ASTM D5441-98(2017)

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 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: Historical
• Publication Date: 30-Sep-2017
• 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)

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: D5441 − 98 (Reapproved 2017)
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
Fischer Reagent Titration Method)
methyl ethyl ketone. Impurities are determined to a minimum
D3700 Practice for Obtaining LPG Samples Using a Float-
concentration of 0.02 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
D4307 Practice for Preparation of Liquid Blends for Use as
1.3 Water cannot be determined by this test method and
Analytical Standards
must be measured by a procedure such as Test Method D1364
D4626 Practice for Calculation of Gas Chromatographic
and the result used to normalize the chromatographic values.
Response Factors
1.4 Amajority of the impurities in MTBE is resolved by the
E355 Practice for Gas ChromatographyTerms and Relation-
test method, however, some co-elution is encountered.
ships
1.5 This test method is inappropriate for impurities that boil
E594 Practice for Testing Flame Ionization Detectors Used
at temperatures higher than 180 °C or for impurities that cause
in Gas or Supercritical Fluid Chromatography
poor or no response in a flame ionization detector, such as
3. Terminology
water.
3.1 Definitions—This test method makes reference to many
1.6 The values stated in SI (metric) units of measurement
common gas chromatographic procedures, terms, and relation-
are preferred and used throughout the standard.
ships. Detailed definitions of these can be found in Practices
1.6.1 Exception—Alternate units, in common usage, are
E355 and E594.
also provided to improve clarity and aid the user of this test
method.
3.2 Definitions of Terms Specific to This Standard:
3.2.1 C to C olefins—commonolefinimpuritiesinMTBE
1.7 This standard does not purport to address all of the 4 12
are unreacted feedstock and dimers or trimers of feed such as
safety concerns, if any, associated with its use. It is the
trimethylpentene or pentamethylheptene.
responsibility of the user of this standard to establish appro-
priate safety, health, and environmental practices and deter-
4. Summary of Test Method
mine the applicability of regulatory limitations prior to use.
4.1 Arepresentative aliquot of the MTBE product sample is
1.8 This international standard was developed in accor-
introduced into a gas chromatograph equipped with a methyl
dance with internationally recognized principles on standard-
silicone bonded phase fused silica open tubular column.
ization established in the Decision on Principles for the
Helium carrier gas transports the vaporized aliquot through the
Development of International Standards, Guides and Recom-
column where the components are separated by the chromato-
graphic process. Components are sensed by a flame ionization
detector as they elute from the column.
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 Oct. 1, 2017. Published November 2017. Originally contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
approved in 1993. Last previous edition approved in 2013 as D5441–98(2013). Standards volume information, refer to the standard’s Document Summary page on
DOI: 10.1520/D5441-98R17. the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
D5441 − 98 (2017)
4.2 The detector signal is processed by an electronic data pressure of approximately 550 kPa (80 psig) is required). A
acquisition system or integrating computer. Each eluting com- hydrogenflameionizationdetectorwithassociatedgascontrols
ponent is identified by
...

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 2013) D5441 − 98 (Reapproved 2017)
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
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 %.
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°C180 °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. Alternate units, in
common usage, are also provided to improve clarity and aid the user of this test method.
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 consult and establish appropriate safety safety, health, and healthenvironmental 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:
D1364 Test Method for Water in Volatile Solvents (Karl Fischer Reagent Titration Method)
D3700 Practice for Obtaining LPG Samples Using a Floating Piston Cylinder
D4057 Practice for Manual Sampling of Petroleum and Petroleum Products
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 can be found in Practices E355 and E594.
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 May 1, 2013Oct. 1, 2017. Published August 2013November 2017. Originally approved in 1993. Last previous edition approved in 20082013
ε1
as D5441–98(2008)D5441–98(2013). . DOI: 10.1520/D5441-98R13.10.1520/D5441-98R17.
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.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
D5441 − 98 (2017)
3.2 Definitions of Terms Specific to This Standard:
3.2.1 C to C olefins—common olefin impurities in MTBE are unreacted feedstock and dimers or trimers of feed such as
4 12
trimethylpentene or pentamethylheptene.
4. Summary of Test Method
4.1 A representative aliquot of the MTBE product sample is introduced into a gas chromatograph equipped with a methyl
silicone bonded phase fused
...