ASTM D4493-94
(Test Method)Standard Test Method for Solidification Point of Bisphenol A (4,4´-Isopropylidenediphenol)
Standard Test Method for Solidification Point of Bisphenol A (4,4´-Isopropylidenediphenol)
SCOPE
1.1 This test method describes the procedure for determination of the solidification point of 4,4`-isopropylidene diphenol, commercially known as bisphenol A, between 150 and 157°C.
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.
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NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
Designation: D 4493 – 94
AMERICAN SOCIETY FOR TESTING AND MATERIALS
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Reprinted from the Annual Book of ASTM Standards. Copyright ASTM
Standard Test Method for
Solidification Point of Bisphenol A
(4,4*-Isopropylidenediphenol)
This standard is issued under the fixed designation D 4493; 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 a relatively small amount of the same substance in its solid
phase.
1.1 This test method describes the procedure for determina-
tion of the solidification point of 4,48-isopropylidene diphenol,
4. Summary of Test Method
commercially known as bisphenol A, between 150 and 157°C.
4.1 Bisphenol A is melted, and then cooled slowly with
1.2 The following applies to all specified limits in this
constant agitation. When crystallization begins, and super-
standard: For purposes of determining conformance with this
cooling occurs, the temperature falls to a minimum, rises to a
standard, an observed value or a calculated value shall be
maximum, and then falls again. The maximum temperature
rounded off “to the nearest unit” in the last right-hand digit
attained after crystallization begins is the solidification point of
used in expressing the specification limit, in accordance with
bisphenol A.
the rounding-off method of Practice E 29.
1.3 This standard does not purport to address all of the
5. Significance and Use
safety concerns, if any, associated with its use. It is the
5.1 The solidification point of bisphenol A is a direct
responsibility of the user of this standard to establish appro-
indication of its purity, although it gives no information as to
priate safety and health practices and determine the applica-
the nature of any impurities present.
bility of regulatory limitations prior to use.
5.2 High purity bisphenol A has a solidification point of
2. Referenced Documents approximately 157°C.
5.3 This test method can be used for internal quality control
2.1 ASTM Standards:
or for setting specifications.
D 1493 Test Method for Solidification Point of Industrial
Organic Chemicals
6. Interference
D 4297 Practice for Sampling and Handling Bisphenol A
2 6.1 Bisphenol A that is not stored or packaged properly may
(4,48–Isopropylidenediphenol)
3 adsorb moisture. Adsorbed moisture will lower the solidifica-
E 1 Specification for ASTM Thermometers
tion point.
E 29 Practice for Using Significant Digits in Test Data to
Determine Conformance with Specifications
7. Apparatus
E 77 Test Method for Inspection and Verification of Ther-
3 7.1 Nessler Tubes , borosilicate, 100 mL, short form,
mometers
32-mm diameter.
2.2 Other Document:
7.2 Electric Heat Block , thermostatically controlled, ca-
OSHA Regulations, 29 CFR, paragraphs 1910.1000 and
pable of reaching 170°C; having flat-bottom holes 34 mm in
1910.1200
diameter by 172 mm deep.
3. Terminology
NOTE 1—A suitable size block is 100 by 110 by 175 mm high, and
3.1 Definitions: made of aluminum.
NOTE 2—A thermostatically controlled hot oil bath may be used.
3.1.1 solidification point—the temperature at which the
liquid phase of a substance is in approximate equilibrium with
7.3 Erlenmeyer Flask, 500-mL.
NOTE 3—The melted sample may be cooled in an air jacket-cooling
This test method is under the jurisdiction of ASTM Committee D-16 on bath, as specified in Test Method D 1493.
Aromatic Hydrocarbons and Related Chemicals and is the direct responsibility of
7.4 Thermometer—ASTM 102C, having a range from 123
Subcommittee D16.0C on Oxygenated Aromatics.
Current edition approved April 15, 1994. Published June 1994. Originally
published as D 4493 – 85. Last previous edition D 4493 – 89.
2 6
Annual Book of ASTM Standards, Vol 06.04. Fisher Scientific Co., No. 7-052 B, available from the local Fischer supplier, or
Annual Book of ASTM Standards, Vol 14.03. its equivalent, has been found to be satisfactory for this purpose.
4 7
Annual Book of ASTM Standards, Vol 14.02. Model 60100 heater available from Precision Scientific, Div. of GCA Corp.,
Available from Superintendent of Documents, U.S. Government Printing 3737 W. Courtland St., Chicago, IL 60647, or its equivalent, has been found to be
Office, Washington, DC 20402. satisfactory for this purpose.
NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
D 4493
FIG. 1 Bisphenol A Solidification Point Apparatus
to 177°C and conforming to the requirements for thermometer 9. Hazards
102C as prescribed in Specification E 1.
9.1 Consult current OSHA Regulations and supplier’s Ma-
terial Safety Data Sheets for all materials used in this test
NOTE 4—Thermometers should be calibrated in accordance with Test
method.
Method E 77 or calibrated from 154 to 157°C versus an NBS thermometer
or platinum resistance thermometer. Preferably, thermometers should be
9.2 When handling molten solids in open tubes, adequate
calibrated and certified by a thermometer manufacturer. An alternative
ventilation must be provided and proper protection should be
thermometer is a platinum resistance thermometer with digital read-out.
used to prevent thermal burns. It is preferable to perform this
7.5 Electric Heater , stir plate, capable of reaching 150°C. test in a
...
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