ASTM D4590-00
(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
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 known to produce color 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 The following applies to all specified limits in this standard: for purposes of determining conformance with this standard, an observed value or a calculated value shall be rounded off "to the nearest unit" in the last right-hand digit used in expressing the specification limit, in accordance with the rounding-off method of Practice E29.
1.3 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 7.
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Designation:D4590–00
Standard Test Method for
Colorimetric Determination of p-tert-Butylcatechol In Styrene
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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 (e) indicates an editorial change since the last revision or reapproval.
1. Scope 3. Summary of Method
1.1 This test method is applicable to the determination of 3.1 Color is developed in the specimen by the addition of
residual 4-tertiary-butylcatechol (TBC) in styrene monomer or caustic in a methanol-octanol solvent. The pink color intensity
AMS in the 1 to 100 ppm range. Any other compound known is measured with a spectrophotometer and compared to a
to produce color when contacted with aqueous sodium hydrox- calibration curve for quantitation.
ide solution will interfere. It may be compensated for by
4. Significance and Use
including it in the preparation of the standard solutions, if its
identity and concentration in the sample are known. 4.1 This test method is suitable for determining the quantity
of TBC inhibitor, both for the protection against polymeriza-
1.2 The following applies to all specified limits in this
standard: for purposes of determining conformance with this tion while in transit and storage, and for internal quality
control.
standard, an observed value or a calculated value shall be
rounded off “to the nearest unit” in the last right-hand digit
5. Apparatus
used in expressing the specification limit, in accordance with
5.1 Visible Range Spectrophotometer, equipped with ab-
the rounding-off method of PracticeE29.
sorption cells providing light paths from 1 to 5 cm for use at
1.3 This standard does not purport to address all of the
approximately 490 nm.
safety concerns, if any, associated with its use. It is the
5.2 Volumetric Pipets, 5 mL.
responsibility of the user of this standard to establish appro-
5.3 Pipetors, 0.1 and 0.2 mL.
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use. For specific
6. Reagents and Materials
statements on hazards, see Section 7.
6.1 Purity of Reagents—Where unspecified, chemicals shall
2. Referenced Documents
be reagent grade and conform to recognized specifications if
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such exist. If found to have no adverse effect on accuracy,
2.1 ASTM Standards:
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other grades may be used.
D 1193 Specification for Reagent Water
6.2 4-Tertiary-Butylcatechol, Mp 52-55°C.
D 3437 Practice for Sampling and Handling Liquid Cyclic
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6.3 Toluene, ACS reagent grade.
Products
6.4 Methanol, reagent grade.
E29 Practice for Using Significant Digits in Test Data to
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6.5 n-Octanol, reagent grade.
Determine Conformance with Specifications
6.6 Sodium Hydroxide Pellets, reagent grade.
2.2 Other Document:
6.7 Alcoholic Sodium Hydroxide, approximately 0.15 N.
OSHA Regulations, 29 CFR, paragraphs 1910.1000 and
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Dissolve 0.3 g NaOH in 25 mL methanol. Add 25 mL of
1910.1200
n-octanol and 100 µLof water. Let this reagent mature for two
days before use. This solution is stable for two weeks.
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This test method is under the jurisdiction of ASTM Committee D16 on
6.8 TBC Stock Standard—Weigh 0.5 g ofTBC into 500 g of
Aromatic Hydrocarbons and Related Chemicals and is the direct responsibility of
toluene. This solution will contain 1000 ppm TBC. This
Subcommittee D16.07 on Styrene, Ethylbenzene, and C and C Aromatic
9 10
Hydrocarbons.
Current edition approved Dec. 10, 2000. Published February 2001. Originally
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published as D 4590 – 86. Last previous edition D 4590 – 95a. Reagent Chemicals, American Chemical Society Specifications, American
2
Annual Book of ASTM Standards, Vol 11.01. Chemical Society, Washington, DC. For suggestions on the testing of reagents not
3
Annual Book of ASTM Standards, Vol 06.04. listed by the American Chemical Society, see Analar Standards for Laboratory
4
Annual Book of ASTM Standards, Vol 14.02. Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
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Available from the Superintendent of Documents, U.S. Government Printing and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
Office, Washington, D.C. 20402. MD.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
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D4590–00
NOTE 5—If a blue color persists before the methanol is added, the
standard should have a shelf life of one year or better if stored
concentration range has been exceeded. Dilute the specimen 1:10 with
in a refrigerator or freezer. Storing standards in amber bottles
toluene and rep
...
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