ASTM E2412-2004 Standard Practice for Condition Monitoring of Used Lubricants by Trend Analysis Using Fourier Transform Infrared (FT-IR) Spectrometry《利用傅立叶变换红外线(FT-IR)光谱测定法通过趋势分析监测.pdf

1、Designation: E 2412 04Standard Practice forCondition Monitoring of Used Lubricants by Trend AnalysisUsing Fourier Transform Infrared (FT-IR) Spectrometry1This standard is issued under the fixed designation E 2412; the number immediately following the designation indicates the year oforiginal adoptio

2、n 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 editorial change since the last revision or reapproval.1. Scope1.1 This practice covers the use of FT-IR in monitoringadditive depletion, con

3、taminant buildup and base stock degra-dation in machinery lubricants, hydraulic fluids and other fluidsused in normal machinery operation. Contaminants monitoredinclude water, soot, ethylene glycol, fuels and incorrect oil.Oxidation, nitration and sulfonation of base stocks are moni-tored as evidenc

4、e of degradation. The objective of this moni-toring activity is to diagnose the operational condition of themachine based on fault conditions observed in the oil. Mea-surement and data interpretation parameters are presented toallow operators of different FT-IR spectrometers to compareresults by emp

5、loying the same techniques.1.2 This practice is based on trending and distributionresponse analysis from mid-infrared absorption measurements.While calibration to generate physical concentration units maybe possible, it is unnecessary or impractical in many cases.Warning or alarm limits (the point w

6、here maintenance actionon a machine being monitored is recommended or required)can be determined through statistical analysis, history of thesame or similar equipment, round robin tests or other methodsin conjunction with correlation to equipment performance.These warning or alarm limits can be a fi

7、xed maximum orminimum value for comparison to a single measurement or canalso be based on a rate of change of the response measured(1).2This practice describes distributions but does not precludeusing rate-of-change warnings and alarms.NOTE 1It is not the intent of this practice to establish or reco

8、mmendnormal, cautionary, warning or alert limits for any machinery. Such limitsshould be established in conjunction with advice and guidance from themachinery manufacturer and maintenance group.1.3 Spectra and distribution profiles presented herein are forillustrative purposes only, and are not to b

9、e construed asrepresenting or establishing lubricant or machinery guidelines.1.4 This practice is designed as a fast, simple spectroscopiccheck for condition monitoring of used lubricants and can beused to assist in the determination of general machinery healththrough measurement of properties obser

10、vable in the mid-infrared spectrum such as water, oil oxidation, and others asnoted in 1.1. The infrared data generated by this practice istypically used in conjunction with other testing methods. Forexample, infrared spectroscopy cannot determine wear metallevels or any other type of elemental anal

11、ysis. The practice aspresented is not intended for the prediction of lubricantphysical properties (for example, viscosity, total base number,total acid number, etc.). This practice is designed for monitor-ing used lubricants and can aid in the determination of generalmachinery health and is not desi

12、gned for the analysis oflubricant composition, lubricant performance or additive pack-age formulations.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 h

13、ealth practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:3D 445 Test Method for Kinematic Viscosity of Transparentand Opaque LiquidsD 2896 Test Method for Base Number of Petroleum Prod-ucts by Potentiometric Perchloric Acid Tit

14、rationD 4057 Practice for Manual Sampling of Petroleum andPetroleum ProductsD 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

15、 (ICP-AES)D 6304 Test Method for Determination of Water in LiquidPetroleum Products by Karl Fischer ReagentE 131 Terminology Relating to Molecular SpectroscopyE 168 Practices for General Techniques of Infrared Quanti-tative Analysis1This practice is under the jurisdiction of ASTM Committee E13 on Mo

16、lecularSpectroscopy and is the direct responsibility of Subcommittee E13.03 on InfraredSpectroscopy.Current edition approved Nov. 1, 2004. Published December 2004.2The boldface numbers in parentheses refer to the list of references at the end ofthis standard.3For referenced ASTM standards, visit the

17、 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.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, U

18、nited States.E 1421 Practice for Describing and Measuring Performanceof Fourier Transform Mid-Infrared (FT-MIR) Spectrom-eters: Level Zero and Level One TestsE 1655 Practice for Infrared, Multivariate, QuantitativeAnalysis2.2 ISO Document:ISO/TC 108 N 605 Terminology for the Field of ConditionMonito

19、ring and Diagnostics of Machines43. Terminology3.1 DefinitionsFor definitions of terms relating to infraredspectroscopy used in this practice, refer to Terminology E 131.3.1.1 Fourier transform infrared (FT-IR) spectrometry,na form of infrared spectrometry in which an interferrogramis obtained; this

20、 interferrogram is then subjected to a Fouriertransform to obtain an amplitude-wavenumber (or wavelength)spectrum. E 1313.2 Definitions of Terms Specific to This Standard:3.2.1 condition monitoring, na field of technical activityin which selected physical parameters associated with anoperating machi

21、ne are periodically or continuously sensed,measured and recorded for the interim purpose of reducing,analyzing, comparing and displaying the data and informationso obtained and for the ultimate purpose of using interim resultto support decisions related to the operation and maintenanceof the machine

22、 (2, 3).3.2.2 machinery health, na qualitative expression of theoperational status of a machine sub-component, component orentire machine, used to communicate maintenance and opera-tional recommendations or requirements in order to continueoperation, schedule maintenance or take immediate mainte-nan

23、ce action.3.2.3 trend analysis, nas applied in this practice, moni-toring of the level and rate of change over operating time ofmeasured parameters (1).3.2.4 used oil, nas applied in this practice, a lubricatingoil that is present in a machine which has been at operatingtemperature for at least one

24、hour.3.2.4.1 DiscussionSampling a used oil after at least onehour of operation will allow for the measurement of a basepoint for later trend analysis.3.2.4.2 DiscussionAny subsequent addition of lubricant(for example, topping off, may change the trending baseline)which may lead to erroneous conclusi

25、ons.3.2.5 new oil, nan oil taken from the original manufac-turers packaging, prior to being added to machinery.3.2.6 reference oil, nsee new oil.4. Summary of Practice4.1 Periodic samples are acquired from the engine ormachine being monitored. An infrared absorbance spectrum ofthe sample is acquired

26、, typically covering the range of 4000 to550 cm-1, with sufficient signal-to-noise (S/N) ratio to measureabsorbance areas of interest. Exact data acquisition parameterswill vary depending on instrument manufacturer but mostsystems should be able to collect an absorbance spectrumadequate for most mea

27、surements in less than one minute.Features in the infrared spectrum indicative of the molecularlevel components of interest (1,8) (that is, water, fuel, anti-freeze, additive, degradation, and so forth) are measured andreported. Condition alerts and alarms can then be triggeredaccording to both the

28、level and the trends from the monitoredsystem.5. Significance and Use5.1 Periodic sampling and analysis of lubricants have longbeen used as a means to determine overall machinery health.Atomic emission (AE) and atomic absorption (AA) spectros-copy are often employed for wear metal analysis (for exam

29、ple,Test Method D 5185). A number of physical property testscompliment wear metal analysis and are used to provideinformation on lubricant condition (for example, Test MethodsD 445, D 2896, and D 6304). Molecular analysis of lubricantsand hydraulic fluids by FT-IR spectroscopy produces directinforma

30、tion on molecular species of interest, including addi-tives, fluid breakdown products and external contaminants, andthus complements wear metal and other analyses used in acondition monitoring program (1,4-8).6. Apparatus6.1 Required Components:6.1.1 Fourier Transform Infrared Spectrometer (FT-IR)In

31、strument is configured with a source, beamsplitter anddetector to adequately cover the mid-infrared range of 4000cm-1to 550 cm-1. Most work has been done on systems usinga room temperature deuterated triglycine sulfate (DTGS)detector, air-cooled source and Germanium coating on Potas-sium Bromide (Ge

32、/KBr) beamsplitter. Alternate source, beam-splitter and detector combinations covering this range arecommercially available but have not been investigated for usein this practice. Other detectors may be suitable but should beused with caution. In particular, liquid nitrogen cooled Mer-cury Cadmium T

33、elluride (MCT) detectors are known to exhibitsignificant nonlinearities.6.1.2 Infrared Liquid Transmission Sampling CellSampling cells can be constructed of zinc selenide (ZnSe),barium fluoride (BaF2), potassium bromide (KBr), or othersuitable window material, with a pathlength of 0.1 mm (100m), par

34、allel (3to5%w/wsolids). As acondition limit (soot) has already triggered, action should betaken irrespective of water. Exact quantitative measurement ofsoot is difficult (that is, % w/w) due to multiple infraredcontributing factors as well as the many different soot mea-surement methods available.A1

35、.2.2 Soot:A1.2.2.1 Soot loading is measured from the baseline offsetat 2000 cm-1as described in the table above. Fig. A1.2 showssome examples of spectra showing low, intermediate, high andvery high soot loading levels (increasing levels from 1 through5).A1.2.2.2 Soot InterferenceHigh water levels ha

36、ve beenobserved to interfere with the measurement of soot in internalcombustion engine crankcases. However, this interference doesnot become significant until the water level is on the order of5 % (50 000 ppm), levels which will immediately condemnthe lubricant and require immediate maintenance acti

37、on irre-spective of any other indicators.A1.2.3 Oxidation, Nitration and Sulfation:A1.2.3.1 Unlike the previous examples, oxidation, nitrationand sulfation breakdown products in crankcase oils can not beeasily quantified by comparison to pure prepared standards.Here, there are a large number of diff

38、erent oxidation andnitration compounds that can be produced and gradually buildup in the oil. Fig. A1.3 shows the measurement areas foroxidation and nitration product buildup monitoring, with thesulfation region highlighted in Fig. A1.4.TABLE A1.1 Petroleum Lubricant (for example, Crankcase) Conditi

39、on Monitoring ParametersDirect TrendingComponent Measurement Area, cm-1Baseline Point(s), cm-1ReportingAWater Area 3500 to 3150 Minima 4000 to 3680 and 2200 to 1900 Report Value as MeasuredSoot Loading Absorbance intensity at 2000 None Value 3 100Oxidation Area 1800 to 1670 Minima 2200 to 1900 and 6

40、50 to 550 Report Value as MeasuredNitration Area from 1650 to 1600 Minima 2200 to 1900 and 650 to 550 Report Value as MeasuredAntiwear Components(Phosphate based, typically ZDDP)Area 1025 to 960 Minima 2200 to 1900 and 650 to 550 Report Value as MeasuredGasoline Area 755 to 745 Minima 780 to 760 and

41、 750 to 730 Report Value as MeasuredDiesel (JP-5, JP-8)BArea 815 to 805 Minima 835 to 825 and 805 to 795 (Value + 2) 3 100Sulfate by-products Area 1180 to 1120 Minima 2200 to 1900 and 650 to 550 Report value as measuredEthylene Glycol Coolant Area 1100 to 1030 Minima 1130 to 1100 and 1030 to 1010 Re

42、port value as measuredAReporting values in absorbance/0.1 mm (see 6.1.2).BSpectral characteristics of diesel and other noted fuels have been found to vary. Work is currently active on other IR measurement areas and techniques. Themeasurement listed can be used as a guideline but is not intended to b

43、e the only infrared based fuel contamination measurement. Checking suspect fuel sources issuggested to verify presence of indicator absorbance bands.FIG. A1.1 Example of Integrated Band Measurement Area for Water in Crankcase OilE2412046A1.2.3.2 Oxidation, Nitration and SulfationInterferencesAs in t

44、he soot measurement, very high waterlevels can generate false positives for oxidation and nitration.However, water levels of this magnitude will immediatelycondemn the lubricant. Very high (5 %) glycol levels in acrankcase oil may start interfering with sulfation measurement,but again contaminant le

45、vels of this magnitude would dictateimmediate maintenance action. Various additive packages,such as detergents, dispersants, antioxidants, overbase addi-tives, etc. may also generate significant absorbance in thecondition monitoring regions of interest. Blends of petroleumlubricants with significant

46、 amounts of ester whether part of thebase stock package or as an additive will absorb strongly in theoxidation area. These lubricants are not presented at this time.A1.2.4 Fuel Contamination:A1.2.4.1 The possibility of fuel contamination may beindicated in diesel crankcase lubricants by measuring th

47、e peakat 810 cm-1. Spectral characteristics of diesel (Fig. A1.6) andFIG. A1.2 Soot Measurement in Diesel Crankcase OilsFIG. A1.3 Oxidation and Nitration Measurement in Crankcase OilsE2412047other fuels noted in Table A1.1 have been found to vary. Workis currently active on other IR measurement area

48、s and tech-niques. The measurement listed can be used as a guideline butis not intended to be the only infrared based fuel contaminationmeasurement. An independent test, such as viscosity change,flash point, or gas chromatography can be used to confirm anindication of fuel presence by the FT-IR.A1.2

49、.5 Glycol Antifreeze Contamination:A1.2.5.1 Glycol contamination is monitored in diesel crank-case lubricants by measuring the carbon-oxygen stretch regionas noted in Table A1.1. Spectral characteristics of glycolcontamination are shown in Fig. A1.6.A1.2.5.2 Ethylene glycol will interfere with the ability toaccurately quantify water level when present since it alsocontains hydroxyl groups. However, the converse is not truesince glycol has other spectral features that are used fordetection and quantification. Therefore, when glycol is present,water can be detected but