ASTM D2426-93(2014)

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

SIGNIFICANCE AND USE
4.1 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 standard. No other units of measurement are included in this standard.  
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. For specific precautionary statements see Sections 6 and 8.

General Information

• Status: Historical
• Publication Date: 30-Apr-2014
• 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

• Replaces: ASTM D2426-93(2009) - Standard Test Method for Butadiene Dimer and Styrene in Butadiene Concentrates by Gas Chromatography
• Effective Date: 01-May-2014
• Referred By: ASTM D5274-00(2019) - Standard Guide for Analysis of 1,3–Butadiene Product
• Effective Date: 01-May-2014

Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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: D2426 − 93 (Reapproved 2014)
Standard Test Method for
Butadiene Dimer and Styrene in Butadiene Concentrates by
Gas Chromatography
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.
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) and styrene in butadiene
concentrates, both recycle and specification grade.
4. Significance and Use
1.2 The values stated in SI units are to be regarded as
4.1 Butadiene dimer and styrene may be present as impuri-
standard. No other units of measurement are included in this
ties in commercial butadiene. This test method is suitable for
standard.
use in internal quality control and in establishing product
1.3 This standard does not purport to address all of the
specifications.
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
5. Apparatus
priate safety and health practices and determine the applica-
5.1 Chromatograph—Any chromatograph having either a
bility of regulatory limitations prior to use. For specific
thermal conductivity or flame ionization detector may be used.
precautionary statements see Sections 6 and 8.
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
2. Referenced Documents
5:1for0.01weight%ofbutadienedimerandstyreneunderthe
2.1 ASTM Standards:
operating conditions prescribed in this test method.
D1657 Test Method for Density or Relative Density of Light
5.2 Recorder—A 0 to 1-mV, 0 to 5-mV, or 0 to 10-mV
Hydrocarbons by Pressure Hydrometer
recorder with a full-scale response time of2sor less, and with
D1945 Test Method for Analysis of Natural Gas by Gas
sufficient sensitivity to meet the requirements of 5.1.
Chromatography
D2593 Test Method for Butadiene Purity and Hydrocarbon
5.3 Column—Any column may be used that is capable of
Impurities by Gas Chromatography
resolving the butadiene dimer and styrene as discrete peaks,
2.2 Other Documents:
quantitatively proportional to concentration and within an
STP 109A Physical Constants of Hydrocarbons C to C
elapsed time sufficiently short to be practical.
1 10
5.4 LiquidSamplingValve—Any liquid sampling valve may
3. Summary of Test Method
be used that will permit the reproducible introduction of the
3.1 The sample is introduced into a gas-liquid partition
butadiene concentrate as a liquid under its vapor pressure or
column. The components of interest are separated as they are
higher and in a quantity sufficient to meet the sensitivity and
transported through the column by a carrier gas, and their
resolution requirements in 5.1 and 5.3, respectively.
presenceintheeffluent is detected and recorded as a chromato-
NOTE 1—Suitable valves are commercially available
gram. Packed columns are used, and either thermal conductiv-
ity or ionization detectors are permissible. The quantity of the
6. Reagents and Materials
6.1 4-vinylcyclohexene-1andStyrene, for calibration, purity
This test method is under the jurisdiction of ASTM Committee D02 on
of not less than 99 %.
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of
Subcommittee D02.D0.04 on C4 Hydrocarbons.
6.2 Carrier Gas—Helium or hydrogen for use on thermal
CurrenteditionapprovedMay1,2014.PublishedJuly2014.Originallyapproved
conductivity detector units; or nitrogen, helium, or argon for
in 1965. Last previous edition approved in 2009 as D2426 – 93 (2009). DOI:
use on ionization detector units. (Warning—Compressed gas.
10.1520/D2426-93R14.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or Hazardous pressure.) (Warning—Hydrogen gas is flammable.
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
Hazardous pressure.)
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. 6.3 Liquid Phase, for column.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D2426 − 93 (2014)
TABLE 1 Columns and Conditions Used Successfully
Carbowax
Dow Silicone Carbowax Carbowax Polyethylene Barecowax
Silicone SE-30 20M + Dow
200 1500 1540 Glycol-6000 1035
Corning Hi Vac
Column length, m 1.5 4.6 3.7 15.2 3.1 3.7 6.1
Column diameter, mm 3.2 4.8 6.4 0.5 6.4 4.8 6.4
Column temperature, °C 85 110 100 75 100–128 155 140
Liquid phase, wt % 10 15 16 . 0.75 each 30 20
Support material Chromosorb P TFE-fluorocarbon Chromosorb P (Coated) Silica Chromosorb P Chromosorb P
Mesh 80–100 40–60 100–120 . . 30–50 60–80
Carrier flow, mL/min 19 60 60 15 30 171 60
A B
Detector HFI T.C. HFI HFI T.C. T.C. T.C.
Sample size, µL 0.77 20 0.07 1.54 1.03 8.69 3.0
Peak measurement triangulation triangulation integrator triangulation triangulation peak height planimeter
A
HFI = hydrogen flame ionization.
B
T.C. = thermal conductivity.
NOTE 2—The following materials have been used successfully as liquid
Pressure the sample cylinder with a suitable gas to a pressure
phases (see Table 1) :
sufficient to ensure no flashing in the line to the sampling valve
Carbowax 400, 1500, 1540
or in the valve itself. Using the same sample size and
General Electric SE-30 silicone gum rubber
instrument conditions, inject the sample into the column and
Polyethylene glycol 6000
Barecowax 1035 recordthep
...

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: D2426 − 93 (Reapproved 2009) D2426 − 93 (Reapproved 2014)
Standard Test Method for
Butadiene Dimer and Styrene in Butadiene Concentrates by
Gas Chromatography
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.
1. 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 standard. No other units of measurement are included in this standard.
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. For specific precautionary statements see Sections 6 and 8.
2. Referenced Documents
2.1 ASTM Standards:
D1657 Test Method for Density or Relative Density of Light Hydrocarbons by Pressure Hydrometer
D1945 Test Method for Analysis of Natural Gas by Gas Chromatography
D2593 Test Method for Butadiene Purity and Hydrocarbon Impurities by Gas Chromatography
2.2 Other Documents:
STP 109A Physical Constants of Hydrocarbons C to C
1 10
3. Summary of Test Method
3.1 The sample is introduced into a gas-liquid partition column. The components of interest are separated as they are transported
through the column by a carrier gas, and their presence in the effluent is detected and recorded as a chromatogram. Packed columns
are used, and either thermal conductivity or ionization detectors are permissible. The quantity of the components of interest present
in the sample is determined from the chromatogram by comparing their peak areas or heights with those obtained from a synthetic
sample.
4. Significance and Use
4.1 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.
5. Apparatus
5.1 Chromatograph—Any chromatograph having either a thermal conductivity or flame ionization detector may be used. 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 5:1 for
0.01 weight % of butadiene dimer and styrene under the operating conditions prescribed in this test method.
5.2 Recorder—A 0 to 1-mV, 0 to 5-mV, or 0 to 10-mV recorder with a full-scale response time of 2 s or less, and with sufficient
sensitivity to meet the requirements of 5.1.
5.3 Column—Any column may be used that is capable of resolving the butadiene dimer and styrene as discrete peaks,
quantitatively proportional to concentration and within an elapsed time sufficiently short to be practical.
This test method 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 1965. Last previous edition approved in 20042009 as
ε1
D2426–93(2004)D2426 – 93 (2009). . DOI: 10.1520/D2426-93R09.10.1520/D2426-93R14.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at [e-mail]. 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
D2426 − 93 (2014)
TABLE 1 Columns and Conditions Used Successfully
Carbowax
Dow Silicone Carbowax Carbowax Polyethylene Barecowax
Silicone SE-30 20M + Dow
200 1500 1540 Glycol-6000 1035
Corning Hi Vac
Column length, m 1.5 4.6 3.7 15.2 3.1 3.7 6.1
Column diameter, mm 3.2 4.8 6.4 0.5 6.4 4.8 6.4
Column temperature, °C 85 110 100 75 100–128 155 140
Liquid phase, wt % 10 15 16 . 0.75 each 30 20
Support material Chromosorb P TFE-fluorocarbon Chromosorb P (Coated) Silica Chromosorb P Chromosorb P
Mesh 80–100 40–60 100–120 . . 30–50 60–80
Carrier flow, mL/min 19 60 60 15 30 171 60
A B
Detector HFI T.C. HFI HFI T.C. T.C. T.C.
Sample size, μL 0.77 20 0.07 1.54 1.03 8.69 3.0
Peak measurement triangulation triangulation integrator triangulation triangulation peak height planimeter
A
HFI = hydrogen flame ionization.
B
T.C. = thermal conductivity.
5.4 Liquid Sampling Valve—Any liquid sampling valve may be used that will permit the reproducible introduction of the
butadiene concentrate as a liquid under its vapor pressure or higher and in a quantity sufficient to meet the sensitivity and resolution
requirements in 5.1 and 5.3, respectively.
NOTE 1—Suitable valves are commercially available
6. Reagents and Materials
6.1 4-vinylcyclohexene-1 and Styrene, for calibration, purity of not less than 99 %.
6.2 Carrier Gas—Helium or hydrogen for use on thermal conductivity detector units; or nitrogen, helium, or argon for use on
ionization detector units. (Warning—Compressed gas. Hazardous pressure.) (Warning—Hydrogen gas is flammable. Hazardous
pressure.)
6.3 Liquid Phase, for column.
NOTE 2—The following materials have been used successfully as liquid phases (see Table 1) :
Carbowax 400, 1500, 1540
General Electric SE-30 silicone gum rubber
Polyethylene glycol 6000
Barecowax 1035
Dow Corning silicone oil
Carbowax 20M + Dow Corning Hi Vac.
6.4 Solid Support, for use in packed column, usually crushed fire brick or diatomaceous earth
...