ASTM D6443-2004 Test Method for Determination of Calcium Chlorine Copper Magnesium Phosphorus Sulfur and Zinc in Unused Lubricating Oils and Additives by Wavelength Dispersive X-ra.pdf
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1、Designation: D 6443 04An American National StandardStandard Test Method forDetermination of Calcium, Chlorine, Copper, Magnesium,Phosphorus, Sulfur, and Zinc in Unused Lubricating Oilsand Additives by Wavelength Dispersive X-ray FluorescenceSpectrometry (Mathematical Correction Procedure)1This stand
2、ard is issued under the fixed designation D 6443; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) indicates an edito
3、rial change since the last revision or reapproval.1. Scope*1.1 This test method covers the determination of calcium,chlorine, copper, magnesium, phosphorus, sulfur, and zinc inunused lubricating oils, additives, and additive packages bywavelength dispersive X-ray fluorescence spectrometry. Ma-trix e
4、ffects are handled with mathematical corrections.1.2 For each element, the upper limit of the concentrationrange covered by this test method is defined by the highestconcentration listed in Table 1. Samples containing higherconcentrations can be analyzed following dilution.1.3 For each element, the
5、lower limit of the concentrationrange covered by this test method can be estimated by the limitof detection (LOD)2(see also 40 CFR 136 Appendix B) orlimit of quantification (LOQ),2both of which can be estimatedfrom Sr, the repeatability standard deviation. LOD and LOQvalues, determined from results
6、obtained in the interlaboratorystudy on precision, are listed in Table 2.1.3.1 LOD and LOQ are not intrinsic constants of this testmethod. LOD and LOQ depend upon the precision attainableby a laboratory when using this test method.1.4 This test method uses regression software to determinecalibration
7、 parameters, which can include influence coeffi-cients (that is, interelement effect coefficients) (Guide E 1361),herein referenced as alphas. Alphas can also be determinedfrom theory using relevant software.1.5 Setup of this test method is intended for persons trainedin the practice of X-ray spectr
8、ometry. Following setup, this testmethod can be used routinely.1.6 The values stated in either SI units or angstrom units areto be regarded separately as standard.1.7 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the
9、user of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:3D 1552 Test Method for Sulfur in Petroleum Products(High-Temperature Method)D 4057 Practice for Manual Sampli
10、ng of Petroleum andPetroleum ProductsD 4177 Practice for Automatic Sampling of Petroleum andPetroleum ProductsD 4307 Practice for Preparation of Liquid Blends for Use asAnalytical StandardsD 4628 Test Method for Analysis of Barium, Calcium,Magnesium, and Zinc in Unused Lubricating Oils byAtomic Abso
11、rption SpectrometryD 4927 Test Methods for Elemental Analysis of Lubricantand Additive ComponentsBarium, Calcium, Phospho-rus, Sulfur, and Zinc by Wavelength-Dispersive X-RayFluorescence SpectroscopyD 4951 Test Method for Determination of Additive Ele-ments in Lubricating Oils by Inductively Coupled
12、 PlasmaAtomic Emission Spectrometry1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products and Lubricants and is the direct responsibility of SubcommitteeD02.03 on Elemental Analysis.Current edition approved Nov. 1, 2004. Published November 2004. Originallyapproved in
13、1999. Last previous edition approved in 1999 as D 644399.2Analytical Chemistry, Vol 55, pp. 2210-2218.3For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards
14、Document Summary page onthe ASTM website.TABLE 1 Calibration Standard Compositions, Concentrations inMass %Std. No. Ca Cl Cu Mg P S Zn1 0.02 0.02 0.01 0.20 0.25 1.00 0.022 0.02 0.02 0.05 0.20 0.02 0.02 0.253 0.02 0.20 0.01 0.05 0.25 0.02 0.254 0.02 0.20 0.05 0.05 0.02 1.00 0.025 0.40 0.02 0.01 0.05
15、0.02 1.00 0.256 0.40 0.02 0.05 0.05 0.25 0.02 0.027 0.40 0.20 0.01 0.20 0.02 0.02 0.028 0.40 0.20 0.05 0.20 0.25 1.00 0.259 0.20 0.10 0.03 0.10 0.10 0.50 0.1010 0001*A Summary of Changes section appears at the end of this standard.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, Wes
16、t Conshohocken, PA 19428-2959, United States.D 5185 Test Method for Determination of Additive Ele-ments, Wear Metals, and Contaminants in Used Lubricat-ing Oils and Determination of Selected Elements in BaseOils by Inductively Coupled Plasma Atomic EmissionSpectrometry (ICP-AES)D 6299 Practice for A
17、pplying Statistical Quality AssuranceTechniques to Evaluate Analytical Measurement SystemPerformanceE 29 Practice for Using Significant Digits in Test Data toDetermine Conformance with SpecificationsE 1361 Guide for Correction of Interelement Effects inX-Ray Spectrometric Analysis2.2 Government Stan
18、dard:440 CFR, 136 Appendix B, Definition and Procedure for theDetermination of the Method Detection LimitRevision1.11, pp. 265-2673. Summary of Test Method3.1 The X-ray fluorescence spectrometer is initially cali-brated by the following procedure. For each element, the slopeand intercept of the cali
19、bration curve are determined byregressing concentration data and intensities measured on a setof physical standards. Empirical alphas can also be determinedby regression when the appropriate set of physical standards isused for calibration. Theoretical alphas, calculated with specialsoftware, can al
20、so be used. In addition, a combination oftheoretical and empirical alphas can be used.3.2 Asample is placed in the X-ray beam, and the intensitiesof the appropriate fluorescence lines are measured. A similarmeasurement is made at a wavelength offset from eachfluorescence line in order to obtain a ba
21、ckground correction.Enhancement or absorption of the X-ray fluorescence of ananalyte by an interfering element in the sample can occur, andthese effects can be handled in the data reduction by imple-mentation of alphas. Concentrations of the analytes are deter-mined by comparison of net signals agai
22、nst calibration curves,which include influence coefficients (that is, alphas) calculatedfrom theory, empirical data, or a combination of theory andempirical data.4. Significance and Use4.1 Lubricating oils can be formulated with additives, whichcan act as detergents, anti-oxidants, anti-wear agents,
23、 and soforth. Some additives can contain one or more of calcium,copper, magnesium, phosphorus, sulfur, and zinc. This testmethod can be used to determine if the oils, additives, andadditive packages meet specification with respect to content ofthese elements.4.2 This test method can also be used to
24、determine iflubricating oils, additives, and additive packages meet specifi-cation with respect to chlorine concentration. In this context,specification can refer to contamination.4.3 This test method is not intended for use on samples thatcontain some component that significantly interferes with th
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