ASTM D7797-12
(Test Method)Test Method for Determination of the Fatty Acid Methyl Esters Content of Aviation Turbine Fuel Using Flow Analysis by Fourier Transform Infrared Spectroscopy – Rapid Screening Method
Test Method for Determination of the Fatty Acid Methyl Esters Content of Aviation Turbine Fuel Using Flow Analysis by Fourier Transform Infrared Spectroscopy – Rapid Screening Method
SIGNIFICANCE AND USE
5.1 The present and growing international governmental requirements to add fatty acid methyl esters (FAME) to diesel fuel has had the unintended side-effect of leading to potential FAME contamination of jet turbine fuel in multifuel transport facilities such as cargo tankers and pipelines, and industry wide concerns.
5.2 Analytical methods have been developed with the capability of measuring down to
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 of aviation turbine fuel (AVTUR), in the range of 20 to 150 mg/kg.Note 1—Specifications falling within the scope of this test method are: Specification D1655 and Defence Standard 91-91.Note 2—This test method detects all FAME components, with peak IR absorbance at approximately 1749 cm-1 and C8 to C22 molecules, as specified in standards such as Specification D6751 and EN 14214. The accuracy of the method is based on the molecular weight of C16 to C18 FAME species; the presence of other FAME species with different molecular weights could affect the accuracy.Note 3—Additives such as antistatic agents, antioxidants and corrosion inhibitors are measured with the FAME by the FTIR spectrometer. However the effects of these additives are removed by the flow analysis processing.Note 4—FAME concentrations from 150 mg/kg to 500 mg/kg, and below 20 mg/kg can be measured but the precision could be affected.
1.2 The values stated in SI units 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 responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.
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Standards Content (Sample)
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation: D7797 − 12 AnAmerican National Standard
Standard Test Method for
Determination of the Fatty Acid Methyl Esters Content of
Aviation Turbine Fuel Using Flow Analysis by Fourier
Transform Infrared Spectroscopy – Rapid Screening
1,2
Method
This standard is issued under the fixed designation D7797; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope 2. Referenced Documents
2.1 ASTM Standards:
1.1 This test method specifies a rapid screening method
D1298 Test Method for Density, Relative Density, or API
using flow analysis by Fourier transform infrared (FA-FTIR)
Gravity of Crude Petroleum and Liquid Petroleum Prod-
spectroscopy with partial least squares (PLS-1) processing for
ucts by Hydrometer Method
the determination of the fatty acid methyl ester (FAME)
D1655 Specification for Aviation Turbine Fuels
content of aviation turbine fuel (AVTUR), in the range of 20 to
D4052 Test Method for Density, Relative Density, and API
150 mg/kg.
Gravity of Liquids by Digital Density Meter
NOTE 1—Specifications falling within the scope of this test method are:
D4057 Practice for Manual Sampling of Petroleum and
Specification D1655 and Defence Standard 91-91.
Petroleum Products
NOTE 2—This test method detects all FAME components, with peak IR
-1
absorbance at approximately 1749 cm and C to C molecules, as D4177 Practice for Automatic Sampling of Petroleum and
8 22
specified in standards such as Specification D6751 and EN 14214. The
Petroleum Products
accuracy of the method is based on the molecular weight of C16 to C18
D6300 Practice for Determination of Precision and Bias
FAME species; the presence of other FAME species with different
Data for Use in Test Methods for Petroleum Products and
molecular weights could affect the accuracy.
Lubricants
NOTE3—Additivessuchasantistaticagents,antioxidantsandcorrosion
D6751 Specification for Biodiesel Fuel Blend Stock (B100)
inhibitors are measured with the FAME by the FTIR spectrometer.
However the effects of these additives are removed by the flow analysis for Middle Distillate Fuels
processing.
E1655 Practices for Infrared Multivariate Quantitative
NOTE 4—FAME concentrations from 150 mg/kg to 500 mg/kg, and
Analysis
below 20 mg/kg can be measured but the precision could be affected. 4
2.2 ISO Standards:
1.2 The values stated in SI units are to be regarded as ISO 4259 Petroleum Products – Determination and applica-
tion of precision data in relation to methods of test
standard. No other units of measurement are included in this
standard.
2.3 CEN Standards:
EN 14214 Specification Automotive fuels – Fatty acid
1.3 This standard does not purport to address all of the
methyl esters (FAME) for diesel engines – Requirements
safety concerns, if any, associated with its use. It is the
and test methods
responsibility of the user of this standard to establish appro-
2.4 Energy Institute Standards:
priate safety and health practices and determine the applica-
IP 583 Test method for Determination of the fatty acid
bility of regulatory limitations prior to use.
methyl esters content of aviation turbine fuel using flow
analysis by Fourier transform infrared spectroscopy –
This test method is under the jurisdiction of ASTM Committee D02 on
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Subcommittee D02.J0.05 on Fuel Cleanliness. contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Current edition approved April 15, 2012. Published June 2012. DOI: 10.1520/ Standards volume information, refer to the standard’s Document Summary page on
D7797-12 the ASTM website.
2 4
This standard has been developed through the cooperative effort between Available fromAmerican National Standards Institute (ANSI), 25 W. 43rd St.,
ASTM International and the Energy Institute, London. The IP and ASTM logos 4th Floor, New York, NY 10036, http://www.ansi.org.
imply that theASTM and IPstandards are technically equivalent, but their use does AvailablefromtheEnergyInstitute,61NewCavendishSt.,London,WIG7AR,
not imply that both standards are editorially identical. U.K., http://www.energyinst.org.uk.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D7797 − 12
Rapid screening method however these are complex, and require specialized personnel
and laboratory facilities. This Rapid Screening method has
2.5 Other Standards:
been developed for use in the supply chain by non specialized
Defence Standard 91-91 Issue 7 (DERD 2494)Turbine Fuel,
personnel to cover the range of 20 to 150 mg/kg.
Aviation Kerosine Type, Jet A1
2.6 ASTM Adjuncts:
6. Apparatus
D2PP Determination of Precision and Bias Data for Use in
Test Methods for Petroleum Products 6.1 Automatically controlled, closely integrated, instrument
comprising FTIR spectrometer with a 2–mm effective optical
3. Terminology
path length flow-through cell, computer controlled pump,
sorbent cartridge holder, control and interface electronics, test
3.1 Definitions:
specimen and waste containers, and solenoid valves.
3.1.1 FAME, n—Fatty acid methyl esters, also known as
biodiesel.
6.2 The processing computer can be integrated into the
3.1.1.1 Discussion—Used as a component in automotive
instrument.
dieselfuelandthepotentialsourceofcontaminationinaviation
6.3 This apparatus and the required sorbent cartridge are
turbine fuel due to multi-fuel tankers and pipelines.
described in more detail in Annex A1.
3.2 Definitions of Terms Specific to This Standard:
6.4 Density Measuring Device (optional)—According to
3.2.1 FA-FTIR, n—flow analysis by FourierTransform Infra
Test Methods D1298,or D4052, or equivalent national
red technique uses a flow-through measurement cell to make a
standards, to determine the density of the aviation fuel test
number of measurements on a stream of test specimen.
sample if required.
3.2.1.1 Discussion—The test specimen is analyzed before
and after passing through a sorbent that is designed to retard
7. Reagents and Materials
the FAME contamination to be measured. The results are
7.1 Cleaning Solvent, heptane, reagent grade.
compared to enable the amount of FAME present in the
aviation fuel to be determined.
7.2 Verification Fluids :
7.2.1 100 mg/kg, containing 100 6 10 mg/kg of FAME,
3.2.2 sorbent cartridge, n—a cartridge, through which the
with a certified value and uncertainty.
test specimen flows, containing a specific sorbent
7.2.2 30 mg/kg, containing 30 6 5 mg/kg of FAME, with a
3.2.2.1 Discussion—The sorbent cartridge is discarded after
certified value and uncertainty.
each test.
7.3 Calibration Fluids :
4. Summary of Test Method
7.3.1 Set of Five Fluids, containing amounts of FAME with
4.1 A test specimen of aviation turbine (AVTUR) fuel is
certified values and uncertainty.
automatically analyzed, by an FTIR spectrometer, ina2mm
7.4 Lint-free Cloth,forcleaninganddryingthesampleinput
effective path length flow-through cell, before and after flow-
tube.
ing through a cartridge containing a sorbent designed to have
a relatively long residence time for FAME. The spectroscopic
8. Sampling
absorbance differences of the IR spectra, between the
8.1 Unless otherwise specified, take a sample of at least 60
measurements, are processed in conjunction with a PLS-1
mL in accordance with Practices D4057 or D4177 or in
model to determine the presence and amplitude of the carbonyl
-1
accordance with the requirements of national standards or
peak of FAME at approximately 1749 cm . Test time is
regulations for the sampling of petroleum products, or both.
typically20min.TheflowanalysisbyFTIRenablestheeffects
of potential interferences to be removed by using their relative
8.2 Use new, opaque glass or epoxy lined metal containers
retardance times through the sorbent in conjunction with their with inert closures.
absorbance at specific wavelengths.
8.2.1 Used sample containers are permitted provided it can
beconfirmedtheyhavenotbeenusedforunknownfluidsorfor
5. Significance and Use
fluids containing >5 % FAME.
5.1 The present and growing international governmental
NOTE 5—New sample containers are strongly recommended due to
requirements to add fatty acid methyl esters (FAME) to diesel
concerns over the difficulty in removing all traces of FAME retained from
fuel has had the unintended side-effect of leading to potential previous samples.
FAME contamination of jet turbine fuel in multifuel transport
8.2.2 Rinse all sample containers with heptane (7.1)or
facilitiessuchascargotankersandpipelines,andindustrywide
another suitable solvent and drain. Then rinse with the product
concerns.
to be sampled at least three times. Each rinse shall use product
with a volume of 10 to 20 % of the container volume. Each
5.2 Analytical methods have been developed with the capa-
bility of measuring down to <5 mg/kg levels of FAME,
The following reagents and materials were used to develop the precision
Available from Procurement Executive DF5 (air), Ministry of Defence, statements: Seta Verification and Calibration fluids for Seta FIJI, Stanhope-Seta,
www.dstan.mod.uk. Chertsey, Surrey, KT16 8AP, UK. This is not an endorsement or certification by
ADJD6300 is no longer available from ASTM International Headquarters. ASTM.
D7797 − 12
NOTE 7—In 10.1.4, R is the reproducibility of the test method at 100 or
rinse shall include closing and shaking the container for a
30 mg/kg, respectively.
minimum of 5 s and then draining the product.
10.1.5 If it is not possible to meet the criteria in 10.1.4 to
9. Preparation of Apparatus
verify the correct operation of the instrument, follow the
manufacturer’s instructions regarding fault finding and calibra-
9.1 Follow the manufacturer’s instructions and on-screen
tion.
instructions for the correct set up and shut down of the
apparatus.
10.2 Calibration:
10.2.1 Calibrate the instrument according to the manufac-
9.2 Run a flushing sequence using heptane (7.1) in accor-
turer’s instructions when it is not possible to meet the criteria
dance with the manufacturer’s instructions if the last test
in 10.1.4 to verify the correct operation of the instrument.
sample contained FAME in excess of 150 mg/kg.
10.2.1.1 Calibration uses 5 calibration standards (7.3) cov-
9.3 Wipe dry the sample input tube with a lint free cloth
ering the scope of the test method, containing known amounts
(7.4) before commencing a test.
(mg/kg) of FAME in a known fluid.
9.4 Ensure that the verification and calibration of the instru-
ment are in accordance with Section 10.
11. Procedure (see Fig. 1)
9.5 Gently swirl the sample for homogeneity before draw-
11.1 Commence the test measurement sequence (see Sec-
ing the test specimen.
tion 9), and input the sample density in kg/m and sample
identification in accordance with the manufacturer’s instruc-
9.6 Determine the density of the sample using the density
tions and the on-screen instructions.
measuring device (6.4) if the density is not known.
NOTE 8—If the density of the aviation fuel is not known, a nominal
9.7 Use a new test specimen container, or if there is enough 3
value of 807.5 kg/m is assumed. This could affect the result by a
test sample available it is permissible to clean and dry the test
maximum of 4 %.
specimen container thoroughly before each test using heptane
11.2 Insert a new sorbent cartridge (A1.1.3) and attach a
and then partially fill with the test sample, swirl and drain,
new filter (A1.1.9) to the exit (bottom) of the sorbent cartridge;
repeat three times.
follow the manufacturer’s instructions to fit the input tube to
NOTE 6—New specimen containers are strongly recommended due to
the cartridge.
concerns over the difficulty in removing all traces of FAME retained from
previous test specimens.
11.3 Pour approximately 50 mL of sample into the test
specimen container (A1.1.4), that has been prepared as de-
10. Calibration and Standardization
scribed in 9.7, locate in position and attach the container lid
10.1 Verification:
and sample input tube.
10.1.1 Follow the apparatus and test specimen preparation
11.4 Ensure that an empty waste container, lid and output
instructions (9) and check the validity of the verification fluids
tube (A1.1.5) are in position.
to be used.
11.5 Start the test to commence the following automatic
10.1.2 Verify the correct operation of the instrument using
sequencesasthetestspecimenisdrawnthroughtheinstrument
the verification fluid (7.2.1), in accordance with the manufac-
by the programmed pump: (see Fig. 1 and Fig. A1.1):
turer’s instructions, at least every six months. More frequent
11.5.1 Prime and flush the tubing and the flow-through
performance checks shall be carried out according to local
measurement cell with the test specimen.
quality control requirements.
11.5.2 Measure the spectrum of the test specimen to check
10.1.3 Verify the correct operation of the instrument using
for contamination and to obtain a reference spectrum.
both verification fluids (7.2.1 and 7.2.2) in accordance with the
11.5.3 Measure the spectra of the output from the sorbent
manufacturer’s instructions at least every 12 months or imme-
diately after any maintenance on the measurement system. cartridge until a stable value is reached and compares with the
reference spectrum.
10.1.4 If the result is not within R/√2 plus the uncertainty of
the verification fluid’s certified value or within the tolerances 11.5.4 Re-measure the spectrum of the test specimen to
supplied with the verification fluid, recheck the validity date of obtain a second reference spectrum.
the verification fluid and run a flushing sequence (9.2) and 11.5.5 Analyze and compare the flow analysis spectra (see
repeat the verification. 11.5.3) with the reference spectrum and determines the FAME
FIG. 1 Test Sequence
D7797 − 12
peak amplitude using a PLS-1 model (see A1.1.10) over the the Merox fuel. Following the addition of a PLS-1 process, the
-1 -1
nominal 1660 cm to 1800 cm range. full spectrographic data from seven of the participating instru-
11.5.6 Calculate the FAME concentration in mg/kg using ments in the round robin were recalculated to give new test
the calibration curve, the determined peak, the stored value of results showing a significant reduction in the previously
the calibrant material’s density and the sample’s density (see observedpositivebias.Theprecisionvaluesgivenin12.1were
9.6). derived
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