1、Designation: D7417 10Standard Test Method forAnalysis of In-Service Lubricants Using Particular Four-PartIntegrated Tester (Atomic Emission Spectroscopy, InfraredSpectroscopy, Viscosity, and Laser Particle Counter)1This standard is issued under the fixed designation D7417; the number immediately fol
2、lowing 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 () indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test metho
3、d covers the quantitative analysis ofin-service lubricants using an automatic testing device thatintegrates these varied technologies: atomic emission spectros-copy, infrared spectroscopy, viscosity, and particle counting.1.2 This is suited for in-service lubricating oils havingviscosities in the ra
4、nge between ISO 10 and ISO 320 andproperties in the ranges given in Tables 1 and 2.1.3 This test method may be used to establish trends in wearand contamination of in-service lubricants and may not giveequivalent numerical results to current ASTM test methods.1.4 This test method is not intended for
5、 use with crude oil.1.5 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.6 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 standa
6、rd to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use. (Specific hazardstatements are given in Section 9 and 11.3.)2. Referenced Documents2.1 ASTM Standards:2D445 Test Method for Kinematic Viscosity of Transparentand Opaque L
7、iquids (and Calculation of Dynamic Viscos-ity)D2270 Practice for Calculating Viscosity Index from Kine-matic Viscosity at 40 and 100CD2896 Test Method for Base Number of Petroleum Prod-ucts by Potentiometric Perchloric Acid TitrationD4057 Practice for Manual Sampling of Petroleum andPetroleum Produc
8、tsD4739 Test Method for Base Number Determination byPotentiometric Hydrochloric Acid TitrationD6595 Test Method for Determination of Wear Metals andContaminants in Used Lubricating Oils or Used HydraulicFluids by Rotating Disc Electrode Atomic Emission Spec-trometryD7042 Test Method for Dynamic Visc
9、osity and Density ofLiquids by Stabinger Viscometer (and the Calculation ofKinematic Viscosity)E2412 Practice for Condition Monitoring of In-ServiceLubricants by Trend Analysis Using Fourier TransformInfrared (FT-IR) Spectrometry2.2 ISO Standards:3ISO 4406:99 Hydraulic Fluid Power Solid Contaminatio
10、nsCodeISO 11171 Automatic Particle Counter Calibration Proce-dures3. Terminology3.1 Definitions:3.1.1 electrode, nin an integrated tester, set of two (upperand lower) used in excitation of wear metals during emissionspectroscopic testing.3.1.2 emission spectrometer, ncomponent used to reportelements
11、 in parts per million in lubricants. This processmeasures 20 different wear/additive metals that can be presentin the used lubricant after the oil has been in service for aperiod of time. Test Method D6595 can be used for referenceor definition.3.1.3 infrared spectrometer, ncomponent used to reportc
12、ondition and contamination of the lubricant (for example,water, oxidation, fuel dilution (gasoline and diesel), nitration,glycol, soot, calculated viscosity, and base number). PracticeE2412 can be used for reference or definition.3.1.4 integrated tester, ninstrument used to analyze in-service lubric
13、ants for maintenance, preventative maintenanceand service recommendations. This instrument utilizes any1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products and Lubricants and is the direct responsibility of SubcommitteeD02.96 on In-Service Lubricant Testing and Cond
14、ition Monitoring Services.Current edition approved Oct. 1, 2010. Published November 2010. DOI:10.1520/D7417-10.2For 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 s
15、tandards Document Summary page onthe ASTM website.3Available from American National Standards Institute (ANSI), 25 W. 43rd St.,4th Floor, New York, NY 10036, http:/www.ansi.org.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United Sbination of th
16、e following: emission spectrometer, infrareddevice, viscometer, and particle counter.43.1.5 sample transport system, nin an integrated tester,computer controlled assembly that directs the oil samplesthroughout the integrated tester.3.1.6 spark chamber, nin an integrated tester, area hous-ing the upp
17、er and lower electrodes for emission spectrometer.3.1.7 viscometer, nin an integrated tester, a viscometerusing calibrated measurements similar to a kinematic viscom-eter capable of reporting viscosity at 40C or 100C incentistokes (cSt), and providing a calculated viscosity index.The results are als
18、o used to determine fuel dilution in diesellubricants. Reference to Test Method D445, Practice D2270,orTest Method D7042 can be used as a reference for viscositydefinition. Although the integrated tester does not print out SIunits for measuring viscosity, reporting in mm2/s can bedetermined.3.2 Defi
19、nitions of Terms Specific to This Standard:3.2.1 electrode gap, nin an integrated tester, specificdistance between the upper and lower electrodes in the sparkchamber.3.2.2 particle counter, ncomponent in this particular in-tegrated tester that is used to count particles using laser andhigh-resolutio
20、n digital counter reporting in 4 m(c), 6 m(c),14 m(c) or 2 m, 5 m, 15 m, using ISO 11171 calibrationmethod and or ISO 4406:99 reporting method.3.2.3 sanitized cleaning swabs, nin an integrated tester,used to clean the electrodes after each sample analysis.3.3 Abbreviations:AES = Atomic Emission Spec
21、troscopyIR = InfraredOEM = Original Equipment Manufacturer4. Summary of Test Method4.1 Asample of in-service lubricant is collected into a clean,new 120 mL sample bottle from the equipment being tested,preferably within 30 min of equipment shutdown. Lubricantdescription and service information shoul
22、d be recorded forproper evaluation. The integrated tester is prepared for analysisaccording to the operations manual and on-screen prompts.The lubricant sample is placed into the sample transport systemand is analyzed using available integrated devices. The appli-cation software guides the entire pr
23、ocedure, controls thetransfer of the sample, stores data, and generates on screen andprinted results with a printed generic recommendation of thelubricants physical condition.5. Significance and Use5.1 The integrated tester is primarily used to perform on-siteanalysis of in-service lubricants used i
24、n the automotive, high-way trucking, mining, construction, off-road “mining,” marine,industrial, power generation, agriculture, and manufacturingindustries.5.2 The immediate results of analysis of in-service lubri-cants are critical when performing proactive and preventative4The sole source of suppl
25、y of the apparatus (OSA Lab Four Part Analyzer andaccessories) known to the committee at this time is On-Site Analysis, Inc., 7108Fairway Drive, Suite 130, Palm Beach Gardens, FL 33418 (manufacturing divisionin Marlborough, MA), www.on-. If you are aware of alternativesuppliers, please provide this
26、information to ASTM International Headquarters.Your comments will receive careful consideration at a meeting of the responsibletechnical committee,1which you may attend.TABLE 1 Element Test Parameters Measured, Calculated, and ReportedElement Low Range, mg/kg High Range, mg/kg Element Low Range, mg/
27、kg High Range, mg/kgAluminum 5 to 100 NA Molybdenum 10 to 1000 NABarium 25 to 150 150 to 2000 Nickel 5 to 100 NABoron 5 to 100 100 to 1000 Phosphorous 100 to 600 600 to 4000Calcium 25 to 500 500 to 9000 Potassium 10 to 1000 1000 to 4000Chromium 8 to 100 NA Silicon 5 to 150 150 to 3000Copper 5 to 500
28、 500 to 1000 Sodium 10 to 1000 NAIron 6 to 1000 1000 to 3000 Tin 6 to 100 NALead 6 to 150 NA Titanium 8 to 100 NAMagnesium 5 to 100 100 to 3000 Vanadium 7 to 100 NAManganese 5 to 100 NA Zinc 8 to 100 100 to 4000TABLE 2 Physical Properties Parameters Measured, Calculated, and ReportedNOTEReview Test
29、Method D4739 and D2896 for particular lubricating oil applications.Physical Property RangeWater, wt% 0.1to3Glycol, wt% 0.1to2Soot, wt% 0.1to4Fuel Dilution, wt% 0.1 to 15Oxidation, abs. 0.1 to 50Nitration, abs. 0.1to35Calculated Viscosity - IR 4 to 35 (100 cSt)Viscosity 40C, cSt (optional) 30 to 320V
30、iscosity 100C, cSt (optional) 5 to 25Viscosity Index 5to150Base Number, mg KOH/g 1.0 to 17D7417 102maintenance. On-site oil analysis, when used in conjunctionwith these programs, allows continuous system monitoring andcontamination control potentially improving equipment “up-time” and equipment life
31、.6. Interferences6.1 Sample SizeUsing less than the required 130 mL ofsample for the analysis may result in erroneous numbers.6.2 High ConcentrationOf a contaminant such as waterand or soot in the IR device might cause other parameters to beblocked out in the IR band resulting in a default returned
32、valueof not applicable or “n/a” for these other parameters.7. Apparatus7.1 Integrated TesterThe particular integrated tester willincorporate two or more of the following sensors: an emissionspectrometer, an infrared device, a viscometer, or a particlecounter.7.2 Emission SpectrometerConsists of an e
33、xcitationsource, spark stand, and optical system.7.3 Infrared DeviceConsists of an infrared source, samplecell, and optical system.7.4 Dual Temperature ViscometerConsists of a tempera-ture controlled sample reservoir and electronic control system.7.5 Particle CounterConsists of a sophisticated senso
34、rcell using red laser light extinction technology utilizing theISO 11171 calibration and ISO 4406:99 reporting.7.6 Sample ContainerSample container of no less than118 mL that is free of contaminants shall be used for thein-service oil samples and shall be discarded after use. Themaximum dimensions o
35、f 10.8 cm high, 8.9 cm in diameter, andan opening of no less than 1.6 cm shall be used.7.7 Sonic BathWater-filled, vibrating tool used to be surethat all of the contamination is in suspension in the lubricantsample. This is mostly used when preparing a lubricant samplefor a particle count analysis p
36、rocedure.7.8 Computer Application Software and OperationsManualThe computer application software provides thefunctionality for the particular integrated tester; an electronicuser with help screens and a condensed reference manual forquick reference, interface, hierarchical equipment database tostore
37、, analyze and manage data, embedded logic for datainterpretation; and automatic reporting tools. A complete op-erations manual and troubleshooting guide accompany thesoftware application.8. Reagents and Materials8.1 The particular integrated tester uses the following sup-plies which are available fr
38、om the manufacturer to ensureaccurate operation of the integrated tester:8.1.1 ElectrodesA high-purity silver electrode set (upperand lower).8.1.2 Cleaning FluidAn environmentally safe mineral oil,to clean the instruments internal flow system. The cleaningsolution in most cases can also be used as t
39、he base oil for thecalibration of the instrument. This product is a nonflammableproduct consisting of technical grade Semtol White MineralOil.58.1.3 Test StandardThis solution is intended for use as acalibration standard for the integrated tester. It is a multi-element solution of Primol N3526that w
40、as prepared withneutral oil as a functional antioxidant for specific concentra-tions. The certified concentrations are based upon the assayedconcentrations of the raw materials and the gravimetric proce-dures used to prepare the final standard. The uncertaintyassociated with each certified concentra
41、tion is 62 mg/kg (partsper million). In order to verify these certified values, the finalsolution was analyzed by plasma emission spectroscopy (ICP).NOTE 1The manufacturer guarantees the accuracy of this solutionuntil the expiration date shown, provided it is kept tightly capped andstored in origina
42、l bottle under normal laboratory conditions. Do notrefrigerate or store in direct sunlight. Minimize exposure to moisture orhigh humidity. It is recommended that the solution be thoroughly mixed,by shaking the bottle, prior to use.8.1.4 High Viscosity FluidFor use with viscometer only.This fluid is
43、blended with known viscosities and is periodicallyanalyzed to confirm calibration or to recalibrate the viscometer.It consists of a highly refined mineral oil and a detergent/dispersant engine oil additive package.8.1.5 Low Viscosity FluidFor use with viscometer only.This fluid is blended with known
44、 viscosities and is periodicallyanalyzed to confirm calibration or to recalibrate the viscometer.It consists of a highly refined mineral oil and a detergent/dispersant engine oil additive package.8.1.6 Reference OilUsed to verify accuracy of physicalproperty test results reported by infrared device.
45、 The referenceoil has known physical properties which are tested against theinfrared device using the software to determine standardiza-tion. It consists of a highly refined mineral oil combined withzinc alkyl dithiophosphate.8.1.7 Sanitary Cleaning SwabsUsed to clean the elec-trodes after each samp
46、le analysis. Operator shall use contami-nant free cotton swabs that are not treated with sodium fromthe hypochlorite bleaching process. Check the manufacturersspecifications of the cleaning swabs before use to determine ifthe bleaching process has been performed.9. Hazards9.1 Used oil can contain ha
47、zardous material from compo-nent source and or the contamination process. Wear appropriatepersonal protective equipment to prevent repeated or prolongedcontact with used oil. Follow proper oil handling procedures5The sole source of supply of the apparatus known to the committee at this timeis Sonneb
48、orn, Inc., 771 Old Saw Mill River Rd., Tarrytown, NY 10591-6716. If youare aware of alternative suppliers, please provide this information to ASTMInternational Headquarters. Your comments will receive careful consideration at ameeting of the responsible technical committee,1which you may attend.6The
49、 sole source of supply of the apparatus known to the committee at this timeis ExxonMobil (Corporate Headquarters), 5959 Las Colinas Blvd., Irving, TX75039-2298. If you are aware of alternative suppliers, please provide this informa-tion to ASTM International Headquarters. Your comments will receive carefulconsideration at a meeting of the responsible technical committee,1which you mayattend.D7417 103during sampling and throughout analytical process. Followapplicable regulations and procedures when disposing of used
