ASTM D7963-22

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Designation: D7963 − 21 D7963 − 22
Standard Test Method for
Determination of Contamination Level of Fatty Acid Methyl
Esters in Middle Distillate and Residual Fuels Using Flow
Analysis by Fourier Transform Infrared Spectroscopy—
Rapid Screening Method
This standard is issued under the fixed designation D7963; 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*
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) processing for the quantitative determination of the fatty acid methyl ester (FAME)
contamination of middle distillates, in the range of 20 mg ⁄kg to 1000 mg ⁄kg, and of middle distillates and residual fuels, following
dilution, for levels above 0.1 %.
NOTE 1—Annex A2 describes a dilution procedure to significantly expand the measurement range above 1000 mg/kg for distillates and to enable
measurement of residual oils
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NOTE 2—This test method detects all FAME components, with peak IR absorbance at approximately 1749 cm and C to C molecules, as specified
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in standards such as D6751 and EN 14214. The accuracy of the test method is based on the molecular mass of C to C FAME species; the presence
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of other FAME species with different molecular masses 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 any
potential interference effects of these additives are eliminated by the flow analysis processing.
NOTE 4—The scope of this test method does not include aviation turbine fuel which is addressed by Test Method D7797.
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, health, and environmental practices and determine the applicability of
regulatory limitations prior to use.
1.4 This international standard was developed in accordance with internationally recognized principles on standardization
established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued
by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
2. Referenced Documents
2.1 ASTM Standards:
This test method is under the jurisdiction of ASTM Committee D02 on Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of Subcommittee
D02.14 on Stability, Cleanliness and Compatibility of Liquid Fuels.
Current edition approved Oct. 15, 2021Dec. 1, 2022. Published November 2021December 2022. Originally approved in 2014. Last previous edition approved in 20192021
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as D7963 – 19D7963 – 21. . DOI: 10.1520/D7963-21.10.1520/D7963-22.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
*A Summary of Changes section appears at the end of this standard
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D7963 − 22
D1298 Test Method for Density, Relative Density, or API Gravity of Crude Petroleum and Liquid Petroleum Products by
Hydrometer Method
D4052 Test Method for Density, Relative Density, and API Gravity of Liquids by Digital Density Meter
D4057 Practice for Manual Sampling of Petroleum and Petroleum Products
D4175 Terminology Relating to Petroleum Products, Liquid Fuels, and Lubricants
D4177 Practice for Automatic Sampling of Petroleum and Petroleum Products
D6300 Practice for Determination of Precision and Bias Data for Use in Test Methods for Petroleum Products, Liquid Fuels, and
Lubricants
D6751 Specification for Biodiesel Fuel Blend Stock (B100) for Middle Distillate Fuels
D7797 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
E1655 Practices for Infrared Multivariate Quantitative Analysis
2.2 CEN Standard:
EN 14214 Automotive Fuels—Fatty Acid Methyl Esters (FAME) for Diesel Engines—Requirements and Test Methods
2.3 Energy Institute Standards:
IP 583 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
2.4 Other Standards:
MIL-DTL-16884 Specification for Fuel, Naval Distillate
3. Terminology
3.1 Definitions:
3.1.1 For definitions of terms used in this test method, refer to Terminology D4175.
3.1.2 FAME, n—fatty acid methyl esters, also known as biodiesel.
3.1.2.1 Discussion—
Used as a component in automotive diesel fuel and the potential source of contamination in fuels due to multi-fuel tankers and
pipelines.
3.2 Definitions of Terms Specific to This Standard:
3.2.1 FA-FTIR, n—flow analysis by Fourier Transform Infrared technique uses a flow-through measurement cell to make a number
of measurements on a stream of test specimen.
3.2.1.1 Discussion—
The test specimen is analyzed before and after passing through a sorbent that is designed to retard the FAME contamination to be
measured. The results are compared to enable the amount of FAME present in the fuel to be determined.
3.2.2 sorbent cartridge, n—a cartridge through which the test specimen flows, containing a specific sorbent.
3.2.2.1 Discussion—
The sorbent cartridge is discarded after each test.
4. Summary of Test Method
4.1 The test specimen is automatically analyzed, by an FTIR spectrometer, in a 2 mm effective path length flow-through cell,
before and after flowing through a cartridge containing a sorbent designed to have a relatively long residence time for FAME.
4.2 The spectroscopic absorbance differences of the IR spectra, between the measurements, are processed in conjunction with a
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PLS-1 model to determine the presence and amplitude of the carbonyl peak of FAME at approximately 1749 cm .
4.3 The flow analysis by FTIR enables the effects of potential interferences to be removed by using their relative retardance times
through the sorbent in conjunction with their absorbance at specific wavelengths.
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4.4 Test time is typically less than 20 min.
5. 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 fuels in multi-fuel transport facilities such as cargo
tankers and pipelines, and industry wide concerns. This has led to a requirement to measure contamination levels in diesel and other
fuels to assist custody transfer issues.
5.2 Analytical methods have been developed with the capability of measuring down to <5 mg/kg levels of FAME in aviation
turbine fuel (AVTUR), however these are complex, and require specialized personnel and laboratory facilities. This Rapid
Screening method has been developed for use in the supply chain by non-specialized personnel to cover the range of 20 mg ⁄kg to
500 000 mg ⁄kg (0.002 % to 50 %).
5.3 A similar procedure, Test Method D7797, is available for AVTUR in the range 10 mg/kg to 150 mg ⁄kg. Test Method D7797
uses the same apparatus, with a specific model developed for AVTUR.
6. Apparatus
6.1 Automatically controlled, closely integrated instrument comprising a FTIR spectrometer with a 2 mm effective optical path
length flow-through cell, computer controlled pump, sorbent cartridge holder, control and interface electronics, test specimen and
waste containers, and solenoid valves.
6.2 The processing computer can be integrated into the instrument.
6.3 This apparatus and the required sorbent cartridge are described in more detail in Annex A1.
6.4 Density measuring device (optional), according to Test Methods D1298 or D4052 or equivalent national standards, to
determine the density of the test specimen if required.
7. Reagents and Materials
7.1 Cleaning Solvent—heptane, reagent grade.
7.2 Verification Fluids:
7.2.1 100 mg/kg—containing 100 mg ⁄kg 6 10 mg/kg of FAME, with a certified value and uncertainty.
7.2.2 30 mg/kg—containing 30 mg/kg 6 5 mg/kg of FAME, with a certified value and uncertainty.
7.2.3 400 mg/kg—containing 400 mg/kg 6 40 mg/kg of FAME, with a certified value and uncertainty.
7.2.4 900 mg/kg—containing 900 mg/kg 6 90 mg/kg of FAME, with a certified value and uncertainty.
7.3 Calibration Fluids:
7.3.1 A Set of Nine Fluids—containing amounts of FAME with certified values and uncertainty.
7.4 Lint-free Cloth—for cleaning and drying the sample input tube.
The following reagents and materials were used to develop the precision statements: Seta Verification and Calibration fluids for Seta FIJI. Stanhope-Seta, Chertsey, Surrey,
KT16 8AP, UK. This is not an endorsement or certification by ASTM. The sole source of supply of Seta Verification and Calibration fluids for Seta FIJI known to the
committee at this time is Stanhope-Seta, Chertsey, Surrey, KT16 8AP, UK. If you are aware of alternative suppliers, please provide this information to ASTM International
Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend.
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7.5 Diluent—for diluting the test sample when the FAME content is >1000 mg/kg (See Annex A2).
7.6 Sorbent Cartridge —see Fig. A1.2, individually packed in a sealed envelope, one per test.
8. Sampling
8.1 Unless otherwise specified, take a sample of at least 60 mL in accordance with Practices D4057 or D4177, and/or in
accordance with the requirements of national standards or regulations for the sampling of petroleum products.
8.2 Use new opaque glass or epoxy-lined metal containers with inert closures.
8.2.1 Used sample containers are permitted provided it can be confirmed they have not been used for unknown fluids or for fluids
containing >5 % FAME.
8.2.1.1 New sample containers are strongly recommended due to concerns over the difficulty in removing all traces of FAME
retained from previous samples.
8.2.2 Rinse all sample containers with heptane (7.1) or another suitable solvent and drain. Then rinse with the product to be
sampled at least three times. Each rinse shall use product with a volume of 10 % to 20 % of the container volume. Each rinse shall
include closing and shaking the container for a minimum of 5 s and then draining the product.
9. Apparatus and Sample Preparation
9.1 Follow the manufacturer’s instructions and on-screen instructions for the correct set-up and shut-down of the apparatus.
9.2 Run a flushing sequence using heptane (7.1) in accordance with the manufacturer’s instructions if the last test sample contained
FAME in excess of 1000 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 verification and calibration of the instrument are in accordance with Section 10.
9.5 Gently swirl the middle distillate sample for homogeneity before drawing the test specimen. For residual fuels, warm the
sample up to 50 °C and agitate the sample to provide mixing, such as orbiting the container horizontally.
9.6 If the expected concentration of FAME is >1000 mg/kg or the sample is residual fuel, follow Annex A2 to dilute the sample.
9.7 Determine the density of the middle distillate sample using the density measuring device (6.4) if the density is not known. For
samples previously diluted according to Annex A2, determine the density of the diluted sample using the density measuring device
(6.4) if the density is not known.
9.8 Use a new test specimen container, or if there is enough test sample available, it is permissible to clean and dry the test
specimen container thoroughly before each test using heptane and then partially fill with the test sample, swirl and drain. Repeat
three times.
NOTE 5—New specimen containers are strongly recommended due to concerns over the difficulty in removing all traces of FAME retained from previous
test specimens.
10. Calibration and Standardization
10.1 Verification:
The sole source of supply of the apparatus known to the committee at this time is Seta FIJI and cartridge (including filter) available from Stanhope-Seta, Chertsey, Surrey,
KT16 8AP, UK. If you are aware of alternative suppliers, please provide this information to ASTM International Headquarters. Your comments will receive careful
consideration at a meeting of the responsible technical committee, which you may attend.
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10.1.1 Follow the apparatus and test specimen preparation instructions (see Section 9) and check the validity of the verification
fluids to be used.
10.1.2 Ver
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