ASTM D4534-99

Standard Test Method for Benzene Content of Cyclic Products by Gas Chromatography (Withdrawn 2006)

SCOPE
1.1 This test method covers the determination of the benzene content of specific cyclic hydrocarbon products.
1.2 Benzene may be determined over a range from 5 to 300 mg/kg.
1.3 The products in which benzene can be determined include cyclohexane, toluene, individual C8 aromatics, cumene, and styrene.
1.4 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.
WITHDRAWN RATIONALE
This test method covers the determination of the benzene content of specific cyclic hydrocarbon products.
Formerly under the jurisdiction of Committee D16 on Aromatic Hydrocarbons and Related Chemicals, this test method was withdrawn in June 2006 in accordance with section 10.5.3.1 of the Regulations Governing ASTM Technical Committees, which requires that standards shall be updated by the end of the eighth year since the last approval date.

General Information

• Status: Withdrawn
• Publication Date: 09-Jun-1999
• Withdrawal Date: 19-Jun-2006
• ICS: 71.080.15 - Aromatic hydrocarbons
• Technical Committee: D16 - Aromatic, Industrial, Specialty and Related Chemicals
• Drafting Committee: D16.04 - Instrumental Analysis

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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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: D 4534 – 99
Standard Test Method for
Benzene Content of Cyclic Products by Gas
Chromatography
This standard is issued under the fixed designation D 4534; 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 Quantitative results are obtained from the measured area of the
recorded benzene peak by using a factor obtained from the
1.1 This test method covers the determination of the ben-
analysis of a blend of known benzene content.
zene content of specific cyclic hydrocarbon products.
1.2 Benzene may be determined over a range from 5 to 300
4. Significance and Use
mg/kg.
4.1 Knowledge of the benzene content is typically required
1.3 The products in which benzene can be determined
for cyclic products used as chemical intermediates and sol-
include cyclohexane, toluene, individual C aromatics,
vents. This test method may be used for final product inspec-
cumene, and styrene.
tions, process control, establishing specifications, and research
1.4 This standard does not purport to address all of the
work.
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 Gas Chromatograph—Any chromatograph having ei-
bility of regulatory limitations prior to use. A specific hazard
ther a flame ionization or other detector that is capable of
statement is given in Section 7.
providing a minimum peak height response of 0.1 mV for 20
mg/kg benzene using a maximum sample injection of 2 µL.
2. Referenced Documents
5.2 Chromatographic Column—The choice of column is
2.1 ASTM Standards:
based on resolution requirements. Any column may be used if
D 3437 Practice for Sampling and Handling Liquid Cyclic
it is capable of resolving benzene from the major component
Products
3 andotherimpurities.ThecolumndescribedinTable1hasbeen
E 260 Practice for Packed Column Gas Chromatography
found satisfactory.
E 355 Practice for Gas Chromatography Terms and Rela-
3 5.3 Integrator—Electronic integration is recommended.
tionships
5.4 Recorder, Strip Chart, 0 to 1-mV range recording
2.2 Other Document:
potentiometerwitharesponsetimeof1sorlessandmaximum
OSHA Regulations, 29 CFR, paragraphs 1910.1000 and
4 noise level of 0.3 % of full scale. If electronic integration is not
1910.1200
used, a minimum chart width of 200 mm and a minimum chart
3. Summary of Test Method speed of 1 cm/min is required.
5.5 Microsyringe, 10-µL capacity.
3.1 A gas chromatograph with a flame ionization or other
5.6 Volumetric Flask, 50-mL capacity.
detector and a column containing a supported polar liquid
phase is used. A reproducible volume of sample is injected.
6. Reagents and Materials
6.1 Carrier Gas, helium or nitrogen, chromatographic
This test method is under the jurisdiction of ASTM Committee D16 on grade.
Aromatic Hydrocarbons and Related Chemicals and is the direct responsibility of
6.2 Hydrogen, zero grade.
Subcommittee D16.04 on Instrumental Analysis.
6.3 Compressed Air, oil free.
Current edition approved June 10, 1999. Published August 1999. Originally
{1
6.4 Benzene, 99 % minimum purity.
published as D 4534 – 85 . Last previous edition D 4534 – 89 (1993) .
Annual Book of ASTM Standards, Vol 06.04.
6.5 Specific Cyclic Hydrocarbon, high-purity (best grade
Annual Book of ASTM Standards, Vol 14.02.
obtainable) benzene content not to exceed 10 % of the level
Available from Superintendent of Documents, U.S. Government Printing
expected in the sample.
Office, Washington, DC 20402.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D 4534
TABLE 1 Instrument Parameters
10. Procedure
Detector Hydrogen flame ionization
10.1 Install the chromatographic column, and establish
Column Copper
stable instrument operation at the proper operating conditions
Length 3.7 m (12 ft)
Outside diameter 3.175 mm ( ⁄8 in.)
as shown in Table 1. Adjust column temperature and flow rate
Stationary phase TCEPE (Tetracyanoethylated
to achieve sufficient resolution. A retention time of 5 to 6 min
pentaerythritol), 10 %
A
for benzene has been found to yield sufficient resolution with
Support Chromosorb P, 60–80 mesh
Temperature, °C the recommended column. Refer to instructions provided by
Sample inlet system 200
the manufacturer of the chromatograph and to Practices E 260
B
Column 75–85
and E 355.
Detector 200
Carrier gas Helium or nitrogen
10.2 Inject a repeatable volume of sample, typically 2 µLor
A
Flow rate 20 mL/min
less, into the chromatograph. The volume of sample injected
Sample size 0.5–2 µL, reproducible
must be exactly the same as the volume of blend injected. Start
A
Chromosorb P is a registered trademark of Johns-Manville Corp.
B the recorder or integration device, or both, and obtain the
Approximate values, see 10.1.
chromatogra
...