ASTM D6443-04

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Designation:D6443–04
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.
TABLE 1 Calibration Standard Compositions, Concentrations in
1. Scope*
Mass%
1.1 This test method covers the determination of calcium,
Std. No. Ca Cl Cu Mg P S Zn
chlorine, copper, magnesium, phosphorus, sulfur, and zinc in
1 0.02 0.02 0.01 0.20 0.25 1.00 0.02
unused lubricating oils, additives, and additive packages by
2 0.02 0.02 0.05 0.20 0.02 0.02 0.25
wavelength dispersive X-ray fluorescence spectrometry. Ma-
3 0.02 0.20 0.01 0.05 0.25 0.02 0.25
trix effects are handled with mathematical corrections. 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
1.2 For each element, the upper limit of the concentration
6 0.40 0.02 0.05 0.05 0.25 0.02 0.02
range covered by this test method is defined by the highest
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
concentration listed in Table 1. Samples containing higher
9 0.20 0.10 0.03 0.10 0.10 0.50 0.10
concentrations can be analyzed following dilution.
10 0 0 0 000 0
1.3 For each element, the lower limit of the concentration
range covered by this test method can be estimated by the limit
2
of detection (LOD) (see also 40 CFR 136 Appendix B) or
priate safety and health practices and determine the applica-
2
limit of quantification (LOQ), both of which can be estimated
bility of regulatory limitations prior to use.
from S , the repeatability standard deviation. LOD and LOQ
r
2. Referenced Documents
values, determined from results obtained in the interlaboratory
3
study on precision, are listed in Table 2.
2.1 ASTM Standards:
1.3.1 LOD and LOQ are not intrinsic constants of this test
D1552 Test Method for Sulfur in Petroleum Products
method. LOD and LOQ depend upon the precision attainable
(High-Temperature Method)
by a laboratory when using this test method.
D4057 Practice for Manual Sampling of Petroleum and
1.4 This test method uses regression software to determine
Petroleum Products
calibration parameters, which can include influence coeffi-
D4177 Practice for Automatic Sampling of Petroleum and
cients (that is, interelement effect coefficients) (Guide E1361),
Petroleum Products
herein referenced as alphas. Alphas can also be determined
D4307 Practice for Preparation of Liquid Blends for Use as
from theory using relevant software.
Analytical Standards
1.5 Setup of this test method is intended for persons trained
D4628 Test Method for Analysis of Barium, Calcium,
inthepracticeofX-rayspectrometry.Followingsetup,thistest
Magnesium, and Zinc in Unused Lubricating Oils by
method can be used routinely.
Atomic Absorption Spectrometry
1.6 The values stated in either SI units or angstrom units are
D4927 Test Methods for Elemental Analysis of Lubricant
to be regarded separately as standard.
and Additive Components—Barium, Calcium, Phospho-
1.7 This standard does not purport to address all of the
rus, Sulfur, and Zinc by Wavelength-Dispersive X-Ray
safety concerns, if any, associated with its use. It is the
Fluorescence Spectroscopy
responsibility of the user of this standard to establish appro-
D4951 Test Method for Determination of Additive Ele-
ments in Lubricating Oils by Inductively Coupled Plasma
Atomic Emission Spectrometry
1
This test method is under the jurisdiction of ASTM Committee D02 on
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
D02.03 on Elemental Analysis.
3
Current edition approved Nov. 1, 2004. Published November 2004. Originally For referenced ASTM standards, visit the ASTM website, www.astm.org, or
approved in 1999. Last previous edition approved in 1999 as D6443–99. DOI: contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
10.1520/D6443-04. 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.
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D6443–04
TABLE 2 Estimated LOD and LOQ, Units are Mass%
4.2 This test method can also be used to determine if
Ca Cl Cu Mg P Zn lubricating oils, additive
...