ASTM D4590-18
(Test Method)Standard Test Method for Colorimetric Determination of p-tert-Butylcatechol In Styrene Monomer or AMS (α–Methylstyrene) by Spectrophotometry
Standard Test Method for Colorimetric Determination of <emph type="ital">p-tert</emph >-Butylcatechol In Styrene Monomer or AMS (α–Methylstyrene) by Spectrophotometry
SIGNIFICANCE AND USE
5.1 This test method is suitable for determining the quantity of TBC inhibitor, both for the protection against polymerization while in transit and storage, and for internal quality control.
SCOPE
1.1 This test method is applicable to the determination of residual 4-tertiary-butylcatechol (TBC) in styrene monomer or AMS in the 1 to 100 mg/kg range. Any other compound producing color at 490 nm when contacted with aqueous sodium hydroxide solution will interfere. It may be compensated for by including it in the preparation of the standard solutions, if its identity and concentration in the sample are known.
1.2 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. The limit of detection is 0.2 mg/kg while the limit of quantitation is 0.8 mg/kg based on the ILS data in Table 1.
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.4 This standard 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 standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use. For specific statements on hazards, see Section 8.
1.5 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.
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Designation: D4590 − 18
Standard Test Method for
Colorimetric Determination of p-tert-Butylcatechol In Styrene
1
Monomer or AMS (α–Methylstyrene) by Spectrophotometry
This standard is issued under the fixed designation D4590; 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 is applicable to the determination of
D1193 Specification for Reagent Water
residual 4-tertiary-butylcatechol (TBC) in styrene monomer or
AMS in the 1 to 100 mg/kg range. Any other compound D3437 Practice for Sampling and Handling Liquid Cyclic
Products
producing color at 490 nm when contacted with aqueous
sodium hydroxide solution will interfere. It may be compen- D4790 Terminology ofAromatic Hydrocarbons and Related
Chemicals
sated for by including it in the preparation of the standard
solutions, if its identity and concentration in the sample are D6809 Guide for Quality Control and Quality Assurance
Procedures for Aromatic Hydrocarbons and Related Ma-
known.
terials
1.2 In determining the conformance of the test results using
E29 Practice for Using Significant Digits in Test Data to
this method to applicable specifications, results shall be
Determine Conformance with Specifications
rounded off in accordance with the rounding-off method of
E691 Practice for Conducting an Interlaboratory Study to
Practice E29. The limit of detection is 0.2 mg/kg while the
Determine the Precision of a Test Method
limit of quantitation is 0.8 mg/kg based on the ILS data in
2.2 Other Document:
Table 1.
OSHA Regulations, 29 CFR paragraphs 1910.1000 and
3
1.3 The values stated in SI units are to be regarded as
1910.1200
standard. No other units of measurement are included in this
3. Terminology
standard.
3.1 See Terminology D4790 for definition of terms used in
1.4 This standard does not purport to address all of the
this standard.
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
4. Summary of Method
priate safety, health, and environmental practices and deter-
4.1 Color is developed in the specimen by the addition of
mine the applicability of regulatory limitations prior to use.
caustic in a methanol-octanol solvent.The intensity of the pink
For specific statements on hazards, see Section 8.
color is measured with a spectrometer and compared to a
1.5 This international standard was developed in accor-
calibration curve for quantitation.
dance with internationally recognized principles on standard-
ization established in the Decision on Principles for the
5. Significance and Use
Development of International Standards, Guides and Recom-
5.1 This test method is suitable for determining the quantity
mendations issued by the World Trade Organization Technical
of TBC inhibitor, both for the protection against polymeriza-
Barriers to Trade (TBT) Committee.
tion while in transit and storage, and for internal quality
control.
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 service@astm.org. 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, 2018. Published June 2018. Originally AvailablefromU.S.GovernmentPrintingOfficeSuperintendentofDocuments,
approved in 1986. Last previous edition approved in 2013 as D4590 – 13. DOI: 732 N. Capitol St., NW, Mail Stop: SDE, Washington, DC 20401, http://
10.1520/D4590-18. 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 ----------------------
D4590 − 18
TABLE 1 Intermediate Precision and Reproducibility
(weighed to the nearest 0.1 g). This solution will have a
TBC Observed concentration of approximately 1000 mg/kg TBC in toluene
Repeatability Reproducibility
Concentration
and the exact concentration can be calculated using Eq 1. This
4.7 0.23 0.94
standard should have a shelf life of one year or better if stored
15.2 0.47 5.08
24.5 1.55 4.91 in a refrigerator or freezer. Storing standards in amber bottles
94.6 3.98 9.94
significantly reduces degradation of standards with time.
mg TBC/kg toluene 5
...
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: D4590 − 13 D4590 − 18
Standard Test Method for
Colorimetric Determination of p-tert-Butylcatechol In Styrene
1
Monomer or AMS (α–Methylstyrene) by Spectrophotometry
This standard is issued under the fixed designation D4590; 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 is applicable to the determination of residual 4-tertiary-butylcatechol (TBC) in styrene monomer or AMS
in the 1 to 100 mg/kg range. Any other compound producing color at 490 nm when contacted with aqueous sodium hydroxide
solution will interfere. It may be compensated for by including it in the preparation of the standard solutions, if its identity and
concentration in the sample are known.
1.2 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. The limit of detection is 0.2 mg/kg while the limit of quantitation
is 0.8 mg/kg based on the ILS data in Table 1.
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.4 This standard 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 standard to establish appropriate safety safety, health, and healthenvironmental practices and determine the
applicability of regulatory limitations prior to use. For specific statements on hazards, see Section 8.
1.5 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:
D1193 Specification for Reagent Water
D3437 Practice for Sampling and Handling Liquid Cyclic Products
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
E691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
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 standard.
4. Summary of Method
4.1 Color is developed in the specimen by the addition of caustic in a methanol-octanol solvent. The intensity of the pink color
is measured with a spectrometer and compared to a calibration curve for quantitation.
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, 2018. Published June 2013June 2018. Originally approved in 1986. Last previous edition approved in 20092013 as
D4590 – 09.D4590 – 13. DOI: 10.1520/D4590-13.10.1520/D4590-18.
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 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 ----------------------
D4590 − 18
TABLE 1 Intermediate Precision and Reproducibility
TBC Observed
Repeatability Reproducibility
Concentration
4.7 0.23 0.94
15.2 0.47 5.08
24.5 1.55 4.91
94.6 3.98 9.94
5. Significance and Use
5.1 This test method is suitable for determining the quantity of TBC inhibitor, both for the protection against polymerization
while in transit and storage, and for internal quality control.
6. A
...
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