ASTM D4590-06
(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 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.
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.
General Information
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Standards Content (Sample)
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Designation:D4590–06
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* D 6809 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 range. Any other compound
Determine Conformance with Specifications
producing color at 490 nm when contacted with aqueous
E 691 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, 29CFR 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 D 4790 for definition of terms used in
PracticeE29.
this standard.
1.3 The values stated in SI units are to be regarded as
standard. No other units of measurement are included in this
4. Summary of Method
standard.
4.1 Color is developed in the specimen by the addition of
1.4 This standard does not purport to address all of the
caustic in a methanol-octanol solvent.The intensity of the pink
safety concerns, if any, associated with its use. It is the
color is measured with a spectrometer and compared to a
responsibility of the user of this standard to establish appro-
calibration curve for quantitation.
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use. For specific
5. Significance and Use
statements on hazards, see Section 8.
5.1 This test method is suitable for determining the quantity
of TBC inhibitor, both for the protection against polymeriza-
2. Referenced Documents
2 tion while in transit and storage, and for internal quality
2.1 ASTM Standards:
control.
D 1193 Specification for Reagent Water
D 3437 Practice for Sampling and Handling Liquid Cyclic
6. Apparatus
Products
6.1 Visible Range Spectrometer, equipped with absorption
D 4790 Terminology of Aromatic Hydrocarbons and Re-
cells providing light paths from 1 to 5 cm for use at approxi-
lated Chemicals
mately 490 nm.
6.2 Volumetric Pipets and Pipetors—The sample pipet vol-
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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
Current edition approved June 1, 2006. Published June 2006. Originally
approved in 1986. Last previous edition approved in 2000 as D 4590 – 00. scaled to usea5mL sample volume.
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
3
Standards volume information, refer to the standard’s Document Summary page on AvailablefromU.S.GovernmentPrintingOfficeSuperintendentofDocuments,
the ASTM website. 732 N. Capitol St., NW, Mail Stop: SDE, Washington, DC 20401.
*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.
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D4590–06
NOTE 1—Both the stock solution and toluene diluent should be at room
Sample Pipet, 0.15 NaOH Pipetor, Methanol Pipetor,
temperature. Temperature differences will cause dilution errors due to
mL µL µL
15 300 600
variations in density.
5 100 200
10.2 Determine the absorbance of each standard solution
7. Reagents and Materials
and one reagent blank in accordance with Section 11.
10.3 Plot absorbance versus concentration on standard
7.1 Purity of Reagents—Where unspecified, chemicals shall
graph paper.
be reagent grade and conform to recognized specifications if
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such exist. If found to have no adv
...
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