ASTM D7754-16
(Test Method)Standard Test Method for Determination of Trace Oxygenates in Automotive Spark-Ignition Engine Fuel by Multidimensional Gas Chromatography
Standard Test Method for Determination of Trace Oxygenates in Automotive Spark-Ignition Engine Fuel by Multidimensional Gas Chromatography
SIGNIFICANCE AND USE
5.1 The analysis of trace oxygenates in automotive spark-ignition engine fuel has become routine in certain areas to ensure compliance whenever oxygenated fuels are used. In addition, test methods to measure trace levels of oxygenates in automotive spark-ignition fuel are necessary to assess product quality.
SCOPE
1.1 This test method covers the determination of trace oxygenates in automotive spark-ignition engine fuel. The method used is a multidimensional gas chromatographic method using 1,2-dimethoxy ethane as the internal standard. The oxygenates that are analyzed are: methyl-tertiary butyl ether (MTBE), ethyl-tertiary butyl ether (ETBE), diisopropyl ether (DIPE), methanol, tertiary-amyl methyl ether (TAME), n-propanol, i-propanol, n-butanol, i-butanol, tert-butyl alcohol, sec-butyl alcohol, and tert-pentanol. Ethanol is usually not measured as a trace oxygenate since ethanol can be used as the main oxygenate compound in finished automotive spark-ignition fuels such as reformulated automotive spark-ignition fuels. The concentration range of the oxygenates covered in the ILS study was from 10 mg/kg to 2000 mg/kg. In addition this method is also suitable for the measurement of the C5 isomeric alcohols (2-methyl-1-butanol, 2-methyl-2-butanol) present from the fermentation of ethanol.
1.2 The ethanol blending concentration for which this test method applies ranges from 1 % to 15% by volume. Higher concentrations of ethanol coelute with methanol in the analytical column. Lower levels of ethanol, similar to the other oxygenate, can be calibrated and analyzed also. If higher ethanol concentrations are expected, the window cutting technique can be used to avoid ethanol from entering the analytical column and interfere with the determination of the other oxygenates of interest. Refer to Appendix X1 for details.
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.3.1 Alternative units, in common usage, are also provided to increase clarity and aid the users of this test method.
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.
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Designation: D7754 − 16
Standard Test Method for
Determination of Trace Oxygenates in Automotive Spark-
Ignition Engine Fuel by Multidimensional Gas
1
Chromatography
This standard is issued under the fixed designation D7754; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope* responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica-
1.1 This test method covers the determination of trace
bility of regulatory limitations prior to use.
oxygenates in automotive spark-ignition engine fuel. The
method used is a multidimensional gas chromatographic
2. Referenced Documents
method using 1,2-dimethoxy ethane as the internal standard.
2
2.1 ASTM Standards:
The oxygenates that are analyzed are: methyl-tertiary butyl
D4057Practice for Manual Sampling of Petroleum and
ether (MTBE), ethyl-tertiary butyl ether (ETBE), diisopropyl
Petroleum Products
ether (DIPE), methanol, tertiary-amyl methyl ether (TAME),
D4307Practice for Preparation of Liquid Blends for Use as
n-propanol,i-propanol,n-butanol,i-butanol,tert-butylalcohol,
Analytical Standards
sec-butyl alcohol, and tert-pentanol. Ethanol is usually not
D4815Test Method for Determination of MTBE, ETBE,
measuredasatraceoxygenatesinceethanolcanbeusedasthe
TAME, DIPE, tertiary-Amyl Alcohol and C to C Alco-
main oxygenate compound in finished automotive spark- 1 4
hols in Gasoline by Gas Chromatography
ignition fuels such as reformulated automotive spark-ignition
D6304Test Method for Determination of Water in Petro-
fuels.Theconcentrationrangeoftheoxygenatescoveredinthe
leum Products, Lubricating Oils, and Additives by Cou-
ILS study was from 10mg⁄kg to 2000mg⁄kg. In addition this
lometric Karl Fischer Titration
methodisalsosuitableforthemeasurementoftheC5isomeric
alcohols (2-methyl-1-butanol, 2-methyl-2-butanol) present
3. Terminology
from the fermentation of ethanol.
3.1 Definitions of Terms Specific to This Standard:
1.2 The ethanol blending concentration for which this test
3.1.1 electronic pressure control, n—electronic pneumatic
method applies ranges from 1% to 15% by volume. Higher
control of carrier gas flows. Can be flow or pressure pro-
concentrations of ethanol coelute with methanol in the analyti-
grammed to speed up elution of components.
cal column. Lower levels of ethanol, similar to the other
3.1.2 flame ionization detector (FID), n—detector used to
oxygenate, can be calibrated and analyzed also. If higher
analyze the components eluting from the column.
ethanol concentrations are expected, the window cutting tech-
niquecanbeusedtoavoidethanolfromenteringtheanalytical
3.1.3 fluidic switch, n—device that reverses the directional
column and interfere with the determination of the other
flow in a union T altering the pressure at the midpoint. In its
oxygenates of interest. Refer to Appendix X1 for details.
simplest design it is also known as a Dean Switch.
1.3 The values stated in SI units are to be regarded as 3.1.4 inlet, n—capillary split/splitless inlet system operated
standard. No other units of measurement are included in this in the split mode is recommended. Operate the inlet within its
standard. linear range.
1.3.1 Alternative units, in common usage, are also provided
3.1.4.1 split ratio, n— in capillary gas chromatography,the
to increase clarity and aid the users of this test method.
ratio of the total flow of carrier gas to the sample inlet versus
1.4 This standard does not purport to address all of the the flow of the carrier gas to the capillary column is expressed
by:
safety concerns, if any, associated with its use. It is the
Splitratio 5 ~S1C!/C (1)
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 Jan. 1, 2016. Published February 2016. Originally contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
ɛ1
approved in 2011. Last previous edition approved in 2011 as D7754–11 . Standards volume information, refer to the standard’s Document Summary page on
DOI:10.1520/D7754-16. 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
1
---------------------- Page: 1 ----------------------
D7754 − 16
where: two flame ionization detectors. In the single detector Configu-
r
...
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: D7754 − 11 D7754 − 16
Standard Test Method for
Determination of Trace Oxygenates in Automotive Spark-
Ignition Engine Fuel by Multidimensional Gas
1
Chromatography
This standard is issued under the fixed designation D7754; 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—Research report information was added editorially to Section 14 in November 2015.
1. Scope Scope*
1.1 This test method covers the determination of trace oxygenates in automotive spark-ignition engine fuel. The method used
is a multidimensional gas chromatographic method using 1,2-dimethoxy ethane as the internal standard. The oxygenates that are
analyzed are: methyl-tertiary butyl ether (MTBE), ethyl-tertiary butyl ether (ETBE), diisopropyl ether (DIPE), methanol,
tertiary-amyl methyl ether (TAME), n-propanol, i-propanol, n-butanol, i-butanol, tert-butyl alcohol, sec-butyl alcohol, and
tert-pentanol. Ethanol is usually not measured as a trace oxygenate since ethanol can be used as the main oxygenate compound
in finished automotive spark-ignition fuels such as reformulated automotive spark-ignition fuels. The concentration range of the
oxygenates covered in the ILS study was from 1010 mg ⁄ μg/Kg kg to 20002000 mg ⁄ μg/Kg. kg. In addition this method is also
suitable for the measurement of the C5 isomeric alcohols (2-methyl-1-butanol, 2-methyl-2-butanol) present from the fermentation
of ethanol.
1.2 The ethanol blending concentration for which this test method applies ranges from 11 % to 15% by volume. Higher
concentrations of ethanol coelute with methanol in the analytical column. Lower levels of ethanol, similar to the other oxygenate,
can be calibrated and analyzed also. If higher ethanol concentrations are expected, the window cutting technique can be used to
avoid ethanol from entering the analytical column and interfere with the determination of the other oxygenates of interest. Refer
to Appendix X1 for details.
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.3.1 AlternateAlternative units, in common usage, are also provided to increase clarity and aid the users of this test method.
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.
2. Referenced Documents
2
2.1 ASTM Standards:
D4057 Practice for Manual Sampling of Petroleum and Petroleum Products
D4307 Practice for Preparation of Liquid Blends for Use as Analytical Standards
D4815 Test Method for Determination of MTBE, ETBE, TAME, DIPE, tertiary-Amyl Alcohol and C to C Alcohols in
1 4
Gasoline by Gas Chromatography
D6304 Test Method for Determination of Water in Petroleum Products, Lubricating Oils, and Additives by Coulometric Karl
Fischer Titration
3. Terminology
3.1 Definitions of Terms Specific to 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 Oct. 1, 2011Jan. 1, 2016. Published November 2011February 2016. DOI:10.1520/D7754-11E01.Originally approved in 2011. Last previous
ɛ1
edition approved in 2011 as D7754 – 11 . DOI:10.1520/D7754-16.
2
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
1
---------------------- Page: 1 ----------------------
D7754 − 16
3.1.1 electronic pressure control, n—electronic pneumatic control of carrier gas flows. Can be flow or pressure programmed to
speed up elution of components.
3.1.2 flame ionization detector (FID), n—detector used to analyze the components eluting from the column.
3.1.3 fluidic switch, n—device that reverses the directional flow in a union T altering the
...
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