ASTM D7754-19
(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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.
1.5 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.
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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: D7754 − 19
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, health, and environmental practices and deter-
1.1 This test method covers the determination of trace
mine the applicability of regulatory limitations prior to use.
oxygenates in automotive spark-ignition engine fuel. The
1.5 This international standard was developed in accor-
method used is a multidimensional gas chromatographic
dance with internationally recognized principles on standard-
method using 1,2-dimethoxy ethane as the internal standard.
ization established in the Decision on Principles for the
The oxygenates that are analyzed are: methyl-tertiary butyl
Development of International Standards, Guides and Recom-
ether (MTBE), ethyl-tertiary butyl ether (ETBE), diisopropyl
mendations issued by the World Trade Organization Technical
ether (DIPE), methanol, tertiary-amyl methyl ether (TAME),
Barriers to Trade (TBT) Committee.
n-propanol,i-propanol,n-butanol,i-butanol,tert-butylalcohol,
sec-butyl alcohol, and tert-pentanol. Ethanol is usually not
2. Referenced Documents
measuredasatraceoxygenatesinceethanolcanbeusedasthe
2
2.1 ASTM Standards:
main oxygenate compound in finished automotive spark-
D4057Practice for Manual Sampling of Petroleum and
ignition fuels such as reformulated automotive spark-ignition
Petroleum Products
fuels.Theconcentrationrangeoftheoxygenatescoveredinthe
D4307Practice for Preparation of Liquid Blends for Use as
ILS study was from 10mg⁄kg to 2000mg⁄kg. In addition this
Analytical Standards
methodisalsosuitableforthemeasurementoftheC5isomeric
D4815Test Method for Determination of MTBE, ETBE,
alcohols (2-methyl-1-butanol, 2-methyl-2-butanol) present
TAME, DIPE, tertiary-Amyl Alcohol and C to C Alco-
1 4
from the fermentation of ethanol.
hols in Gasoline by Gas Chromatography
1.2 The ethanol blending concentration for which this test
D6304Test Method for Determination of Water in Petro-
method applies ranges from 1% to 15% by volume. Higher
leum Products, Lubricating Oils, and Additives by Cou-
concentrations of ethanol coelute with methanol in the analyti-
lometric Karl Fischer Titration
cal column. Lower levels of ethanol, similar to the other
oxygenate, can be calibrated and analyzed also. If higher
3. Terminology
ethanol concentrations are expected, the window cutting tech-
3.1 Definitions of Terms Specific to This Standard:
niquecanbeusedtoavoidethanolfromenteringtheanalytical
3.1.1 electronic pressure control, n—electronic pneumatic
column and interfere with the determination of the other
control of carrier gas flows. Can be flow or pressure pro-
oxygenates of interest. Refer to Appendix X1 for details.
grammed to speed up elution of components.
1.3 The values stated in SI units are to be regarded as
3.1.2 flame ionization detector (FID), n—detector used to
standard. No other units of measurement are included in this
analyze the components eluting from the column.
standard.
3.1.3 fluidic switch, n—device that reverses the directional
1.3.1 Alternative units, in common usage, are also provided
flow in a union T altering the pressure at the midpoint. In its
to increase clarity and aid the users of this test method.
simplest design it is also known as a Dean Switch.
1.4 This standard does not purport to address all of the
3.1.4 inlet, n—capillary split/splitless inlet system operated
safety concerns, if any, associated with its use. It is the
in the split mode is recommended. Operate the inlet within its
linear range.
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, 2019. Published December 2019. Originally contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
approved in 2011. Last previous edition approved in 2016 as D7754–16. Standards volume information, refer to the standard’s Document Summary page on
DOI:10.1520/D7754-19. the ASTM website.
*A Summary of Changes section appears at th
...
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.
Designation: D7754 − 16 D7754 − 19
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. 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 safety, health, and healthenvironmental practices and determine the
applicability of regulatory limitations prior to use.
1.5 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 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 Jan. 1, 2016Nov. 1, 2019. Published February 2016December 2019. Originally approved in 2011. Last previous edition approved in 20112016
ɛ1
as D7754 – 11D7754 – 16. . DOI:10.1520/D7754-16. DOI:10.1520/D7754-19.
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 − 19
3.1.1 electronic pressure control, n—electronic pneumatic control of carrier gas flows. Can be flow or pressure program
...
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: D7754 − 19
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. Scope* responsibility of the user of this standard to establish appro-
priate safety, health, and environmental practices and deter-
1.1 This test method covers the determination of trace
mine the applicability of regulatory limitations prior to use.
oxygenates in automotive spark-ignition engine fuel. The
1.5 This international standard was developed in accor-
method used is a multidimensional gas chromatographic
dance with internationally recognized principles on standard-
method using 1,2-dimethoxy ethane as the internal standard.
ization established in the Decision on Principles for the
The oxygenates that are analyzed are: methyl-tertiary butyl
Development of International Standards, Guides and Recom-
ether (MTBE), ethyl-tertiary butyl ether (ETBE), diisopropyl
mendations issued by the World Trade Organization Technical
ether (DIPE), methanol, tertiary-amyl methyl ether (TAME),
Barriers to Trade (TBT) Committee.
n-propanol, i-propanol, n-butanol, i-butanol, tert-butyl alcohol,
sec-butyl alcohol, and tert-pentanol. Ethanol is usually not
2. Referenced Documents
measured as a trace oxygenate since ethanol can be used as the
2
2.1 ASTM Standards:
main oxygenate compound in finished automotive spark-
D4057 Practice for Manual Sampling of Petroleum and
ignition fuels such as reformulated automotive spark-ignition
Petroleum Products
fuels. The concentration range of the oxygenates covered in the
D4307 Practice for Preparation of Liquid Blends for Use as
ILS study was from 10 mg ⁄kg to 2000 mg ⁄kg. In addition this
Analytical Standards
method is also suitable for the measurement of the C5 isomeric
D4815 Test Method for Determination of MTBE, ETBE,
alcohols (2-methyl-1-butanol, 2-methyl-2-butanol) present
TAME, DIPE, tertiary-Amyl Alcohol and C to C Alco-
1 4
from the fermentation of ethanol.
hols in Gasoline by Gas Chromatography
1.2 The ethanol blending concentration for which this test
D6304 Test Method for Determination of Water in Petro-
method applies ranges from 1 % to 15% by volume. Higher
leum Products, Lubricating Oils, and Additives by Cou-
concentrations of ethanol coelute with methanol in the analyti-
lometric Karl Fischer Titration
cal column. Lower levels of ethanol, similar to the other
oxygenate, can be calibrated and analyzed also. If higher 3. Terminology
ethanol concentrations are expected, the window cutting tech-
3.1 Definitions of Terms Specific to This Standard:
nique can be used to avoid ethanol from entering the analytical
3.1.1 electronic pressure control, n—electronic pneumatic
column and interfere with the determination of the other
control of carrier gas flows. Can be flow or pressure pro-
oxygenates of interest. Refer to Appendix X1 for details.
grammed to speed up elution of components.
1.3 The values stated in SI units are to be regarded as
3.1.2 flame ionization detector (FID), n—detector used to
standard. No other units of measurement are included in this
analyze the components eluting from the column.
standard.
3.1.3 fluidic switch, n—device that reverses the directional
1.3.1 Alternative units, in common usage, are also provided
flow in a union T altering the pressure at the midpoint. In its
to increase clarity and aid the users of this test method.
simplest design it is also known as a Dean Switch.
1.4 This standard does not purport to address all of the
3.1.4 inlet, n—capillary split/splitless inlet system operated
safety concerns, if any, associated with its use. It is the
in the split mode is recommended. Operate the inlet within its
linear range.
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, 2019. Published December 2019. Originally contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
approved in 2011. Last previous edition approved in 2016 as D7754 – 16. Standards volume information, refer to the standard’s Document Summary page on
DOI:10.1520/D7754-19. 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
...
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