ASTM D4590-09
(Test Method)Standard Test Method for Colorimetric Determination of p-tert-Butylcatechol In Styrene Monomer or AMS (alpha-Methylstyrene) by Spectrophotometry
Standard Test Method for Colorimetric Determination of <i>p-tert</i>-Butylcatechol In Styrene Monomer or AMS (alpha-Methylstyrene) by Spectrophotometry
SIGNIFICANCE AND USE
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 ppm (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 E 29.
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 and health practices and determine the applicability of regulatory limitations prior to use. For specific statements on hazards, see Section 8.
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Designation: D4590 − 09
StandardTest 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* D6809 Guide for Quality Control and Quality Assurance
Procedures for Aromatic Hydrocarbons and Related Ma-
1.1 This test method is applicable to the determination of
terials
residual 4-tertiary-butylcatechol (TBC) in styrene monomer or
E29 Practice for Using Significant Digits in Test Data to
AMS in the 1 to 100 ppm (mg/kg) range.Any other compound
Determine Conformance with Specifications
producing color at 490 nm when contacted with aqueous
E691 Practice for Conducting an Interlaboratory Study to
sodium hydroxide solution will interfere. It may be compen-
Determine the Precision of a Test Method
sated for by including it in the preparation of the standard
2.2 Other Document:
solutions, if its identity and concentration in the sample are
OSHA Regulations, 29 CFR paragraphs 1910.1000 and
known.
3
1910.1200
1.2 In determining the conformance of the test results using
this method to applicable specifications, results shall be 3. Terminology
rounded off in accordance with the rounding-off method of
3.1 See Terminology D4790 for definition of terms used in
Practice E29.
this standard.
1.3 The values stated in SI units are to be regarded as
4. Summary of Method
standard. No other units of measurement are included in this
standard.
4.1 Color is developed in the specimen by the addition of
caustic in a methanol-octanol solvent.The intensity of the pink
1.4 This standard does not purport to address all of the
color is measured with a spectrometer and compared to a
safety concerns, if any, associated with its use. It is the
calibration curve for quantitation.
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica-
5. Significance and Use
bility of regulatory limitations prior to use. For specific
5.1 This test method is suitable for determining the quantity
statements on hazards, see Section 8.
of TBC inhibitor, both for the protection against polymeriza-
2. Referenced Documents
tion while in transit and storage, and for internal quality
2
control.
2.1 ASTM Standards:
D1193 Specification for Reagent Water
6. Apparatus
D3437 Practice for Sampling and Handling Liquid Cyclic
6.1 Visible Range Spectrometer , equipped with absorption
Products
cells providing light paths from 1 to 5 cm for use at approxi-
D4790 Terminology ofAromatic Hydrocarbons and Related
mately 490 nm.
Chemicals
6.2 Volumetric Pipets and Pipetors—The sample pipet vol-
1
ume should be sized to fill the spectrometer absorption cell.
This test method is under the jurisdiction of ASTM Committee D16 on
Aromatic Hydrocarbons and Related Chemicals and is the direct responsibility of
Pipetor volumes must be scaled to the sample volume. This
Subcommittee D16.07 on Styrene, Ethylbenzene and C9 and C10 Aromatic
procedure is written using a 15 mL sample volume. The
Hydrocarbons.
following table shows how reagent pipetor volumes could be
CurrenteditionapprovedJune1,2009.PublishedJuly2009.Originallyapproved
scaled to usea5mL sample volume.
in 1986. Last previous edition approved in 2006 as D4590 – 06. DOI: 10.1520/
D4590-09.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
3
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM AvailablefromU.S.GovernmentPrintingOfficeSuperintendentofDocuments,
Standards volume information, refer to the standard’s Document Summary page on 732 N. Capitol St., NW, Mail Stop: SDE, Washington, DC 20401, http://
the ASTM website. 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 − 09
8.3 Flammable Hazards—Styrene monomer is flammable
Sample Pipet, 0.15 NaOH Pipe- Methanol Pipetor,
mL tor, µL
and polymerizes exothermally in the presence of peroxide,
µL
mineral acids, and aluminum chloride.
15 300 600
5 100 200
9. Sampling
9.1 Collect the samples in accordance with Practice D3437.
7. Reagents and Materials
7.1 Purity of Reagents—Where unspecified, chemicals shall
10. Preparation of Calibration Curve
be reagent grade and conform to recognized specifications if
10.1 Prepare standards of 5, 10, 20, 30, 40, 50, 70, and 100
4
such exist. If
...
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:D4590–06 Designation: D 4590 – 09
Standard Test Method for
Colorimetric Determination of p-tert-Butylcatechol In Styrene
1
Monomer or AMS (a–Methylstyrene) by Spectrophotometry
This standard is issued under the fixed designation D 4590; 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 orAMS
in the 1 to 100 ppm (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 E 29.
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 and health practices and determine the applicability of regulatory
limitations prior to use. For specific statements on hazards, see Section 8.
2. Referenced Documents
2
2.1 ASTM Standards:
D 1193 Specification for Reagent Water
D 3437 Practice for Sampling and Handling Liquid Cyclic Products
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
E29 Practice for Using Significant Digits in Test Data to Determine Conformance with Specifications
E 691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
2.2 Other Document:
3
OSHA Regulations, 29CFR paragraphs 1910.1000 and 1910.1200
3. Terminology
3.1 See Terminology D 4790 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.
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. Apparatus
6.1 Visible Range Spectrometer , equipped with absorption cells providing light paths from 1 to 5 cm for use at approximately
490 nm.
6.2 Volumetric Pipets and Pipetors —The sample pipet volume should be sized to fill the spectrometer absorption cell. Pipetor
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 and C Aromatic Hydrocarbons.
9 10
Current edition approved June 1, 2006.2009. Published June 2006.July 2009. Originally approved in 1986. Last previous edition approved in 20002006 as D 4590 – 006.
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 ----------------------
D4590–09
volumes must be scaled to the sample volume.This procedure is written using a 15 mLsample volume.The following table shows
how reagent pipetor volumes could be scaled to usea5mL sample volume.
2
---------------------- Page: 2 ----------------------
D4590–09
Sample Pipet, 0.15 NaOH Pipetor, Methanol Pipetor,
mL µL µL
15 300 600
5 100 200
7. Reagents and Materials
7.1 Purity of Reagents—Where unspecified, chemicals shall be reagent grade an
...
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