ASTM D6144-22

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

SIGNIFICANCE AND USE
5.1 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.  
5.2 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 (TBC or PTBC) 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 2.) Based on the results in ASTM Research Report RR:D16-1022, summarized in Table 2, the limit of quantitation for these impurities averages 4 mg/kg, while the limit of detection averages 1.2 mg/kg.  
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 E29.  
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, health, and environmental practices and determine the applicability of regulatory limitations prior to use. For specific hazard statements, see Section 8.  
1.6 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

General Information

• Status: Published
• Publication Date: 31-Dec-2021
• ICS: 71.040.50 - Physicochemical methods of analysis
• Technical Committee: D16 - Aromatic, Industrial, Specialty and Related Chemicals
• Drafting Committee: D16.07 - Styrene, Ethylbenzene and C9 and C10 Aromatic Hydrocarbons

Standards Content (Sample)

This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation: D6144 − 22
Standard Test 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* 1.6 This international standard was developed in accor-
dance with internationally recognized principles on standard-
1.1 This test method covers the determination of the purity
ization established in the Decision on Principles for the
ofAMS (α-methylstyrene) by gas chromatography. Calibration
Development of International Standards, Guides and Recom-
of the gas chromatography system is done by the external
mendations issued by the World Trade Organization Technical
standard calibration technique.
Barriers to Trade (TBT) Committee.
1.2 This test method has been found applicable to the
measurement of impurities such as cumene, 3-methyl-2-
2. Referenced Documents
cyclopentene-1-one, n-propylbenzene, tert-butylbenzene, sec-
2
2.1 ASTM Standards:
butylbenzene, cis-2-phenyl-2-butene, acetophenone, 1-phenyl-
D3437 Practice for Sampling and Handling Liquid Cyclic
1-butene, 2-phenyl-2-propanol, trans-2-phenyl-2-butene,
Products
m-cymene, p-cymene, and phenol, which are common to the
manufacturing process of AMS. The method has also been D4307 Practice for Preparation of Liquid Blends for Use as
found applicable for the determination of para-tertiary- Analytical Standards
butylcatechol (TBC or PTBC) typically added as a stabilizer to D4790 Terminology ofAromatic Hydrocarbons and Related
AMS. The impurities inAMS can be analyzed over a range of
Chemicals
5 to 800 mg/kg by this method. (See Table 2.) Based on the D6809 Guide for Quality Control and Quality Assurance
results in ASTM Research Report RR:D16-1022, summarized
Procedures for Aromatic Hydrocarbons and Related Ma-
in Table 2, the limit of quantitation for these impurities
terials
averages 4 mg/kg, while the limit of detection averages
E29 Practice for Using Significant Digits in Test Data to
1.2 mg⁄kg.
Determine Conformance with Specifications
E355 Practice for Gas Chromatography Terms and Relation-
1.3 In determining the conformance of the test results using
ships
this method to applicable specifications, results shall be
E691 Practice for Conducting an Interlaboratory Study to
rounded off in accordance with the rounding-off method of
Determine the Precision of a Test Method
Practice E29.
E1510 Practice for Installing Fused Silica Open Tubular
1.4 The values stated in SI units are to be regarded as
Capillary Columns in Gas Chromatographs
standard. No other units of measurement are included in this
2.2 Other Document:
standard.
OSHA Regulations, 29 CFR paragraphs 1910.1000 and
1.5 This standard does not purport to address all the safety
3
1910.1200
concerns, if any, associated with its use. It is the responsibility
of the user of this standard to establish appropriate safety,
3. Terminology
health, and environmental practices and determine the appli-
cability of regulatory limitations prior to use. For specific 3.1 See Terminology D4790 for definition of terms used in
hazard statements, see Section 8. this test method.
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, Industrial, Specialty and Related Chemicals and is the direct responsi- contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
bility of Subcommittee D16.07 on Styrene, Ethylbenzene and C9 and C10Aromatic Standards volume information, refer to the standard’s Document Summary page on
Hydrocarbons. the ASTM website.
3
Current edition approved Jan. 1, 2022. Published January 2022. Originally AvailablefromU.S.GovernmentPrintingOfficeSuperintendentofDocuments,
approved in 1997. Last previous edition approved in 2017 as D6144 – 17. DOI: 732 N. Capitol St., NW, Mail Stop: SDE, Washington, DC 20401, http://
10.1520/D6144-22. 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 − 22
4. Summary of Test Method strate that the results are consistent with the precision state-
ment. Recorders are not considered adequate for meeting the
4.1 AMS (α-methylstyrene) is analyzed by a gas chromato
...

This document is not an ASTM standard and is intended only to provide the user of an ASTM 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 − 17 D6144 − 22
Standard Test 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*
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 (TBC or PTBC) 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
Table 2.) Based on the results in ASTM Research Report RR:D16-1022, summarized in Table 2, the limit of quantitation for these
these impurities averages 4 mg/kg, while the limit of detection averages 1.21.2 mg mg/kg. (See ⁄kg. 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 E29.
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 safety, health, and healthenvironmental practices and determine the
applicability of regulatory limitations prior to use. For specific hazard statements, see Section 8.
1.6 This international standard was developed in accordance with internationally recognized principles on standardization
established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued
by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
2. Referenced Documents
2
2.1 ASTM Standards:
D3437 Practice for Sampling and Handling Liquid Cyclic Products
D4307 Practice for Preparation of Liquid Blends for Use as Analytical Standards
D4790 Terminology of Aromatic Hydrocarbons and Related Chemicals
D6809 Guide for Quality Control and Quality Assurance Procedures for Aromatic Hydrocarbons and Related Materials
1
This test method is under the jurisdiction of ASTM Committee D16 on Aromatic, Industrial, Specialty and Related Chemicals and is the direct responsibility of
Subcommittee D16.07 on Styrene, Ethylbenzene and C9 and C10 Aromatic Hydrocarbons.
Current edition approved June 1, 2017Jan. 1, 2022. Published June 2017January 2022. Originally approved in 1997. Last previous edition approved in 20132017 as
D6144D6144 – 17. – 13. DOI: 10.1520/D6144-17.10.1520/D6144-22.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
*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 − 22
TABLE 12 Summary of Precision Data (mg/kg)
Compound Repeatability (r) Reproducibility (R) 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
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
n-Propylbenzene (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
tert-Butylbenzene (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
sec-Butylbenzene
...