ASTM D5274-00(2014)
(Guide)Standard Guide for Analysis of 1,3–Butadiene Product
Standard Guide for Analysis of 1,3–Butadiene Product
SIGNIFICANCE AND USE
4.1 This guide is intended to provide information on the possible composition of 1,3-butadiene products and possible ways to test them. Since there are currently not enough ASTM standards for determining all components of interest, this guide provides information on other potentially available test methods.
4.2 Although this guide is not to be used for specifications, it can provide a starting point for parties to develop mutually agreed-upon specifications that meet their respective requirements. It can also be used as a starting point in finding suitable test methods for 1,3-butadiene components.
SCOPE
1.1 This guide covers the analysis of 1,3–butadiene products produced in North America. It includes possible components and test methods, both ASTM and other, either actually used or believed to be in use, to test for these components. This guide is not intended to be used or construed as a set of specifications for butadiene products.
1.2 The values stated in SI units are to be regarded as standard. The values given in parentheses are for information only.
1.3 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: D5274 − 00 (Reapproved 2014)
Standard Guide for
Analysis of 1,3–Butadiene Product
This standard is issued under the fixed designation D5274; 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 D4178 Practice for Calibrating Moisture Analyzers
D4423 Test Method for Determination of Carbonyls in C
1.1 This guide covers the analysis of 1,3–butadiene prod-
Hydrocarbons
ucts produced in North America. It includes possible compo-
D4468 Test Method for Total Sulfur in Gaseous Fuels by
nents and test methods, both ASTM and other, either actually
Hydrogenolysis and Rateometric Colorimetry
used or believed to be in use, to test for these components.This
D4629 Test Method for Trace Nitrogen in Liquid Petroleum
guide is not intended to be used or construed as a set of
HydrocarbonsbySyringe/InletOxidativeCombustionand
specifications for butadiene products.
Chemiluminescence Detection
1.2 The values stated in SI units are to be regarded as
D4864 Test Method for Determination of Traces of Metha-
standard. The values given in parentheses are for information
nol in Propylene Concentrates by Gas Chromatography
only.
D5799 Test Method for Determination of Peroxides in Buta-
1.3 This standard does not purport to address all of the diene
safety concerns, if any, associated with its use. It is the
3. Terminology
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica-
3.1 Definitions:
bility of regulatory limitations prior to use.
3.1.1 1,3-butadiene—hydrocarbon product containing more
than 99 % 1,3-butadiene.
2. Referenced Documents
3.2 Symbols:
2.1 ASTM Standards:
3.2.1 BHT—butyl hydroxy toluene.
D1025 Test Method for Nonvolatile Residue of
3.2.2 GC—gas chromatography.
Polymerization-Grade Butadiene
3.2.3 pTBC—paratertiary butyl catechol.
D1157 Test Method for Total Inhibitor Content (TBC) of
Light Hydrocarbons
3.2.4 4VCH-1—4-vinylcyclohexene(1,3-butadienedimer).
D1550 Standard ASTM Butadiene Measurement Tables
D2384 Test Methods for Traces of Volatile Chlorides in
4. Significance and Use
Butane-Butene Mixtures
4.1 This guide is intended to provide information on the
D2426 Test Method for Butadiene Dimer and Styrene in
possible composition of 1,3-butadiene products and possible
Butadiene Concentrates by Gas Chromatography
ways to test them. Since there are currently not enoughASTM
D2593 Test Method for Butadiene Purity and Hydrocarbon
standards for determining all components of interest, this guide
Impurities by Gas Chromatography
provides information on other potentially available test meth-
D3246 Test Method for Sulfur in Petroleum Gas by Oxida-
ods.
tive Microcoulometry
4.2 Although this guide is not to be used for specifications,
D3700 Practice for Obtaining LPG Samples Using a Float-
it can provide a starting point for parties to develop mutually
ing Piston Cylinder
agreed-upon specifications that meet their respective require-
ments. It can also be used as a starting point in finding suitable
1 test methods for 1,3-butadiene components.
This guide is under the jurisdiction of ASTM Committee D02 on Petroleum
Products, Liquid Fuels, and Lubricants and is the direct responsibility of Subcom-
mittee D02.D0.04 on C4 Hydrocarbons.
5. Sampling
CurrenteditionapprovedMay1,2014.PublishedJuly2014.Originallyapproved
5.1 General:
in 1992. Last previous edition approved in 2009 as D5274 – 00 (2009). DOI:
10.1520/D5274-00R14.
5.1.1 1,3-butadiene is a very reactive hydrocarbon. It reacts
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
with oxygen to form peroxides and to polymerize. It also
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
dimerizes at a rate that is temperature dependent. Below 10°C
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. (50°F), the dimerization rate is less than 1 mg/kg by mass/h;
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D5274 − 00 (2014)
but, at 20°C (77°F), it increases to 3 to 4 mg/kg mass/h; and at of heavier components, if present, and concentration of lighter
40°C (104°F), to 14 to 20 mg/kg mass/h. 1,3-butadiene is also ones.Also, since 1,3-butadiene is so reactive, the heat required
classified as toxic and as a potential health hazard, having been to vaporize may cause undesirable changes in the composition
found carcinogenic to laboratory animals. Therefore, sampling of the sample. For these reasons, vaporization is not recom-
of 1,3-butadiene must adhere to the following three principles: mended for 1,3-butadiene.
5.1.1.1 Minimize personnel exposure. See the appropriate
5.5 Reactive Components—Determination of reactive
OSHA Material Safety Data Sheet for guidance,
components, such as certain sulfur compounds, is generally
5.1.1.2 Eliminate or keep to an absolute minimum the
believed to require special sample containers, such as TFE-
inclusion of oxygen during and after sampling, and
fluorocarbon-lined cylinders.
5.1.1.3 Sample the product at as low a temperature as
possible, maintain the sample at a low temperature, and
6. Composition and Test Methods
analyze it as soon as possible. Do not allow it to sit outdoors in
6.1 Table 1 indicates possible composition ranges and
the sun after sampling.
ASTM methods for 1,3-butadiene product. Table 2 lists other
5.1.2 In addition to 5.1.1.1 – 5.1.1.3, 1,3-butadiene to be
test methods known or
...
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: D5274 − 00 (Reapproved 2009) D5274 − 00 (Reapproved 2014)
Standard Guide for
Analysis of 1,3–Butadiene Product
This standard is issued under the fixed designation D5274; 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 guide covers the analysis of 1,3–butadiene products produced in North America. It includes possible components and
test methods, both ASTM and other, either actually used or believed to be in use, to test for these components. This guide is not
intended to be used or construed as a set of specifications for butadiene products.
1.2 The values stated in SI units are to be regarded as standard. The values given in parentheses are for information only.
1.3 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
2.1 ASTM Standards:
D1025 Test Method for Nonvolatile Residue of Polymerization-Grade Butadiene
D1157 Test Method for Total Inhibitor Content (TBC) of Light Hydrocarbons
D1550 Standard ASTM Butadiene Measurement Tables
D2384 Test Methods for Traces of Volatile Chlorides in Butane-Butene Mixtures
D2426 Test Method for Butadiene Dimer and Styrene in Butadiene Concentrates by Gas Chromatography
D2593 Test Method for Butadiene Purity and Hydrocarbon Impurities by Gas Chromatography
D3246 Test Method for Sulfur in Petroleum Gas by Oxidative Microcoulometry
D3700 Practice for Obtaining LPG Samples Using a Floating Piston Cylinder
D4178 Practice for Calibrating Moisture Analyzers
D4423 Test Method for Determination of Carbonyls in C Hydrocarbons
D4468 Test Method for Total Sulfur in Gaseous Fuels by Hydrogenolysis and Rateometric Colorimetry
D4629 Test Method for Trace Nitrogen in Liquid Petroleum Hydrocarbons by Syringe/Inlet Oxidative Combustion and
Chemiluminescence Detection
D4864 Test Method for Determination of Traces of Methanol in Propylene Concentrates by Gas Chromatography
D5799 Test Method for Determination of Peroxides in Butadiene
3. Terminology
3.1 Definitions:
3.1.1 1,3-butadiene—hydrocarbon product containing more than 99 % 1,3-butadiene.
3.2 Symbols:
3.2.1 BHT—butyl hydroxy toluene.
3.2.2 GC—gas chromatography.
3.2.3 pTBC—paratertiary butyl catechol.
3.2.4 4VCH-1—4-vinyl cyclo hexene (1,3-butadiene dimer).
This guide is under the jurisdiction of ASTM Committee D02 on Petroleum Products Products, Liquid Fuels, and Lubricants and is the direct responsibility of
Subcommittee D02.D0.04 on C4 Hydrocarbons.
Current edition approved July 1, 2009May 1, 2014. Published November 2009July 2014. Originally approved in 1992. Last previous edition approved in 20052009 as
D5274–00(2005).D5274 – 00 (2009). DOI: 10.1520/D5274-00R09.10.1520/D5274-00R14.
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.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D5274 − 00 (2014)
4. Significance and Use
4.1 This guide is intended to provide information on the possible composition of 1,3-butadiene products and possible ways to
test them. Since there are currently not enough ASTM standards for determining all components of interest, this guide provides
information on other potentially available test methods.
4.2 Although this guide is not to be used for specifications, it can provide a starting point for parties to develop mutually
agreed-upon specifications that meet their respective requirements. It can also be used as a starting point in finding suitable test
methods for 1,3-butadiene components.
5. Sampling
5.1 General:
5.1.1 1,3-butadiene is a very reactive hydrocarbon. It reacts with oxygen to form peroxides and to polymerize. It also dimerizes
at a rate that is temperature dependent. Below 10°C (50°F), the dimerization rate is less than 1 mg/kg by mass/h; but, at 20°C
(77°F), it increases to 3 to 4 mg/kg mass/h; and at 40°C (104°F), to 14 to 20 mg/kg mass/h. 1,3-butadiene is also classified as toxic
and as a potential health hazard, having been found carcinogenic to laboratory animals. Therefore, sampling of 1,3-butadiene must
adhere to the following three principles:
5.1.1.1 Minimize personnel exposure. See the appropriate OSHA Material Safety Data Sheet for guidance,
5.1.1.2 Eliminate or keep to an absolute minimum the inclusion of oxygen during and after sampling, and
5.1.1.3 Sample the product at as low a temperature as possible, maintain the sample at a low temperature, and analyze it as soon
as possible. Do not allow it to sit outdoors in the sun after sampling.
5.1.2 In addition to 5.1.1.1 – 5.1.1.3, 1,3-butadiene to be analyzed for trace components should be sampled by a technique that
minimizes or eliminates loss of light components and concentration of heavy ones. The subsections below list some different
sampling methods and principles. However, it is not the intent of this guide to list procedures that are applicable to all sampling
situations. It is strongly recommended that samples be obtained under the supervision of a person with wide knowledge and
experience in sampling 1,3-butadiene.
5.1.3 Also, even though this guide does not address the location of a sampling point in a line or vessel, the importance of the
proper sampling location cannot be overemphasized.
5.2 Floating Piston Cylinder—Practice D3700 meets the criterion of minimizing or eliminating loss of light components and
concentration of heavy ones. However, some labs have safety codes preventing use of rupture-disc piston containers. Alternative
procedures must be used in these labs.
5.3 Conventional “Outaging” Method—The widely used “outaging” technique (that is, the practice of removing a portion of
the fluid contents from a conventional sampling cylinder after filling in order to provide expansion room) causes a partial loss of
light components into the vapor space. Subsequent handling to recapture these light ends in the liquid phase of the sample, such
as repressurization of the cylinder contents with an inert gas, is usually successful, since 1,3-butadiene seldom contains
noncondensables. However, if permanent gases are present
...
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