ASTM D4927-01
(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
SCOPE
1.1 These test methods cover the determination of barium, calcium, phosphorus, sulfur, and zinc in unused lubricating oils at element concentration ranges from 0.03 to 1.0 mass % (0.01 to 2.0 mass % for sulfur). 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 1-12, and 19).
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 13-19).
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
Relations
Standards Content (Sample)
NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
An American National Standard
Designation: D 4927 – 01
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.
1. Scope * 2.2 Test Method A (Internal Standard Procedure)—Internal
standards are used with the standards and sample specimens to
1.1 These test methods cover the determination of barium,
compensate for the potential interelement effects.
calcium, phosphorus, sulfur, and zinc in unused lubricating oils
2.2.1 Barium, Calcium, Phosphorus, and Zinc—A sample
at element concentration ranges from 0.03 to 1.0 mass % (0.01
specimen that has been blended with a single internal standard
to 2.0 mass % for sulfur). The range can be extended to higher
solution (containing tin or titanium for barium and calcium,
concentrations by dilution of sample specimens. Additives can
zirconium for phosphorus, and nickel for zinc) is poured into
also be determined after dilution. Two different methods are
an X-ray cell. Total net counts (peak intensity—background)
presented in these test methods.
for each element and its respective internal standard are
1.2 Test Method A (Internal Standard Procedure)—Internal
collected at their appropriate wavelengths. The ratios between
standards are used to compensate for interelement effects of
elemental and internal standard counts are calculated and
X-ray excitation and fluorescence (see Sections 1-12, and 19).
converted into barium, calcium, phosphorus, or zinc concen-
1.3 Test Method B (Mathematical Correction Procedure)—
trations, or a combination thereof, from calibration curves.
The measured X-ray fluorescence intensity for a given element
2.2.2 Sulfur—A sample specimen is mixed with a lead
is mathematically corrected for potential interference from
internal standard solution and analyzed as described in 2.2.1.
other elements present in the sample (see Sections 1-6, and
2.3 Test Method B (Mathematical Correction Procedure)—
13-19).
The measured intensity for a given element is mathematically
1.4 The preferred concentration units are mass percent
corrected for the interference from other elements in the
barium, calcium, phosphorus, sulfur, or zinc.
sample specimen. This requires that intensities from all ele-
1.5 This standard does not purport to address all of the
ments in the specimen be obtained.
safety concerns, if any, associated with its use. It is the
2.3.1 The sample specimen is placed in the X-ray beam and
responsibility of the user of this standard to establish appro-
the intensities of the fluorescence lines of barium, calcium,
priate safety and health practices and determine the applica-
phosphorus, sulfur, and zinc are measured. A similar measure-
bility of regulatory limitations prior to use.
ment is made away from the fluorescence lines in order to
2. Summary of the Test Methods
obtain a background correction. Concentrations of the elements
of interest are determined by comparison of net signals against
2.1 A sample specimen is placed in the X-ray beam and the
appropriate interelement correction factors developed from
intensity of the appropriate fluorescence lines of barium,
responses of calibration standards.
calcium, phosphorus, sulfur, and zinc are measured. Instrument
2.3.2 The X-ray fluorescence spectrometer is initially cali-
response factors related to the concentration of standards
brated with a suite of standards in order to determine by
enable the determination of the concentration of elements in
regression analysis, interelement correction factors and instru-
the tested sample specimens. Enhancement or depression of the
ment response factors.
X-ray fluorescence of a given element by an interfering
2.3.3 Subsequent calibration is achieved using a smaller
element in the sample may occur. Two test methods (A and B)
number of standards since only the instrument response factors
are described for compensating any interference effect.
need to be redetermined. One of these standards (or an optional
synthetic pellet) can be used to monitor instrumental drift when
1
These test methods are under the jurisdiction of ASTM Committee D02 on
performing a high volume of analyses.
Petroleum Products and Lubricants and are the direct responsibility of Subcommit-
2.4 Additives and additive packages can be determined after
tee D02.03 on Elemental Anal
...
Questions, Comments and Discussion
Ask us and Technical Secretary will try to provide an answer. You can facilitate discussion about the standard in here.