ASTM D5135-95

Standard Test Method for Analysis of Styrene by Capillary Gas Chromatography

SCOPE
1.1 This test method covers the determination of the impurities in, and the purity of styrene by gas chromatography. It is applicable to styrene in the range from 99 to 100% purity and to impurities at concentrations of 0.001 to  
1.00%. This test method may be used for lower purity but not all the impurities may be readily identified and the use of an internal standard becomes more difficult.
1.2 The following applies to all specified limits in this standard: for purposes of determining conformance with this standard, an observed value or a calculated value shall be rounded off "to the nearest unit" in the last right-hand digit used in expressing the specification limit, in accordance with the rounding-off method of Practice E29.
1.3 This standard does not purport to address all 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 a specific hazard statement, see Section 6.

General Information

• Status: Historical
• Publication Date: 31-Dec-1994
• ICS: 71.080.15 - Aromatic hydrocarbons
• Technical Committee: D16 - Aromatic, Industrial, Specialty and Related Chemicals
• Drafting Committee: D16.07 - Styrene, Ethylbenzene and C9 and C10 Aromatic Hydrocarbons

Relations

• Replaced By: ASTM D5135-02 - Standard Test Method for Analysis of Styrene by Capillary Gas Chromatography
• Effective Date: 10-Jun-2002
• Referred By: ASTM D7504-23 - Standard Test Method for Trace Impurities in Monocyclic Aromatic Hydrocarbons by Gas Chromatography and Effective Carbon Number
• Effective Date: 01-Jan-1995
• Referred By: ASTM D2827-19 - Standard Specification for Styrene Monomer
• Effective Date: 01-Jan-1995

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NOTICE: This standard has either been superseded and replaced by a new version or discontinued.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 5135 – 95
Standard Test Method for
Analysis of Styrene by Capillary Gas Chromatography
This standard is issued under the fixed designation D 5135; 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 impurity is compared to the peak area of the internal standard
(n-heptane or other suitable known) added to the sample. From
1.1 This test method covers the determination of the impu-
the response factors of these impurities relative to that of the
rities in, and the purity of styrene by gas chromatography. It is
internal standard and the amount of internal standard added,
applicable to styrene in the range from 99 to 100 % purity and
the concentration of the impurities are calculated. The styrene
to impurities at concentrations of 0.001 to 1.00 %. This test
content is obtained by subtracting the total amount of all
method may be used for lower purity but not all the impurities
impurities from 100.00.
may be readily identified and the use of an internal standard
becomes more difficult.
4. Significance and Use
1.2 The following applies to all specified limits in this
4.1 This test method is designed to obtain styrene purity on
standard: for purposes of determining conformance with this
the basis of impurities normally present in styrene and may be
standard, an observed value or a calculated value shall be
used for final product inspections and process control.
rounded off “to the nearest unit” in the last right-hand digit
4.2 This test method will detect the following impurities:
used in expressing the specification limit, in accordance with
non-aromatic hydrocarbons containing ten carbons or less,
the rounding-off method of Practice E 29.
ethylbenzene, p- and m-xylene, cumene, o-xylene,
1.3 This standard does not purport to address all the safety
n-propylbenzene, m- and p-ethyltoluene, alpha-methyl-styrene,
concerns, if any, associated with its use. It is the responsibility
m- and p-vinyltoluene and others where specific impurity
of the user of this standard to establish appropriate safety and
standards are available. Absolute purity cannot be determined
health practices and determine the applicability of regulatory
if unknown impurities are present.
limitations prior to use. For a specific hazard statement, see
Section 7.
5. Apparatus
2. Referenced Documents 5.1 Gas Chromatograph—Any gas chromatograph having a
flame ionization detector and a splitter injector suitable for use
2.1 ASTM Standards:
with a fused silica capillary column may be used, provided the
D 3437 Practice for Sampling and Handling Liquid Cyclic
2 system has sufficient sensitivity to obtain a minimum peak
Products
height response of 0.1 mV for 0.010 % internal standard when
E 29 Practice for Using Significant Digits in Test Data to
3 operated at the stated conditions. Background noise at these
Determine Conformance with Specifications
conditions is not to exceed 3 μV.
E 1510 Practice for Installing Fused Silica Open Tubular
3 5.2 Column—Capillary columns have been found to be
Capillary Columns in Gas Chromatographs
satisfactory. For example, 60 m of 0.32-mm inside diameter
2.2 Other Document
polar-fused silica capillary internally coated to a 0.5-μm
OSHA Regulations—29CFR paragraphs 1910.1000 and
4 thickness with a bonded (cross-linked) polyethylene glycol can
1910.1200
be used (see Table 1 for parameters). Other columns may be
3. Summary of Test Method used after it has been established that such a column is capable
of separating all major impurities and the internal standard
3.1 In this test method, the chromatogram peak area for each
from the styrene under operating conditions appropriate for the
column (see Practice E 1510).
This test method is under the jurisdiction of ASTM Committee D16 on
5.3 Electronic Integration, with tangent capabilities is rec-
Aromatic Hydrocarbons and Related Chemicals and is the direct responsibility of
Subcommittee D16.07 on Styrene, Ethylbenzene, and C and C Aromatic
ommended.
9 10
Hydrocarbons.
5.4 100-mL Volumetric Flask.
Current edition approved May 15, 1995. Published July 1995. Originally
5.5 Microsyringes, assorted volumes.
published as D 5135 – 90. Last previous edition D 5135 – 93.
Annual Book of ASTM Standards, Vol 06.04.
6. Reagents and Materials
Annual Book of ASTM Standards, Vol 14.02.
Available from Superintendent of Documents, U.S. Government Printing
6.1 Carrier Gas—a carrier gas (minimum purity of 99.95
Office, Washington, DC 20402.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D 5135
TABLE 1 Typical Instrument Parameters
9.4 Inject an appropriate amount of sample into the chro-
Carrier gas helium matograph and obtain a chromatogram.
Carrier gas flow rate at 110°C, mL/min 1.2
9.5 Measure the areas of all peaks, including the internal
Detector flame ionization
standard, except the styrene peak.
Detector temperature, °C 240
Injection port temperature, °C 230 9.6 Calculate the response factors for each impurity relative
Hydrogen flow rate, mL/min 30
to the internal standard as follows:
Air flow rate, mL/min 275
Make up gas nitrogen
C
i
RF 5 (1)
Make up gas flow rate, mL/min 23 i
A A
i b
Split flow, mL/min 150
~C ! 2
S D
s
A A
si sb
Column 60 m 3 0.32 mm ID 3 0.5 μm
bonded polyethylene glycol-
fused silica capillary
where:
Column temperature, °C 110
Chart speed, cm/min 1
RF = response factor relative to the internal standard,
i
Sample size, μL 0.6
A = area of internal standard in calibration mixture,
si
A = area of impurity peak in calibration mixture,
i
A = area of internal standard in styrene used in making
sb
mol %) appropriate to the type of detector used should be
calibration mixture,
em
...