ASTM D4927-2015 Standard Test Methods for Elemental Analysis of Lubricant and Additive Components&x2014 Barium Calcium Phosphorus Sulfur and Zinc by Wavelength-Dispersive X-Ray Flu.pdf
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1、Designation: D4927 15Standard Test Methods forElemental Analysis of Lubricant and Additive ComponentsBarium, Calcium, Phosphorus, Sulfur, and Zinc byWavelength-Dispersive X-Ray Fluorescence Spectroscopy1This standard is issued under the fixed designation D4927; the number immediately following the d
2、esignation 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 () indicates an editorial change since the last revision or reapproval.This standard has been approved for use
3、 by agencies of the U.S. Department of Defense.1. Scope*1.1 These test methods cover the determination of barium,calcium, phosphorus, sulfur, and zinc in unused lubricating oilsat element concentration ranges shown in Table 1. The rangecan be extended to higher concentrations by dilution of samplesp
4、ecimens. Additives can also be determined after dilution.Two different methods are presented in these test methods.1.2 Test Method A (Internal Standard Procedure)Internalstandards are used to compensate for interelement effects ofX-ray excitation and fluorescence (see Sections 8 through 13).1.3 Test
5、 Method B (Mathematical Correction Procedure)The measured X-ray fluorescence intensity for a given elementis mathematically corrected for potential interference fromother elements present in the sample (see Sections 14 through19).1.4 The preferred concentration units are mass % barium,calcium, phosp
6、horus, sulfur, or zinc.1.5 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the user of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior
7、 to use.2. Referenced Documents2.1 ASTM Standards:2D6299 Practice for Applying Statistical Quality Assuranceand Control Charting Techniques to Evaluate AnalyticalMeasurement System Performance3. Summary of the Test Methods3.1 A sample specimen is placed in the X-ray beam and theintensity of the appr
8、opriate fluorescence lines of barium,calcium, phosphorus, sulfur, and zinc are measured. Instrumentresponse factors related to the concentration of standardsenable the determination of the concentration of elements inthe tested sample specimens. Enhancement or depression of theX-ray fluorescence of
9、a given element by an interferingelement in the sample may occur. Two test methods (A and B)are described for compensating any interference effect.3.2 Test Method A (Internal Standard Procedure)Internalstandards are used with the standards and sample specimens tocompensate for the potential interele
10、ment effects.3.2.1 Barium, Calcium, Phosphorus, and ZincA samplespecimen that has been blended with a single internal standardsolution (containing tin or titanium for barium and calcium,zirconium for phosphorus, and nickel for zinc) is poured intoan X-ray cell. Total net counts (peak intensitybackgr
11、ound)for each element and its respective internal standard arecollected at their appropriate wavelengths. The ratios betweenelemental and internal standard counts are calculated andconverted into barium, calcium, phosphorus, or zincconcentrations, or a combination thereof, from calibrationcurves.3.2
12、.2 SulfurA sample specimen is mixed with a leadinternal standard solution and analyzed as described in 3.2.1.3.3 Test Method B (Mathematical Correction Procedure)The measured intensity for a given element is mathematicallycorrected for the interference from other elements in thesample specimen. This
13、 requires that intensities from all ele-ments in the specimen be obtained.3.3.1 The sample specimen is placed in the X-ray beam andthe intensities of the fluorescence lines of barium, calcium,phosphorus, sulfur, and zinc are measured. A similar measure-ment is made away from the fluorescence lines i
14、n order toobtain a background correction. Concentrations of the elementsof interest are determined by comparison of net signals againstappropriate interelement correction factors developed fromresponses of calibration standards.1These test methods are under the jurisdiction of ASTM Committee D02 onP
15、etroleum Products, Liquid Fuels, and Lubricants and are the direct responsibilityof Subcommittee D02.03 on Elemental Analysis.Current edition approved Dec. 1, 2015. Published December 2015. Originallyapproved in 1989. Last previous edition approved in 2014 as D4927 14. DOI:10.1520/D4927-15.2For refe
16、renced 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 Document Summary page onthe ASTM website.*A Summary of Changes section appears at the end of this standardCopyr
17、ight ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States13.3.2 The X-ray fluorescence spectrometer is initially cali-brated with a suite of standards in order to determine byregression analysis, interelement correction factors and instru-ment respo
18、nse factors.3.3.3 Subsequent calibration is achieved using a smallernumber of standards since only the instrument response factorsneed to be redetermined. One of these standards (or an optionalsynthetic pellet) can be used to monitor instrumental drift whenperforming a high volume of analyses.3.4 Ad
19、ditives and additive packages can be determined afterdilution with base oil to place the elemental concentrations inthe range described in 1.1.4. Significance and Use4.1 Some oils are formulated with organo-metallic additiveswhich act as detergents, antioxidants, antiwear agents, and soforth. Some o
20、f these additives contain one or more of theseelements: barium, calcium, phosphorus, sulfur, and zinc. Thesetest methods provide a means of determining the concentrationof these elements which in turn provides an indication of theadditive content of these oils.4.2 Several additive elements and their
21、 compounds areadded to the lubricating oils to give beneficial performance (seeTable 2).5. Interferences5.1 The additive elements found in lubricating oils willaffect the measured intensities from the elements of interest toa varying degree. In general for lubricating oils, the X-radiationemitted by
22、 the element of interest is absorbed by the otherelements in the sample matrix. Also, the X-radiation emittedfrom one element can further excite another element. Theseeffects are significant at concentrations varying from0.03 mass % due to the heavier elements to 1 mass % for thelighter elements. Th
23、e measured intensity for a given elementcan be mathematically corrected for the absorption of theemitted radiation by the other elements present in the samplespecimen. Suitable internal standards can also compensate forX-ray inter-element effects. If an element is present at signifi-cant concentrati
24、ons and an interelement correction for thatelement is not employed, the results can be low due toabsorption or high due to enhancement.6. Apparatus6.1 X-Ray Spectrometer, equipped for soft X-ray detectionof radiation in the range from 1 Ato 10 A. For optimumsensitivity, the spectrometer is equipped
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