ASTM D4493-03
(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)
SIGNIFICANCE AND USE
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.
High purity bisphenol A has a solidification point of approximately 157°C.
This test method can be used for internal quality control or for setting specifications.
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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Designation: D 4493 – 03
Standard Test Method for
Solidification Point of Bisphenol A
1
(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 3. Terminology
1.1 This test method describes the procedure for determina- 3.1 Definitions:
tion of the solidification point of 4,48-isopropylidene diphenol, 3.1.1 solidification point—the temperature at which the
commercially known as bisphenolA, between 150 and 157°C. liquid phase of a substance is in approximate equilibrium with
1.2 The following applies to all specified limits in this a relatively small amount of the same substance in its solid
standard: For purposes of determining conformance with this phase.
standard, an observed value or a calculated value shall be
4. Summary of Test Method
rounded off “to the nearest unit” in the last right-hand digit
4.1 Bisphenol A is melted, and then cooled slowly with
used in expressing the specification limit, in accordance with
the rounding-off method of PracticeE29. constant agitation. When crystallization begins, and super-
cooling occurs, the temperature falls to a minimum, rises to a
1.3 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the maximum, and then falls again. The maximum temperature
attained after crystallization begins is the solidification point of
responsibility of the user of this test method. For specific
hazard statements, see Section 9. bisphenol A.
5. Significance and Use
2. Referenced Documents
2.1 ASTM Standards: 5.1 The solidification point of bisphenol A is a direct
indication of its purity, although it gives no information as to
D 1493 Test Method for Solidification Point of Industrial
2
Organic Chemicals the nature of any impurities present.
D 4297 Practice for Sampling and Handling Bisphenol A 5.2 High purity bisphenol A has a solidification point of
2
approximately 157°C.
(4,48–Isopropylidenediphenol)
3
E1 Specification for ASTM Thermometers 5.3 This test method can be used for internal quality control
or for setting specifications.
E29 Practice for Using Significant Digits in Test Data to
4
Determine Conformance with Specifications
6. Interference
E77 Test Method for Inspection and Verification of Ther-
3
6.1 BisphenolAthat is not stored or packaged properly may
mometers
adsorb moisture. Adsorbed moisture will lower the solidifica-
E 691 Practice for Conducting an Interlaboratory Study to
4
tion point.
Determine the Precision of a Test Method
2.2 Other Document:
7. Apparatus
OSHA Regulations,29 CFR, paragraphs 1910.1000 and
5
7.1 Nessler Tubes, borosilicate, 100 mL, short form, 32-mm
1910.1200
diameter.
7.2 Electric Heat Block, thermostatically controlled, ca-
pable of reaching 170°C; having flat-bottom holes 34 mm in
1
This test method is under the jurisdiction of ASTM Committee D16 on
diameter by 172 mm deep.
Aromatic Hydrocarbons and Related Chemicals and is the direct responsibility of
Subcommittee D16.02 on Oxygenated Aromatics.
NOTE 1—A suitable size block is 100 by 110 by 175 mm high, and
Current edition approved Jan. 10, 2003. Published March 2003. Originally
made of aluminum.
approved in 1985. Last previous edition approved in 1994 as D 4493 – 94.
NOTE 2—A thermostatically controlled hot oil bath may be used.
2
Annual Book of ASTM Standards, Vol 06.04.
3
Annual Book of ASTM Standards, Vol 14.03.
7.3 Erlenmeyer Flask, 500-mL.
4
Annual Book of ASTM Standards, Vol 14.02.
5
NOTE 3—The melted sample may be cooled in an air jacket-cooling
Available from Superintendent of Documents, U.S. Government Printing
Office, Washington, DC 20402. bath, as specified in Test Method D 1493.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
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D4493–03
FIG. 1 Bisphenol A Solidification Point Apparatus
7.4 Thermometer—ASTM 102C, having a range from 123 9.2 When handling molten solids in open tubes, adequate
to 177°C and conforming to the requirements for thermometer ventilation must be provided and proper protection should be
102C as prescribed in SpecificationE1. used to prevent thermal burns. It is preferable to perform this
test in a fume hood.
NOTE 4—Thermometers should be calibrated in accordance with Test
MethodE77orcalibratedfrom154to157°CversusanNBSthermometer
10. Sampling
or platinum resistance thermometer. Preferably, thermometers should be
calibrated and certified by a thermometer manufacturer. An alternative
10.1 Sample the material
...
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