ASTM D7797-2012 0625 Test Method for Determination of the Fatty Acid Methyl Esters Content of Aviation Turbine Fuel Using Flow Analysis by Fourier Transform Infrared Spectroscopy &.pdf

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1、Designation: D7797 12583Test Method forDetermination of the Fatty Acid Methyl Esters Content ofAviation Turbine Fuel Using Flow Analysis by FourierTransform Infrared Spectroscopy Rapid ScreeningMethod1,2This standard is issued under the fixed designation ; the number immediately following the design

2、ation indicates the year of originaladoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscriptepsilon () indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method specifies a rap

3、id 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 of 20 to150 mg/kg.NOTE 1Specifications falling wit

4、hin 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 Specification D6751 and EN 14214. Theaccuracy of the metho

5、d is based on the molecular weight of C16 to 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 with the FAME by the FTIR spectrometer.However the e

6、ffects of these additives are removed by the flow analysisprocessing.NOTE 4FAME concentrations from 150 mg/kg to 500 mg/kg, andbelow 20 mg/kg can be measured but the precision could be affected.1.2 The values stated in SI units are to be regarded asstandard. No other units of measurement are include

7、d 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 applica-bility of regulatory limitations prior to u

8、se.2. Referenced Documents2.1 ASTM Standards:3D1298 Test Method for Density, Relative Density (SpecificGravity), or API Gravity of Crude Petroleum and LiquidPetroleum Products by Hydrometer MethodD1655 Specification for Aviation Turbine FuelsD4052 Test Method for Density, Relative Density, and APIGr

9、avity 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 Petroleum Products andLubricant

10、sD6751 Specification for Biodiesel Fuel Blend Stock (B100)for Middle Distillate FuelsE1655 Practices for Infrared Multivariate QuantitativeAnalysis2.2 ISO Standards:4ISO 4259 Petroleum Products Determination and applica-tion of precision data in relation to methods of test2.3 CEN Standards:4EN 14214

11、 Specification Automotive fuels Fatty acidmethyl esters (FAME) for diesel engines Requirementsand test methods2.4 Energy Institute Standards:5IP 583 Test method for Determination of the fatty acidmethyl esters content of aviation turbine fuel using flowanalysis by Fourier transform infrared spectros

12、copy 1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products and Lubricants and is the direct responsibility of SubcommitteeD02.J0.05 on Fuel Cleanliness.Current edition approved April 15, 2012. Published June 2012. DOI: 10.1520/D7797-122This standard has been develope

13、d 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, visit the ASTM

14、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 York, NY 10036,

15、http:/www.ansi.org.5Available from the Energy Institute, 61 New Cavendish St., London, WIG 7AR,U.K., http:/www.energyinst.org.uk.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States1Rapid screening method2.5 Other Standards:6Defence Standa

16、rd 91-91 Issue 7 (DERD 2494) Turbine Fuel,Aviation Kerosine Type, Jet A12.6 ASTM Adjuncts:7D2PP Determination of Precision and Bias Data for Use inTest Methods for Petroleum Products3. Terminology3.1 Definitions:3.1.1 FAME, nFatty acid methyl esters, also known asbiodiesel.3.1.1.1 DiscussionUsed as

17、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 Fourier Transform Infrared technique uses a flow-through measurement cell

18、 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 arecompared to enable the amount of FAME present in theaviation fuel to

19、 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 specimen of aviation turbine (AVTUR) fuel isautomatically analyzed, by an F

20、TIR 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 differences of the IR spectra, between the measure-ments, are processed in conjun

21、ction with a PLS-1 model todetermine the presence and amplitude of the carbonyl peak ofFAME at approximately 1749 cm-1. Test time is typically 20min. The flow analysis by FTIR enables the effects of potentialinterferences to be removed by using their relative retardancetimes through the sorbent in c

22、onjunction with their absorbanceat 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-effect of leading to potentialFAME contamination of jet turbine fuel in m

23、ultifuel 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 recommended due toconcerns over the difficulty in removing all traces of

24、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 of 10 to 20 % of the container volume. Each6Available from Procurement

25、 Executive DF5 (air), Ministry of Defence,www.dstan.mod.uk.7ADJD6300 is no longer available from ASTM International Headquarters.8The following reagents and materials were used to develop the precisionstatements: Seta Verification and Calibration fluids for Seta FIJI, Stanhope-Seta,Chertsey, Surrey,

26、 KT16 8AP, UK. This is not an endorsement or certification byASTM.D7797 122rinse shall include closing and shaking the container for aminimum of 5 s and then draining the product.9. Preparation of Apparatus9.1 Follow the manufacturers instructions and on-screeninstructions for the correct set up and

27、 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 lint free cloth(7.4) before commencing a test.9.4 Ensure that the verif

28、ication 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 (6.4) if the density is not known.9.7 Use a new test specimen container

29、, 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.NOTE 6New specimen containers are strongly recommended due toconcerns o

30、ver 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 validity of the verification fluidsto be used.10.1.2 Verify the correct

31、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 control requirements.10.1.3 Verify the correct operation of the instrument us

32、ingboth 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 the uncertaintyof the verification fluids certified value or within the

33、 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 at 100 or30 mg/kg, respectively.10.1.5 If it is not possible to meet the crite

34、ria 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 instructions when it is not possible to meet the criteriain 10.1.4 to verify

35、the correct operation of the instrument.10.2.1.1 Calibration uses 5 calibration standards (7.3) cov-ering the scope of the test method, containing known amounts(mg/kg) of FAME in a known fluid.11. Procedure (see Fig. 1)11.1 Commence the test measurement sequence (see Sec-tion 9), and input the sampl

36、e density in kg/m3and sampleidentification in accordance with the manufacturers instruc-tions and the on-screen instructions.NOTE 8If the density of the aviation fuel is not known, a nominalvalue of 807.5 kg/m3is assumed. This could affect the result by amaximum of 4 %.11.2 Insert a new sorbent cart

37、ridge (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 50 mL of sample into the testspecimen container (A1.1.4), that has been prepared as de-scribed in 9.7, loca

38、te 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 following automaticsequences as the test specimen is drawn through the instrumentby the programmed pump: (see Fi

39、g. 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 to obtain a reference spectrum.11.5.3 Measure the spectra of the output from the sorbentcartridge until a s

40、table 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 analysis spectra (see11.5.3) with the reference spectrum and determines the FAMEFIG. 1 Test SequenceD7797 123pea

41、k amplitude using a PLS-1 model (see A1.1.10) over thenominal 1660 cm-1to 1800 cm-1range.11.5.6 Calculate the FAME concentration in mg/kg usingthe calibration curve, the determined peak, the stored value ofthe calibrant materials density and the samples density (see9.6).11.5.7 Flush the system with

42、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 the manufacturersinstructions to remove and dispose of the used sorbent car-tridge and filter.12. Calculatio

43、n12.1FAME mg/kg 5 (Cm) 3 (PcPs) (1)where:Cm= value directly from the integral calibration curvemg/kg,Ps= density of the sample in kg/m3,Pc= density of the calibrant material in kg/m3.Report the amount of FAME in the sample to the nearest 0.1mg/kg.13. Report13.1 The test report shall contain at least

44、 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),13.1.4 Any deviations, by agreement or otherwise, from theprocedures specified, and13.1.5 The time and date of th

45、e test.14. Precision and Bias914.1 GeneralThe precision was obtained from a 2009Energy Institute ILS carried out in Europe using nineinstruments/operators, located in separate laboratories, and asample set comprising 13 aviation turbine fuel samples induplicate blended with known amounts of FAME. Te

46、n sampleswere based on one hydro-treated fuel and three samples werebased on one Merox treated fuel. Initial analysis of the resultsshowed a positive bias with three of the test samples based onthe Merox fuel. Following the addition of a PLS-1 process, thefull spectrographic data from seven of the p

47、articipating instru-ments in the round robin were recalculated to give new testresults showing a significant reduction in the previouslyobserved positive bias. The precision values given in 12.1 werederived from statistical analysis of these test results. Thecalculated values were validated by tests

48、 on a full sample setfrom the round robin.14.1.1 The precision was obtained by statistical examina-tion of the ILS test results according to Practice D6300 (ISO4259) using ADJD6300 D2PP.14.2 RepeatabilityThe difference between successive testresults obtained by the same operator with the same appara

49、tusunder constant operating 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 0.01921(X 1 150) (2)where X is the average of two results being compared, inmg/kg. See Table 1 for a tabular illustration of precision.14.3 ReproducibilityThe difference between two test re-sults independently obtained by different operators usingdifferent apparatus on nominally identical test material would,in the normal and correct operation of the test met