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

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.
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.

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Historical
Publication Date
31-Jul-2007
Current Stage
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ASTM D7347-07 - Standard Test Method for Determination of Olefin Content in Denatured Ethanol by Supercritical Fluid Chromatography
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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An American National Standard
Designation: D 7347 – 07
Standard Test Method for
Determination of Olefin Content in Denatured Ethanol by
1
Supercritical Fluid Chromatography
This standard is issued under the fixed designation D 7347; 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 (e) indicates an editorial change since the last revision or reapproval.
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 thermo-
1.2 This test method can be used for the analysis of dynamic state above its critical temperature and critical pres-
denatured ethanol that is intended to be used as an oxygenate sure.
additive in commercial spark ignition engine fuels. 3.1.4 supercritical fluid chromatography, n—class of chro-
1.3 The values stated in SI units are to be regarded as the matography that employs supercritical fluids as mobile phases.
standard. The values given in parentheses are for information
4. Summary of Test Method
only.
4.1 A small aliquot of the denatured alcohol sample is
1.4 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the injectedontoasetofthreeanalyticalchromatographiccolumns
connected in series. The sample is transported through the
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica- columns using supercritical carbon dioxide (CO)asthe
2
mobile phase. The first column is packed with polyvinyl
bility of regulatory limitations prior to use.
alcohol(PVA).Thesecondcolumnintheseriesisananalytical
2. Referenced Documents
column packed with high surface area silica gel particles, and
2
2.1 ASTM Standards: the third column is packed with silica particles coated with
D 4052 Test Method for Density and Relative Density of strong cation exchange material loaded with silver ions.
Liquids by Digital Density Meter 4.2 Two six-port switching valves are used to direct the
D 5186 Test Method for Determination of the Aromatic different classes of components through the chromatographic
ContentandPolynuclearAromaticContentofDieselFuels system to the detector. In a forward flow mode, saturates,
and Aviation Turbine Fuels By Supercritical Fluid Chro- aromatics,andolefinspassontotheanalyticalsilicagelcolumn
matography whilethealcoholisretainedonthePVAcolumn.Thesaturates,
D 6550 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
mode is resumed after the alcohol is eliminated and saturates
1
This test method is under the jurisdiction of ASTM Committee D02 on
are carried to the detector, while the aromatics are retained on
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
the silica column and the olefinic species are trapped on the
D02.04.0C on Liquid Chromatography.
Current edition approved Aug. 1, 2007. Published September 2007.
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

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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 Column Type: PVA Silica Silver-loaded silica
Vendor: Selerity, Selerity, Merck Selerity,
signal for olefins, r
...

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