Standard Test Method for Butadiene Dimer and Styrene in Butadiene Concentrates by Gas Chromatography

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 Notes 1, 2, and 4.

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09-Apr-1998
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ASTM D2426-93(1998) - Standard Test Method for Butadiene Dimer and Styrene in Butadiene Concentrates by Gas Chromatography
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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.
An American National Standard
Designation:D2426–93 (Reapproved 1998)
Standard Test Method for
Butadiene Dimer and Styrene in Butadiene Concentrates by
GasChromatography
This standard is issued under the fixed designation D 2426; 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 4. Significance and Use
1.1 This test method covers the determination of butadiene 4.1 Butadiene dimer and styrene may be present as impuri-
dimer(4-vinylcyclohexene-1)andstyreneinbutadieneconcen- ties in commercial butadiene. This test method is suitable for
trates, both “recycle” and specification grade. use in internal quality control and in establishing product
1.2 The values stated in SI units are to be regarded as the specifications.
standard.
5. Apparatus
1.3 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the 5.1 Chromatograph—Any chromatograph having either a
thermal conductivity or flame ionization detector may be used.
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica- The detector system shall have sufficient sensitivity to obtain a
deflection of at least 2 mm at a signal-to-noise ratio of at least
bility of regulatory limitations prior to use. For specific
precautionary statements see Note 1, Note 2, and Note 4. 5:1for0.01weight%ofbutadienedimerandstyreneunderthe
operating conditions prescribed in this test method.
2. Referenced Documents
5.2 Recorder—A 0 to 1-mV, 0 to 5-mV, or 0 to 10-mV
2.1 ASTM Standards: recorder with a full-scale response time of2sor less, and with
D 1657 Test Method for Density or Relative Density of sufficient sensitivity to meet the requirements of 5.1.
Light Hydrocarbons by Pressure Thermohydrometer 5.3 Column—Any column may be used that is capable of
D 1945 Test Method for Analysis of Natural Gas by Gas resolving the butadiene dimer and styrene as discrete peaks,
Chromatography quantitatively proportional to concentration and within an
D 2593 Test Method for Butadiene Purity and Hydrocarbon elapsed time sufficiently short to be practical. (See Note 1.)
Impurities by Gas Chromatography 5.4 LiquidSamplingValve—Anyliquidsamplingvalvemay
be used that will permit the reproducible introduction of the
3. Summary of Test Method
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
6. Reagents and Materials
presence in the effluent is detected and recorded as a chromato-
gram. Packed columns are used, and either thermal conductiv- 6.1 4-Vinylcyclohexene-1andStyrene,forcalibration,purity
ity or ionization detectors are permissible. The quantity of the of not less than 99 %.
components of interest present in the sample is determined 6.2 Carrier Gas—Helium or hydrogen for use on thermal
from the chromatogram by comparing their peak areas or conductivity detector units; or nitrogen, helium, or argon for
heights with those obtained from a synthetic sample. use on ionization detector units.
NOTE 1—Warning: Compressed gas. Hazardous pressure.
NOTE 2—Warning: Hydrogen gas is flammable. Hazardous pressure.
6.3 Liquid Phase, for column.
This test method is under the jurisdiction of ASTM Committee D-2 on
Petroleum Products and Lubricantsand is the direct responsibility of Subcommittee
NOTE 3—The following materials have been used successfully as liquid
D02.D0.04on C Hydrocarbons.
phases:
Current edition approved Feb. 15, 1993. Published May 1993. Originally
published as D 2426 – 65 T. Last previous edition D 2426 – 86.
Annual Book of ASTM Standards, Vol 05.01.
3 4
Annual Book of ASTM Standards, Vol 05.05. Suitable valves are commercially available.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
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.
D2426
Carbowax 400, 1500, 1540
9. Calculation
General Electric SE-30 silicone gum rubber
9.1 PeakMeasurement—Measure the peak area or height of
Polyethylene glycol 6000
each component of interest in both the synthetic blend and the
Barecowax 1035
sample. Measurement may be accomplished by any method
Dow Corning silicone oil
Carbowax 20M + Dow Corning Hi Vac. that meets the precision requirements of Section 10. Area
methods found to be acceptable include planimetering, inte-
6.4 Solid Support, for use in packed column, usually
gration, and triangulation (multiplying the peak height by the
crushed fire brick or diatomaceous earth. Sieve size will
width at the half-height). In peak area or height methods care
dependonthediameterofthecolumnusedandsupportloading
must be taken so that chromatograph operating parameters
and should be such as to give optimum resolution and analysis
such as column temperature and carrier gas flow rate are kept
time.
at the same conditions on both the synthetic standa
...

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