ASTM D8274-20a

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Designation: D8274 − 20 D8274 − 20a
Standard Test Method for
Determination of Biodiesel (Fatty Acid Methyl Esters)
Content in Diesel Fuel Oil by Portable Rapid Mid-Infrared
Analyzer
This standard is issued under the fixed designation D8274; 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 covers the determination of the content of biodiesel (fatty acid methyl esters (FAME)) in diesel fuel oils for
volume fractions of 0.1 % to 31.0 % by mid-infrared analyzer with a resolution of 0.1 %.
NOTE 1—ASTM and ISO specification fuels falling within the scope of this test method include Specifications: D975 grades No. 1D and No. 2D, D7467,
distillate grades of D396, MIL-DTL-16884, and distillate grades of marine fuel specification ISO 8217.
1.2 The accuracy of this test method is based on the molecular weight of C16 and C18 FAME species.
1.2.1 Discussion—Biodiesel contains a variety of species with different molecular weights. Typical market FAMEs from North
America and Europe, which are predominantly soy, rapeseed, and used cooking oil derived FAME were included in the pilot study.
FAME derived from coconut, which predominantly contains C12, will over-read by approximately 30 %.
1.3 It is not possible to This method cannot distinguish between vegetable oils, animal fats, FAEE, compounds containing carbonyl
groups, and FAME. For more information, see Section 6.
1.4 This test method has interim repeatability precision only, see Section 14 for more information.
1.5 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.6 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.
1.7 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
D02.04.0F on Absorption Spectroscopic Methods.
Current edition approved Aug. 1, 2020Oct. 1, 2020. Published August 2020October 2020. Originally approved in 2019. Last previous edition approved in 20192020 as
D8274 – 19.D8274 – 20. DOI: 10.1520/D8274-20.10.1520/D8274-20A.
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
D8274 − 20a
D86 Test Method for Distillation of Petroleum Products and Liquid Fuels at Atmospheric Pressure
D396 Specification for Fuel Oils
D445 Test Method for Kinematic Viscosity of Transparent and Opaque Liquids (and Calculation of Dynamic Viscosity)
D975 Specification for Diesel Fuel
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
D4307 Practice for Preparation of Liquid Blends for Use as Analytical Standards
D6299 Practice for Applying Statistical Quality Assurance and Control Charting Techniques to Evaluate Analytical Measure-
ment System Performance
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
D7371 Test Method for Determination of Biodiesel (Fatty Acid Methyl Esters) Content in Diesel Fuel Oil Using Mid Infrared
Spectroscopy (FTIR-ATR-PLS Method)
D7467 Specification for Diesel Fuel Oil, Biodiesel Blend (B6 to B20)
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
D7806 Test Method for Determination of Biodiesel (Fatty Acid Methyl Ester) and Triglyceride Content in Diesel Fuel Oil Using
Mid-Infrared Spectroscopy (FTIR Transmission Method)
D7963 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
2.2 ISO Standard:
ISO 8217 Petroleum products—Fuels (class F)—Specifications of marine fuels
2.3 Other Standard:
MIL-DTL-16884 Specification for Naval distillate fuel (NATO designation F76)
3. Terminology
3.1 Definitions—For definitions of terms used in this test method, refer to Terminology D4175.
3.2 Abbreviations:
3.2.1 FAME, n—fatty acid methyl esters
4. Summary of Test Method
4.1 This test method describes a rapid procedure to determine the volume concentration of biodiesel in diesel. The test specimen
is introduced into a liquid cell of a mid-infrared analyzer. The absorbance of the sample is measured in two spectroscopic bands.
-1
The amount of biodiesel is determined by the absorbance in a band which includes 1749 cm , where the carbonyl stretching
-1
frequency is located. The second band, centered around 1890 cm is used to correct for the non-biodiesel matrix of the test
specimen. The test takes less than one minute, including introducing the test specimen and removing the previous test specimen.
5. Significance and Use
5.1 Biodiesel is a fuel commodity primarily used as a blending component with diesel fuel. It is important to check the
concentration of biodiesel in the diesel fuel in order to verify it is within limits or does not exceed the maximum allowable limit.
5.2 This test method is applicable for quality control in the production and distribution of diesel fuel and biodiesel blends.
5.3 This test is simple to run, completed in less than one minute, with no dilution of the test sample, no cleaning solvents are
required, and the analyzer is portable and self-contained.
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D8274 − 20a
6. Interferences
6.1 Undissolved Water and Particulates—Samples containing undissolved water or particulates can result in erroneous results. If
the sample is cloudy or water saturated after it has been equilibrated between 10 °C to 30 °C, filter the sample through a qualitative
filter paper until clear prior to its measurement.
6.2 Vegetable Oils—It is not possible to This method cannot distinguish between vegetable oils, animal fats, and FAME by this
test method. FAME. Measurements of vegetable oils and animal fats will give a similar response as that of FAME.
6.3 Fatty Acid Ethyl Esters (FAEE)—It is not possible to distinguish between FAEE and FAME by this test method. Measurements
of FAEE and animal fats will give a similar response as that of FAME.
6.4 Carbonyl Groups—This method cannot distinguish FAME from compounds containing carbonyl groups, such as aldehydes
and ketones. The results for samples containing volume fractions of these compounds less than 0.1 % would not be affected.
7. Apparatus
7.1 Mid-Infrared Analyzer, comprising of a liquid cell, infrared emitter, detectors, a display, microprocessor, and a sample loading
mechanism.
7.2 The apparatus is further described in Annex A1.
8. Reagents and Materials
8.1 Absorbent paper towel.
8.2 Verification sample, containing a known concentration of FAME between 3 % and 7 % (volume fraction). Refer to Annex A2
on the preparation of verification samples.
8.3 Calibration standards, containing known concentrations of FAME between 0 % and 40 %. Refer to Annex A2 on the
preparation of calibration samples.
9. Sampling
9.1 General Requirements:
9.1.1 Obtain samples using procedures outlined in Practice D4057 or D4177. Do not use “sampling by water displacement.”
FAME is more water-soluble than the hydrocarbon base in a biodiesel blend.
9.1.2 Protect samples from excessive temperatures prior to testing.
9.1.3 Avoid using plastic materials for sampling, and do not use rubber caps or plastic bottles for storage of the sample.
10. Preparation of Apparatus
10.1 Switch on the analyzer.
10.2 Place the inlet tube over a waste container, and empty the analyzer by depressing the fill button.
NOTE 2—During this step, any remaining test specimen is ejected into the waste container.
The sole source of supply of the apparatus, SetaCheck Bio (part number SA5500), 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.
D8274 − 20a
10.3 Allow the fill button to come up slowly. Repeat 10.2 and 10.3 a minimum of three times.
10.4 Wipe the inlet tube with absorbent paper towel (8.1).
11. Calibration and Standardization
11.1 Follow the manufacturer’s instructions to calibrate the analyzer.
11.2 The analyzer is calibrated using calibration standards blended as described in Annex A2.
11.3 Verify the correct operation of the analyzer by testing a verification sample (8.2) at least once per year, and following
recalibration or repair. If a result more than 0.5 % (volume fraction) from the expected is obtained, then follow the manufacturer’s
instructions to recalibrate the analyzer.
11.4 Confirm the in-statistical-control status of the test method each day it is used by measuring the biodiesel concentration of at
least one quality control sample that is similar in composition and matrix to samples routinely analyzed. For details on quality
control sample selection, preparation, testing, and control charting, refer to Practice D6299. Follow the manufacturer’s instructions
if the analyzer is out of statistical control.
12. Procedure
12.1 Allow the samples and analyzer to reach a temperature between 18 °C and 24 °C before analysis.
NOTE 3—The FAME concentration of the sample can be measured with the analyzer and sample in the temperature range 5 °C to 40 °C, but the precision
has not bee
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