ASTM D6144-08
(Test Method)Standard Test Method for Analysis of AMS (α-Methylstyrene) by Capillary Gas Chromatography
Standard Test Method for Analysis of AMS (<span class='unicode'>α</span>-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 (α-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 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.5 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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Designation: D6144 − 08
StandardTest Method for
Analysis of AMS (α-Methylstyrene) by Capillary Gas
1
Chromatography
This standard is issued under the fixed designation D6144; 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* 2. Referenced Documents
2
2.1 ASTM Standards:
1.1 This test method covers the determination of the purity
D3437 Practice for Sampling and Handling Liquid Cyclic
ofAMS (α-methylstyrene) by gas chromatography. Calibration
Products
of the gas chromatography system is done by the external
D4307 Practice for Preparation of Liquid Blends for Use as
standard calibration technique.
Analytical Standards
1.2 This test method has been found applicable to the
D4790 Terminology ofAromatic Hydrocarbons and Related
measurement of impurities such as cumene, 3-methyl-2- Chemicals
cyclopentene-1-one, n-propylbenzene, tert-butylbenzene, sec- D6809 Guide for Quality Control and Quality Assurance
Procedures for Aromatic Hydrocarbons and Related Ma-
butylbenzene, cis-2-phenyl-2-butene, acetophenone, 1-phenyl-
terials
1-butene, 2-phenyl-2-propanol, trans-2-phenyl-2-butene,
E29 Practice for Using Significant Digits in Test Data to
m-cymene, p-cymene, and phenol, which are common to the
Determine Conformance with Specifications
manufacturing process of AMS. The method has also been
E355 Practice for Gas Chromatography Terms and Relation-
found applicable for the determination of para-tertiary-
ships
butylcatechol typically added as a stabilizer to AMS. The
E691 Practice for Conducting an Interlaboratory Study to
impurities in AMS can be analyzed over a range of 5 to 800
Determine the Precision of a Test Method
mg/kg by this method. (See Table 1.)The limit of detection for
E1510 Practice for Installing Fused Silica Open Tubular
these impurities is typically in the range of 5 to 10 mg/kg. (See
Capillary Columns in Gas Chromatographs
Table 1.)
2.2 Other Document:
1.3 In determining the conformance of the test results using
OSHA Regulations, 29 CFR paragraphs 1910.1000 and
3
this method to applicable specifications, results shall be
1910.1200
rounded off in accordance with the rounding-off method of
Practice E29. 3. Terminology
3.1 See Terminology D4790 for definition of terms used in
1.4 The values stated in SI units are to be regarded as
this test method.
standard. No other units of measurement are included in this
standard.
4. Summary of Test Method
1.5 This standard does not purport to address all the safety
4.1 AMS (α-methylstyrene) is analyzed by a gas chromato-
concerns, if any, associated with its use. It is the responsibility
graph (GC) equipped with a flame ionization detector (FID).A
of the user of this standard to establish appropriate safety and
precisely repeatable volume of the sample to be analyzed is
health practices and determine the applicability of regulatory
injected onto the gas chromatograph. The peak areas of the
limitations prior to use. For specific hazard statements, see
impurities are measured and converted to concentrations via an
Section 8.
external standard methodology. Purity by GC (the AMS
1 2
This test method is under the jurisdiction of ASTM Committee D16 on For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Aromatic Hydrocarbons and Related Chemicals and is the direct responsibility of contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Subcommittee D16.07 on Styrene, Ethylbenzene and C9 and C10 Aromatic Standards volume information, refer to the standard’s Document Summary page on
Hydrocarbons. the ASTM website.
3
Current edition approved June 1, 2008. Published June 2008. Originally AvailablefromU.S.GovernmentPrintingOfficeSuperintendentofDocuments,
approved in 1997. Last previous edition approved in 2004 as D6144 - 04. DOI: 732 N. Capitol St., NW, Mail Stop: SDE, Washington, DC 20401, http://
10.1520/D6144-08. www.access.gpo.gov.
*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
---------------------- Page: 1 ----------------------
D6144 − 08
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
nPropylbenzene (NPB) 2.11 + 0.03*NPB −7.81 + 0.37*NPB 55 – 195
Phenol 1.84 3.65 + 0.58*Phenol 1 – 40
tertButylbenzene (TBB) −1.22 + 0.035*TBB 3.63 + 0.087*TBB 150 – 650
secButylbenzene (SBB) 4.23 + 0.019*SBB 21.60 + 0.25*SBB 200 – 765
mCymene 0
...
This document is not anASTM standard and is intended only to provide the user of anASTM 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:D6144–04 Designation: D 6144 – 08
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 (´) indicates an editorial change since the last revision or reapproval.
1. Scope*
1.1 This test method covers the determination of the purity of AMS (a-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,andphenol,whicharecommontothemanufacturingprocessofAMS.
The method has also been found applicable for the determination of para-tertiary-butylcatechol typically added as a stabilizer to
AMS.The impurities inAMS can be analyzed over a range of 5 to 800 mg/kg by this method. (SeeTable 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
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.5 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.
2. Referenced Documents
2
2.1 ASTM Standards:
D 3437 Practice for Sampling and Handling Liquid Cyclic Products
D 4307 Practice for Preparation of Liquid Blends for Use as Analytical Standards
D 4790 Terminology of Aromatic Hydrocarbons and Related Chemicals
D 6809 Guide for Quality Control and Quality Assurance Procedures for Aromatic Hydrocarbons and Related Materials
E 29 Practice for Using Significant Digits in Test Data to Determine Conformance with Specifications
E 355 Practice for Gas Chromatography Terms and Relationships
E 691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
E 1510 Practice for Installing Fused Silica Open Tubular Capillary Columns in Gas Chromatographs
2.2 Other Document:
OSHA Regulations, 29CFR, paragraphs 1910.1000 and 1910.1200OSHA Regulations, 29CFR paragraphs 1910.1000 and
3
1910.1200
3. Terminology
3.1 See Terminology D 4790 for definition of terms used in this test method.
4. Summary of Test Method
4.1 AMS (alpha-methylstyrene)(a-methylstyrene) is analyzed by a gas chromatograph (GC) equipped with a flame ionization
detector (FID).Aprecisely repeatable volume of the sample to be analyzed is injected onto the gas chromatograph.The peak areas
1
This test method is under the jurisdiction ofASTM Committee D16 onAromatic Hydrocarbons and Related Chemicals and is the direct responsibility of Subcommittee
D16.07 on Styrene, Ethylbenzene, and C C9 and C Aromatic Hydrocarbons.C10 Atomatic Hydrocarbons .
9 10
Current edition approved Jan.June 1, 2004.2008. Published January 2004.June 2008. Originally approved in 1997. Last previous edition approved in 19972004 as
D6144-97.D 6144 - 04.
2
For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
3
Available from U.S. Government Printing Office Superintendent of Documents, 732 N. Capitol St., NW, Mail Stop: SDE, Washington, DC 20401, http://
www.access.gpo.gov.
*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
---------------------- Page: 1 ----------------------
D6144–08
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
Cu
...
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