ASTM D4927-14
(Test Method)Standard Test Methods for Elemental Analysis of Lubricant and Additive Components—Barium, Calcium, Phosphorus, Sulfur, and Zinc by Wavelength-Dispersive X-Ray Fluorescence Spectroscopy
Standard Test Methods for Elemental Analysis of Lubricant and Additive Components—Barium, Calcium, Phosphorus, Sulfur, and Zinc by Wavelength-Dispersive X-Ray Fluorescence Spectroscopy
SIGNIFICANCE AND USE
4.1 Some oils are formulated with organo-metallic additives which act as detergents, antioxidants, antiwear agents, and so forth. Some of these additives contain one or more of these elements: barium, calcium, phosphorus, sulfur, and zinc. These test methods provide a means of determining the concentration of these elements which in turn provides an indication of the additive content of these oils.
4.2 Several additive elements and their compounds are added to the lubricating oils to give beneficial performance (see Table 2).
SCOPE
1.1 These test methods cover the determination of barium, calcium, phosphorus, sulfur, and zinc in unused lubricating oils at element concentration ranges shown in Table 1. The range can be extended to higher concentrations by dilution of sample specimens. Additives can also be determined after dilution. Two different methods are presented in these test methods.
1.2 Test Method A (Internal Standard Procedure)—Internal standards are used to compensate for interelement effects of X-ray excitation and fluorescence (see Sections 8 through 13).
1.3 Test Method B (Mathematical Correction Procedure)—The measured X-ray fluorescence intensity for a given element is mathematically corrected for potential interference from other elements present in the sample (see Sections 14 through 19).
1.4 The preferred concentration units are mass % barium, calcium, phosphorus, sulfur, or zinc.
1.5 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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Designation: D4927 − 14
StandardTest Methods for
Elemental Analysis of Lubricant and Additive Components—
Barium, Calcium, Phosphorus, Sulfur, and Zinc by
1
Wavelength-Dispersive X-Ray Fluorescence Spectroscopy
This standard is issued under the fixed designation D4927; 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. Scope* 3. Summary of the Test Methods
1.1 These test methods cover the determination of barium,
3.1 Asample specimen is placed in the X-ray beam and the
calcium,phosphorus,sulfur,andzincinunusedlubricatingoils intensity of the appropriate fluorescence lines of barium,
at element concentration ranges shown in Table 1. The range
calcium,phosphorus,sulfur,andzincaremeasured.Instrument
can be extended to higher concentrations by dilution of sample response factors related to the concentration of standards
specimens. Additives can also be determined after dilution.
enable the determination of the concentration of elements in
Two different methods are presented in these test methods. thetestedsamplespecimens.Enhancementordepressionofthe
X-ray fluorescence of a given element by an interfering
1.2 Test Method A (Internal Standard Procedure)—Internal
element in the sample may occur. Two test methods (A and B)
standards are used to compensate for interelement effects of
are described for compensating any interference effect.
X-ray excitation and fluorescence (see Sections 8 through 13).
3.2 Test Method A (Internal Standard Procedure)—Internal
1.3 Test Method B (Mathematical Correction Procedure)—
standards are used with the standards and sample specimens to
The measured X-ray fluorescence intensity for a given element
compensate for the potential interelement effects.
is mathematically corrected for potential interference from
3.2.1 Barium, Calcium, Phosphorus, and Zinc—A sample
other elements present in the sample (see Sections 14 through
specimen that has been blended with a single internal standard
19).
solution (containing tin or titanium for barium and calcium,
1.4 The preferred concentration units are mass % barium,
zirconium for phosphorus, and nickel for zinc) is poured into
calcium, phosphorus, sulfur, or zinc.
an X-ray cell. Total net counts (peak intensity—background)
1.5 This standard does not purport to address all of the
for each element and its respective internal standard are
safety concerns, if any, associated with its use. It is the
collected at their appropriate wavelengths. The ratios between
responsibility of the user of this standard to establish appro-
elemental and internal standard counts are calculated and
priate safety and health practices and determine the applica-
converted into barium, calcium, phosphorus, or zinc
bility of regulatory limitations prior to use.
concentrations, or a combination thereof, from calibration
curves.
2. Referenced Documents
3.2.2 Sulfur—A sample specimen is mixed with a lead
2
internal standard solution and analyzed as described in 3.2.1.
2.1 ASTM Standards:
D6299 Practice for Applying Statistical Quality Assurance
3.3 Test Method B (Mathematical Correction Procedure)—
and Control Charting Techniques to Evaluate Analytical
The measured intensity for a given element is mathematically
Measurement System Performance
corrected for the interference from other elements in the
sample specimen. This requires that intensities from all ele-
ments in the specimen be obtained.
1
These test methods are under the jurisdiction of ASTM Committee D02 on
3.3.1 The sample specimen is placed in the X-ray beam and
Petroleum Products, Liquid Fuels, and Lubricants and are the direct responsibility
the intensities of the fluorescence lines of barium, calcium,
of Subcommittee D02.03 on Elemental Analysis.
phosphorus, sulfur, and zinc are measured.Asimilar measure-
Current edition approved Dec. 1, 2014. Published January 2015. Originally
ment is made away from the fluorescence lines in order to
approved in 1989. Last previous edition approved in 2010 as D4927 – 10. DOI:
10.1520/D4927-14.
obtainabackgroundcorrection.Concentrationsoftheelements
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
of interest are determined by comparison of net signals against
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
appropriate interelement correction factors developed from
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. responses of calibration standards.
*A Summary of Changes section appears at the
...
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: D4927 − 10 D4927 − 14
Standard Test Methods for
Elemental Analysis of Lubricant and Additive Components—
Barium, Calcium, Phosphorus, Sulfur, and Zinc by
1
Wavelength-Dispersive X-Ray Fluorescence Spectroscopy
This standard is issued under the fixed designation D4927; 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. Scope*
1.1 These test methods cover the determination of barium, calcium, phosphorus, sulfur, and zinc in unused lubricating oils at
element concentration ranges shown in Table 1. The range can be extended to higher concentrations by dilution of sample
specimens. Additives can also be determined after dilution. Two different methods are presented in these test methods.
1.2 Test Method A (Internal Standard Procedure)—Internal standards are used to compensate for interelement effects of X-ray
excitation and fluorescence (see Sections 8 through 13).
1.3 Test Method B (Mathematical Correction Procedure)—The measured X-ray fluorescence intensity for a given element is
mathematically corrected for potential interference from other elements present in the sample (see Sections 14 through 19).
1.4 The preferred concentration units are mass % barium, calcium, phosphorus, sulfur, or zinc.
1.5 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:
D6299 Practice for Applying Statistical Quality Assurance and Control Charting Techniques to Evaluate Analytical Measure-
ment System Performance
3. Summary of the Test Methods
3.1 A sample specimen is placed in the X-ray beam and the intensity of the appropriate fluorescence lines of barium, calcium,
phosphorus, sulfur, and zinc are measured. Instrument response factors related to the concentration of standards enable the
determination of the concentration of elements in the tested sample specimens. Enhancement or depression of the X-ray
fluorescence of a given element by an interfering element in the sample may occur. Two test methods (A and B) are described for
compensating any interference effect.
3.2 Test Method A (Internal Standard Procedure)—Internal standards are used with the standards and sample specimens to
compensate for the potential interelement effects.
3.2.1 Barium, Calcium, Phosphorus, and Zinc—A sample specimen that has been blended with a single internal standard
solution (containing tin or titanium for barium and calcium, zirconium for phosphorus, and nickel for zinc) is poured into an X-ray
cell. Total net counts (peak intensity—background) for each element and its respective internal standard are collected at their
appropriate wavelengths. The ratios between elemental and internal standard counts are calculated and converted into barium,
calcium, phosphorus, or zinc concentrations, or a combination thereof, from calibration curves.
3.2.2 Sulfur—A sample specimen is mixed with a lead internal standard solution and analyzed as described in 3.2.1.
1
These test methods are under the jurisdiction of ASTM Committee D02 on Petroleum Products Products, Liquid Fuels, and Lubricants and are the direct responsibility
of Subcommittee D02.03 on Elemental Analysis.
Current edition approved July 1, 2010Dec. 1, 2014. Published July 2010January 2015. Originally approved in 1989. Last previous edition approved in 20052010 as
D4927D4927 – 10.–05. DOI: 10.1520/D4927-10.10.1520/D4927-14.
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
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D4927 − 14
TABLE 1 Range of Applicability
Element Range, Mass %
Barium 0.04-8.5
Calcium 0.01-1.0
Phosphorus 0.01-0.5
Sulfur 0.1-4.0
Zinc 0.01-0.6
3.3 Tes
...
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