ASTM D6443-14
(Test Method)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)
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)
SIGNIFICANCE AND USE
4.1 Lubricating oils can be formulated with additives, which can act as detergents, anti-oxidants, anti-wear agents, and so forth. Some additives can contain one or more of calcium, copper, magnesium, phosphorus, sulfur, and zinc. This test method can be used to determine if the oils, additives, and additive packages meet specification with respect to content of these elements.
4.2 Several additive elements and their compounds are added to the lubricating oils to give beneficial performance (Table 3).
4.3 This test method can also be used to determine if lubricating oils, additives, and additive packages meet specification with respect to chlorine concentration. In this context, specification can refer to contamination.
4.4 This test method is not intended for use on samples that contain some component that significantly interferes with the analysis of the elements specified in the scope.
4.5 This test method can complement other test methods for lube oils and additives, including Test Methods D4628, D4927, D4951, and D5185.
SCOPE
1.1 This test method covers the determination of calcium, chlorine, copper, magnesium, phosphorus, sulfur, and zinc in unused lubricating oils, additives, and additive packages by wavelength dispersive X-ray fluorescence spectrometry. Matrix effects are handled with mathematical corrections.
1.2 For each element, the upper limit of the concentration range covered by this test method is defined by the highest concentration listed in Table 1. Samples containing higher concentrations can be analyzed following dilution.
1.3 For each element, the lower limit of the concentration range covered by this test method can be estimated by the limit of detection (LOD)2 (see also 40 CFR 136 Appendix B) or limit of quantification (LOQ),2 both of which can be estimated from Sr, the repeatability standard deviation. LOD and LOQ values, determined from results obtained in the interlaboratory study on precision, are listed in Table 2.
1.3.1 LOD and LOQ are not intrinsic constants of this test method. LOD and LOQ depend upon the precision attainable by a laboratory when using this test method.
1.4 This test method uses regression software to determine calibration parameters, which can include influence coefficients (that is, interelement effect coefficients) (Guide E1361), herein referenced as alphas. Alphas can also be determined from theory using relevant software.
1.5 Setup of this test method is intended for persons trained in the practice of X-ray spectrometry. Following setup, this test method can be used routinely.
1.6 The values stated in either SI units or angstrom units are to be regarded separately as standard.
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 prior to use.
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Designation: D6443 − 14
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
1
Spectrometry (Mathematical Correction Procedure)
This standard is issued under the fixed designation D6443; 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* 1.7 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
1.1 This test method covers the determination of calcium,
responsibility of the user of this standard to establish appro-
chlorine, copper, magnesium, phosphorus, sulfur, and zinc in
priate safety and health practices and determine the applica-
unused lubricating oils, additives, and additive packages by
bility of regulatory limitations prior to use.
wavelength dispersive X-ray fluorescence spectrometry. Ma-
trix effects are handled with mathematical corrections.
2. Referenced Documents
1.2 For each element, the upper limit of the concentration
3
2.1 ASTM Standards:
range covered by this test method is defined by the highest
D1552 Test Method for Sulfur in Petroleum Products (High-
concentration listed in Table 1. Samples containing higher
Temperature Method)
concentrations can be analyzed following dilution.
D4057 Practice for Manual Sampling of Petroleum and
1.3 For each element, the lower limit of the concentration
Petroleum Products
range covered by this test method can be estimated by the limit
D4177 Practice for Automatic Sampling of Petroleum and
2
of detection (LOD) (see also 40 CFR 136 Appendix B) or
Petroleum Products
2
limit of quantification (LOQ), both of which can be estimated
D4307 Practice for Preparation of Liquid Blends for Use as
from S , the repeatability standard deviation. LOD and LOQ
Analytical Standards
r
values, determined from results obtained in the interlaboratory
D4628 Test Method for Analysis of Barium, Calcium,
study on precision, are listed in Table 2.
Magnesium, and Zinc in Unused Lubricating Oils by
1.3.1 LOD and LOQ are not intrinsic constants of this test
Atomic Absorption Spectrometry
method. LOD and LOQ depend upon the precision attainable
D4927 Test Methods for Elemental Analysis of Lubricant
by a laboratory when using this test method.
and Additive Components—Barium, Calcium,
Phosphorus, Sulfur, and Zinc by Wavelength-Dispersive
1.4 This test method uses regression software to determine
X-Ray Fluorescence Spectroscopy
calibration parameters, which can include influence coeffi-
D4951 Test Method for Determination ofAdditive Elements
cients (that is, interelement effect coefficients) (Guide E1361),
in Lubricating Oils by Inductively Coupled Plasma
herein referenced as alphas. Alphas can also be determined
Atomic Emission Spectrometry
from theory using relevant software.
D5185 Test Method for Multielement Determination of
1.5 Setup of this test method is intended for persons trained
Used and Unused Lubricating Oils and Base Oils by
inthepracticeofX-rayspectrometry.Followingsetup,thistest
Inductively Coupled Plasma Atomic Emission Spectrom-
method can be used routinely.
etry (ICP-AES)
1.6 The values stated in either SI units or angstrom units are
D6299 Practice for Applying Statistical Quality Assurance
to be regarded separately as standard. and Control Charting Techniques to Evaluate Analytical
Measurement System Performance
E29 Practice for Using Significant Digits in Test Data to
Determine Conformance with Specifications
1
This test method is under the jurisdiction of ASTM Committee D02 on
Petroleum Products, Liquid Fuels, and Lubricantsand is the direct responsibility of
Subcommittee D02.03 on Elemental Analysis.
3
Current edition approved Dec. 1, 2014. Published January 2015. Originally For referenced ASTM standards, visit the ASTM website, www.astm.org, or
approved in 1999. Last previous edition approved in 2010 as D6443 – 04 (2010). contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
DOI: 10.1520/D6443-14. Standards volume information, refer to the standard’s Document Summary page on
2
Analytical Chemistry, Vol 55, pp. 2210-2218. 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
1
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D6443 − 14
TABLE 1 Calibration Standard Compositions, Concentrations in
method can be used to determine if the oils, additives, and
Mass %
additive packages meet sp
...
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: D6443 − 04 (Reapproved 2010) D6443 − 14
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
1
Spectrometry (Mathematical Correction Procedure)
This standard is issued under the fixed designation D6443; 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 determination of calcium, chlorine, copper, magnesium, phosphorus, sulfur, and zinc in unused
lubricating oils, additives, and additive packages by wavelength dispersive X-ray fluorescence spectrometry. Matrix effects are
handled with mathematical corrections.
1.2 For each element, the upper limit of the concentration range covered by this test method is defined by the highest
concentration listed in Table 1. Samples containing higher concentrations can be analyzed following dilution.
1.3 For each element, the lower limit of the concentration range covered by this test method can be estimated by the limit of
2 2
detection (LOD) (see also 40 CFR 136 Appendix B) or limit of quantification (LOQ), both of which can be estimated from S ,
r
the repeatability standard deviation. LOD and LOQ values, determined from results obtained in the interlaboratory study on
precision, are listed in Table 2.
1.3.1 LOD and LOQ are not intrinsic constants of this test method. LOD and LOQ depend upon the precision attainable by a
laboratory when using this test method.
1.4 This test method uses regression software to determine calibration parameters, which can include influence coefficients (that
is, interelement effect coefficients) (Guide E1361), herein referenced as alphas. Alphas can also be determined from theory using
relevant software.
1.5 Setup of this test method is intended for persons trained in the practice of X-ray spectrometry. Following setup, this test
method can be used routinely.
1.6 The values stated in either SI units or angstrom units are to be regarded separately as standard.
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
D6443D6443 – 04 (2010).–04. DOI: 10.1520/D6443-04R10.10.1520/D6443-14.
2
Analytical Chemistry, Vol 55, pp. 2210-2218.
TABLE 1 Calibration Standard Compositions, Concentrations in
Mass %
Std. No. Ca Cl Cu Mg P S Zn
1 0.02 0.02 0.01 0.20 0.25 1.00 0.02
2 0.02 0.02 0.05 0.20 0.02 0.02 0.25
3 0.02 0.20 0.01 0.05 0.25 0.02 0.25
4 0.02 0.20 0.05 0.05 0.02 1.00 0.02
5 0.40 0.02 0.01 0.05 0.02 1.00 0.25
6 0.40 0.02 0.05 0.05 0.25 0.02 0.02
7 0.40 0.20 0.01 0.20 0.02 0.02 0.02
8 0.40 0.20 0.05 0.20 0.25 1.00 0.25
9 0.20 0.10 0.03 0.10 0.10 0.50 0.10
10 0 0 0 0 0 0 0
*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
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D6443 − 14
TABLE 2 Estimated LOD and LOQ, Units are Mass %
Ca Cl Cu Mg P Zn
LOD 0.0002 0.0004 0.0002 0.0039 0.0006 0.0002
LOQ 0.0008 0.0015 0.0007 0.0130 0.0020 0.0007
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 prior to use.
2. Referenced Documents
3
2.1 ASTM Standards:
D1552 Test Method for Sulfur in Petroleum Products (High-Temperature Method)
D4057 Practice for Manual Sampling of Petroleum and Petroleum Products
D4177 Practice for Automatic Sampling of Petroleum and Petroleum Products
D4307 Practice for Preparation of Liquid Blends for Use as Analytical Standards
D4628 Test Method for Analysis of Barium, Calcium, Magnesium, and Zinc in Unused Lubricating Oils by Atomic Absorption
Spectrometry
D4927 Test Methods for Elemental Analysis of Lubricant and Additive Components—Barium, Calcium, Phosphorus, Sulfur,
and Zinc by Wavelength-Dispersive
...
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