ASTM D6481-24
(Test Method)Standard Test Method for Determination of Phosphorus, Sulfur, Calcium, and Zinc in Lubrication Oils by Energy Dispersive X-ray Fluorescence Spectroscopy
Standard Test Method for Determination of Phosphorus, Sulfur, Calcium, and Zinc in Lubrication Oils by Energy Dispersive X-ray Fluorescence Spectroscopy
SIGNIFICANCE AND USE
5.1 Some oils are formulated with organo-metallic additives, which act, for example, as detergents, antioxidants, and antiwear agents. Some of these additives contain one or more of these elements: calcium, phosphorus, sulfur, and zinc. 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 This test method is primarily intended to be used at a manufacturing location for monitoring of additive elements in lubricating oils. It can also be used in central and research laboratories.
SCOPE
1.1 This test method covers the quantitative determination of additive elements in unused lubricating oils, as shown in Table 1.
1.2 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.
1.3 This test method uses interelement correction factors calculated from empirical calibration data.
1.4 This test method is not suitable for the determination of magnesium and copper at the concentrations present in lubricating oils.
1.5 This test method excludes lubricating oils that contain chlorine or barium as an additive element.
1.6 This test method can be used by persons who are not skilled in X-ray spectrometry. It is intended to be used as a routine test method for production control analysis.
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, health, and environmental practices and determine the applicability of regulatory limitations to use.
1.8 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: D6481 − 24
Standard Test Method for
Determination of Phosphorus, Sulfur, Calcium, and Zinc in
Lubrication Oils by Energy Dispersive X-ray Fluorescence
1
Spectroscopy
This standard is issued under the fixed designation D6481; 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. Scope* 2. Referenced Documents
2
1.1 This test method covers the quantitative determination 2.1 ASTM Standards:
of additive elements in unused lubricating oils, as shown in D4175 Terminology Relating to Petroleum Products, Liquid
Table 1. Fuels, and Lubricants
1.2 This test method is limited to the use of energy
3. Terminology
dispersive X-ray fluorescence (EDXRF) spectrometers em-
3.1 Definitions:
ploying an X-ray tube for excitation in conjunction with the
3.1.1 For definitions of terms used in this test method, refer
ability to separate the signals of adjacent elements.
to Terminology D4175.
1.3 This test method uses interelement correction factors
calculated from empirical calibration data.
4. Summary of Test Method
1.4 This test method is not suitable for the determination of 4.1 A specimen is placed in the X-ray beam, and the
magnesium and copper at the concentrations present in lubri-
appropriate regions of its spectrum are measured to give the
cating oils. fluorescent intensities of phosphorus, sulfur, calcium, and zinc.
Other regions of the spectrum are measured to compensate for
1.5 This test method excludes lubricating oils that contain
varying background. If the detector does not completely
chlorine or barium as an additive element.
resolve all the elements in a single measurement, then to
1.6 This test method can be used by persons who are not
improve selectivity, there is a combination of sequential and
skilled in X-ray spectrometry. It is intended to be used as a
simultaneous measurements employing primary and secondary
routine test method for production control analysis.
beam filters. There can be correction of measured intensities
1.7 This standard does not purport to address all of the
for spectral overlap. Concentrations of the elements of interest
safety concerns, if any, associated with its use. It is the
are determined by comparison of these intensities against a
responsibility of the user of this standard to establish appro-
calibration curve using empirical interelement correction fac-
priate safety, health, and environmental practices and deter-
tors and ratio to backscatter.
mine the applicability of regulatory limitations to use.
4.2 The EDXRF spectrometer is initially calibrated using a
1.8 This international standard was developed in accor-
set of prepared standards to collect the necessary intensity data.
dance with internationally recognized principles on standard-
Each calibration line and any correction coefficient are ob-
ization established in the Decision on Principles for the
tained by a regression of this data, using the program supplied
Development of International Standards, Guides and Recom-
with the spectrometer.
mendations issued by the World Trade Organization Technical
Barriers to Trade (TBT) Committee.
5. Significance and Use
5.1 Some oils are formulated with organo-metallic
additives, which act, for example, as detergents, antioxidants,
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
2
Subcommittee D02.03 on Elemental Analysis. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved March 1, 2024. Published March 2024. Originally contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
approved in 1999. Last previous edition approved in 2019 as D6481 – 14 (2019). Standards volume information, refer to the standard’s Document Summary page on
DOI: 10.1520/D6481-24. 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 ----------------------
D6481 − 24
TABLE 1 Elements and Range of Concentrations Determined
6.4 There can be spectral overlap of one element onto
Element Concentration Range another, especially for phosphorus on sulfur, and the instru-
Phosphorus 0.02 % to 0.3 % by mass ment must include correction procedures for any such overlaps.
Sulfur 0.05 % to 1.0 % by mass
Calciu
...
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.
Designation: D6481 − 14 (Reapproved 2019) D6481 − 24
Standard Test Method for
Determination of Phosphorus, Sulfur, Calcium, and Zinc in
Lubrication Oils by Energy Dispersive X-ray Fluorescence
1
Spectroscopy
This standard is issued under the fixed designation D6481; 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. Scope Scope*
1.1 This test method covers the quantitative determination of additive elements in unused lubricating oils, as shown in Table 1.
1.2 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.
1.3 This test method uses interelement correction factors calculated from empirical calibration data.
1.4 This test method is not suitable for the determination of magnesium and copper at the concentrations present in lubricating
oils.
1.5 This test method excludes lubricating oils that contain chlorine or barium as an additive element.
1.6 This test method can be used by persons who are not skilled in X-ray spectrometry. It is intended to be used as a routine test
method for production control analysis.
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, health, and environmental practices and determine the applicability of
regulatory limitations to use.
1.8 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.
2. Referenced Documents
2
2.1 ASTM Standards:
D4175 Terminology Relating to Petroleum Products, Liquid Fuels, and Lubricants
3. Terminology
3.1 Definitions:
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 May 1, 2019March 1, 2024. Published July 2019March 2024. Originally approved in 1999. Last previous edition approved in 20142019 as
D6481 – 14.D6481 – 14 (2019). DOI: 10.1520/D6481-14R19.10.1520/D6481-24.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on 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 ----------------------
D6481 − 24
TABLE 1 Elements and Range of Concentrations Determined
Element Concentration Range
Phosphorus 0.02 mass % to 0.3 mass %
Sulfur 0.05 mass % to 1.0 mass %
Calcium 0.02 mass % to 1.0 mass %
Zinc 0.01 mass % to 0.3 mass %
TABLE 1 Elements and Range of Concentrations Determined
Element Concentration Range
Phosphorus 0.02 % to 0.3 % by mass
Sulfur 0.05 % to 1.0 % by mass
Calcium 0.02 % to 1.0 % by mass
Zinc 0.01 % to 0.3 % by mass
3.1.1 For definitions of terms used in this test method, refer to Terminology D4175.
4. Summary of Test Method
4.1 A specimen is placed in the X-ray beam, and the appropriate regions of its spectrum are measured to give the fluorescent
intensities of phosphorus, sulfur, calcium, and zinc. Other regions of the spectrum are measured to compensate for varying
background. If the detector does not completely resolve all the elements in a single measurement, then to improve selectivity, there
is a combination of sequential and simultaneous measurements employing primary and secondary beam filters. There can be
correction of measured intensities for spectral overlap. Concentrations of the elements of interest are determined by comparison
of these intensities against a calibration curve using empirical interelement correction factors and ratio to backscatter.
4.2 The EDXRF spectrometer is initially calibrated using a set of prepared standards to collect the necessary intensity
...
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