1、Designation: D 4493 03Standard Test Method forSolidification Point of Bisphenol A(4,4*-Isopropylidenediphenol)1This standard is issued under the fixed designation D 4493; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of
2、last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method describes the procedure for determina-tion of the solidification point of 4,48-isopropylidene diphen
3、ol,commercially known as bisphenol A, between 150 and 157C.1.2 The following applies to all specified limits in thisstandard: For purposes of determining conformance with thisstandard, an observed value or a calculated value shall berounded off “to the nearest unit” in the last right-hand digitused
4、in expressing the specification limit, in accordance withthe rounding-off method of Practice E 29.1.3 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the user of this test method. For specifichazard statements, see Sect
5、ion 9.2. Referenced Documents2.1 ASTM Standards:D 1493 Test Method for Solidification Point of IndustrialOrganic Chemicals2D 4297 Practice for Sampling and Handling Bisphenol A(4,48Isopropylidenediphenol)2E 1 Specification for ASTM Thermometers3E 29 Practice for Using Significant Digits in Test Data
6、 toDetermine Conformance with Specifications4E 77 Test Method for Inspection and Verification of Ther-mometers3E 691 Practice for Conducting an Interlaboratory Study toDetermine the Precision of a Test Method42.2 Other Document:OSHA Regulations, 29 CFR, paragraphs 1910.1000 and1910.120053. Terminolo
7、gy3.1 Definitions:3.1.1 solidification pointthe temperature at which theliquid phase of a substance is in approximate equilibrium witha relatively small amount of the same substance in its solidphase.4. Summary of Test Method4.1 Bisphenol A is melted, and then cooled slowly withconstant agitation. W
8、hen crystallization begins, and super-cooling occurs, the temperature falls to a minimum, rises to amaximum, and then falls again. The maximum temperatureattained after crystallization begins is the solidification point ofbisphenol A.5. Significance and Use5.1 The solidification point of bisphenol A
9、 is a directindication of its purity, although it gives no information as tothe nature of any impurities present.5.2 High purity bisphenol A has a solidification point ofapproximately 157C.5.3 This test method can be used for internal quality controlor for setting specifications.6. Interference6.1 B
10、isphenol A that is not stored or packaged properly mayadsorb moisture. Adsorbed moisture will lower the solidifica-tion point.7. Apparatus7.1 Nessler Tubes, borosilicate, 100 mL, short form, 32-mmdiameter.7.2 Electric Heat Block, thermostatically controlled, ca-pable of reaching 170C; having flat-bo
11、ttom holes 34 mm indiameter by 172 mm deep.NOTE 1A suitable size block is 100 by 110 by 175 mm high, andmade of aluminum.NOTE 2A thermostatically controlled hot oil bath may be used.7.3 Erlenmeyer Flask, 500-mL.NOTE 3The melted sample may be cooled in an air jacket-coolingbath, as specified in Test
12、Method D 1493.1This test method is under the jurisdiction of ASTM Committee D16 onAromatic Hydrocarbons and Related Chemicals and is the direct responsibility ofSubcommittee D16.02 on Oxygenated Aromatics.Current edition approved Jan. 10, 2003. Published March 2003. Originallyapproved in 1985. Last
13、previous edition approved in 1994 as D 4493 94.2Annual Book of ASTM Standards, Vol 06.04.3Annual Book of ASTM Standards, Vol 14.03.4Annual Book of ASTM Standards, Vol 14.02.5Available from Superintendent of Documents, U.S. Government PrintingOffice, Washington, DC 20402.1Copyright ASTM International
14、 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.7.4 ThermometerASTM 102C, having a range from 123to 177C and conforming to the requirements for thermometer102C as prescribed in Specification E 1.NOTE 4Thermometers should be calibrated in accordance with TestMeth
15、od E 77 or calibrated from 154 to 157C versus an NBS thermometeror platinum resistance thermometer. Preferably, thermometers should becalibrated and certified by a thermometer manufacturer. An alternativethermometer is a platinum resistance thermometer with digital read-out.7.5 Electric Heater, stir
16、 plate, capable of reaching 150C.7.6 Magnetic Spinner, starhead.NOTE 5A wire stirrer, as specified in Test Method D 1493, may beused.7.7 Chloroprene Rubber Stopper, number 6, with hole to fitthermometer. If wire stirrer is used, an additional hole isneeded.NOTE 6Stoppers made of cork or other materi
17、als should not be used.7.8 Ring Stand and Clamp.8. Reagents and Materials8.1 Methyl Silicone Oil, suitable for continuous use at200C.9. Hazards9.1 Consult current OSHA Regulations, suppliers MaterialSafety Data Sheets, and local regulations for all materials usedin this test method.9.2 When handling
18、 molten solids in open tubes, adequateventilation must be provided and proper protection should beused to prevent thermal burns. It is preferable to perform thistest in a fume hood.10. Sampling10.1 Sample the material in accordance with PracticeD 4297.11. Procedure11.1 Place a Nessler tube, filled w
19、ith bisphenol A, andcontaining the magnetic spinner, the stopper, and thermometer,in an electric heat block, preheated to 170 6 5C, to meltbisphenol A.NOTE 7The solidification point is determined on the specimen asreceived, with no drying procedure.11.2 As the bisphenol A melts, add more to the Ness
20、ler tube,if necessary, so that the immersion requirement of the ther-mometer will be met. It takes approximately 30 to 45 min tomelt enough bisphenol A to run the test. In order to minimizethe loss of volatile components, it is advisable to begin thesolidification point determination within 5 min af
21、ter the bisphe-nol A is molten.11.3 After the bisphenol A has melted, remove the Nesslertube from the heat block and place in the Erlenmeyer flask,which has been clamped to a ring stand (see Fig. 1). It may benecessary to wrap aluminum foil around the top portion of theFIG. 1 Bisphenol A Solidificat
22、ion Point ApparatusD4493032Nessler tube, before placing in the Erlenmeyer flask, to preventthe tube from turning in the flask. The flask contains 400 mLof silicone oil that has been preheated to 140 6 2C, and is ona heater-stir plate. It is advisable to set the flask in a smallaluminum foil pan to c
23、atch the oil in the event of a flask failure.11.4 Submerge the thermometer to the immersion mark andensure that the bulb of the thermometer is approximately 20mm above the bottom of the Nessler tube, clearing themagnetic spinner.11.5 Start the magnetic spinner stirring at a rate to create avortex, a
24、nd continue stirring until the liquid becomes solidenough to prevent the spinner from stirring. The cooling rateshould be adjusted to maintain a constant temperature for about3 min. The cooling rate may or may not be critical, dependingupon the product purity.11.6 Observe and record the thermometer
25、readings at 30-sintervals to the nearest 0.1C until the temperature rises fromthe minimum, due to super cooling, to a maximum, and finallybegins to drop. Further stirring will be impossible at this point.The maximum temperature after crystallization begins is thesolidification point.NOTE 8Taking tem
26、perature readings 30 s apart will ensure againstmistaking a temporary plateau for the maximum temperature. Plotting thetemperature readings against time will also help to identify a temporaryplateau.11.7 Correct the observed solidification point for the cali-bration of the thermometer.12. Report12.1
27、 Report the solidification point as the maximum tem-perature attained after crystallization begins. Report to thenearest 0.1C.13. Precision and Bias13.1 PrecisionThe following criteria should be used tojudge the acceptability (95 % confidence level) of resultsobtained by this test method. An interla
28、boratory study6wasconducted by four laboratories to determine solidificationpoints on three separate materials. Duplicates were run by eachlaboratory on two different days. Results of the interlaboratorystudy were calculated using Practice E 691.13.1.1 RepeatabilityResults submitted by the same labo
29、ratory should not be considered suspect unless they differ bymore than 0.5C. On the basis of test error alone, the differencebetween two test results obtained in the same laboratory on thesame material on the same day will be expected to exceed thisvalue only 5 % of the time.13.1.2 ReproducibilityR
30、esults submitted by each of twolaboratories should not be considered suspect unless they differby more than 1.8C. On the basis of test error alone, thedifference between two test results obtained in different labo-ratories on the same material will be expected to exceed thisvalue only 5 % of the tim
31、e.13.2 BiasNo statement is made about bias of the testmethod since there is no absolute method available as a refereemethod.14. Keywords14.1 bisphenol-A; isopropylidenediphenol; solidificationpointASTM International takes no position respecting the validity of any patent rights asserted in connectio
32、n with any item mentionedin this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the riskof infringement of such rights, are entirely their own responsibility.This standard is subject to revision at any time by the responsible
33、technical committee and must be reviewed every five years andif not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standardsand should be addressed to ASTM International Headquarters. Your comments will receive careful consid
34、eration at a meeting of theresponsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you shouldmake your views known to the ASTM Committee on Standards, at the address shown below.This standard is copyrighted by ASTM International, 100 Bar
35、r Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the aboveaddress or at 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm.org).6Supporting data are available from ASTM International Headquarters. RequestRR: D16-1008.D4493033
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