ASTM D5274-92(1997)

Standard Guide for Analysis of 1,3-Butadiene Product

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.

General Information

• Status: Historical
• Publication Date: 09-Dec-2000
• ICS: 71.080.10 - Aliphatic hydrocarbons
• Technical Committee: D02 - Petroleum Products, Liquid Fuels, and Lubricants
• Drafting Committee: D02.D0.04 - C4 and C5 Hydrocarbons

Relations

• Replaced By: ASTM D5274-00 - Standard Guide for Analysis of 1,3-Butadiene Product
• Effective Date: 10-Dec-2000

Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
Designation: D 5274 – 92 (Reapproved 1997) An American National Standard
Standard Guide for
Analysis of 1,3–Butadiene Product
This standard is issued under the fixed designation D 5274; 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 (e) indicates an editorial change since the last revision or reapproval.
1. Scope D 4468 Test Method for Total Sulfur in Gaseous Fuels by
Hydrogenolysis and Rateometric Colorimetry
1.1 This guide covers the analysis of 1,3–butadiene prod-
D 4629 Test Method for Trace Nitrogen in Liquid Petro-
ucts produced in North America. It includes possible compo-
leum Hydrocarbons by Syringe/Inlet Oxidative Combus-
nents and test methods, both ASTM and other, either actually
tion and Chemiluminescence Detection
used or believed to be in use, to test for these components. This
D 4864 Test Method for Determination of Traces of Metha-
guide is not intended to be used or construed as a set of
nol in Propylene Concentrates by Gas Chromatography
specifications for butadiene products.
1.2 The values given in SI units are to be regarded as the
3. Terminology
standard. The inch-pound units given in parentheses are for
3.1 Definitions:
information only.
3.1.1 1,3-butadiene—hydrocarbon product containing more
1.3 This standard does not purport to address all of the
than 99 % 1,3-butadiene.
safety concerns, if any, associated with its use. It is the
3.2 Symbols:
responsibility of the user of this standard to establish appro-
3.2.1 BHT—butyl hydroxy toluene.
priate safety and health practices and determine the applica-
3.2.2 GC—gas chromatography.
bility of regulatory limitations prior to use.
3.2.3 pTBC—paratertiary butyl catechol.
2. Referenced Documents 3.2.4 4VCH-1—4-vinyl cyclo hexene (1,3-butadiene
dimer).
2.1 ASTM Standards:
D 1022 Test Method for Peroxide Content of Light Hydro-
4. Significance and Use
carbons
4.1 This guide is intended to provide information on the
D 1025 Test Method for Nonvolatile Residue of Polymer-
3 possible composition of 1,3-butadiene products and possible
ization Grade Butadiene
ways to test them. Since there are currently not enough ASTM
D 1157 Test Method for Total Inhibitor Content (TBC) of
3 standards for determining all components of interest, this guide
Light Hydrocarbons
provides information on other potentially available test meth-
D 1550 ASTM Butadiene Measurement Tables
ods.
D 2384 Test Methods for Traces of Volatile Chlorides in
4.2 Although this guide is not to be used for specifications,
Butane-Butene Mixtures
it can provide a starting point for parties to develop mutually
D 2426 Test Method for Butadiene Dimer and Styrene in
agreed-upon specifications that meet their respective require-
Butadiene Concentrates by Gas Chromatography
ments. It can also be used as a starting point in finding suitable
D 2593 Test Method for Butadiene Purity and Hydrocarbon
3 test methods for 1,3-butadiene components.
Impurities by Gas Chromatography
D 3246 Test Method for Sulfur in Petroleum Gas by Oxi-
5. Sampling
dative Microcoulometry
5.1 General:
D 3700 Practice for Containing Hydrocarbon Fluid Samples
4 5.1.1 1,3-butadiene is a very reactive hydrocarbon. It reacts
Using a Floating Piston Cylinder
with oxygen to form peroxides and to polymerize. It also
D 4178 Practice for Calibrating Moisture Analyzers
dimerizes at a rate that is temperature dependent. Below 10°C
D 4423 Test Method for Determination of Carbonyls in C
(50°F), the dimerization rate is less than 1 mg/kg by mass/h;
Hydrocarbons
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
1 classified as toxic and as a potential health hazard, having been
This guide is under the jurisdiction of ASTM Committee D-2 on Petroleum
found carcinogenic to laboratory animals. Therefore, sampling
Products and Lubricants and is the direct responsibility of Subcommittee D02.D0.04
on C Hydrocarbons.
5 of 1,3-butadiene must adhere to the following three principles:
Current edition approved Aug. 15, 1992. Published October 1992.
Discontinued; see 1982 Annual Book of ASTM Standards, Vol 05.01.
3 5
Annual Book of ASTM Standards, Vol 05.01. Annual Book of ASTM Standards, Vol 05.05.
4 6
Annual Book of ASTM Standards, Vol 05.02. Annual Book of ASTM Standards, Vol 05.03.
Copyright © ASTM, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959, United States.
D 5274
TABLE 1 1,3-Butadiene Test Methods (ASTM)
5.1.1.1 Minimize personnel exposure. See the appropriate
OSHA Material Safety Data Sheet for guidance, Concentration
Property Units Test Method
Range
5.1.1.2 Eliminate or keep to an absolute minimum the
Amines mg/kg See Table 2 <1 to 25
inclusion of oxygen during and after sampling, and
Ammonia mg/kg See Table 2 <1 to 25
5.1.1.3 Sample the product at as low a temperature as
Benzene mg/kg See Table 2 <0.1 to 10
possible, maintain the sample at a low temperature, and
1,2-butadiene mg/kg D 2593 <1 to 100
1,3-butadiene dimer mg/kg D 2426 <100 to 200
analyze it as soon as possible. Do not allow it to sit outdoors in
(4VCH-1)
the sun after sampling.
C hydrocarbons mg/kg D 2593 <1 to 1000
5.1.2 In addition to 5.1.1.1-5.1.1.3, 1,3-butadiene to be
C hydrocarbons mg/kg See Table 2 <1 to 1000
6+
Carbonyls mg/kg D 4423 <1 to 100
analyzed for trace components should be sampled by a
Chlorides mg/kg See Table 2 <1 to 25
technique that minimizes or eliminates loss of light compo-
Ethylene glycol mg/kg See Table 2 <1 to 100
nents and concentration of heavy ones. The subsections below
Inhibito
...