1、Designation: D7797 16aD7797 17 An American National Standard583583/15Standard 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 desi
2、gnation D7797; 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
3、or reapproval.1. Scope*1.1 This test method specifies a rapid screening method using flow analysis by Fourier transform infrared (FA-FTIR)spectroscopy with partial least squares (PLS-1) processing for the determination of the fatty acid methyl ester (FAME) content ofaviation turbine fuel (AVTUR), in
4、 the range of 10 mgkg to 150 mgkg.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 IR absorbance at approximately 1749 cm-1 and C8 to C22 molecules, as specifiedin stand
5、ards such as Specification D6751 and EN 14214. The accuracy of the method is based on the molecular weight of C16 to C18 FAME species; thepresence of other FAME species with different molecular weights could affect the accuracy.NOTE 3Additives such as antistatic agents, antioxidants and corrosion in
6、hibitors are measured with the FAME by the FTIR spectrometer. Howeverthe effects of these additives are removed by the flow analysis processing.NOTE 4FAME concentrations from 150 mg/kg to 500 mg/kg, and below 10 mg/kg can be measured but the precision could be affected.1.2 The values stated in SI un
7、its are to be regarded as standard. No other units of measurement are included in this standard.1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibilityof the user of this standard to establish appropriate safety and health p
8、ractices and determine the applicability of regulatorylimitations prior to use.1.4 This international standard was developed in accordance with internationally recognized principles on standardizationestablished in the Decision on Principles for the Development of International Standards, Guides and
9、 Recommendations issuedby the World Trade Organization Technical Barriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:3D1298 Test Method for Density, Relative Density, or API Gravity of Crude Petroleum and Liquid Petroleum Products byHydrometer MethodD1655 Specification for Av
10、iation Turbine FuelsD4052 Test Method for Density, Relative Density, and API Gravity of Liquids by Digital Density MeterD4057 Practice for Manual Sampling of Petroleum and Petroleum ProductsD4177 Practice for Automatic Sampling of Petroleum and Petroleum ProductsD6300 Practice for Determination of P
11、recision and Bias Data for Use in Test Methods for Petroleum Products and LubricantsD6751 Specification for Biodiesel Fuel Blend Stock (B100) for Middle Distillate FuelsE1655 Practices for Infrared Multivariate Quantitative Analysis1 This test method is under the jurisdiction ofASTM Committee D02 on
12、 Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of SubcommitteeD02.J0.05 on Fuel Cleanliness.Current edition approved Oct. 1, 2016May 1, 2017. Published October 2016June 2017. Originally approved in 2012. Last previous edition approved in 2016 asD7797 16.D7797 16a.
13、 DOI: 10.1520/D7797-16A.10.1520/D7797-17.2 This standard has been developed through the cooperative effort between ASTM International and the Energy Institute, London. The IP and ASTM logos imply that theASTM and IP standards are technically equivalent, but their use does not imply that both standar
14、ds are editorially identical.3 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM website.This document is not an ASTM sta
15、ndard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Becauseit may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cas
16、es only the current versionof the standard as published by ASTM is to be considered the official document.*A Summary of Changes section appears at the end of this standardCopyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States12.2 CEN Standar
17、ds:4EN 14214 Specification Automotive FuelsFatty Acid Methyl Esters (FAME) for Diesel EnginesRequirements and TestMethods2.3 Energy Institute Standards:5IP 583 Test Method for Determination of the Fatty Acid Methyl Esters Content of Aviation Turbine Fuel Using Flow Analysisby Fourier Transform Infra
18、red SpectroscopyRapid Screening Method2.4 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 Bias Data for Use in Test Methods for Petroleum Products3. Terminology3.1 Definitions:3.
19、1.1 FAME, nFatty acid methyl esters, also known as biodiesel.3.1.1.1 DiscussionUsed as a component in automotive diesel fuel and the potential source of contamination in aviation turbine fuel due to multi-fueltankers and pipelines.3.2 Definitions of Terms Specific to This Standard:3.2.1 FA-FTIR, nfl
20、ow analysis by Fourier Transform Infra red 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 before and after passing through a sorbent that is designed to retard the FAME contamination to bemea
21、sured. The results are compared to enable the amount of FAME present in the aviation fuel to be determined.3.2.2 sorbent cartridge, na cartridge, through which the test specimen flows, containing a specific sorbent3.2.2.1 DiscussionThe sorbent cartridge is discarded after each test.4. Summary of Tes
22、t Method4.1 A test specimen of aviation turbine (AVTUR) fuel is automatically analyzed, by an FTIR spectrometer, in a 2 mm effectivepath length flow-through cell, before and after flowing through a cartridge containing a sorbent designed to have a relatively longresidence time for FAME. The spectros
23、copic absorbance differences of the IR spectra, between the measurements, are processedin conjunction with a PLS-1 model to determine the presence and amplitude of the carbonyl peak of FAME at approximately 1749cm-1. Test time is typically 20 min. The flow analysis by FTIR enables the effects of pot
24、ential interferences to be removed by usingtheir relative retardance times through the sorbent in conjunction with their absorbance at specific wavelengths.5. Significance and Use5.1 The present and growing international governmental requirements to add fatty acid methyl esters (FAME) to diesel fuel
25、 hashad the unintended side-effect of leading to potential FAME contamination of jet turbine fuel in multifuel transport facilities suchas cargo tankers and pipelines, and industry wide concerns.5.2 Analytical methods have been developed with the capability of measuring down to 5 % FAME.NOTE 5New sa
26、mple containers are strongly recommended due to concerns over the difficulty in removing all traces of FAME retained from previoussamples.8.2.2 Rinse all sample containers with heptane (7.1) or another suitable solvent and drain. Then rinse with the product to besampled at least three times. Each ri
27、nse shall use product with a volume of 10 % to 20 % of the container volume. Each rinse shallinclude closing and shaking the container for a minimum of 5 s and then draining the product.9. Preparation of Apparatus9.1 Follow the manufacturers instructions and on-screen instructions for the correct se
28、t up and shut down of the apparatus.9.2 Run a flushing sequence using heptane (7.1) in accordance with the manufacturers instructions if the last test samplecontained FAME in excess of 150 mgkg.9.3 Wipe dry the sample input tube with a lint free cloth (7.4) before commencing a test.9.4 Ensure that t
29、he verification and calibration of the instrument are in accordance with Section 10.9.5 Gently swirl the sample for homogeneity before drawing the test specimen.9.6 Determine the density of the sample using the density measuring device (6.4) if the density is not known.9.7 Use a new test specimen co
30、ntainer, or if there is enough test sample available it is permissible to clean and dry the testspecimen container thoroughly before each test using heptane and then partially fill with the test sample, swirl and drain, repeatthree times.NOTE 6New specimen containers are strongly recommended due to
31、concerns 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 preparation instructions (9) and check the validity of the verification fluids to beused.10.1.2 Verify t
32、he correct operation of the instrument using the verification fluid (7.2.1), in accordance with the manufacturersinstructions, at least every six months. More frequent performance checks shall be carried out according to local quality controlrequirements.8 The following reagents and materials were u
33、sed to develop the precision statements: SetaVerification and Calibration fluids for Seta FIJI, Stanhope-Seta, Chertsey, Surrey,KT16 8AP, UK. This is not an endorsement or certification by ASTM.D7797 17310.1.3 Verify the correct operation of the instrument using both verification fluids (7.2.1 and 7
34、.2.2) in accordance with themanufacturers instructions at least every 12 months or immediately after any maintenance on the measurement system.10.1.4 If the result is not within R/2 plus the uncertainty of the verification fluids certified value or within the tolerancessupplied with the verification
35、 fluid, recheck the validity date of the verification fluid and run a flushing sequence (9.2) and repeatthe verification.NOTE 7In 10.1.4, R is the reproducibility of the test method at 100 mg kg or 30 mg kg, respectively.10.1.5 If it is not possible to meet the criteria in 10.1.4 to verify the corre
36、ct operation of the instrument, follow themanufacturers instructions regarding fault finding and calibration.10.2 Calibration:10.2.1 Calibrate the instrument according to the manufacturers instructions when it is not possible to meet the criteria in 10.1.4to verify the correct operation of the instr
37、ument.10.2.1.1 Calibration uses five (5) calibration standards (7.3) covering 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 Section 9), and input the sample density in kilograms per cu
38、bic metre(kg/m3) and sample identification in accordance with the manufacturers instructions and the on-screen instructions.NOTE 8If the density of the aviation fuel is not known, a nominal value of 807.5 kg m3 is assumed. This could affect the result by a maximum of4 %.11.2 Insert a new sorbent car
39、tridge (A1.1.3) and attach a new filter (A1.1.9) to the exit (bottom) of the sorbent cartridge; followthe manufacturers instructions to fit the input tube to the cartridge.11.3 Pour approximately 50 mL of sample into the test specimen container (A1.1.4), that has been prepared as described in 9.7,lo
40、cate in position and attach the container lid and sample input tube.11.4 Ensure that an empty waste container, lid and output tube (A1.1.5) are in position.11.5 Start the test to commence the following automatic sequences as the test specimen is drawn through the instrument by theprogrammed pump: (s
41、ee Fig. 1 and Fig. A1.1):11.5.1 Prime and flush the tubing and the flow-through measurement cell with the test specimen.11.5.2 Measure the spectrum of the test specimen to check for contamination and to obtain a reference spectrum.11.5.3 Measure the spectra of the output from the sorbent cartridge u
42、ntil a stable value is reached and compares with thereference spectrum.11.5.4 Re-measure the spectrum of the test specimen to obtain a second reference spectrum.11.5.5 Analyze and compare the flow analysis spectra (see 11.5.3) with the reference spectrum and determines the FAME peakamplitude using a
43、 PLS-1 model (see A1.1.10) over the nominal 1660 cm-1 to 1800 cm-1 range.11.5.6 Calculate the FAME concentration in mg/kg using the calibration curve, the determined peak, the stored value of thecalibrant materials density and the samples density (see 9.6).11.5.7 Flush the system with the remainder
44、of the test specimen and finally purges with air.11.5.8 Display the result numerically and graphically (see Fig. A1.1 for a typical example).11.6 Record the test result and follow the manufacturers instructions to remove and dispose of the used sorbent cartridge andfilter.12. Calculation12.1FAME mg/
45、kg5Cm! 3Pc Ps! (1)where:Cm = value directly from the integral calibration curve mg/kg,FIG. 1 Test SequenceD7797 174Ps = 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 0.1 mgkg.13. Report13.1 The test report shall
46、contain at least the following information:13.1.1 A reference to this standard,13.1.2 All details necessary for complete identification of the product tested,13.1.3 The result of the test (see Section 12),13.1.4 Any deviations, by agreement or otherwise, from the procedures specified, and13.1.5 The
47、time and date of the test.14. Precision and Bias914.1 GeneralThe precision was obtained from a 2013 Energy Institute ILS carried out in Europe using eight instruments/operators, located in separate laboratories, and a sample set comprising 13 aviation turbine fuel samples in duplicate blended withkn
48、own amounts of FAME. Samples included hydro-treated fuel, non-hydro-treated fuel, and synthetic fuel and were sourced fromthe U.S., U.K., and Europe. The precision values given in 12.1 were derived from statistical analysis of these test results.14.1.1 The precision was obtained by statistical exami
49、nation of the ILS test results according to Practice D6300 usingADJD6300 D2PP.14.2 RepeatabilityThe difference between successive test results obtained by the same operator with the same apparatus underconstant operating conditions on nominally identical test material would, in the normal and correct operation of the test method,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 results independently obtained by diffe
