ASTM D2426-93(2004)e1
(Test Method)Standard Test Method for Butadiene Dimer and Styrene in Butadiene Concentrates by Gas Chromatography
Standard Test Method for Butadiene Dimer and Styrene in Butadiene Concentrates by Gas Chromatography
SIGNIFICANCE AND USE
Butadiene dimer and styrene may be present as impurities in commercial butadiene. This test method is suitable for use in internal quality control and in establishing product specifications.
SCOPE
1.1 This test method covers the determination of butadiene dimer (4-vinylcyclohexene-1) and styrene in butadiene concentrates, both recycle and specification grade.
1.2 The values stated in SI units are to be regarded as the standard.
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. For specific precautionary statements see Sections 6 and 8.
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Designation:D2426–93 (Reapproved 2004)
Standard Test Method for
Butadiene Dimer and Styrene in Butadiene Concentrates by
GasChromatography
This standard is issued under the fixed designation D2426; 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.
´ NOTE—Warning notes were moved into text editorially in November 2004.
1. Scope components of interest present in the sample is determined
from the chromatogram by comparing their peak areas or
1.1 This test method covers the determination of butadiene
heights with those obtained from a synthetic sample.
dimer(4-vinylcyclohexene-1)andstyreneinbutadieneconcen-
trates, both recycle and specification grade.
4. Significance and Use
1.2 The values stated in SI units are to be regarded as the
4.1 Butadiene dimer and styrene may be present as impuri-
standard.
ties in commercial butadiene. This test method is suitable for
1.3 This standard does not purport to address all of the
use in internal quality control and in establishing product
safety concerns, if any, associated with its use. It is the
specifications.
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica-
5. Apparatus
bility of regulatory limitations prior to use. For specific
5.1 Chromatograph—Any chromatograph having either a
precautionary statements see Sections 6 and 8.
thermal conductivity or flame ionization detector may be used.
The detector system shall have sufficient sensitivity to obtain a
2. Referenced Documents
deflection of at least 2 mm at a signal-to-noise ratio of at least
2.1 ASTM Standards:
5:1for0.01weight%ofbutadienedimerandstyreneunderthe
D1657 Test Method for Density or Relative Density of
operating conditions prescribed in this test method.
Light Hydrocarbons by Pressure Hydrometer
5.2 Recorder—A0 to 1-mV, 0 to 5-mV, or 0 to 10-mV
D1945 Test Method for Analysis of Natural Gas by Gas
recorder with a full-scale response time of2sor less, and with
Chromatography
sufficient sensitivity to meet the requirements of 5.1.
D2593 Test Method for Butadiene Purity and Hydrocarbon
5.3 Column—Any column may be used that is capable of
Impurities by Gas Chromatography
2 resolving the butadiene dimer and styrene as discrete peaks,
2.2 Other Documents:
quantitatively proportional to concentration and within an
STP 109 A , Physical Constants of Hydrocarbons C
elapsed time sufficiently short to be practical.
to C
5.4 LiquidSamplingValve—Anyliquidsamplingvalvemay
3. Summary of Test Method be used that will permit the reproducible introduction of the
butadiene concentrate as a liquid under its vapor pressure or
3.1 The sample is introduced into a gas-liquid partition
higher and in a quantity sufficient to meet the sensitivity and
column. The components of interest are separated as they are
resolution requirements in 5.1 and 5.3, respectively.
transported through the column by a carrier gas, and their
presenceintheeffluentisdetectedandrecordedasachromato-
6. Reagents and Materials
gram. Packed columns are used, and either thermal conductiv-
6.1 4-vinylcyclohexene-1andStyrene, for calibration, purity
ity or ionization detectors are permissible. The quantity of the
of not less than 99 %.
6.2 Carrier Gas—Helium or hydrogen for use on thermal
This test method is under the jurisdiction of ASTM Committee D02 on
conductivity detector units; or nitrogen, helium, or argon for
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
use on ionization detector units. (Warning—Compressed gas.
D02.D0 on Hydrocarbons for Chemical and Special Uses.
Hazardous pressure.) (Warning—Hydrogen gas is flammable.
Current edition approved Nov. 1, 2004. Published November 2004. Originally
approved in 1965. Last previous edition approved in 1998 as D2426 – 93 (1998). Hazardous pressure.)
DOI: 10.1520/D2426-93R04E01.
6.3 Liquid Phase, for column.
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. Suitable valves are commercially available.
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D2426–93 (2004)
NOTE 1—Thefollowingmaterialshavebeenusedsuccessfullyasliquid
recordthepeaks.(SeeTable1fortypicaloperatingconditions.)
phases (see Table 1):
(Warning—Butadiene gas is flammable under pressure.)
Carbowax 400, 1500, 1540
General Electric SE-30 silicone gum rubber
9. Calculation
Polyethylene glycol 6000
Barecowax 1035
9.1 PeakMeasurement—Measure the peak area or height of
Dow Corning silicone oil
each component of interest in both the synthetic blend and the
Carbowax 20M + Dow Corning Hi Vac.
sample. Measurement may be accomplished by any method
6.4 Solid Support, for use in packed column, usually
that meets the precision requirements of Section 10. Area
crushed fire brick or diatomaceous earth. Sieve size will
methods found to be acceptable include planimetering, inte-
dependonthediameterofthecolumnusedandsupportloading
gration, and triangulation (multiplying the peak height by the
and should be such as to give optimum resolution and analysis
width at the half-height). In peak area or height methods care
time.
must be taken so that chromatograph
...
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