ASTM D4927-02

Standard Test Methods for Elemental Analysis of Lubricant and Additive Components—Barium, Calcium, Phosphorus, Sulfur, and Zinc by Wavelength-Dispersive X-Ray Fluorescence Spectroscopy

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 . 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 1-11, and 17).
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 1-6, and 12-17).
1.4 The preferred concentration units are mass percent 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.

General Information

• Status: Historical
• Publication Date: 09-Nov-2002
• ICS: 75.100 - Lubricants, industrial oils and related products
• Technical Committee: D02 - Petroleum Products, Liquid Fuels, and Lubricants
• Drafting Committee: D02.03 - Elemental Analysis

Relations

• Replaces: ASTM D4927-01 - Standard Test Methods for Elemental Analysis of Lubricant and Additive Components—Barium, Calcium, Phosphorus, Sulfur, and Zinc by Wavelength-Dispersive X-Ray Fluorescence Spectroscopy
• Effective Date: 10-Nov-2002
• Replaced By: ASTM D4927-05 - Standard Test Methods for Elemental Analysis of Lubricant and Additive Components—Barium, Calcium, Phosphorus, Sulfur, and Zinc by Wavelength-Dispersive X-Ray Fluorescence Spectroscopy
• Effective Date: 01-Apr-2005
• Referred By: ASTM D6443-14(2019)e1 - Standard Test Method for Determination of Calcium, Chlorine, Copper, Magnesium, Phosphorus, Sulfur, and Zinc in Unused Lubricating Oils and Additives by Wavelength Dispersive X-ray Fluorescence Spectrometry (Mathematical Correction Procedure)
• Effective Date: 10-Nov-2002
• Referred By: ASTM D4951-14(2019) - Standard Test Method for Determination of Additive Elements in Lubricating Oils by Inductively Coupled Plasma Atomic Emission Spectrometry
• Effective Date: 10-Nov-2002
• Referred By: ASTM D5185-18 - Standard Test Method for Multielement Determination of Used and Unused Lubricating Oils and Base Oils by Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES)
• Effective Date: 10-Nov-2002
• Referred By: ASTM D7455-19 - Standard Practice for Sample Preparation of Petroleum and Lubricant Products for Elemental Analysis
• Effective Date: 10-Nov-2002
• Referred By: ASTM D7343-20 - Standard Practice for Optimization, Sample Handling, Calibration, and Validation of X-ray Fluorescence Spectrometry Methods for Elemental Analysis of Petroleum Products and Lubricants
• Effective Date: 10-Nov-2002
• Referred By: ASTM D7040-04(2020) - Standard Test Method for Determination of Low Levels of Phosphorus in ILSAC GF 4 and Similar Grade Engine Oils by Inductively Coupled Plasma Atomic Emission Spectrometry
• Effective Date: 10-Nov-2002
• Referred By: ASTM D2622-21 - Standard Test Method for Sulfur in Petroleum Products by Wavelength Dispersive X-ray Fluorescence Spectrometry
• Effective Date: 10-Nov-2002
• Referred By: ASTM D7578-20 - Standard Guide for Calibration Requirements for Elemental Analysis of Petroleum Products and Lubricants
• Effective Date: 10-Nov-2002
• Referred By: ASTM D8110-17 - Standard Test Method for Elemental Analysis of Distillate Products by Inductively Coupled Plasma Mass Spectrometry (ICP-MS)
• Effective Date: 10-Nov-2002
• Referred By: ASTM D6074-15(2022) - Standard Guide for Characterizing Hydrocarbon Lubricant Base Oils
• Effective Date: 10-Nov-2002

Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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An American National Standard
Designation:D4927–02
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 D 4927; 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.
TABLE 1 Range of Applicability
1. Scope *
Element Range, Mass %
1.1 These test methods cover the determination of barium,
calcium,phosphorus,sulfur,andzincinunusedlubricatingoils
Barium 0.04 - 8.5
at element concentration ranges shown in Table 1. The range
Calcium 0.01 - 1.0
can be extended to higher concentrations by dilution of sample
Phosphorus 0.01 - 0.5
Sulfur 0.1 - 4.0
specimens. Additives can also be determined after dilution.
Zinc 0.01 - 0.6
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
response factors related to the concentration of standards
X-ray excitation and fluorescence (see Sections 1-11, and 17).
enable the determination of the concentration of elements in
1.3 Test Method B (Mathematical Correction Procedure)—
thetestedsamplespecimens.Enhancementordepressionofthe
The measured X-ray fluorescence intensity for a given element
X-ray fluorescence of a given element by an interfering
is mathematically corrected for potential interference from
element in the sample may occur. Two test methods (A and B)
other elements present in the sample (see Sections 1-6, and
are described for compensating any interference effect.
12-17).
3.2 Test Method A (Internal Standard Procedure)—Internal
1.4 The preferred concentration units are mass percent
standards are used with the standards and sample specimens to
barium, calcium, phosphorus, sulfur, or zinc.
compensate for the potential interelement effects.
1.5 This standard does not purport to address all of the
3.2.1 Barium, Calcium, Phosphorus, and Zinc—A sample
safety concerns, if any, associated with its use. It is the
specimen that has been blended with a single internal standard
responsibility of the user of this standard to establish appro-
solution (containing tin or titanium for barium and calcium,
priate safety and health practices and determine the applica-
zirconium for phosphorus, and nickel for zinc) is poured into
bility of regulatory limitations prior to use.
an X-ray cell. Total net counts (peak intensity—background)
for each element and its respective internal standard are
2. Referenced Documents
collected at their appropriate wavelengths. The ratios between
2.1 ASTM Standards:
elemental and internal standard counts are calculated and
D 6299 Practice for Applying Statistical Quality Assurance
converted into barium, calcium, phosphorus, or zinc concen-
Techniques to Evaluate Analytical Measurement System
trations, or a combination thereof, from calibration curves.
2
Performance
3.2.2 Sulfur—A sample specimen is mixed with a lead
internal standard solution and analyzed as described in 3.2.1.
3. Summary of the Test Methods
3.3 Test Method B (Mathematical Correction Procedure)—
3.1 Asample specimen is placed in the X-ray beam and the
The measured intensity for a given element is mathematically
intensity of the appropriate fluorescence lines of barium,
corrected for the interference from other elements in the
calcium,phosphorus,sulfur,andzincaremeasured.Instrument
sample specimen. This requires that intensities from all ele-
ments in the specimen be obtained.
1
3.3.1 The sample specimen is placed in the X-ray beam and
These test methods are under the jurisdiction of ASTM Committee D02 on
Petroleum Products and Lubricants and are the direct responsibility of Subcommit-
the intensities of the fluorescence lines of barium, calcium,
tee D02.03on Elemental Analysis.
phosphorus, sulfur, and zinc are measured.Asimilar measure-
Current edition approved Nov. 10, 2002. Published February 2003. Originally
ment is made away from the fluorescence lines in order to
approved in 1989. Last previous edition approved in 2001 as D 4927–01.
2
Annual Book of ASTM Standards, Vol 05.03. obtainabackgroundcorrection.Concentrationsoftheelements
*A Summary of Changes section appears at the end of this standard.
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D4927–02
of interest are determined by
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