ASTM D6481-14
(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
3.1 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.
3.2 Several additive elements and their compounds are added to the lubricating oils to give beneficial performance (Table 2).
3.3 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 and health practices and determine the applicability of regulatory limitations to use.
General Information
Relations
Buy Standard
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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: D6481 − 14
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* simultaneous measurements employing primary and secondary
beam filters. There can be correction of measured intensities
1.1 This test method covers the quantitative determination
for spectral overlap. Concentrations of the elements of interest
of additive elements in unused lubricating oils, as shown in
are determined by comparison of these intensities against a
Table 1.
calibration curve using empirical interelement correction fac-
1.2 This test method is limited to the use of energy
tors and ratio to backscatter.
dispersive X-ray fluorescence (EDXRF) spectrometers em-
2.2 The EDXRF spectrometer is initially calibrated using a
ploying an X-ray tube for excitation in conjunction with the
setofpreparedstandardstocollectthenecessaryintensitydata.
ability to separate the signals of adjacent elements.
Each calibration line and any correction coefficient are ob-
1.3 This test method uses interelement correction factors
tained by a regression of this data, using the program supplied
calculated from empirical calibration data.
with the spectrometer.
1.4 This test method is not suitable for the determination of
3. Significance and Use
magnesium and copper at the concentrations present in lubri-
cating oils.
3.1 Some oils are formulated with organo-metallic
additives, which act, for example, as detergents, antioxidants,
1.5 This test method excludes lubricating oils that contain
and antiwear agents. Some of these additives contain one or
chlorine or barium as an additive element.
more of these elements: calcium, phosphorus, sulfur, and zinc.
1.6 This test method can be used by persons who are not
This test method provides a means of determining the concen-
skilled in X-ray spectrometry. It is intended to be used as a
trations of these elements, which in turn provides an indication
routine test method for production control analysis.
of the additive content of these oils.
1.7 This standard does not purport to address all of the
3.2 Several additive elements and their compounds are
safety concerns, if any, associated with its use. It is the
added to the lubricating oils to give beneficial performance
responsibility of the user of this standard to establish appro-
(Table 2).
priate safety and health practices and determine the applica-
bility of regulatory limitations to use. 3.3 This test method is primarily intended to be used at a
manufacturing location for monitoring of additive elements in
2. Summary of Test Method
lubricating oils. It can also be used in central and research
laboratories.
2.1 A specimen is placed in the X-ray beam, and the
appropriate regions of its spectrum are measured to give the
4. Interferences
fluorescent intensities of phosphorus, sulfur, calcium, and zinc.
4.1 The additive elements found in lubricating oils will
Other regions of the spectrum are measured to compensate for
affect the measured intensities from the elements of interest to
varying background. If the detector does not completely
a varying degree. In general, for lubricating oils, the
resolve all the elements in a single measurement, then to
X-radiation emitted by the element of interest can be absorbed
improve selectivity, there is a combination of sequential and
by itself (self-absorption) or by the other elements present in
the sample matrix. Also the X-radiation emitted from one
1
element can further excite (enhance) another element. These
This test method is under the jurisdiction of ASTM Committee D02 on
Petroleum Products, Liquid Fuels, and Lubricantsand is the direct responsibility of
interelement effects are significant at concentrations varying
Subcommittee D02.03 on Elemental Analysis.
from 0.03 mass %, due to the heavier elements, to 1 mass %,
Current edition approved Dec. 1, 2014. Published January 2015. Originally
forthelighterelements.Enhancementeffectscanbeminimised
approved in 1999. Last previous edition approved in 2010 as D6481 – 99 (2010).
DOI: 10.1520/D6481-14. byselectiveexcitation.Themeasuredconcentrationforagiven
*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 − 14
TABLE 1 Elements and Range of Concentrations Deter
...
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 − 99 (Reapproved 2010) D6481 − 14
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 and health practices and determine the applicability of regulatory
limitations to use.
2. Summary of Test Method
2.1 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.
2.2 The EDXRF spectrometer is initially calibrated using a set of prepared standards to collect the necessary intensity data. Each
calibration line and any correction coefficient are obtained by a regression of this data, using the program supplied with the
spectrometer.
3. Significance and Use
3.1 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.
3.2 Several additive elements and their compounds are added to the lubricating oils to give beneficial performance (Table 2).
3.3 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.
1
This test method is under the jurisdiction of ASTM Committee D02 on Petroleum Products Products, Liquid Fuels, and Lubricantsand is the direct responsibility of
Subcommittee D02.03 on Elemental Analysis.
Current edition approved May 1, 2010Dec. 1, 2014. Published May 2010January 2015. Originally approved in 1999. Last previous edition approved in 20042010 as
D6481 - 99 (2004).D6481 – 99 (2010). DOI: 10.1520/D6481-99R10.10.1520/D6481-14.
*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 − 14
TABLE 1 Elements and Range of Concentrations Determined
Element Concentration Range
Phosphorus 0.02 to 0.3 mass %
Sulfur 0.05 to 1.0 mass %
Calcium 0.02 to 1.0 mass %
Zinc 0.01 to 0.3 mass %
4. Interferences
4.1 The additive elements found in lubricating oils will affect the measured intensities from the elements of interest to a varying
deg
...
Questions, Comments and Discussion
Ask us and Technical Secretary will try to provide an answer. You can facilitate discussion about the standard in here.