ASTM D6144-97
(Test Method)Standard Test Method for Analysis of AMS (alpha-Methylstyrene) by Capillary Gas Chromatography
Standard Test Method for Analysis of AMS (alpha-Methylstyrene) by Capillary Gas Chromatography
SCOPE
1.1 This test method covers the determination of the purity of AMS (alpha-methylstyrene) by gas chromatography.
1.2 This test method has been found applicable to the measurement of impurities such as cumene, 3-methyl-2-cyclopentene-1-one, n-propylbenzene, tert-buytlbenzene, sec-butylbenzene, cis-2-phenyl-2-butene, acetophenone, 1-phenyl-1-butene, 2-phenyl-2-propanol, and trans-2-phenyl-2-butene, which are common to the manufacturing process of AMS. The limit of detection for these impurities is 0.01 wt%.
1.3 The following applies to all specified limits in this test method: for purposes of determining conformance with this test method, 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 E 29.
1.4 This Test Method 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 Test Method to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. For specific hazard statements, see Section 8.
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Designation: D 6144 – 97
Standard Test Method for
Analysis of AMS (a-Methylstyrene) by Capillary Gas
Chromatography
This standard is issued under the fixed designation D 6144; 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 OSHA Regulations, 29CFR, paragraphs 1910.1000 and
1910.1200
1.1 This test method covers the determination of the purity
of AMS (a-methylstyrene) by gas chromatography.
3. Terminology
1.2 This test method has been found applicable to the
3.1 See Terminology D 4790 for definition of terms used in
measurement of impurities such as cumene, 3-methyl-2-
this test method.
cyclopentene-1-one, n-propylbenzene, tert-buytlbenzene, sec-
butylbenzene, cis-2-phenyl-2-butene, acetophenone, 1-phenyl-
4. Summary of Test Method
1-butene, 2-phenyl-2-propanol, and trans-2-phenyl-2-butene,
4.1 A known amount of internal standard is added to a
which are common to the manufacturing process of AMS. The
sample of AMS. The prepared sample is mixed and analyzed
limit of detection for these impurities is 0.01 wt %.
by a gas chromatograph (GC) equipped with a flame ionization
1.3 The following applies to all specified limits in this test
detector (FID). The peak area of each impurity and the internal
method: for purposes of determining conformance with this
standard is measured and the amount of each impurity is
test method, an observed value or a calculated value shall be
calculated from the ratio of the peak area of the internal
rounded off “to the nearest unit” in the last right-hand digit
standard versus the peak area of the impurity. Purity by GC
used in expressing the specification limit, in accordance with
(the AMS content) is calculated by subtracting the sum of the
the rounding-off method of Practice E 29.
impurities from 100.00. Results are reported in weight percent.
1.4 This standard does not purport to address all the safety
concerns, if any, associated with its use. It is the responsibility
5. Significance and Use
of the user of this standard to establish appropriate safety and
5.1 This test method is suitable for setting specification on
health practices and determine the applicability of regulatory
the materials referenced in 1.2 and for use as an internal quality
limitations prior to use. For specific hazard statements, see
control tool where AMS is produced or is used in a manufac-
Section 8.
turing process. It may also be used in development or research
work involving AMS.
2. Referenced Documents
5.2 This test method is useful in determining the purity of
2.1 ASTM Standards:
AMS with normal impurities present. If extremely high boiling
D 3437 Practice for Sampling and Handling Liquid Cyclic
2 or unusual impurities are present in the AMS, this test method
Products
would not necessarily detect them and the purity calculation
D 4790 Terminology of Aromatic Hydrocarbons and Re-
2 would be erroneous.
lated Chemicals
E 29 Practice for Using Significant Digits in Test Data to
6. Apparatus
Determine Conformance with Specifications
6.1 Gas Chromatograph—Any instrument having a flame
E 355 Practice for Gas Chromatography Terms and Rela-
ionization detector that can be operated at the conditions given
tionships
in Table 1. The system should have sufficient sensitivity to
E 1510 Practice for Installing Fused Silica Open Tubular
obtain a minimum peak height response for 0.01 % n-octane of
Columns in Gas Chromatographs
twice the height of the signal background noise.
2.2 Other Document:
6.2 Columns—The choice of column is based on resolution
requirements. Any column may be used that is capable of
resolving all significant impurities from AMS and the internal
This test method is under the jurisdiction of ASTM Committee D16 on
Aromatic Hydrocarbons and Related Chemicals and is the direct responsibility of
standard. The column described in Table 1 has been used
Subcommittee D16.07 on Styrene, Ethylbenzene, and C and C Aromatic
9 10
Hydrocarbons.
Current edition approved June 10, 1997. Published August 1997.
2 4
Annual Book of ASTM Standards, Vol 06.04. Available from the Superintendent of Documents, U.S. Government Printing
Annual Book of ASTM Standards, Vol 14.02. Office, Washington, DC 20402.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D 6144
TABLE 1 Instrumental Parameters
10. Preparation of Apparatus
Detector flame ionization
10.1 Follow manufacturer’s instructions for mounting and
Injection Port capillary splitter
conditioning the column into the chromatograph and adjusting
Column A:
Tubing fused silica
the instrument to the conditions described in Table 1 allowing
Stationary phase crosslinked methylsilicone
sufficient time for the equipment to reach equilibrium. See
Film thickness, μm 1.0
Practice E 1510 for more information on column installation.
Length, m 60
Diameter, mm 0.25 See Practice E 355 for additional information on gas chroma-
tography practices and terminology.
Temperatures:
Injector, °C 250
11. Procedure
Detector, °C 250
Oven, °C 125
11.1 Into a 100-mL volumetric flask, add 100 μL of n-octane
to 99.90 mL of AMS. Mix well. Assuming a density of 0.704
Carrier gas helium
for n-octane and 0.910 for AMS, the resulting n-octane
Flow rate, mls/min 2
concentration will be 0.0774 weight %.
Split ratio 70:1 11.2 Inject into the gas chromatograph, an appropriate
amount of sample as previously determined according to 6.1
Sample size, μl 1.0
and start the analysis.
11.3 Obtain a chromatgram and peak integration report. Fig.
1 illustrates a typical analysis of AMS using Column A and
successfully. Unless the analyst can be sure of peak identity
conditions listed in Table 1.
(for example by gas chromatography-mass spectrometry (GC-
MS)), the use of the column in Table 1 is strongly recom- 12. Calculations
mended.
12.1
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