ASTM D7797-2016 1607 Standard Test Method for Determination of the Fatty Acid Methyl Esters Content of Aviation Turbine Fuel Using Flow Analysis by Fourier Transform Infrared Spect.pdf

1、Designation: D7797 16 An American National Standard583Standard Test Method forDetermination of the Fatty Acid Methyl Esters Content ofAviation Turbine Fuel Using Flow Analysis by FourierTransform Infrared SpectroscopyRapid ScreeningMethod1,2This standard is issued under the fixed designation D7797;

2、the number immediately following 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

3、. Scope*1.1 This test method specifies a rapid screening methodusing flow analysis by Fourier transform infrared (FA-FTIR)spectroscopy with partial least squares (PLS-1) processing forthe determination of the fatty acid methyl ester (FAME)content of aviation turbine fuel (AVTUR), in the range of10 m

4、g kg to 150 mg kg.NOTE 1Specifications falling within the scope of this test method are:Specification D1655 and Defence Standard 91-91.NOTE 2This test method detects all FAME components, with peak IRabsorbance at approximately 1749 cm-1and C8to C22molecules, asspecified in standards such as Specific

5、ation D6751 and EN 14214. Theaccuracy of the method is based on the molecular weight of C16to C18FAME species; the presence of other FAME species with differentmolecular weights could affect the accuracy.NOTE 3Additives such as antistatic agents, antioxidants and corrosioninhibitors are measured wit

6、h the FAME by the FTIR spectrometer.However the effects of these additives are removed by the flow analysisprocessing.NOTE 4FAME concentrations from 150 mg/kg to 500 mg/kg, andbelow 10 mg/kg can be measured but the precision could be affected.1.2 The values stated in SI units are to be regarded asst

7、andard. No other units of measurement are included in thisstandard.1.3 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 ap

8、plica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:3D1298 Test Method for Density, Relative Density, or APIGravity of Crude Petroleum and Liquid Petroleum Prod-ucts by Hydrometer MethodD1655 Specification for Aviation Turbine FuelsD4052 Test Method for Dens

9、ity, Relative Density, and APIGravity of Liquids by Digital Density MeterD4057 Practice for Manual Sampling of Petroleum andPetroleum ProductsD4177 Practice for Automatic Sampling of Petroleum andPetroleum ProductsD6300 Practice for Determination of Precision and BiasData for Use in Test Methods for

10、 Petroleum Products andLubricantsD6751 Specification for Biodiesel Fuel Blend Stock (B100)for Middle Distillate FuelsE1655 Practices for Infrared Multivariate QuantitativeAnalysis2.2 CEN Standards:4EN 14214 Specification Automotive FuelsFatty AcidMethyl Esters (FAME) for Diesel EnginesRequirementsan

11、d Test Methods2.3 Energy Institute Standards:5IP 583 Test Method for Determination of the Fatty AcidMethyl Esters Content of Aviation Turbine Fuel UsingFlow Analysis by Fourier Transform InfraredSpectroscopyRapid Screening Method1This test method is under the jurisdiction of ASTM Committee D02 onPet

12、roleum Products, Liquid Fuels, and Lubricants and is the direct responsibility ofSubcommittee D02.J0.05 on Fuel Cleanliness.Current edition approved May 15, 2016. Published June 2016. Originallyapproved in 2012. Last previous edition approved in 2012 as D7797 12. DOI:10.1520/D7797-16.2This standard

13、has been developed through the cooperative effort betweenASTM International and the Energy Institute, London. The IP and ASTM logosimply that the ASTM and IP standards are technically equivalent, but their use doesnot imply that both standards are editorially identical.3For referenced ASTM standards

14、, 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.4Available from American National Standards Institute (ANSI), 25 W. 43rd St.,4th Floor, New

15、 York, NY 10036, http:/www.ansi.org.5Available from the Energy Institute, 61 New Cavendish St., London, WIG 7AR,U.K., http:/www.energyinst.org.uk.*A Summary of Changes section appears at the end of this standardCopyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 1

16、9428-2959. United States12.4 Other Standards:6Defence Standard 91-91 Issue 7 (DERD 2494) Turbine Fuel,Aviation Kerosine Type, Jet A12.5 ASTM Adjuncts:7ADJD6300 (D2PP) Determination of Precision and BiasData for Use in Test Methods for Petroleum Products3. Terminology3.1 Definitions:3.1.1 FAME, nFatt

17、y acid methyl esters, also known asbiodiesel.3.1.1.1 DiscussionUsed as a component in automotivediesel fuel and the potential source of contamination in aviationturbine fuel due to multi-fuel tankers and pipelines.3.2 Definitions of Terms Specific to This Standard:3.2.1 FA-FTIR, nflow analysis by Fo

18、urier Transform Infrared technique uses a flow-through measurement cell to make anumber of measurements on a stream of test specimen.3.2.1.1 DiscussionThe test specimen is analyzed beforeand after passing through a sorbent that is designed to retardthe FAME contamination to be measured. The results

19、arecompared to enable the amount of FAME present in theaviation fuel to be determined.3.2.2 sorbent cartridge, na cartridge, through which thetest specimen flows, containing a specific sorbent3.2.2.1 DiscussionThe sorbent cartridge is discarded aftereach test.4. Summary of Test Method4.1 A test spec

20、imen of aviation turbine (AVTUR) fuel isautomatically analyzed, by an FTIR spectrometer, ina2mmeffective path length flow-through cell, before and after flow-ing through a cartridge containing a sorbent designed to havea relatively long residence time for FAME. The spectroscopicabsorbance difference

21、s of the IR spectra, between themeasurements, are processed in conjunction with a PLS-1model to determine the presence and amplitude of the carbonylpeak of FAME at approximately 1749 cm-1. Test time istypically 20 min. The flow analysis by FTIR enables the effectsof potential interferences to be rem

22、oved by using their relativeretardance times through the sorbent in conjunction with theirabsorbance at specific wavelengths.5. Significance and Use5.1 The present and growing international governmentalrequirements to add fatty acid methyl esters (FAME) to dieselfuel has had the unintended side-effe

23、ct of leading to potentialFAME contamination of jet turbine fuel in multifuel transportfacilities such as cargo tankers and pipelines, and industry wideconcerns.5.2 Analytical methods have been developed with the capa-bility of measuring down to 5 % FAME.NOTE 5New sample containers are strongly reco

24、mmended due toconcerns over the difficulty in removing all traces of FAME retained fromprevious samples.8.2.2 Rinse all sample containers with heptane (7.1)oranother suitable solvent and drain. Then rinse with the productto be sampled at least three times. Each rinse shall use productwith a volume o

25、f 10 % to 20 % of the container volume. Eachrinse shall include closing and shaking the container for aminimum of 5 s and then draining the product.6Available from Procurement Executive DF5 (air), Ministry of Defence,www.dstan.mod.uk.7ADJD6300 is no longer available from ASTM International Headquart

26、ers.8The following reagents and materials were used to develop the precisionstatements: Seta Verification and Calibration fluids for Seta FIJI, Stanhope-Seta,Chertsey, Surrey, KT16 8AP, UK. This is not an endorsement or certification byASTM.D7797 1629. Preparation of Apparatus9.1 Follow the manufact

27、urers instructions and on-screeninstructions for the correct set up and shut down of theapparatus.9.2 Run a flushing sequence using heptane (7.1) in accor-dance with the manufacturers instructions if the last testsample contained FAME in excess of 150 mg kg.9.3 Wipe dry the sample input tube with a

28、lint free cloth(7.4) before commencing a test.9.4 Ensure that the verification and calibration of the instru-ment are in accordance with Section 10.9.5 Gently swirl the sample for homogeneity before draw-ing the test specimen.9.6 Determine the density of the sample using the densitymeasuring device

29、(6.4) if the density is not known.9.7 Use a new test specimen container, or if there is enoughtest sample available it is permissible to clean and dry the testspecimen container thoroughly before each test using heptaneand then partially fill with the test sample, swirl and drain,repeat three times.

30、NOTE 6New specimen containers are strongly recommended due toconcerns over the difficulty in removing all traces of FAME retained fromprevious test specimens.10. Calibration and Standardization10.1 Verification:10.1.1 Follow the apparatus and test specimen preparationinstructions (9) and check the v

31、alidity of the verification fluidsto be used.10.1.2 Verify the correct operation of the instrument usingthe verification fluid (7.2.1), in accordance with the manufac-turers instructions, at least every six months. More frequentperformance checks shall be carried out according to localquality contro

32、l requirements.10.1.3 Verify the correct operation of the instrument usingboth verification fluids (7.2.1 and 7.2.2) in accordance with themanufacturers instructions at least every 12 months or imme-diately after any maintenance on the measurement system.10.1.4 If the result is not within R/2 plus t

33、he uncertainty ofthe verification fluids certified value or within the tolerancessupplied with the verification fluid, recheck the validity date ofthe verification fluid and run a flushing sequence (9.2) andrepeat the verification.NOTE 7In 10.1.4, R is the reproducibility of the test method at100 mg

34、 kg or 30 mg kg, respectively.10.1.5 If it is not possible to meet the criteria in 10.1.4 toverify the correct operation of the instrument, follow themanufacturers instructions regarding fault finding and calibra-tion.10.2 Calibration:10.2.1 Calibrate the instrument according to the manufac-turers i

35、nstructions when it is not possible to meet the criteriain 10.1.4 to verify the correct operation of the instrument.10.2.1.1 Calibration uses five (5) calibration standards (7.3)covering the scope of the test method, containing knownamounts (mg/kg) of FAME in a known fluid.11. Procedure (see Fig. 1)

36、11.1 Commence the test measurement sequence (see Sec-tion 9), and input the sample density in kilograms per cubicmetre (kg/m3) and sample identification in accordance with themanufacturers instructions and the on-screen instructions.NOTE 8If the density of the aviation fuel is not known, a nominalva

37、lue of 807.5 kg m3is assumed. This could affect the result by amaximum of 4 %.11.2 Insert a new sorbent cartridge (A1.1.3) and attach anew filter (A1.1.9) to the exit (bottom) of the sorbent cartridge;follow the manufacturers instructions to fit the input tube tothe cartridge.11.3 Pour approximately

38、 50 mL of sample into the testspecimen container (A1.1.4), that has been prepared as de-scribed in 9.7, locate in position and attach the container lidand sample input tube.11.4 Ensure that an empty waste container, lid and outputtube (A1.1.5) are in position.11.5 Start the test to commence the foll

39、owing automaticsequences as the test specimen is drawn through the instrumentby the programmed pump: (see Fig. 1 and Fig. A1.1):11.5.1 Prime and flush the tubing and the flow-throughmeasurement cell with the test specimen.11.5.2 Measure the spectrum of the test specimen to checkfor contamination and

40、 to obtain a reference spectrum.11.5.3 Measure the spectra of the output from the sorbentcartridge until a stable value is reached and compares with thereference spectrum.11.5.4 Re-measure the spectrum of the test specimen toobtain a second reference spectrum.11.5.5 Analyze and compare the flow anal

41、ysis spectra (see11.5.3) with the reference spectrum and determines the FAMEpeak amplitude using a PLS-1 model (see A1.1.10) over thenominal 1660 cm-1to 1800 cm-1range.FIG. 1 Test SequenceD7797 16311.5.6 Calculate the FAME concentration in mg/kg usingthe calibration curve, the determined peak, the s

42、tored value ofthe calibrant materials density and the samples density (see9.6).11.5.7 Flush the system with the remainder of the testspecimen and finally purges with air.11.5.8 Display the result numerically and graphically (seeFig. A1.1 for a typical example).11.6 Record the test result and follow

43、the manufacturersinstructions to remove and dispose of the used sorbent car-tridge and filter.12. Calculation12.1FAME mg/kg 5 Cm! 3 Pc Ps! (1)where:Cm= value directly from the integral calibration curve mg/kg,Ps= density of the sample in kg/m3,Pc= density of the calibrant material in kg/m3.Report th

44、e amount of FAME in the sample to the nearest0.1 mg kg.13. Report13.1 The test report shall contain at least the followinginformation:13.1.1 A reference to this standard,13.1.2 All details necessary for complete identification ofthe product tested,13.1.3 The result of the test (see Section 12),13.1.

45、4 Any deviations, by agreement or otherwise, from theprocedures specified, and13.1.5 The time and date of the test.14. Precision and Bias914.1 GeneralThe precision was obtained from a 2013Energy Institute ILS carried out in Europe using eightinstruments/operators, located in separate laboratories, a

46、nd asample set comprising 13 aviation turbine fuel samples induplicate blended with known amounts of FAME. Samplesincluded hydro-treated fuel, non-hydro-treated fuel, and syn-thetic fuel and were sourced from the U.S., U.K., and Europe.The precision values given in 12.1 were derived from statistical

47、analysis of these test results.14.1.1 The precision was obtained by statistical examina-tion of the ILS test results according to Practice D6300 usingADJD6300 D2PP.14.2 RepeatabilityThe difference between successive testresults obtained by the same operator with the same apparatusunder constant oper

48、ating conditions on nominally identical testmaterial would, in the normal and correct operation of the testmethod, exceed the value below only in one case in 20:r 5 4.589 mg/kg (2)See Table 1 for a tabular illustration of precision.14.3 ReproducibilityThe difference between two test re-sults indepen

49、dently obtained by different operators usingdifferent apparatus on nominally identical test material would,in the normal and correct operation of the test method, exceedthe value below only in one case in 20:R 5 0.04967X 1 100! (3)where X is the average of two results being compared, inmg/kg. See Table 1 for a tabular illustration of precision.14.4 BiasSince there is no accepted reference material fordetermining the bias for the procedure in this test method, abias cannot be determined. The evaluation of 100 separate fuelsamples to d