ASTM D5185-18
(Test Method)Standard Test Method for Multielement Determination of Used and Unused Lubricating Oils and Base Oils by Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES)
Standard Test Method for Multielement Determination of Used and Unused Lubricating Oils and Base Oils by Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES)
SIGNIFICANCE AND USE
5.1 This test method covers the rapid determination of 22 elements in used and unused lubricating oils and base oils, and it provides rapid screening of used oils for indications of wear. Test times approximate a few minutes per test specimen, and detectability for most elements is in the low mg/kg range. In addition, this test method covers a wide variety of metals in virgin and re-refined base oils. Twenty-two elements can be determined rapidly, with test times approximating several minutes per test specimen.
5.2 When the predominant source of additive elements in used lubricating oils is the additive package, significant differences between the concentrations of the additive elements and their respective specifications can indicate that the incorrect oil is being used. The concentrations of wear metals can be indicative of abnormal wear if there are baseline concentration data for comparison. A marked increase in boron, sodium, or potassium levels can be indicative of contamination as a result of coolant leakage in the equipment. This test method can be used to monitor equipment condition and define when corrective actions are needed.
5.2.1 The significance of metal analysis in used lubricating oils is tabulated in Table 4.
5.3 The concentrations of metals in re-refined base oils can be indicative of the efficiency of the re-refining process. This test method can be used to determine if the base oil meets specifications with respect to metal content.
SCOPE
1.1 This test method covers the determination of additive elements, wear metals, and contaminants in used and unused lubricating oils and base oils by inductively coupled plasma atomic emission spectrometry (ICP-AES). The specific elements are listed in Table 1. (A) These wavelengths are only suggested and do not represent all possible choices.
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.2
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. (A) where: X = mean concentration, μg/g. (A) where: X = mean concentration, μg/g.
1.7 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
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, health, and environmental practices and determine the applicability of regulatory limitations prior to use. Specific warning statements are given in 6.1, 8.2, and 8.4.
1.9 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.
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Standards Content (Sample)
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: D5185 − 18
Standard Test Method for
Multielement Determination of Used and Unused Lubricating
Oils and Base Oils by Inductively Coupled Plasma Atomic
1
Emission Spectrometry (ICP-AES)
This standard is issued under the fixed designation D5185; 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.
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
varietyofusedoilsthistestmethodcan,inprinciple,beusedfortheanalysisofunusedoilstoprovide
more complete elemental composition data than Test Methods D4628, D4927,or D4951.
1. Scope* 1.6 For elements other than calcium, sulfur, and zinc, the
lowlimitslistedinTable2andTable3wereestimatedtobeten
1.1 This test method covers the determination of additive
times the repeatability standard deviation. For calcium, sulfur,
elements, wear metals, and contaminants in used and unused
and zinc, the low limits represent the lowest concentrations
lubricating oils and base oils by inductively coupled plasma
tested in the interlaboratory study.
atomic emission spectrometry (ICP-AES). The specific ele-
1.7 The values stated in SI units are to be regarded as
ments are listed in Table 1.
standard. No other units of measurement are included in this
1.2 This test method covers the determination of selected
standard.
elements, listed in Table 1, in re-refined and virgin base oils.
1.8 This standard does not purport to address all of the
1.3 For analysis of any element using wavelengths below
safety concerns, if any, associated with its use. It is the
190 nm, a vacuum or inert-gas optical path is required. The
responsibility of the user of this standard to establish appro-
determinationofsodiumandpotassiumisnotpossibleonsome
priate safety, health, and environmental practices and deter-
instruments having a limited spectral range.
mine the applicability of regulatory limitations prior to use.
Specific warning statements are given in 6.1, 8.2, and 8.4.
1.4 This test method uses oil-soluble metals for calibration
1.9 This international standard was developed in accor-
and does not purport to quantitatively determine insoluble
dance with internationally recognized principles on standard-
particulates.Analytical results are particle size dependent, and
ization established in the Decision on Principles for the
low results are obtained for particles larger than a few
2
Development of International Standards, Guides and Recom-
micrometers.
mendations issued by the World Trade Organization Technical
1.5 Elementspresentatconcentrationsabovetheupperlimit
Barriers to Trade (TBT) Committee.
of the calibration curves can be determined with additional,
appropriate dilutions and with no degradation of precision.
2. Referenced Documents
3
2.1 ASTM Standards:
C1109 Practice for Analysis of Aqueous Leachates from
1
This test method is under the jurisdiction of ASTM Committee D02 on
Nuclear Waste Materials Using Inductively Coupled
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of
Subcommittee D02.03 on Elemental Analysis.
Current edition approved April 1, 2018. Published April 2018. Originally
ɛ1
3
approved in 1991. Last previous edition approved in 2013 as D5185 – 13 . DOI: For referenced ASTM standards, visit the ASTM website, www.astm.org, or
10.1520/D5185-18. contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
2
Eisentraut, K. J., Newman, R. W., Saba, C. S., Kauffman, R. E., and Rhine, W. Standards volume information, refer to the standard’s Document Summary page on
E., Analytical Chemistry, Vol 56, 1984. the ASTM website.
*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
1
---------------------- Page: 1 ----------------------
D5185 − 18
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
...
This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
´1
Designation: D5185 − 13 D5185 − 18
Standard Test Method for
Multielement Determination of Used and Unused Lubricating
Oils and Base Oils by Inductively Coupled Plasma Atomic
1
Emission Spectrometry (ICP-AES)
This standard is issued under the fixed designation D5185; 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
ε NOTE—Table 4 was editorially corrected in April 2014.
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 D4628, D4927, or D4951.
1. Scope*
1.1 This test method covers the determination of additive elements, wear metals, and contaminants in used and unused
lubricating oils and base 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, 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
2
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 units are to be regarded as standard. No other units of measurement are included in this standard.
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 safety, health, and healthenvironmental practices and determine the
applicability of regulatory limitations prior to use. Specific warning statements are given in 6.1, 8.2, and 8.4.
1.9 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.
1
This test method is under the jurisdiction of ASTM Committee D02 on Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of Subcommittee
D02.03 on Elemental Analysis.
Current edition approved Sept. 15, 2013April 1, 2018. Published September 2013April 2018. Originally approved in 1991. Last previous edition approved in 20092013
ɛ1
as D5185 – 09.D5185 – 13 . DOI: 10.1520/D5185-13E01.10.1520/D5185-18.
2
Eisentraut, K. J., Newman, R. W., Saba, C. S., Kauffman, R. E., and Rhine, W. E., Analytical Chemistry, Vol 56, 1984.
*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
1
---------------------- Page: 1 ----------------------
D5185 − 18
A
TABLE 1 Elements Determined and Suggested Wavelengths
Element Wavelength, nm
Aluminum 308.22, 396.15, 309.27
Barium 233.53, 455.40, 493.41
Boron 249.77
Calcium 315.89, 317.93, 364.44, 422.67
Chromium 205.55, 267.72
Copper 324.75
Iron 259.94, 238.20
Lead 220.3
...
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