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

SIGNIFICANCE AND USE
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.
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 through ).
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 through ).
1.4 The preferred concentration units are mass % barium, calcium, phosphorus, sulfur, or zinc.
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: 31-Mar-2005
• 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 D4927-02 - Standard Test Methods for Elemental Analysis of Lubricant and Additive Components—Barium, Calcium, Phosphorus, Sulfur, and Zinc by Wavelength-Dispersive X-Ray Fluorescence Spectroscopy
• Effective Date: 01-Apr-2005
• 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: 01-Apr-2005
• Referred By: ASTM D7578-20 - Standard Guide for Calibration Requirements for Elemental Analysis of Petroleum Products and Lubricants
• Effective Date: 01-Apr-2005
• 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: 01-Apr-2005
• Referred By: ASTM D7455-19 - Standard Practice for Sample Preparation of Petroleum and Lubricant Products for Elemental Analysis
• Effective Date: 01-Apr-2005
• Referred By: ASTM D2622-21 - Standard Test Method for Sulfur in Petroleum Products by Wavelength Dispersive X-ray Fluorescence Spectrometry
• Effective Date: 01-Apr-2005
• Referred By: ASTM D8110-17 - Standard Test Method for Elemental Analysis of Distillate Products by Inductively Coupled Plasma Mass Spectrometry (ICP-MS)
• Effective Date: 01-Apr-2005
• 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: 01-Apr-2005
• 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: 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: 01-Apr-2005
• Referred By: ASTM D6074-15(2022) - Standard Guide for Characterizing Hydrocarbon Lubricant Base Oils
• Effective Date: 01-Apr-2005

Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation:D4927–05
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 Department of Defense.
TABLE 1 Range of Applicability
1. Scope*
Element Range, Mass %
1.1 These test methods cover the determination of barium,
Barium 0.04-8.5
calcium,phosphorus,sulfur,andzincinunusedlubricatingoils
Calcium 0.01-1.0
at element concentration ranges shown in Table 1. The range
Phosphorus 0.01-0.5
can be extended to higher concentrations by dilution of sample
Sulfur 0.1-4.0
Zinc 0.01-0.6
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
3. Summary of the Test Methods
standards are used to compensate for interelement effects of
3.1 Asample specimen is placed in the X-ray beam and the
X-ray excitation and fluorescence (see Sections 8 through 13).
intensity of the appropriate fluorescence lines of barium,
1.3 Test Method B (Mathematical Correction Procedure)—
calcium,phosphorus,sulfur,andzincaremeasured.Instrument
The measured X-ray fluorescence intensity for a given element
response factors related to the concentration of standards
is mathematically corrected for potential interference from
enable the determination of the concentration of elements in
other elements present in the sample (see Sections 14 through
thetestedsamplespecimens.Enhancementordepressionofthe
19).
X-ray fluorescence of a given element by an interfering
1.4 The preferred concentration units are mass % barium,
element in the sample may occur. Two test methods (A and B)
calcium, phosphorus, sulfur, or zinc.
are described for compensating any interference effect.
1.5 This standard does not purport to address all of the
3.2 Test Method A (Internal Standard Procedure)—Internal
safety concerns, if any, associated with its use. It is the
standards are used with the standards and sample specimens to
responsibility of the user of this standard to establish appro-
compensate for the potential interelement effects.
priate safety and health practices and determine the applica-
3.2.1 Barium, Calcium, Phosphorus, and Zinc—A sample
bility of regulatory limitations prior to use.
specimen that has been blended with a single internal standard
2. Referenced Documents
solution (containing tin or titanium for barium and calcium,
2
zirconium for phosphorus, and nickel for zinc) is poured into
2.1 ASTM Standards:
an X-ray cell. Total net counts (peak intensity—background)
D6299 Practice for Applying Statistical Quality Assurance
for each element and its respective internal standard are
and Control Charting Techniques to Evaluate Analytical
collected at their appropriate wavelengths. The ratios between
Measurement System Performance
elemental and internal standard counts are calculated and
converted into barium, calcium, phosphorus, or zinc concen-
1
These test methods are under the jurisdiction of ASTM Committee D02 on
trations, or a combination thereof, from calibration curves.
Petroleum Products and Lubricants and are the direct responsibility of Subcommit-
3.2.2 Sulfur—A sample specimen is mixed with a lead
tee D02.03 on Elemental Analysis.
internal standard solution and analyzed as described in 3.2.1.
Current edition approved April 1, 2005. Published April 2005. Originally
3.3 Test Method B (Mathematical Correction Procedure)—
approved in 1989. Last previous edition approved in 2002 as D4927 – 02. DOI:
10.1520/D4927-05.
The measured intensity for a given element is mathematically
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
corrected for the interference from other elements in the
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
sample specimen. This requires that intensities from all ele-
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. ments in the specimen be obtained.
*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 ----------------------
D4927–05
3.3.1 The sample specimen is placed in the X-ray beam and 6.1.4 Pulse-Height Analyzer, or other means of energy
the intensities
...