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ASTM D7347-07e1

(Test Method)

Standard Test Method for Determination of Olefin Content in Denatured Ethanol by Supercritical Fluid Chromatography

Standard Test Method for Determination of Olefin Content in Denatured Ethanol by Supercritical Fluid Chromatography

SIGNIFICANCE AND USE
Olefinic hydrocarbons that may be present in denatured ethanol have been demonstrated to contribute to photochemical reactions in the atmosphere, and this can result in the formation of smog in susceptible urban areas.
The California Air Resources Board (CARB) has specified a maximum allowable limit of total olefins in spark ignition engine fuel. Denatured ethanol will be added at the terminals as an oxygenate additive and can contain olefinic species contributing to the total olefins present in spark ignition engine fuel. An analytical method is therefore necessary to determine total olefins in denatured ethanol intended for spark ignition engine fuel use. The test method is intended to be used by both regulators and producers.
The present test method is automated, does not require any sample preparation, and has a relatively short analysis time of approximately 20 min.
SCOPE
1.1 This test method covers the determination of the total amount of olefins in denatured ethanol to be used as an oxygenate additive in blended spark ignition engine fuels. The method of determination is supercritical fluid chromatography (SFC). The application range is from 0.1 to 1.0 mass percent total olefins. Results are expressed in terms of mass percent olefins.
1.2 This test method can be used for the analysis of denatured ethanol that is intended to be used as an oxygenate additive in commercial spark ignition engine fuels.
1.3 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.
1.4 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.

General Information

Status
Historical
Publication Date
31-Jul-2007
ICS
75.160.20 - Liquid fuels
Technical Committee
D02 - Petroleum Products, Liquid Fuels, and Lubricants
Drafting Committee
D02.04.0C - Liquid Chromatography
Current Stage
Ref Project

Relations

Replaces
ASTM D7347-07 - Standard Test Method for Determination of Olefin Content in Denatured Ethanol by Supercritical Fluid Chromatography
Effective Date
01-Aug-2007
Replaced By
ASTM D7347-15 - Standard Test Method for Determination of Olefin Content in Denatured Ethanol by Supercritical Fluid Chromatography
Effective Date
01-Dec-2015
Referred By
ASTM D4806-21a - Standard Specification for Denatured Fuel Ethanol for Blending with Gasolines for Use as Automotive Spark-Ignition Engine Fuel
Effective Date
01-Aug-2007
Referred By
ASTM D8011-19 - Standard Specification for Natural Gasoline as a Blendstock in Ethanol Fuel Blends or as a Denaturant for Fuel Ethanol
Effective Date
01-Aug-2007

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ASTM D7347-07e1 - Standard Test Method for Determination of Olefin Content in Denatured Ethanol by Supercritical Fluid ChromatographyASTM D7347-07e1 - Standard Test Method for Determination of Olefin Content in Denatured Ethanol by Supercritical Fluid Chromatography
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ASTM D7347-07e1 - Standard Test Method for Determination of Olefin Content in Denatured Ethanol by Supercritical Fluid Chromatography
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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
´1
Designation:D7347 −07
StandardTest Method for
Determination of Olefin Content in Denatured Ethanol by
1
Supercritical Fluid Chromatography
This standard is issued under the fixed designation D7347; 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—Added research report footnote to Section 13 editorially in October 2008.
1. Scope 3. Terminology
1.1 This test method covers the determination of the total
3.1 Definitions:
amount of olefins in denatured ethanol to be used as an
3.1.1 critical pressure, n—that pressure needed to condense
oxygenate additive in blended spark ignition engine fuels. The
a gas at the critical temperature.
method of determination is supercritical fluid chromatography
3.1.2 critical temperature, n—highest temperature at which
(SFC). The application range is from 0.1 to 1.0 mass percent
a gaseous fluid can be converted to a liquid by means of
total olefins. Results are expressed in terms of mass percent
compression.
olefins.
3.1.3 supercritical fluid, n—fluid maintained in a thermody-
1.2 This test method can be used for the analysis of
namic state above its critical temperature and critical pressure.
denatured ethanol that is intended to be used as an oxygenate
additive in commercial spark ignition engine fuels.
3.1.4 supercritical fluid chromatography, n— class of chro-
matography that employs supercritical fluids as mobile phases.
1.3 The values stated in SI units are to be regarded as the
standard. The values given in parentheses are for information
4. Summary of Test Method
only.
1.4 This standard does not purport to address all of the
4.1 A small aliquot of the denatured alcohol sample is
safety concerns, if any, associated with its use. It is the
injectedontoasetofthreeanalyticalchromatographiccolumns
responsibility of the user of this standard to establish appro-
connected in series. The sample is transported through the
priate safety and health practices and determine the applica-
columns using supercritical carbon dioxide (CO)asthe
2
bility of regulatory limitations prior to use.
mobile phase. The first column is packed with polyvinyl
alcohol(PVA).Thesecondcolumnintheseriesisananalytical
2. Referenced Documents
column packed with high surface area silica gel particles, and
2
the third column is packed with silica particles coated with
2.1 ASTM Standards:
strong cation exchange material loaded with silver ions.
D4052 Test Method for Density, Relative Density, and API
Gravity of Liquids by Digital Density Meter
4.2 Two six-port switching valves are used to direct the
D5186 Test Method for Determination of the Aromatic
different classes of components through the chromatographic
Content and Polynuclear Aromatic Content of Diesel
system to the detector. In a forward flow mode, saturates,
Fuels and Aviation Turbine Fuels By Supercritical Fluid
aromatics,andolefinspassontotheanalyticalsilicagelcolumn
Chromatography
whilethealcoholisretainedonthePVAcolumn.Thesaturates,
D6550 Test Method for Determination of Olefin Content of
aromatics, and olefins are maintained on the silica column,
Gasolines by Supercritical-Fluid Chromatography
whilethealcoholisback-flushedtothedetector.Thisstepfrees
the flow path of alcohol species allowing for the separation of
the olefins from saturates and aromatics. The forward flow
1
This test method is under the jurisdiction of ASTM Committee D02 on
mode is resumed after the alcohol is eliminated and saturates
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of
are carried to the detector, while the aromatics are retained on
Subcommittee D02.04.0C on Liquid Chromatography.
the silica column and the olefinic species are trapped on the
Current edition approved Aug. 1, 2007. Published September 2007. DOI:
10.1520/D7347-07E01.
silver-loaded column. The next step is to back-flush the olefins
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
from the silver-loaded column to the detector. Finally the
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
aromatics are carried from the silica column to the detector in
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. a forward flow mode, bypassing the silver-loaded column.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
´1
D7347−07
TABLE 1 Typical Columns
4.3 A flame ionization detector (FID) is used for quantita-
tion. Calibration is based on the area of the chromatographic
...

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SCOPE
1.1 This test method covers the quantitative determination of total vanadium and nickel in crude and residual oil in the concentration ranges shown in Table 1 using X-ray fluorescence (XRF) spectrometry.  
1.2 Sulfur is measured for analytical purposes only for the compensation of X-ray absorption matrix effects affecting the vanadium and nickel X-rays. For measurement of sulfur by standard test method use Test Methods D4294, D2622 or other suitable standard test method for sulfur in crude and residual oils.  
1.3 This test method is limited to the use of X-ray fluorescence (XRF) spectrometers employing an X-ray tube for excitation in conjunction with wavelength dispersive detection system or energy dispersive high resolution semiconductor detector with the ability to separate signals of adjacent and near-adjacent elements.  
1.4 This test method uses inter-element correction factors calculated from XRF theory, the fundamental parameters (FP) approach, or best fit regression.  
1.5 Samples containing higher concentrations than shown in Table 1 must be diluted to bring the elemental concentration of the diluted material within the scope of this test method.  
1.6 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.6.1 The preferred concentrations units are mg/kg for vanadium and nickel.  
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.

  • Standard
    7 pages
    English language
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  • Standard
    7 pages
    English language
    sale 15% off