ASTM D5441-21

Standard Test Method for Analysis of Methyl Tert-Butyl Ether (MTBE) by Gas Chromatography

SIGNIFICANCE AND USE
5.1 The presence of impurities in MTBE product can have a deleterious effect upon the value of MTBE as a gasoline additive. Oxygenate and olefin contents are of primary concern. This test method provides a knowledge of the composition of MTBE product. This is useful in the evaluation of process operations control, in the valuation of the product, and for regulatory purposes.  
5.2 Open tubular column gas chromatography with a flame ionization detector, used by the test method, is a technique that is sensitive to the contaminants commonly found in MTBE, and a technique that is widely used.
SCOPE
1.1 This test method covers the determination of the purity of methyl tert-butyl ether (MTBE) by gas chromatography. It also provides a procedure to measure impurities in MTBE such as C4 to C12 olefins, methyl, isopropyl and tert-butyl alcohols, methyl sec-butyl and methyl tert-amyl ethers, acetone, and methyl ethyl ketone. Impurities are determined to a minimum concentration of 0.02 % by mass.  
1.2 This test method is not applicable to the determination of MTBE in gasoline.  
1.3 Water cannot be determined by this test method and must be measured by a procedure such as Test Method D1364 and the result used to normalize the chromatographic values.  
1.4 A majority of the impurities in MTBE is resolved by the test method, however, some co-elution is encountered.  
1.5 This test method is inappropriate for impurities that boil at temperatures higher than 180 °C or for impurities that cause poor or no response in a flame ionization detector, such as water.  
1.6 The values stated in SI (metric) units of measurement are preferred and used throughout the standard.  
1.6.1 Exception—Alternate units, in common usage, are also provided to improve clarity and aid the user of this test method.  
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.

General Information

• Status: Published
• Publication Date: 30-Nov-2021
• ICS: 71.080.60 - Alcohols. Ethers
• Technical Committee: D02 - Petroleum Products, Liquid Fuels, and Lubricants
• Drafting Committee: D02.04.0L - Gas Chromatography Methods

Standards Content (Sample)

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: D5441 − 21
Standard Test Method for
Analysis of Methyl Tert-Butyl Ether (MTBE) by Gas
1
Chromatography
This standard is issued under the fixed designation D5441; 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* mendations issued by the World Trade Organization Technical
Barriers to Trade (TBT) Committee.
1.1 This test method covers the determination of the purity
of methyl tert-butyl ether (MTBE) by gas chromatography. It
2. Referenced Documents
alsoprovidesaproceduretomeasureimpuritiesinMTBEsuch
2
2.1 ASTM Standards:
as C to C olefins, methyl, isopropyl and tert-butyl alcohols,
4 12
D1364 Test Method for Water in Volatile Solvents (Karl
methyl sec-butyl and methyl tert-amyl ethers, acetone, and
3
Fischer Reagent Titration Method) (Withdrawn 2021)
methyl ethyl ketone. Impurities are determined to a minimum
D3700 Practice for Obtaining LPG Samples Using a Float-
concentration of 0.02 % by mass.
ing Piston Cylinder
1.2 This test method is not applicable to the determination
D4057 Practice for Manual Sampling of Petroleum and
of MTBE in gasoline.
Petroleum Products
D4175 Terminology Relating to Petroleum Products, Liquid
1.3 Water cannot be determined by this test method and
must be measured by a procedure such as Test Method D1364 Fuels, and Lubricants
D4307 Practice for Preparation of Liquid Blends for Use as
and the result used to normalize the chromatographic values.
Analytical Standards
1.4 Amajority of the impurities in MTBE is resolved by the
D4626 Practice for Calculation of Gas Chromatographic
test method, however, some co-elution is encountered.
Response Factors
1.5 This test method is inappropriate for impurities that boil
E355 Practice for Gas ChromatographyTerms and Relation-
at temperatures higher than 180 °C or for impurities that cause
ships
poor or no response in a flame ionization detector, such as
E594 Practice for Testing Flame Ionization Detectors Used
water.
in Gas or Supercritical Fluid Chromatography
1.6 The values stated in SI (metric) units of measurement
3. Terminology
are preferred and used throughout the standard.
3.1 Definitions—This test method makes reference to many
1.6.1 Exception—Alternate units, in common usage, are
common gas chromatographic procedures, terms, and relation-
also provided to improve clarity and aid the user of this test
ships. Detailed definitions of these and other terms used in this
method.
test method can be found in Practices E355 and E594, and
1.7 This standard does not purport to address all of the
Terminology D4175.
safety concerns, if any, associated with its use. It is the
3.2 Definitions of Terms Specific to This Standard:
responsibility of the user of this standard to establish appro-
3.2.1 C to C olefins, n—common olefin impurities in
priate safety, health, and environmental practices and deter-
4 12
MTBE are unreacted feedstock and dimers or trimers of feed
mine the applicability of regulatory limitations prior to use.
such as trimethylpentene or pentamethylheptene.
1.8 This international standard was developed in accor-
dance with internationally recognized principles on standard-
4. Summary of Test Method
ization established in the Decision on Principles for the
Development of International Standards, Guides and Recom- 4.1 Arepresentative aliquot of the MTBE product sample is
introduced into a gas chromatograph equipped with a methyl
1 2
This test method is under the jurisdiction of ASTM Committee D02 on For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
Subcommittee D02.04.0L on Gas Chromatography Methods. Standards volume information, refer to the standard’s Document Summary page on
Current edition approved Dec. 1, 2021. Published December 2021. Originally the ASTM website.
3
approved in 1993. Last previous edition approved in 2017 as D5441 – 98 (2017). The last approved version of this historical standard is referenced on
DOI: 10.1520/D5441-21. www.astm.org.
*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 ----------------------
D5441 − 21
silicone bonded phase fused silica open tubular column. duction. Carrier gas cont
...

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: D5441 − 98 (Reapproved 2017) D5441 − 21
Standard Test Method for
Analysis of Methyl Tert-Butyl Ether (MTBE) by Gas
1
Chromatography
This standard is issued under the fixed designation D5441; 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 Scope*
1.1 This test method covers the determination of the purity of methyl tert-butyl ether (MTBE) by gas chromatography. It also
provides a procedure to measure impurities in MTBE such as C to C olefins, methyl, isopropyl and tert-butyl alcohols, methyl
4 12
sec-butyl and methyl tert-amyl ethers, acetone, and methyl ethyl ketone. Impurities are determined to a minimum concentration
of 0.02 mass %.0.02 % by mass.
1.2 This test method is not applicable to the determination of MTBE in gasoline.
1.3 Water cannot be determined by this test method and must be measured by a procedure such as Test Method D1364 and the
result used to normalize the chromatographic values.
1.4 A majority of the impurities in MTBE is resolved by the test method, however, some co-elution is encountered.
1.5 This test method is inappropriate for impurities that boil at temperatures higher than 180 °C or for impurities that cause poor
or no response in a flame ionization detector, such as water.
1.6 The values stated in SI (metric) units of measurement are preferred and used throughout the standard.
1.6.1 Exception—Alternate units, in common usage, are also provided to improve clarity and aid the user of this test method.
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.
2. Referenced Documents
2
2.1 ASTM Standards:
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, 2017Dec. 1, 2021. Published November 2017December 2021. Originally approved in 1993. Last previous edition approved in 20132017
as D5441–98(2013).D5441 – 98 (2017). DOI: 10.1520/D5441-98R17.10.1520/D5441-21.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at [e-mail]. 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 ----------------------
D5441 − 21
3
D1364 Test Method for Water in Volatile Solvents (Karl Fischer Reagent Titration Method) (Withdrawn 2021)
D3700 Practice for Obtaining LPG Samples Using a Floating Piston Cylinder
D4057 Practice for Manual Sampling of Petroleum and Petroleum Products
D4175 Terminology Relating to Petroleum Products, Liquid Fuels, and Lubricants
D4307 Practice for Preparation of Liquid Blends for Use as Analytical Standards
D4626 Practice for Calculation of Gas Chromatographic Response Factors
E355 Practice for Gas Chromatography Terms and Relationships
E594 Practice for Testing Flame Ionization Detectors Used in Gas or Supercritical Fluid Chromatography
3. Terminology
3.1 Definitions—This test method makes reference to many common gas chromatographic procedures, terms, and relationships.
Detailed definitions of these and other terms used in this test method can be found in Practices E355 and E594, and Terminology
D4175.
3.2 Definitions of Terms Specific to This Standard:
3.2.1 C to C olefins—olefins, n—common olefin impurities in MTBE are unreacted feedstock and dimers or trimers of feed such
4 12
as trimethylpentene or pentamethylheptene.
4. Summary of Test Method
4.1 A representative aliquot of the MTBE product s
...