ASTM D7751-14e1
(Test Method)Standard Test Method for Determination of Additive Elements in Lubricating Oils by EDXRF Analysis
Standard Test Method for Determination of Additive Elements in Lubricating Oils by EDXRF Analysis
SIGNIFICANCE AND USE
5.1 Lubricating oils are formulated with organo-metallic additives, which act, for example, as detergents, antioxidants, antifoaming, or antiwear agents, or a combination thereof. Some of these additives contain one or more of the following elements: magnesium, phosphorus, sulfur, chlorine, calcium, zinc, and molybdenum. This test method provides a means of determining the concentrations of these elements, which in turn provides an indication of the additive content of these oils.
5.2 Several additive elements and their compounds are added to the lubricating oils to give beneficial performance (Table 2).
5.3 Additive packages are the concentrates that are used to blend lubricating oils.
5.4 This test method is primarily intended to be used for the monitoring of additive elements in lubricating oils.
5.5 If this test method is applied to lubricating oils with matrices significantly different from the calibration materials specified in this test method, the cautions and recommendations in Section 6 should be observed when interpreting the results.
SCOPE
1.1 This test method covers the quantitative determination of additive elements in unused lubricating oils and additive packages, as shown in Table 1. The pooled limit of quantitation of this test method as obtained by statistical analysis of interlaboratory test results is 0.02 % for magnesium, 0.003 % for phosphorus, 0.002 % for sulfur, 0.001 % for chlorine, 0.003 % for calcium, 0.001 % for zinc, and 0.002 % for molybdenum.
1.2 Additive packages require dilution with a contamination free diluent (base oil) prior to analysis. The dilution factor has to be calculated from the expected concentrations to bring the concentrations for all elements into the ranges listed in Table 1.
1.3 Some lubrication oils will contain higher concentrations than the maximum concentrations listed in Table 1. These samples require dilution with a contamination free diluent (base oil) prior to analysis. The dilution factor has to be calculated from the expected concentrations to bring the concentrations for all elements into the ranges listed in Table 1.
1.4 This test method is limited to the use of energy dispersive X-ray fluorescence (EDXRF) spectrometers employing an X-ray tube for excitation in conjunction with the ability to separate the signals of adjacent elements by using a high resolution semiconductor detector.
1.5 This test method uses inter-element correction factors calculated from a fundamental parameters (FP) approach or from another matrix correction method.
1.6 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.6.1 The preferred concentration units are mg/kg or mass %.
1.7 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.
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´1
Designation: D7751 − 14
Standard Test Method for
Determination of Additive Elements in Lubricating Oils by
1
EDXRF Analysis
This standard is issued under the fixed designation D7751; 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.
1
ε NOTE—Table 4 was corrected editorially in November 2015.
1. Scope* 1.7 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
1.1 This test method covers the quantitative determination
responsibility of the user of this standard to establish appro-
of additive elements in unused lubricating oils and additive
priate safety and health practices and determine the applica-
packages,asshowninTable1.Thepooledlimitofquantitation
bility of regulatory limitations prior to use.
of this test method as obtained by statistical analysis of
interlaboratory test results is 0.02 % for magnesium, 0.003 %
2. Referenced Documents
for phosphorus, 0.002 % for sulfur, 0.001 % for chlorine,
2
2.1 ASTM Standards:
0.003 % for calcium, 0.001 % for zinc, and 0.002 % for
D4057 Practice for Manual Sampling of Petroleum and
molybdenum.
Petroleum Products
1.2 Additivepackagesrequiredilutionwithacontamination
D4177 Practice for Automatic Sampling of Petroleum and
free diluent (base oil) prior to analysis. The dilution factor has
Petroleum Products
to be calculated from the expected concentrations to bring the
D6299 Practice for Applying Statistical Quality Assurance
concentrationsforallelementsintotherangeslistedinTable1.
and Control Charting Techniques to Evaluate Analytical
1.3 Some lubrication oils will contain higher concentrations
Measurement System Performance
than the maximum concentrations listed in Table 1. These
D6300 Practice for Determination of Precision and Bias
samples require dilution with a contamination free diluent
Data for Use in Test Methods for Petroleum Products and
(base oil) prior to analysis. The dilution factor has to be
Lubricants
calculated from the expected concentrations to bring the
D6792 Practice for Quality System in Petroleum Products
concentrationsforallelementsintotherangeslistedinTable1.
and Lubricants Testing Laboratories
D7343 Practice for Optimization, Sample Handling,
1.4 This test method is limited to the use of energy
Calibration, and Validation of X-ray Fluorescence Spec-
dispersive X-ray fluorescence (EDXRF) spectrometers em-
trometry Methods for Elemental Analysis of Petroleum
ploying an X-ray tube for excitation in conjunction with the
Products and Lubricants
ability to separate the signals of adjacent elements by using a
E1621 Guide for ElementalAnalysis by Wavelength Disper-
high resolution semiconductor detector.
sive X-Ray Fluorescence Spectrometry
1.5 This test method uses inter-element correction factors
3
2.2 ISO Standards:
calculated from a fundamental parameters (FP) approach or
ISO 4259 Determination and application of precision data in
from another matrix correction method.
relation to methods of test
1.6 The values stated in SI units are to be regarded as
standard. No other units of measurement are included in this
3. Terminology
standard.
3.1 Definitions:
1.6.1 The preferred concentration units are mg/kg or mass
3.1.1 energy dispersive X-ray spectrometry, n—XRF spec-
%.
trometry applying energy dispersive selection of radiation.
1 2
This test method is under the jurisdiction of ASTM Committee D02 on For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Subcommittee D02.03 on Elemental Analysis. Standards volume information, refer to the standard’s Document Summary page on
Current edition approved Dec. 1, 2014. Published January 2015. Originally the ASTM website.
3
approved in 2011. Last previous edition approved in 2012 as D7751 – 12. Available from International Organization for Standardization (ISO), 1, ch. de
DOI:10.1520/D7751-14E01. la Voie-Creuse, CP 56, CH-1211 Geneva 20, Switzerland, http://www.iso.org.
*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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D7751 − 14
TABLE 1 Elements and Range of Applicability
Some of these additives contain one or more of the following
Element Concentration Range in mass % elements: magnesium, phosphorus, sulfur, chlorine, calcium,
Magnesium 0.02 to 0.4 zinc, and molybdenum. This
...
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: D7751 − 14 D7751 − 14
Standard Test Method for
Determination of Additive Elements in Lubricating Oils by
1
EDXRF Analysis
This standard is issued under the fixed designation D7751; 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.
1
ε NOTE—Table 4 was corrected editorially in November 2015.
1. Scope*
1.1 This test method covers the quantitative determination of additive elements in unused lubricating oils and additive packages,
as shown in Table 1. The pooled limit of quantitation of this test method as obtained by statistical analysis of interlaboratory test
results is 0.02 % for magnesium, 0.003 % for phosphorus, 0.002 % for sulfur, 0.001 % for chlorine, 0.003 % for calcium, 0.001 %
for zinc, and 0.002 % for molybdenum.
1.2 Additive packages require dilution with a contamination free diluent (base oil) prior to analysis. The dilution factor has to
be calculated from the expected concentrations to bring the concentrations for all elements into the ranges listed in Table 1.
1.3 Some lubrication oils will contain higher concentrations than the maximum concentrations listed in Table 1. These samples
require dilution with a contamination free diluent (base oil) prior to analysis. The dilution factor has to be calculated from the
expected concentrations to bring the concentrations for all elements into the ranges listed in Table 1.
1.4 This test method is limited to the use of energy dispersive X-ray fluorescence (EDXRF) spectrometers employing an X-ray
tube for excitation in conjunction with the ability to separate the signals of adjacent elements by using a high resolution
semiconductor detector.
1.5 This test method uses inter-element correction factors calculated from a fundamental parameters (FP) approach or from
another matrix correction method.
1.6 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.6.1 The preferred concentration units are mg/kg or mass %.
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 Dec. 1, 2014. Published January 2015. Originally approved in 2011. Last previous edition approved in 2012 as D7751 – 12.
DOI:10.1520/D7751-14.DOI:10.1520/D7751-14E01.
TABLE 1 Elements and Range of Applicability
Element Concentration Range in mass %
Magnesium 0.02 to 0.4
Phosphorous 0.003 to 0.25
Sulfur 0.002 to 1.5
Chlorine 0.001 to 0.4
Calcium 0.003 to 1.0
Zinc 0.001 to 0.25
Molybdenum 0.002 to 0.05
*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 ----------------------
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D7751 − 14
1.7 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.
2. Referenced Documents
2
2.1 ASTM Standards:
D4057 Practice for Manual Sampling of Petroleum and Petroleum Products
D4177 Practice for Automatic Sampling of Petroleum and Petroleum Products
D6299 Practice for Applying Statistical Quality Assurance and Control Charting Techniques to Evaluate Analytical Measure-
ment System Performance
D6300 Practice for Determination of Precision and Bias Data for Use in Test Methods for Petroleum Products and Lubricants
D6792 Practice for Quality System in Petroleum Products and Lubricants Testing Laboratories
D7343 Practice for Optimization, Sample Handling, Calibration, and Validation of X-ray Fluorescence Spectrometry Methods
for Elemental Analysis of Petroleum Products and Lubricants
E1621 Guide for Elemental Analysis by Wavelength Dispersive X-Ray Fluorescence Spectrometry
3
2.2 ISO Standards:
ISO 4259 Determination and application of precision data in relation to methods of test
3. Terminology
3.1 Definitions:
3.1.1 energy dispersive X-ray spectrometry, n—XRF spectrometry applying energy dispersive selection of radiation.
3.2 Abbreviations:
3.2.1 EDXRF—Energy Dispersive X-ray Fluorescence Spectromet
...
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