Standard Test Method for Separation and Determination of Aromatics, Nonaromatics, and FAME Fractions in Middle Distillates by Solid-Phase Extraction and Gas Chromatography

SIGNIFICANCE AND USE
5.1 For the middle distillates whose boiling range is between 170 °C and 400 °C by such distillation methods like Test Method D2887, Procedure A can separate and determine the content of total aromatics and total nonaromatics by SPE and GC analysis of the resulting fractions. The determination of the total content of saturates and aromatics in petroleum middle distillates is useful to investigate the effects of petroleum processes on production of various finished fuels.  
5.2 The total aromatics content and polycyclic aromatics content are important to characterize the quality of diesel fuels. This test method is demonstrated to be time-saving and eco-friendly by reducing the amount of reagent consumption and avoiding the necessity of solvent evaporation step as required, for example, in such Test Method D2549.  
5.3 The determination of detailed hydrocarbon composition by mass spectrometry requires a preliminary separation of the sample into representative aromatics and nonaromatics, as in Test Method D2425, where Test Method D2549 is used to separate the distillate fuel. The SPE fractionation procedure described herein may provide a suitable fractionation alternative approach for these mass spectrometric types of methods.  
5.4 Biodiesel is a blendstock commodity primarily used as a value-added blending component with diesel fuel. Procedure B can provide a separation and determination technique to monitor the FAME content for FAME biodiesel blends.
SCOPE
1.1 This test method covers the separation and determination of representative aromatics, nonaromatics, and fatty acid methyl ester (FAME) fractions in middle distillates that boil between 170 °C and 400 °C, including biodiesel blends with up to 20 % by volume of FAME, by solid phase extraction and gas chromatography.  
1.2 This test method provides two procedures, A and B. Procedure A is applicable to the petroleum-based middle distillates fuel, and Procedure B is applicable to the biodiesel blends with up to 20 % by volume of FAME.  
1.3 This test method is applicable to middle distillates samples with aromatics content ranging from 5 % to 50 % by mass and biodiesel blends with FAME content in the range of 0.5 % to 20 % by volume. This test method may apply to concentrations outside these ranges, but the precision has not been determined.  
1.4 For Procedure B, biodiesels in the form of fatty acid ethyl ester (FAEE) can also fully elute into the FAME fraction, and they have the similar FID (flame ionization detector) relative response factors with that of FAME. The determined content of FAME fractions are the sum of concentrations of FAME and FAEE by this test method (see 3.2.5).  
1.5 From the investigation results obtained for FAME determination, the low concentrations of monoglycerides (usually less than 0.5 % by mass in biodiesel blends) are not detectable under the gas chromatographic (GC) condition of this test method and will not interfere with the determination of FAME by Procedure B. As a result, biodiesel blends, conforming to the requirements of Specification D7467, containing up to 20 % by volume of biodiesel blendstock meeting the requirements in Specification D6751, typically contain concentrations of monoglycerides of less than 0.1 % by mass. The diglycerides and triglycerides, if present, are not detected under the GC condition of this test method due to their higher boiling points.
Note 1: If a sample is suspected of containing an abnormal FAME biodiesel feedstock than specified in Specification D6751, for example, a sample contaminated with vegetable oil with a high level of total triglycerides, the content of mono-, di-, or tri-glycerides in the isolated FAME fraction may be determined using Test Method D6584. Samples containing biodiesels with a high amount of glycerides than specified in Specification D6751 may contaminate the GC column and not recommended for this test method.  
1.6 The values stated in a...

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ASTM D8144-22 - Standard Test Method for Separation and Determination of Aromatics, Nonaromatics, and FAME Fractions in Middle Distillates by Solid-Phase Extraction and Gas Chromatography
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Standards Content (Sample)

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.
Designation: D8144 − 22
Standard Test Method for
Separation and Determination of Aromatics, Nonaromatics,
and FAME Fractions in Middle Distillates by Solid-Phase
1
Extraction and Gas Chromatography
This standard is issued under the fixed designation D8144; 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* diglyceridesandtriglycerides,ifpresent,arenotdetectedunder
the GC condition of this test method due to their higher boiling
1.1 This test method covers the separation and determina-
points.
tion of representative aromatics, nonaromatics, and fatty acid
NOTE 1—If a sample is suspected of containing an abnormal FAME
methyl ester (FAME) fractions in middle distillates that boil
biodiesel feedstock than specified in Specification D6751, for example, a
between170 °Cand400 °C,includingbiodieselblendswithup
sample contaminated with vegetable oil with a high level of total
to20 %byvolumeofFAME,bysolidphaseextractionandgas
triglycerides, the content of mono-, di-, or tri-glycerides in the isolated
FAME fraction may be determined using Test Method D6584. Samples
chromatography.
containing biodiesels with a high amount of glycerides than specified in
1.2 This test method provides two procedures, A and B.
Specification D6751 may contaminate the GC column and not recom-
Procedure A is applicable to the petroleum-based middle mended for this test method.
distillates fuel, and Procedure B is applicable to the biodiesel
1.6 The values stated in acceptable SI units are to be
blends with up to 20 % by volume of FAME.
regarded as the standard. No other units of measurement are
included in this standard
1.3 This test method is applicable to middle distillates
samples with aromatics content ranging from 5 % to 50 % by
1.7 This standard does not purport to address all of the
mass and biodiesel blends with FAME content in the range of
safety concerns, if any, associated with its use. It is the
0.5 % to 20 % by volume. This test method may apply to
responsibility of the user of this standard to establish appro-
concentrations outside these ranges, but the precision has not
priate safety, health, and environmental practices and deter-
been determined.
mine the applicability of regulatory limitations prior to use.
1.8 This international standard was developed in accor-
1.4 For Procedure B, biodiesels in the form of fatty acid
dance with internationally recognized principles on standard-
ethyl ester (FAEE) can also fully elute into the FAME fraction,
ization established in the Decision on Principles for the
and they have the similar FID (flame ionization detector)
Development of International Standards, Guides and Recom-
relative response factors with that of FAME. The determined
mendations issued by the World Trade Organization Technical
content of FAME fractions are the sum of concentrations of
Barriers to Trade (TBT) Committee.
FAME and FAEE by this test method (see 3.2.5).
1.5 From the investigation results obtained for FAME
2. Referenced Documents
determination, the low concentrations of monoglycerides (usu-
2
2.1 ASTM Standards:
ally less than 0.5 % by mass in biodiesel blends) are not
D2425 Test Method for Hydrocarbon Types in Middle Dis-
detectable under the gas chromatographic (GC) condition of
tillates by Mass Spectrometry
thistestmethodandwillnotinterferewiththedeterminationof
D2549 Test Method for Separation of Representative Aro-
FAME by Procedure B.As a result, biodiesel blends, conform-
matics and Nonaromatics Fractions of High-Boiling Oils
ing to the requirements of Specification D7467, containing up
by Elution Chromatography
to 20 % by volume of biodiesel blendstock meeting the
D2887 Test Method for Boiling Range Distribution of Pe-
requirementsinSpecificationD6751,typicallycontainconcen-
troleum Fractions by Gas Chromatography
trations of monoglycerides of less than 0.1 % by mass. The
D4052 Test Method for Density, Relative Density, and API
Gravity of Liquids by Digital Density Meter
1
This test method is under the jurisdiction of ASTM Committee D02 on
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of
2
Subcommittee D02.04.0L on Gas Chromatography Methods. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved Nov. 1, 2022. Published November 2022. Originally contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
ɛ1
approved in 2018. Last previous edition
...

This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
´1
Designation: D8144 − 18 D8144 − 22
Standard Test Method for
Separation and Determination of Aromatics, Nonaromatics,
and FAME Fractions in Middle Distillates by Solid-Phase
1
Extraction and Gas Chromatography
This standard is issued under the fixed designation D8144; 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
ε NOTE—Footnote 4 was updated editorially in June 2019.
1. Scope Scope*
1.1 This test method covers the separation and determination of representative aromatics, nonaromatics, and fatty acid methyl ester
(FAME) fractions in middle distillates that boil between 170 °C and 400 °C, including biodiesel blends with up to 20 % by volume
of FAME, by solid phase extraction and gas chromatography.
1.2 This test method provides two procedures, A and B. Procedure A is applicable to the petroleum-based middle distillates fuel,
and Procedure B is applicable to the biodiesel blends with up to 20 % by volume of FAME.
1.3 This test method is applicable to middle distillates samples with aromatics content ranging from 5 % to 50 % by mass and
biodiesel blends with FAME content in the range of 0.5 % to 20 % by volume. This test method may apply to concentrations
outside these ranges, but the precision has not been determined.
1.4 For Procedure B, biodiesels in the form of fatty acid ethyl ester (FAEE) can also fully elute into the FAME fraction, and they
have the similar FID (flame ionization detector) relative response factors with that of FAME. The determined content of FAME
fractions are the sum of concentrations of FAME and FAEE by this test method (see 3.1.53.2.5).
1.5 From the investigation results obtained for FAME determination, the low concentrations of monoglycerides (usually less than
0.5 % by mass in biodiesel blends) are not detectable under the gas chromatographic (GC) condition of this test method and will
not interfere with the determination of FAME by Procedure B. As a result, biodiesel blends, conforming to the requirements of
Specification D7467, containing up to 20 % by volume of biodiesel blendstock meeting the requirements in Specification D6751,
typically contain concentrations of monoglycerides of less than 0.1 % by mass. The diglycerides and triglycerides, if present, are
not detected under the GC condition of this test method due to their higher boiling points.
NOTE 1—If a sample is suspected of containing an abnormal FAME biodiesel feedstock than specified in Specification D6751, for example, a sample
contaminated with vegetable oil with a high level of total triglycerides, the content of mono-, di-, or tri-glycerides in the isolated FAME fraction may
be determined using Test Method D6584. Samples containing biodiesels with a high amount of glycerides than specified in Specification D6751 may
contaminate the GC column and not recommended for this test method.
1.6 The values stated in acceptable SI units are to be regarded as the standard. No other units of measurement are included in this
standard
1
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
D02.04.0L on Gas Chromatography Methods.
Current edition approved March 1, 2018Nov. 1, 2022. Published April 2018November 2022. Originally approved in 2018. Last previous edition approved in 2018 as
ɛ1
D8144 – 18 . DOI: 10.1520/D8144-18E01.10.1520/D8144-22.
*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
1

---------------------- Page: 1 ----------------------
D8144 − 22
1.7 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.
1.8 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
2.1 AST
...

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