ASTM D4493-20

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Designation: D4493 − 16 D4493 − 20
Standard Test Method for
Solidification Point of Bisphenol A
(4,4'-Isopropylidenediphenol)
This standard is issued under the fixed designation D4493; 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 describes the procedure for determination of the solidification point of bisphenol A (4,4'-isopropylidene
diphenol).
1.2 The test method has been found applicable for determination of the solidification point between 150 and 157°C.
1.3 In determining 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 Warning—Mercury has been designated by many regulatory agencies as a hazardous substance that can cause serious
medical issues. Mercury, or its vapor, has been demonstrated to be hazardous to health and corrosive to materials. Use caution
when handling mercury and mercury-containing products. See the applicable product Safety Data Sheet (SDS) for additional
information. The potential exists that selling mercury or mercury-containing products, or both, is prohibited by local or national
law. Users must determine legality of sales in their location.
1.6 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 hazard statements, see Section 9.
1.7 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
2.1 ASTM Standards:
D1493 Test Method for Solidification Point of Industrial Organic Chemicals (Withdrawn 2004)
D4297 Practice for Sampling and Handling Bisphenol A(4,4' -Isopropylidinediphenol)
D6809 Guide for Quality Control and Quality Assurance Procedures for Aromatic Hydrocarbons and Related Materials
E1 Specification for ASTM Liquid-in-Glass Thermometers
E29 Practice for Using Significant Digits in Test Data to Determine Conformance with Specifications
E77 Test Method for Inspection and Verification of Thermometers
E691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
2.2 Other Documents:
OSHA Regulations, 29 CFR paragraphs 1910.1000 and 1910.1200
3. Terminology
3.1 Definitions:
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 D16.02 on Oxygenated Aromatics.
Current edition approved June 1, 2016June 1, 2020. Published June 2016June 2020. Originally approved in 1985. Last previous edition approved in 20122016 as
D4493 – 12.D4493 – 16. DOI: 10.1520/D4493-16.10.1520/D4493-20.
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’s Document Summary page on the ASTM website.
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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
D4493 − 20
3.1.1 solidification point, n—the temperature at which the liquid phase of a substance is in approximate equilibrium with a
relatively small amount of the same substance in its solid phase.
4. Summary of Test Method
4.1 Bisphenol A is melted, and then cooled slowly with constant agitation. When crystallization begins, and super-cooling
occurs, the temperature falls to a minimum, rises to a maximum, and then falls again. The maximum temperature attained after
crystallization begins is the solidification point of bisphenol A.
5. Significance and Use
5.1 The solidification point of bisphenol A is a direct indication of its purity, although it gives no information as to the nature
of any impurities present.
5.2 High purity bisphenol A has a solidification point of approximately 157°C.
5.3 This test method can be used for internal quality control or for setting specifications.
6. Interference
6.1 Bisphenol A that is not stored or packaged properly may absorb moisture. Absorbed moisture will lower the solidification
point.
7. Apparatus
7.1 Nessler Tubes, borosilicate, 100 mL, short form, 32-mm diameter.
7.2 Electric Heat Block, thermostatically controlled, capable of reaching 170°C; having flat-bottom holes 34 mm in diameter
by 172 mm deep. A suitable block is 100 by 110 by 175 mm high, and made of aluminum. Alternatively, a thermostatically
controlled hot oil bath may be used.
7.3 Thermometer—ASTM 102C, having a range from 123 to 177°C and conforming to the requirements for thermometer 102C
as prescribed in Specification E1. Thermometers should be calibrated in accordance with Test Method E77 or calibrated from 154
to 157°C versus an NBS thermometer or platinum resistance thermometer. Preferably, thermometers should be calibrated and
certified by a thermometer manufacturer. An alternative thermometer is a platinum resistance thermometer with digital read-out.
7.4 Electric Heater, stir plate, capable of reaching 150°C.
7.5 Magnetic Spinner, starhead. A wire stirrer, as specified in Test Method D1493, may be used as well.
7.6 Chloroprene Rubber Stopper, number 6, with hole to fit thermometer. If wire stirrer is used, an additional hole is needed.
Stoppers made of cork or other materials should not be used.
8. Reagents and Materials
8.1 Methyl Silicone Oil, suitable for continuous use at 200°C.
9. Hazards
9.1 Consult current OSHA Regulations, supplier’s Safety Data Sheets, and local regulations for all materials used in this test
method.
9.2 When handling molten solids in open tubes, adequate ventilation must be provided and proper protection should be used
to prevent thermal burns. It is preferable to perform this test in a fume hood.
9.3 Warning—Caution should be taken when cleaning up mercury from broken thermometers. Mercury or its vapor has been
designated as a hazardous substance which has demonstrated to be hazardous to health, corrosive to materials, and therefore can
cause serious medical issues. Mercury has been designated by many regulatory agencies as a hazardous substance that can cause
serious medical issues. See the applicable product Safety Data Sheet (SDS) for additional information. Users should be aware that
selling mercury and/or mercury containing products into your state or country may be prohibited by law.
10. Sampling
...