ASTM D6144-17

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 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 quantitation for these these impurities averages 4 mg/kg, while the limit of detection averages 1.2 mg/kg. (See Table 1.)  
TABLE 1 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  
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  
0.31 + 0.035*mCymene  
2.34 + 0.35*mCymene  
2 – 50  
oCymene  
1.63  
8.00  
29 – 31  
pCymene  
5.12  
15.79  
10 – 18  
cis-2-Phenyl-2-Butene (CPB)  
0.17 + 0.030*CPB  
5.39 + 0.11*CPB  
50 – 225  
trans-2-Phenyl-2-Butene (TPB)  
1.57  
0.54 + 0.20*TPB  
19 – 70  
1-Phenyl-1-Butene (PB)  
4.00 + 0.018*PB  
0.17 + 0.19*PB  
0.2 – 735  
Acetophenone (AP)  
–1.09 + 0.15*AP  
1.17 + 0.63*AP  
15 – 115  
para-tert-Butylcatechol (PTBC)  
2.21  
17.82  
10 – 19  
2-Methylbenzofuran (MBF)  
0.33 + 0.76*MBF  
0.75 + 0.60*MBF  
1 – 2  
2-Phenylpropion aldehyde (PPA)  
0.59 + 0.11*PPA  
0.29 + 0.23*PPA  
1.5 – 15  
α-Methylstyrene Oxide (AMSO)  
4.61  
6.51 + 0.23*AMSO  
13 – 32  
DimethylBenzyl Alcohol (DMBA)  
0.38  
0.55 + 2.03*DMBA  
0.1 – 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 and health 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: Historical
• Publication Date: 31-May-2017
• 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)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation: D6144 − 17
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* Development of International Standards, Guides and Recom-
mendations issued by the World Trade Organization Technical
1.1 This test method covers the determination of the purity
Barriers to Trade (TBT) Committee.
ofAMS (α-methylstyrene) by gas chromatography. Calibration
of the gas chromatography system is done by the external
2. Referenced Documents
standard calibration technique.
2
2.1 ASTM Standards:
1.2 This test method has been found applicable to the
D3437 Practice for Sampling and Handling Liquid Cyclic
measurement of impurities such as cumene, 3-methyl-2-
Products
cyclopentene-1-one, n-propylbenzene, tert-butylbenzene, sec-
D4307 Practice for Preparation of Liquid Blends for Use as
butylbenzene, cis-2-phenyl-2-butene, acetophenone, 1-phenyl-
Analytical Standards
1-butene, 2-phenyl-2-propanol, trans-2-phenyl-2-butene,
D4790 Terminology ofAromatic Hydrocarbons and Related
m-cymene, p-cymene, and phenol, which are common to the
Chemicals
manufacturing process of AMS. The method has also been
D6809 Guide for Quality Control and Quality Assurance
found applicable for the determination of para-tertiary-
Procedures for Aromatic Hydrocarbons and Related Ma-
butylcatechol typically added as a stabilizer to AMS. The
terials
impurities in AMS can be analyzed over a range of 5 to 800
E29 Practice for Using Significant Digits in Test Data to
mg/kg by this method. (See Table 1.) The limit of quantitation
Determine Conformance with Specifications
for these these impurities averages 4 mg/kg, while the limit of
E355 Practice for Gas Chromatography Terms and Relation-
detection averages 1.2 mg/kg. (See Table 1.)
ships
1.3 In determining the conformance of the test results using
E691 Practice for Conducting an Interlaboratory Study to
this method to applicable specifications, results shall be
Determine the Precision of a Test Method
rounded off in accordance with the rounding-off method of
E1510 Practice for Installing Fused Silica Open Tubular
Practice E29.
Capillary Columns in Gas Chromatographs
2.2 Other Document:
1.4 The values stated in SI units are to be regarded as
OSHA Regulations, 29 CFR paragraphs 1910.1000 and
standard. No other units of measurement are included in this
3
1910.1200
standard.
1.5 This standard does not purport to address all the safety
3. Terminology
concerns, if any, associated with its use. It is the responsibility
3.1 See Terminology D4790 for definition of terms used in
of the user of this standard to establish appropriate safety and
this test method.
health practices and determine the applicability of regulatory
limitations prior to use. For specific hazard statements, see
4. Summary of Test Method
Section 8.
4.1 AMS (α-methylstyrene) is analyzed by a gas chromato-
1.6 This international standard was developed in accor-
graph (GC) equipped with a flame ionization detector (FID).A
dance with internationally recognized principles on standard-
precisely repeatable volume of the sample to be analyzed is
ization established in the Decision on Principles for the
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 June 1, 2017. Published June 2017. Originally AvailablefromU.S.GovernmentPrintingOfficeSuperintendentofDocuments,
approved in 1997. Last previous edition approved in 2013 as D6144 – 13. DOI: 732 N. Capitol St., NW, Mail Stop: SDE, Washington, DC 20401, http://
10.1520/D6144-17. 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 − 17
TABLE 1 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
nPropylbenzene (NPB) 2.11 + 0.03*NPB
...

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 − 13 D6144 − 17
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 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
detectionquantitation for these impurities is typically in the range of 5 to 10these impurities averages 4 mg/kg, while the limit of
detection averages 1.2 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 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 and health 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
E29 Practice for Using Significant Digits in Test Data to Determine Conformance with Specifications
E355 Practice for Gas Chromatography Terms and Relationships
E691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
E1510 Practice for Installing Fused Silica Open Tubular Capillary Columns in Gas Chromatographs
2.2 Other Document:
3
OSHA Regulations, 29 CFR paragraphs 1910.1000 and 1910.1200
3. Terminology
3.1 See Terminology D4790 for definition of terms used in this test method.
1
This test method is under the jurisdiction of ASTM Committee D16 on Aromatic Hydrocarbons 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, 2013June 1, 2017. Published June 2013June 2017. Originally approved in 1997. Last previous edition approved in 20122013 as D6144 –
12.13. DOI: 10.1520/D6144-13.10.1520/D6144-17.
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’sstandard’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 − 17
TABLE 1 Summary of Precision Data (mg
...