Standard Guide for Analysis of 1,3-Butadiene Product

SIGNIFICANCE AND USE
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.
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 given in SI units are to be regarded as the standard. The inch-pound units given in parentheses are for information only.
1.3 This standard does not purport to address all of the safety problems, 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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Publication Date
31-Oct-2005
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ASTM D5274-00(2005) - Standard Guide for Analysis of 1,3-Butadiene Product
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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:D5274–00 (Reapproved 2005)
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 D4423 Test Method for Determination of Carbonyls In C
Hydrocarbons
1.1 This guide covers the analysis of 1,3–butadiene prod-
D4468 Test Method for Total Sulfur in Gaseous Fuels by
ucts produced in North America. It includes possible compo-
Hydrogenolysis and Rateometric Colorimetry
nents and test methods, both ASTM and other, either actually
D4629 Test Method forTrace Nitrogen in Liquid Petroleum
used or believed to be in use, to test for these components.This
Hydrocarbons by Syringe/Inlet Oxidative Combustion and
guide is not intended to be used or construed as a set of
Chemiluminescence Detection
specifications for butadiene products.
D4864 Test Method for Determination of Traces of Metha-
1.2 The values stated in SI units are to be regarded as
nol in Propylene Concentrates by Gas Chromatography
standard. The values given in parentheses are for information
D5799 Test Method for Determination of Peroxides in
only.
Butadiene
1.3 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
3. Terminology
responsibility of the user of this standard to establish appro-
3.1 Definitions:
priate safety and health practices and determine the applica-
3.1.1 1,3-butadiene—hydrocarbon product containing more
bility of regulatory limitations prior to use.
than 99 % 1,3-butadiene.
2. Referenced Documents 3.2 Symbols:
3.2.1 BHT—butyl hydroxy toluene.
2.1 ASTM Standards:
3.2.2 GC—gas chromatography.
D1025 Test Method for Nonvolatile Residue of
3.2.3 pTBC—paratertiary butyl catechol.
Polymerization-Grade Butadiene
3.2.4 4VCH-1—4-vinyl cyclo hexene (1,3-butadiene
D1157 Test Method for Total Inhibitor Content (TBC) of
dimer).
Light Hydrocarbons
D1550 Standard ASTM Butadiene Measurement Tables
4. Significance and Use
D2384 Test Methods for Traces of Volatile Chlorides in
4.1 This guide is intended to provide information on the
Butane-Butene Mixtures
possible composition of 1,3-butadiene products and possible
D2426 Test Method for Butadiene Dimer and Styrene in
ways to test them. Since there are currently not enoughASTM
Butadiene Concentrates by Gas Chromatography
standards for determining all components of interest, this guide
D2593 Test Method for Butadiene Purity and Hydrocarbon
provides information on other potentially available test meth-
Impurities by Gas Chromatography
ods.
D3246 Test Method for Sulfur in Petroleum Gas by Oxida-
4.2 Although this guide is not to be used for specifications,
tive Microcoulometry
it can provide a starting point for parties to develop mutually
D3700 Practice for Obtaining LPG Samples Using a Float-
agreed-upon specifications that meet their respective require-
ing Piston Cylinder
ments. It can also be used as a starting point in finding suitable
D4178 Practice for Calibrating Moisture Analyzers
test methods for 1,3-butadiene components.
5. Sampling
This guide is under the jurisdiction of ASTM Committee D02 on Petroleum
ProductsandLubricantsandisthedirectresponsibilityofSubcommitteeD02.D0.04
5.1 General:
on C Hydrocarbons.
5.1.1 1,3-butadiene is a very reactive hydrocarbon. It reacts
Current edition approved Nov. 1, 2005. Published November 2005. Originally
with oxygen to form peroxides and to polymerize. It also
approved in 1992. Last previous edition approved in 2000 as D5274 – 00. DOI:
10.1520/D5274-00R05.
dimerizes at a rate that is temperature dependent. Below 10°C
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
(50°F), the dimerization rate is less than 1 mg/kg by mass/h;
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
but, at 20°C (77°F), it increases to 3 to 4 mg/kg mass/h; and at
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. 40°C (104°F), to 14 to 20 mg/kg mass/h. 1,3-butadiene is also
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D5274–00 (2005)
TABLE 1 1,3-Butadiene Test Methods (ASTM)
5.1.1.2 Eliminate or keep to an absolute minimum the
Concentration inclusion of oxygen during and after sampling, and
Property Units Test Method
Range
5.1.1.3 Sample the product at as low a temperature as
Amines mg/kg See Table 2 <1 to 25
possible, maintain the sample at a low temperature, and
Ammonia mg/kg See Table 2 <1 to 25
analyze it as soon as possible. Do not allow it to sit outdoors in
Benzene mg/kg See Table 2 <0.1to10
1,2-butadiene mg/kg D2593 <1 to 100
the sun after sampling.
1,3-butadiene dimer mg/kg D2426 <100 to 200
5.1.2 In addition to 5.1.1.1-5.1.1.3, 1,3-butadiene to be
(4VCH-1)
analyzed for trace components should be sampled by a
C hydrocarbons mg/kg D2593 <1 to 1000
C hydrocarbons mg/kg See Table 2 <1 to 1000
6+
technique that minimizes or eliminates loss of light compo-
Carbonyls mg/kg D4423 <1 to 100
nents and concentration of heavy ones. The subsections below
Chlorides mg/kg See Table 2 <1 to 25
Ethylene glycol mg/kg See Table 2 <1 to 100 list some different sampling methods and principles. However,
Inhibitor (p-TBC) mg/kg D1157 <1 to 500
it is not the intent of this guide to list procedures that are
See Table 2
applicable to al
...

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