1、Designation: D8182 18Standard Test Method forAlloy Classification of Wear Debris using Laser-InducedBreakdown Spectroscopy (LIBS)1This standard is issued under the fixed designation D8182; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revi
2、sion, 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.1. Scope1.1 This test method describes a means for quantitativedetermination of wear debris found in in-service
3、lubricants bylaser-induced breakdown spectroscopy (LIBS). LIBS is ananalytical technology that uses short laser pulses to createmicro hot-plasma ablation of a material and then employsspectroscopic tools for analysis.21.2 This method covers the means for alloy classificationand sizing of wear debris
4、. Wear debris sources can include, butare not limited to: (1) chip collector and chip detector devices,(2) filters, (3) ferrograms, and (4) loose particles. The 23 testedalloys and metals included in the default material library of theinstrument are listed in Table 1.1.3 The method for alloy classif
5、ication and sizing of weardebris is not limited to the list of alloys in Table 1. Theinstrument has the capability of including additional alloys andmetals as required.1.4 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.5 This
6、 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, health, and environmental practices and deter-mine the applicability of regulatory limitations prior to use.1.6 Thi
7、s international standard was developed in accor-dance with internationally recognized principles on standard-ization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recom-mendations issued by the World Trade Organization TechnicalBarriers to Trade
8、(TBT) Committee.2. Referenced Documents2.1 ASTM Standards:3D7669 Guide for Practical Lubricant Condition Data TrendAnalysisD7720 Guide for Statistically Evaluating Measurand AlarmLimits when Using Oil Analysis to Monitor Equipmentand Oil for Fitness and ContaminationE177 Practice for Use of the Term
9、s Precision and Bias inASTM Test Methods3. Terminology3.1 Definitions:3.1.1 alloy, nunique composition of two or more metalsthat has one or more of the metals treated or processed in aspecial way to confer enhanced performance characteristics onthe resulting material.3.1.2 debris, nsolid particulate
10、 matter introduced to lubri-cant (or machinery/equipment fluid) through contamination ordetached from a surface due to wear, corrosion, or erosionprocess.3.1.3 in-service oil, nlubricating oil that is present in amachine that has been at operating temperature for at least onehour.3.1.4 wear, ndamage
11、 to a solid surface, usually involvingprogressive loss or displacement of material, due to relativemotion between that surface and a contacting substance orsubstances.3.1.5 wear debris, nparticles that have become detachedin wear or erosion processes.3.2 Definitions of Terms Specific to This Standar
12、d:3.2.1 alloy classification, nthe automated process thatuses the LIBS technology in conjunction with an artificialneural network (ANN) to determine the specific alloy or alloygrouping for a given sample.3.2.2 alloy grouping, nwithin a given LIBS training set,when two or more alloys are significantl
13、y similar in elemental1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility ofSubcommittee D02.96.06 on Practices and Techniques for Prediction and Determi-nation of Microscopic Wear and Wear-related Prop
14、erties.Current edition approved June 1, 2018. Published July 2018. DOI: 10.1520/D8182-18.2Hill, R., Lawrence, R., Toms, A.; “A New Approach to Elemental and WearDebris Analysis,” STLE, Las Vegas, NV, 2016.3For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer S
15、ervice at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United StatesThis international standard was developed i
16、n accordance with internationally recognized principles on standardization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.1composition, the alloy cl
17、assification capabilities of the instru-ment may not be able to distinguish them as separate orindividual alloys; when this occurs, such alloys are combinedunder a more general classification referred to as an “alloygrouping” (for example, 52100 and 4130 may be combinedwithin a single alloy grouping
18、 of “52100/4130”).3.2.3 laser-induced breakdown spectroscopy (LIBS), narapid chemical analysis technology that uses a short laser pulseto create a micro-plasma on the sample surface.3.2.4 material library, nthe material library is the instru-ments collection of alloy and metal classification outputs
19、; thematerial library is a subset of the training set and may containindividual alloys or alloy groupings.3.2.5 sample, ntest specimen or a collection of weardebris that is first placed on a sample patch and then insertedinto the instrument for analysis.3.2.6 sample patch, ncustomized plastic insert
20、 used forLIBS analysis.3.2.6.1 DiscussionA given sample patch contains a 0.5 in.by 0.5 in. clear window with semi-permanent adhesive forwear debris retention. Sample patches are populated withsamples of wear debris and then inserted into the instrument foranalysis.3.2.7 training set, nthe collection
21、 of certified alloy andmetal samples and the LIBS spectra acquired from these alloys,which are used to define and configure the instrumentsmaterial library.4. Summary of Test Method4.1 Wear debris is extracted from a chip detector or othersource and placed onto a transparent adhesive sample patch,Fi
22、g. 1. The patch is transferred to an instrument that uses acombination of LIBS, an artificial neural network (ANN) anddigital imaging technologies to determine specific alloy clas-sification and size. To determine the size of a given piece ofwear debris, the transparent sample patch is back lit to c
23、reate asilhouette of the wear debris and a high-resolution image isprocessed using an image binarization and processing algo-rithm. In the case of large pieces of wear debris, the softwareallows for each particle to be analyzed in several locations.This option allows the instrument to determine if t
24、he image ofthe wear debris is one piece or several overlapping pieces ofdifferent alloys or metals.4.2 The LIBS instrument uses short laser pulses to createmicro hot-plasma ablation on the surface of the wear debris andthen employs spectroscopic tools to analyze the materialscomposition. A plasma fi
25、eld from the ablation spot emitsvarious wavelengths of light unique to the elements present inthe sample being analyzed.Aspectrometer is used to determineintensities of each element present in the sample and anartificial neural network (ANN) analyses this data to output thespecific alloy classificat
26、ion for each individual piece of weardebris analyzed.4.2.1 Alloy classification is determined based on the com-position of the wear debris under analysis.4.3 Instrument calibration is supplied by the manufacturervia measurement of the following, and is maintained in serviceas defined in 13.2:4.3.1 A
27、n alloy training set comprised of all of the alloysrequired in the instruments material library is used as refer-ences to calibrate the instrument for alloy classification. Wherepossible, certified alloy or metals are sourced from multiplevendors and accompanied by third party certification. A large
28、number of spectra are collected over a range of intensities andthis aggregate collection of data is used to calibrate theinstruments ANN.4.3.2 For image calibration, a USAir Force 1951 ResolutionTarget is used to configure the imaging optics at the factory.For field operation, a field calibration st
29、andard is used toestablish the ratio between image pixel and wear debris size.5. Significance and Use5.1 In many cases, equipment failure modes are identifiedby wear debris that is not captured in used lubricating oilsamples but captured on chip detectors, filters or by othermeans. Users of this tec
30、hnique include, but are not limited to,original equipment manufacturers (OEMs), commercialairlines, civil aerospace operators, maintenance repair andoverhaul (MRO) facilities, and military maintenance person-nel.6. Interferences6.1 For optimum wear debris classification and instrumentperformance, th
31、e following guidelines should be followed toreduce interferences.TABLE 1 List of 23 Alloys and MetalsAlloys1010 Carbon Steel17-4PH Stainless Steel300 Series Stainless Steel(316, 321, 347)400 Series Stainless Steel(416, 410)52100 / 4130 Alloy Steel9310 / 4340 Alloy SteelA286 Stainless SteelAluminum 2
32、024Aluminum 6061Aluminum 7075BrassCopperInconel 718M50 NiL SteelM50 SteelSilverTitanium 6Al-2Sn-4Zr-6MoTitanium 6Al-4VFIG. 1 Transparent Adhesive Sample Patch with Chip DebrisD8182 1826.1.1 Residual oil on the wear debris may weaken the signalintensity. An isopropyl alcohol rinse of the debris is re
33、com-mended prior to applying the wear debris to the sample patch.Applying a drop or two of isopropyl alcohol to the samplepatch, after the wear debris is applied, is allowed.6.1.2 When preparing the sample patch for analysis, con-centrated clumps of wear debris should be avoided. Overlap-ping debris
34、 may hinder proper identification of some particles.If needed, excessive debris all from one source can be placedon multiple patches.6.1.3 When preparing the sample patch for analysis, weardebris should lay as flat as possible on the sample patch forproper identification.6.1.4 Avoid placing wear deb
35、ris thicker than 0.5 mm on asample patch. Wear debris thicker than 0.5 mm should bebroken into smaller pieces for proper identification.6.1.5 Alloys not in the material library will be classified as“unclassified” or if their elemental composition is similar to analloy in the library, they may be inc
36、orrectly classified.6.1.6 The operation, maintenance, service and all relatedactivities regarding the instrument shall be performed inaccordance with the manufacturers manual and technicalspecification.7. Apparatus7.1 LIBS Instrument.47.2 Sample Tray, to hold the transparent adhesive samplepatch con
37、taining the wear debris sample during analysis.8. Reagents and Materials8.1 Transparent adhesive sample patches.8.2 Optional patch preparation tools and materials(tweezers, probe set, wash bottle, isopropyl alcohol).8.3 Standardization standard that allows for the standardiza-tion procedure to be co
38、mpleted verifying the instrument isstandardized.8.4 Calibration standard that allows for the calibrationprocedure to be completed ensuring instrument calibration.9. Hazards9.1 Potential hazards arising from the use of a laser havebeen mitigated by the design and manufacturing process. Theinstrument
39、is designated as a Class 1 laser product andcomplies with US FDA performance standards for laser prod-ucts except for deviations pursuant to Laser Notice No. 50,dated June 24, 2007. Only manufacturer authorized technicianscan complete laser service on the instrument. Manufacturerrecommended safety p
40、rocedures must be followed duringinstrument service.10. Sampling, Test Specimens, and Test Units10.1 For alloy classification, wear debris particles with aminimum dimension larger than 70 m are classified. Particlessmaller than these dimensions are not classified.10.2 Test specimens and wear debris
41、samples should be nothicker than 0.5 mm. Any sample that is thicker than 0.5 mmshould be broken into smaller pieces.10.3 Residual oil on the wear debris should be removedprior to applying the wear debris to the sample patch. Anisopropyl alcohol rinse of the debris is recommended.10.4 For proper iden
42、tification, test specimens and weardebris samples must be alloys or metals included in thematerial library and training set.10.5 Test specimens and wear debris samples should be flatfor proper identification.11. Preparation of Apparatus11.1 Refer to the manufacturers manual for the mechanicalsetup a
43、nd power up procedures.11.2 Ensure that no alerts, which indicate a fault with themeasurement hardware or software, are generated duringpowerup.12. Conditioning12.1 The instrument self-conditions upon start-up. The in-strument will initiate and automatically notify the operatorwhen ready.13. Calibra
44、tion and Standardization13.1 StandardizationIn-service standardization is com-pleted by the operator in order to verify the status of theinstrument. Standardization is completed through the use of anautomated standardization process using manufacturer pro-vided standardization standard. The standard
45、ization procedureshould be completed once each day prior to use of theinstrument. Refer to the manufacturers manual for the stan-dardization procedure.13.2 CalibrationThe instrument is factory-calibratedupon receipt. In-service calibration, if required, is completedby the operator through the use of
46、 an automated calibrationprocess using manufacturer provided calibration standard.Refer to the manufacturers manual for the calibration proce-dure.14. Analysis Procedures14.1 The instrument shall be used, operated and maintainedin accordance with the instruments manufacturersrequirements, manual and
47、 technical specifications. The follow-ing is a high-level summary of the most critical proceduresrequired to ensure optimal performance from the instrument.Refer to the manufacturers manual for all other proceduresincluding transportation, maintenance and service.14.1.1 Sample Patch PreparationThere
48、 are several poten-tial sources of wear debris. The process of transferring weardebris from the collection source to the sample patch largelydepends on how the debris was collected from the equipment.4The sole source of supply of the apparatus known to the committee at this timeis GasTOPS, Ltd., Pol
49、ytek St., Ottawa, Ontario K1J 9J3, Canada. If you are awareof alternative suppliers, please provide this information to ASTM InternationalHeadquarters. Your comments will receive careful consideration at a meeting of theresponsible technical committee,1which you may attend.D8182 183The following procedure defines the recommended process oftransferring wear debris while considering the cautions out-lined in Section 6.14.1.1.1 Cleaning Wear Debris from a Chip Detector, ChipCollector, or Magnetic PlugRemove the collection devicefrom the equipment and subm
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