1、Designation: D7889 13Standard Test Method forField Determination of In-Service Fluid Properties Using IRSpectroscopy1This standard is issued under the fixed designation D7889; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the yea
2、r 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 the use of a grating spec-trometer to analyze properties of an in-service fluid sample
3、which are indicative of the status of that fluid and relatedmachinery.1.2 This test method provides a means for the assessment ofin-service fluid properties using infrared spectroscopy. It de-scribes a methodology for sampling, performing analysis, andproviding key in-service fluid properties with a
4、 self-containedunit that is meant for field use. It provides analysis of in-servicefluids at any stage of their useful life, including newly utilizedfluid.1.3 In particular, these key in-service fluid properties in-clude oxidation, nitration, sulfation, soot, and antiwear addi-tives. They are applic
5、able for hydrocarbon type (API GroupI-IV) fluids from machinery lubricants, including reciprocatingengine oils, turbine oils, hydraulic oils, and gear oils.1.4 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.4.1 ExceptionThe u
6、nit for wavenumbers is in cm-1.1.5 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 limitatio
7、ns prior to use.2. Referenced Documents2.1 ASTM Standards:2D4057 Practice for Manual Sampling of Petroleum andPetroleum ProductsD7412 Test Method for Condition Monitoring of PhosphateAntiwear Additives in In-Service Petroleum and Hydro-carbon Based Lubricants by Trend Analysis Using FourierTransform
8、 Infrared (FT-IR) SpectrometryD7414 Test Method for Condition Monitoring of Oxidationin In-Service Petroleum and Hydrocarbon Based Lubri-cants by Trend Analysis Using Fourier Transform Infrared(FT-IR) SpectrometryD7415 Test Method for Condition Monitoring of SulfateBy-Products in In-Service Petroleu
9、m and HydrocarbonBased Lubricants by Trend Analysis Using Fourier Trans-form Infrared (FT-IR) SpectrometryD7418 Practice for Set-Up and Operation of Fourier Trans-form Infrared (FT-IR) Spectrometers for In-Service OilCondition MonitoringD7624 Test Method for Condition Monitoring of Nitration inIn-Se
10、rvice Petroleum and Hydrocarbon-Based Lubricantsby Trend Analysis Using Fourier Transform Infrared(FT-IR) SpectrometryD7669 Guide for Practical Lubricant Condition Data TrendAnalysisD7720 Guide for Statistically Evaluating Measurand AlarmLimits when Using Oil Analysis to Monitor Equipmentand Oil for
11、 Fitness and ContaminationD7844 Test Method for Condition Monitoring of Soot inIn-Service Lubricants by Trend Analysis using FourierTransform Infrared (FT-IR) SpectrometryE131 Terminology Relating to Molecular SpectroscopyE168 Practices for General Techniques of Infrared Quanti-tative AnalysisE932 P
12、ractice for Describing and Measuring Performance ofDispersive Infrared SpectrometersE1655 Practices for Infrared Multivariate QuantitativeAnalysisE2412 Practice for Condition Monitoring of In-Service Lu-bricants by Trend Analysis Using Fourier TransformInfrared (FT-IR) SpectrometryE2617 Practice for
13、 Validation of Empirically Derived Mul-tivariate Calibrations3. Terminology3.1 For definitions of terms relating to infrared spectroscopyused in this test method, refer to Terminology E131. For1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products, Liquid Fuels, and L
14、ubricants and is the direct responsibility ofSubcommittee D02.96.03 on FTIR Testing Practices and Techniques Related toIn-Service Lubricants.Current edition approved Oct. 1, 2013. Published October 2013. DOI: 10.1520/D7889-13.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orco
15、ntact ASTM Customer Service 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 States1definition of terms r
16、elated to infrared-based in-service fluidcondition monitoring, refer to Practice D7418.3.2 Definitions of Terms Specific to This Standard:3.2.1 absorbance units (AU), nunits of measurement ofthe raw absorbance spectrum which is obtained using thedefinition described in Section 8 (Theory for a Single
17、 Com-pound Analysis) of Practice E168, which is not normalized forpathlength.3.2.2 cell background, na single-beam spectrum that isobtained on a clean, empty wipe-clean transmission cell.3.2.3 mid-infrared grating spectrometer, na spectrometerwhich operates in the mid-infrared spectral range, betwee
18、n atleast 960 cm-1and 3040 cm-1and creates an infrared spectrumby means of a reflective diffraction grating.3.2.3.1 DiscussionSuch a grating spectrometer may be ofany of a variety of designs and optical configurations. Exampledesigns include monochrometer-type systems wherein thegrating is rotated t
19、o a single point infrared detector, orarray-type systems which utilize an infrared detector array atthe output and a fixed grating. Example optical configurationsinclude Rowland-Circle and Czerny-Turner systems. Typicalinfrared detectors are uncooled thermal detectors such asthermopile or pyroelectr
20、ic-based sensors.3.2.4 reporting units, nspecifies the reporting units of thefluid analysis property.3.2.5 self-contained field apparatus, na mid-infrared grat-ing spectrometer which is of the form factor to allow it tooperate as an independent device suitable for field use.3.2.6 wipe-clean transmis
21、sion cell, nan infrared transmis-sion cell which is specifically tailored for field use.3.2.6.1 DiscussionIn particular, the cell may be utilizedand cleaned with a towel or rag and without the use of reagentsor chemicals of any sort, making it convenient for use as a fielddevice. Such transmission c
22、ells may accomplish this usingmechanisms for quick open/close of the cell such as by meansof a mechanical lever, demountable screw or press fit, ormagnetic coupling. To correct for any cell fringing effects, thecell utilizes a wedged design both on the interior faces andexterior faces of the cell wi
23、ndows: The cell windows them-selves are wedged at an angle of less than 0.5 degrees. Thespacing between the two windows is wedged at an angle ofapproximately 0.013 degrees. The cell is designed to benominally 100 m in pathlength, with ZnSe windows.4. Summary of Test Method4.1 This test method utiliz
24、es a self-contained field apparatusto provide detailed information concerning the condition statusof in-service fluids. In particular, it provides readings ofoxidation, antiwear additive, sulfation, nitration and soot levelsin hydrocarbon type (API Group I-IV) fluids.4.1.1 An absorbance spectrum of
25、the sample under test isobtained. For the background spectrum, the cell background isused.4.1.1.1 Test Methods have been developed for Fourier-transform infrared (FTIR) devices using absorbance spectraobtained using Practice D7418. Particular Test Methods devel-oped for in-service monitoring of hydr
26、ocarbon type (APIGroup I-IV) fluids include those established for Oxidation(Test Method D7414, Procedure A), Antiwear Additive (TestMethod D7412, Procedure A), Sulfation (Test Method D7415,Procedure A), Nitration (Test Method D7624, Procedure A),and Soot (Test Method D7844, Procedure A). These testm
27、ethods have served to establish the signature infrared spec-troscopic behavior associated with key in-service monitoringproperties. This test method provides property values based onthe examination of each propertys signature infrared spectro-scopic behavior. The essence of this test method is to ca
28、pturethe underlying chemical trends associated with each propertyfor in-service fluid analysis using a self-contained field appa-ratus and coupled wipe-clean transmission cell.4.1.2 From the infrared absorbance spectrum obtained withthe self-contained field apparatus, properties of the in-serviceflu
29、id are calculated. In particular, those properties in Table 1are calculated by the device and presented to the user on thedisplay. Additional properties using infrared calibration meth-ods may be calculated and displayed depending on the particu-lar fluid being analyzed and availability of calibrati
30、ons for thatfluid.4.1.2.1 Infrared spectra generated by the described instru-ment type can be used to provide a further set of properties ofinterest to in-service fluid analysis of hydrocarbon type (APIGroup I-IV) fluids. Such properties must be calibrated to theparticular fluid blend, and may be ge
31、nerated using ASTMguidelines which govern the creation of such calibrations. Suchcalibrations may be built from either standard regressionmethods as described in Practice E168 or as described inPractice E2412. Further, they may also be multivariatecalibrations, described in Practice E1655 and Practi
32、ce E2617.Example properties include Acid Number (AN), Base Number(BN), water contamination, ethylene glycol, fluid mixturecontent, and antioxidant depletion. It should be noted that, dueto the fact that these calibrations are sample-specific, this testmethod does not provide a prescription for calcu
33、lating suchproperties.4.2 The results of the test method can be compared againstpre-defined or user-defined limits so as to judge the conditionof the in-service lubricant. Warning and alarm limits ex-ceedences which may be pre-defined or set by the user areindicated by the property and associated va
34、lue being high-lighted using coding established in Guide D7720, with eithergreen (favorable alarm level designation showing acceptablecondition), yellow (intermediate level alarm designation warn-ing a fault condition is present and will likely need attention inthe future), or red (high level alarm
35、designation showingsignificant deterioration) indicated by the self-contained fieldapparatus.TABLE 1 In-Service Lubricant Properties Reported by the TestMethodProperty Reporting UnitsOxidation Abs/0.1 mmAntiwear Additive Abs/0.1 mmSulfation Abs/0.1 mmNitration Abs/cmSoot Abs/cmD7889 1325. Significan
36、ce and Use5.1 This test method provides a means for obtaining usefulin-service fluid analysis properties in the field. It is not to beconfused with laboratory or portable FTIR devices whichprovide measurements per the existing Test Methods listed in4.1.1.1. Each of these monitored properties has bee
37、n shownover time to indicate either contamination in the fluid system ora particular breakdown modality of the fluid, which is criticalinformation to assess the health of the fluid as well as themachinery. By utilizing the field device, it is possible for thoseoperating machinery, in locations and s
38、ituations where it is notpractical to gather a sample for the laboratory, to obtain qualityin-service fluid analysis. This may be due to the need to havean analysis done in real-time, on-the-spot to maximize theoperational hours of equipment, or to have the analysisperformed at a location where no l
39、aboratory analysis isavailable.6. Interferences6.1 Spectral interferences due to very high levels of externalcontamination in the fluid can yield errors with these measure-ments. Common contaminants include the presence of APIGroup V lubricants at levels exceeding 5 % and antifreezemixes at similar
40、levels.7. Apparatus7.1 A self-contained mid-infrared grating spectrometer witha coupled wipe-clean transmission cell as defined in Section 3.7.2 This spectrometer shall have specific performance char-acteristics indicated in 7.3 7.5, with a Spectral Format in theform of absorbance as a function of w
41、avenumber reported at adigital resolution of 2 cm-1.7.3 Signal-to-Noise Ratio (S/N)shall be adequate to pro-vide the desired precision as indicated in Section 17.Practically, this means that, over the range of measurement, thestandard deviation of the obtained absorbance should be lessthan 0.001 AU.
42、 Based on the capabilities of the spectrometersystem, this may be achieved by co-adding a number of scansto improve the S/N as needed.7.4 Spectral Resolutionshall be approximately 1.5 % offrequency being measured across the measurement range. Forexample, at 1000 cm-1, the spectral resolution should
43、be15 cm-1. In order to qualify this resolution, a simple test usinga 40 micron film of polystyrene, a standard reference materialfor grating instruments as discussed in Practice E932 may beperformed. The absorbance spectrum of this material measuredwith the spectrometer should show a peak at band nu
44、mber 12(1028 cm-1) of approximately 0.29 AU and a peak at bandnumber 2 (2924 cm-1) of approximately 0.56 AU. Otherspectral resolutions may provide accurate results as well butthe calculation parameters listed in Table 2 and Section 17 maybe different from those listed.7.5 Spectral Rangeshall cover t
45、he frequencies necessaryfor calculation of all properties described in the method, whichis 960 cm-1to 3040 cm-1.8. Reagents and Materials8.1 The only materials required to make a measurement areeither a shop rag or lint-free paper towel to clean the wipe-clean transmission cell. No other materials o
46、r reagents arenecessary.9. Hazards9.1 The apparatus utilizes a certified Li-Ion battery.10. Sampling, Test Specimens, and Test Units10.1 A sample of in-service fluid should be obtained. Aminimum quantity of approximately 50 L is needed to obtainone set of measurements as defined in Table 2. The samp
47、leshould be representative of the system. If such equipment isavailable, the sample is preferably obtained as described inPractice D4057.11. Preparation of Apparatus11.1 A quality collection of the infrared absorbance spec-trum is assured by several internal quality checks, whichinclude check fluid,
48、 pathlength, clean cell, and loaded cellmonitoring.11.1.1 Check fluid and pathlength monitoring (described inPractice D7418) are performed on a periodic basis according tomanufacturers recommendations.11.1.2 In order to verify that the wipe-clean transmissioncell is empty and clean, a cell backgroun
49、d is taken in real-timeand a raw absorbance spectrum is calculated using a previouslyarchived, known, empty, and clean cell background.11.1.2.1 By measuring the maximum peak height between3000 cm-1and 2800 cm-1relative to a baseline at 2700 cm-1,itcan be determined whether the cell is clean. When theabsorbance value is greater than a pre-set limit of 0.2 AU, thecell is considered not clean.11.1.2.2 This check is performed before any cell back-ground to be used in the calculation of fluid properties isobtained, and the user is warned if the check fails.11.1.3 Acell lo
