Standard Test Method for Analysis of AMS (alpha-Methylstyrene) by Capillary Gas Chromatography

SIGNIFICANCE AND USE
This test method is suitable for setting specifications on the materials referenced in 1.2 and for use as an internal quality control tool where AMS is produced or is used in a manufacturing process. It may also be used in development or research work involving AMS.
This test method is useful in determining the purity of AMS with normal impurities present. If extremely high boiling or unusual impurities are present in the AMS, this test method would not necessarily detect them and the purity calculation would be erroneous.
SCOPE
1.1 This test method covers the determination of the purity of AMS (-methylstyrene) by gas chromatography. Calibration of the gas chromatography system is done by the external standard calibration technique.
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-butylbenzene, sec-butylbenzene, cis-2-phenyl-2-butene, acetophenone, 1-phenyl-1-butene, 2-phenyl-2-propanol,  trans-2-phenyl-2-butene, m-cymene, p-cymene, and phenol, which are common to the manufacturing process of AMS. The method has also been found applicable for the determination of para-tertiary-butylcatechol typically added as a stabilizer to AMS. The impurities in AMS can be analyzed over a range of 5 to 800 mg/kg by this method. (See Table 1.) The limit of detection for these impurities is typically in the range of 5 to 10 mg/kg. (See Table 1.)
1.3 In determining the conformance of the test results using this method to applicable specifications, results shall be rounded off in accordance with the rounding-off method of Practice E 29.
1.4 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 specific hazard statements, see Section 8.

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Historical
Publication Date
31-Dec-2003
Current Stage
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ASTM D6144-04 - Standard Test Method for Analysis of AMS (alpha-Methylstyrene) by Capillary Gas Chromatography
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation: D 6144 – 04
Standard Test Method for
Analysis of AMS (a-Methylstyrene) by Capillary Gas
1
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* D 4307 PracticeforPreparationofLiquidBlendsforUseas
Analytical Standards
1.1 This test method covers the determination of the purity
D 4790 Terminology of Aromatic Hydrocarbons and Re-
ofAMS(a-methylstyrene)bygaschromatography.Calibration
lated Chemicals
of the gas chromatography system is done by the external
D 6809 Guide for Quality Control and Quality Assurance
standard calibration technique.
Procedures for Aromatic Hydrocarbons and Related Ma-
1.2 This test method has been found applicable to the
terials
measurement of impurities such as cumene, 3-methyl-2-
E 29 Practice for Using Significant Digits in Test Data to
cyclopentene-1-one, n-propylbenzene, tert-butylbenzene, sec-
Determine Conformance with Specifications
butylbenzene, cis-2-phenyl-2-butene, acetophenone, 1-phenyl-
E 355 Practice for Gas Chromatography Terms and Rela-
1-butene, 2-phenyl-2-propanol, trans-2-phenyl-2-butene,
tionships
m-cymene, p-cymene, and phenol, which are common to the
E 691 Practice for Conducting an Interlaboratory Study to
manufacturing process of AMS. The method has also been
Determine the Precision of a Test Method
found applicable for the determination of para-tertiary-
E 1510 Practice for Installing Fused Silica Open Tubular
butylcatechol typically added as a stabilizer to AMS. The
Capillary Columns in Gas Chromatographs
impurities in AMS can be analyzed over a range of 5 to 800
2.2 Other Document:
mg/kg by this method. (SeeTable 1.)The limit of detection for
OSHA Regulations, 29 CFR, paragraphs 1910.1000 and
these impurities is typically in the range of 5 to 10 mg/kg. (See
3
1910.1200
Table 1.)
1.3 In determining the conformance of the test results using
3. Terminology
this method to applicable specifications, results shall be
3.1 See Terminology D 4790 for definition of terms used in
rounded off in accordance with the rounding-off method of
this test method.
Practice E 29.
1.4 This standard does not purport to address all the safety
4. Summary of Test Method
concerns, if any, associated with its use. It is the responsibility
4.1 AMS (alpha-methylstyrene) is analyzed by a gas chro-
of the user of this standard to establish appropriate safety and
matograph (GC) equipped with a flame ionization detector
health practices and determine the applicability of regulatory
(FID). A precisely repeatable volume of the sample to be
limitations prior to use. For specific hazard statements, see
analyzed is injected onto the gas chromatograph. The peak
Section 8.
areas of the impurities are measured and converted to concen-
2. Referenced Documents trations via an external standard methodology. Purity by GC
2 (the AMS content) is calculated by subtracting the sum of the
2.1 ASTM Standards:
impurities from 100.00. Results are reported in weight percent.
D 3437 Practice for Sampling and Handling Liquid Cyclic
Products
5. Significance and Use
5.1 This test method is suitable for setting specifications on
1
This test method is under the jurisdiction of ASTM Committee D16 on
thematerialsreferencedin1.2andforuseasaninternalquality
Aromatic Hydrocarbons and Related Chemicals and is the direct responsibility of
control tool where AMS is produced or is used in a manufac-
Subcommittee D16.07 on Styrene, Ethylbenzene, and C and C Aromatic
9 10
turing process. It may also be used in development or research
Hydrocarbons.
Current edition approved Jan. 1, 2004. Published January 2004. Originally
work involving AMS.
approved in 1997. Last previous edition approved in 1997 as D 6144 - 97.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
3
Standards volume information, refer to the standard’s Document Summary page on AvailablefromU.S.GovernmentPrintingOfficeSuperintendentofDocuments,
the ASTM website. 732 N. Capitol St., NW, Mail Stop: SDE, Washington, DC 20401.
*A Summary of Changes section appears at the end of this standard.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1

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D6144–04
TABLE 1 Summary of Precision Data (mg/kg)
Compound Repeatability Reproducibility Range Studied
Acetone 1.61 + 0.035*Acetone 0.47 + 1.10*Acetone 0.5 – 26
Cumene −0.46 + 0.031*Cumene 7.88 + 0.19*Cumene 45 – 290
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