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 Plasma Atomic Emission Spectrometry (ICP-AES)

SCOPE
1.1 This test method covers the determination of additive elements, wear metals, and contaminants in used lubricating oils by inductively coupled plasma atomic emission spectrometry (ICP-AES). The specific elements are listed in Table 1.
1.2 This test method covers the determination of selected elements, listed in Table 1, in re-refined and virgin base oils.
1.3 For analysis of any element using wavelengths below 190 nm, a vacuum or inert-gas optical path is required. The determination of sodium and potassium is not possible on some instruments having a limited spectral range.
1.4 This test method uses oil-soluble metals for calibration and does not purport to quantitatively determine insoluble particulates. Analytical results are particle size dependent, and low results are obtained for particles larger than a few micrometers.
1.5 Elements present at concentrations above the upper limit of the calibration curves can be determined with additional, appropriate dilutions and with no degradation of precision.
1.6 For elements other than calcium, sulfur, and zinc, the low limits listed in Table 2 and Table 3 were estimated to be ten times the repeatability standard deviation. For calcium, sulfur, and zinc, the low limits represent the lowest concentrations tested in the interlaboratory study.
1.7 The values stated in SI (metric) units are to be regarded as the standard. The inch-pound units given in parentheses are for information only.
1.8 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. Specific precautionary statements are given in 6.1, 8.2, and 8.4

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ASTM D5185-97 - 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 Plasma Atomic Emission Spectrometry (ICP-AES)
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NOTICE: This standard has either been superseded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
Designation: D 5185 – 97 An American National Standard
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
1
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.
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 1.7 The values stated in SI (metric) units are to be regarded
as the standard. The inch-pound units given in parentheses are
1.1 This test method covers the determination of additive
for information only.
elements, wear metals, and contaminants in used lubricating
1.8 This standard does not purport to address all of the
oils by inductively coupled plasma atomic emission spectrom-
safety concerns, if any, associated with its use. It is the
etry (ICP-AES). The specific elements are listed in Table 1.
responsibility of the user of this standard to establish appro-
1.2 This test method covers the determination of selected
priate safety and health practices and determine the applica-
elements, listed in Table 1, in re-refined and virgin base oils.
bility of regulatory limitations prior to use. Specific precau-
1.3 For analysis of any element using wavelengths below
tionary statements are given in Note 1, Note 2, and Note 3.
190 nm, a vacuum or inert-gas optical path is required. The
determination of sodium and potassium is not possible on some
2. Referenced Documents
instruments having a limited spectral range.
2.1 ASTM Standards:
1.4 This test method uses oil-soluble metals for calibration
C 1109 Test Method for Analysis of Aqueous Leachates
and does not purport to quantitatively determine insoluble
from Nuclear Waste Materials Using Inductively Coupled
particulates. Analytical results are particle size dependent, and
3
Plasma-Atomic Emission Spectrometry
low results are obtained for particles larger than a few
2 D 1552 Test Method for Sulfur in Petroleum Products
micrometers.
4
(High-Temperature Method)
1.5 Elements present at concentrations above the upper limit
D 4057 Practice for Manual Sampling of Petroleum and
of the calibration curves can be determined with additional,
5
Petroleum Products
appropriate dilutions and with no degradation of precision.
D 4307 Practice for Preparation of Liquid Blends for Use as
1.6 For elements other than calcium, sulfur, and zinc, the
5
Analytical Standards
low limits listed in Table 2 and Table 3 were estimated to be ten
D 4628 Test Method for Analysis of Barium, Calcium,
times the repeatability standard deviation. For calcium, sulfur,
Magnesium, and Zinc in Unused Lubricating Oils by
and zinc, the low limits represent the lowest concentrations
5
Atomic Absorption Spectrometry
tested in the interlaboratory study.
D 4927 Test Methods for Elemental Analysis of Lubricant
and Additive Components—Barium, Calcium, Phospho-
1
rus, Sulfur, and Zinc by Wavelength-Dispersive X-Ray
This test method is under the jurisdiction of ASTM Committee D-2 on
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
D02.03.0B on Spectrometric Methods.
3
Annual Book of ASTM Standards, Vol 12.01.
Current edition approved Apr. 10, 1997. Published October 1997. Originally
4
Annual Book of ASTM Standards, Vol 05.01.
published as D 5185 – 91. Last previous edition D 5185 – 95.
5
2 Annual Book of ASTM Standards, Vol 05.02.
Eisentraut, K. J., Newman, R. W., Saba, C. S., Kauffman, R. E., and Rhine, W.
E., Analytical Chemistry, Vol 56, 1984.
Copyright © ASTM, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959, United States.
1

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D 5185
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.
...

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