ASTM D7576-16
(Test Method)Standard Test Method for Determination of Benzene and Total Aromatics in Denatured Fuel Ethanol by Gas Chromatography (Withdrawn 2022)
Standard Test Method for Determination of Benzene and Total Aromatics in Denatured Fuel Ethanol by Gas Chromatography (Withdrawn 2022)
SIGNIFICANCE AND USE
5.1 Regulations in some jurisdictions, such as California, limit the concentration of benzene and total aromatic content of denatured fuel ethanol in order to reduce the ozone reactivity and toxicity of automotive evaporative and exhaust emissions. Results from this test method may be used to assess product quality and to meet new fuel regulations.
SCOPE
1.1 This test method covers the determination of benzene and total aromatics in finished denatured fuel ethanol by gas chromatography.
1.2 Total aromatics are determined by adding the concentrations of benzene, toluene, ethylbenzene, o-xylene, m-xylene, p-xylene, and C9 and heavier aromatics.
1.3 The aromatic hydrocarbons are separated without interferences from other hydrocarbons in denatured fuel ethanol. Nonaromatic hydrocarbons having boiling point greater than that of n-dodecane can cause interferences with the determination of the C9 and heavier aromatics. For the C8 aromatics, p-xylene and m-xylene co-elute while ethylbenzene and o-xylene are separated. The C9 and heavier aromatics are determined as a single group.
1.4 This test method covers the following concentration ranges: benzene, 0.01 % to 0.08 % by mass and total aromatics, 0.29 % to 2.67 % by mass.
1.5 Results are reported to the nearest 0.01 % by mass or liquid volume.
1.6 The values stated in SI units are to be regarded as standard.
1.6.1 Exception—The values given in parentheses are provided for information only; they may not be exact equivalents.
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 and health practices and determine the applicability of regulatory limitations prior to use.
WITHDRAWN RATIONALE
This test method covered the determination of benzene and total aromatics in finished denatured fuel ethanol by gas chromatography.
Formerly under the jurisdiction of Committee D02 on Petroleum Products, Liquid Fuels, and Lubricants, this test method was withdrawn in July 2022. This standard is being balloted for withdrawal with no replacement because D7576 was originally approved with a temporary precision in 2010. In 2016 after an ILS was conducted it was updated with a precision; however, the precision obtained did not have sufficient degrees of freedom for benzene and total aromatics. Since 2016, several attempts have been made to expand the ILS to attain the degrees of freedom needed (30). However, sufficient laboratories could not be obtained. It was recently re-balloted asking for an additional five years to complete it but a negative was received because the test method was extended once and in total it has been approximately 11 years since first approved. Therefore, this ballot is being balloted for withdrawal with no replacement. The test method is a regulatory requirement in California and current version will be retained by the regulatory agency but not ASTM.
General Information
Standards Content (Sample)
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation: D7576 − 16
Standard Test Method for
Determination of Benzene and Total Aromatics in Denatured
1
Fuel Ethanol by Gas Chromatography
This standard is issued under the fixed designation D7576; 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
2.1 ASTM Standards:
1.1 This test method covers the determination of benzene
D1298 Test Method for Density, Relative Density, or API
and total aromatics in finished denatured fuel ethanol by gas
Gravity of Crude Petroleum and Liquid Petroleum Prod-
chromatography.
ucts by Hydrometer Method
1.2 Total aromatics are determined by adding the concen-
D4052 Test Method for Density, Relative Density, and API
trationsofbenzene,toluene,ethylbenzene, o-xylene, m-xylene,
Gravity of Liquids by Digital Density Meter
p-xylene, and C and heavier aromatics.
9
D4057 Practice for Manual Sampling of Petroleum and
1.3 The aromatic hydrocarbons are separated without inter-
Petroleum Products
ferences from other hydrocarbons in denatured fuel ethanol. D4307 Practice for Preparation of Liquid Blends for Use as
Nonaromatic hydrocarbons having boiling point greater than
Analytical Standards
that of n-dodecane can cause interferences with the determi-
D5580 Test Method for Determination of Benzene, Toluene,
nation of the C and heavier aromatics. For the C aromatics,
Ethylbenzene, p/m-Xylene, o-Xylene, C and Heavier
9 8
9
p-xylene and m-xylene co-elute while ethylbenzene and
Aromatics, and Total Aromatics in Finished Gasoline by
o-xylene are separated. The C and heavier aromatics are
Gas Chromatography
9
determined as a single group.
D6300 Practice for Determination of Precision and Bias
Data for Use in Test Methods for Petroleum Products and
1.4 This test method covers the following concentration
Lubricants
ranges:benzene,0.01 %to0.08%bymassandtotalaromatics,
E355 Practice for Gas ChromatographyTerms and Relation-
0.29 % to 2.67 % by mass.
ships
1.5 Results are reported to the nearest 0.01 % by mass or
3. Terminology
liquid volume.
3.1 Definitions of Terms Specific to This Standard:
1.6 The values stated in SI units are to be regarded as
3.1.1 1,2,3-tris-2-cyanoethoxypropane (TCEP)—polar gas
standard.
chromatographic liquid phase.
1.6.1 Exception—The values given in parentheses are pro-
3.1.2 aromatic, n—any organic compound containing a
vided for information only; they may not be exact equivalents.
benzene ring.
1.7 This standard does not purport to address all of the
3.1.3 low-volume connector, n—special union for connect-
safety concerns, if any, associated with its use. It is the
ing two lengths of narrow bore tubing 1.6 mm (0.06 in.)
responsibility of the user of this standard to establish appro-
outside diameter and smaller; sometimes this is referred to as
priate safety and health practices and determine the applica-
zero dead volume union.
bility of regulatory limitations prior to use.
3.1.4 narrow bore tubing—tubing used to transfer compo-
nents prior to or after separation; usually 0.5 mm (0.02 in.)
inside diameter and smaller.
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 April 1, 2016. Published April 2016. Originally contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
approved in 2010. Last previous edition approved in 2010 as D7576 – 10. DOI: Standards volume information, refer to the standard’s Document Summary page on
10.1520/D7576-16. 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
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D7576 − 16
FIG. 1 Valve Diagram, Aromatics in Denatured Fuel Ethanol
3.1.5 split ratio—in capillary gas chromatography, the ratio columnisreversedtobackflushtheC andheavieraromaticsto
9
of the total flow of carrier gas to the sample inlet versus the the flame ionization detector.
flow of the carrier gas to the capillary column, expressed by:
4.3 From the first analysis, the peak areas of benzene,
split ratio 5 ~S1C!/C (1)
toluene, and the internal standard (2-hexanone) are measured
and recorded. Peak areas for ethylbenzene, p/m-xylene,
where:
o-xylene, the C and heavier aromatics, and internal standard
9
S = flow rate at the splitter vent, and
are measured and recorded
...
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