport to address all of the
elements, listed in Table 1, in re-refined and virgin base oils.
safety concerns, if any, associated with its use. It is the
1.3 For analysis of any element using wavelengths below
responsibility of the user of this standard to establish appro-
190 nm, a vacuum or inert-gas optical path is required. The
priate safety and health practices and determine the applica-
determination of sodium and potassium is not possible on some
bility of regulatory limitations prior to use. Specific precau-
instruments having a limited spectral range.
tionary statements are given in 6.1, 8.2, and 8.4.
1.4 This test method uses oil-soluble metals for calibration
and does not purport to quantitatively determine insoluble
2. Referenced Documents
particulates. Analytical results are particle size dependent, and
2.1 ASTM Standards:
low results are obtained for particles larger than a few
2 C 1109 Test Method for Analysis of Aqueous Leachates
micrometers.
from Nuclear Waste Materials Using Inductively Coupled
1.5 Elements present at concentrations above the upper limit
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Plasma-Atomic Emission Spectrometry
of the calibration curves can be determined with additional,
D 1552 Test Method for Sulfur in Petroleum Products
appropriate dilutions and with no degradation of precision.
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(High-Temperature Method)
1.6 For elements other than calcium, sulfur, and zinc, the
D 4057 Practice for Manual Sampling of Petroleum and
low limits listed in Table 2 and Table 3 were estimated to be ten
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Petroleum Products
D 4307 Practice for Preparation of Liquid Blends for Use as
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Analytical Standards
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This test method is under the jurisdiction of ASTM Committee D02 on
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
D02.03 on Elemental Analysis.
Current edition approved January 10, 2002. Published March 2002. Originally
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published as D 5185 – 91. Last previous edition D 5185 – 97. Annual Book of ASTM Standards, Vol 12.01.
2 4
Eisentraut, K. J., Newman, R. W., Saba, C. S., Kauffman, R. E., and Rhine, W. Annual Book of ASTM Standards, Vol 05.01.
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E., Analytical Chemistry, Vol 56, 1984. Annual Book of ASTM Standards, Vol 05.02.
*A Summary of Changes section appears at the end of this standard.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
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D5185–02
A
TABLE 1 Elements Determined and Suggested Wavelengths TABLE 3 Reproducibility
A
Element Wavelength, nm Element Range, mg/kg Reproducibility, μg/g
0.26
Aluminum 308.22, 396.15, 309.27 Aluminum 6–40 3.8 X
0.92
Barium 233.53, 455.40, 493.41 Barium 0.5–4 0.59 X
0.01
Boron 249.77 Boron 4–30 13 X
1.3
Calcium 315.89, 317.93, 364.44, 422
...