1、Designation: D449308D449312 Standard Test Method for Solidication Point of Bisphenol A (4,4-Isopropylidenediphenol)(4,4-Isopropylidenediphenol) 1 This standard is issued under the xed designation D4493; the number immediately following the designation indicates the year of original adoption or, in t
2、he case of revision, the year of last revision.Anumber 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 Thistestmethoddescribestheprocedurefordeterminationofthesolidicationpointofbisphenol
3、A(4,4-isopropylidene(4, 4-isopropylidene diphenol). 1.2 The method is test method has been found applicable for determination of the solidication point between 150 and 157C. 1.3 In determining conformance of the test results using this method to applicable specications, results shall be rounded off
4、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 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is
5、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 specic hazard statements, see Section 9. 2. Referenced Documents 2.1 ASTM Standards: 2 D1493Test Method for Solidication Po
6、int of Industrial Organic Chemicals (Withdrawn 2004) 3 D4297Practice for Sampling and Handling Bisphenol A (4,4 -Isopropylidinediphenol) D6809Guide for Quality Control and Quality Assurance Procedures for Aromatic Hydrocarbons and Related Materials E1Specication for ASTM Liquid-in-Glass Thermometers
7、 E29Practice for Using Signicant Digits in Test Data to Determine Conformance with Specications E77Test Method for Inspection and Verication of Thermometers E691Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method 2.2 Other Documents: OSHA Regulations, 29 CFRp
8、aragraphs 1910.1000 and 1910.1200 4 3. Terminology 3.1 Denitions: 3.1.1 solidicationpointpoint,nthetemperatureatwhichtheliquidphaseofasubstanceisinapproximateequilibriumwith a relatively small amount of the same substance in its solid phase. 4. Summary of Test Method 4.1 Bisphenol A is melted, and t
9、hen 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 solidication point of bisphenol A. 1 This test method i
10、s under the jurisdiction ofASTM Committee D16 on Aromatic Hydrocarbons and Related Chemicals and is the direct responsibility of Subcommittee D16.02 on Oxygenated Aromatics. Current edition approved June 1, 2012. Published January 2008June 2012. Originally approved in 1985. Last previous edition app
11、roved in 20032008 as D449303.D449308. DOI: 10.1520/D4493-08.10.1520/D4493-12. 2 ForreferencedASTMstandards,visittheASTMwebsite,www.astm.org,orcontactASTMCustomerServiceatserviceastm.org.For Annual Book ofASTM Standards volume information, refer to the standards Document Summary page on the ASTM webs
12、ite. 3 The last approved version of this historical standard is referenced on www.astm.org. 4 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. This document is not anASTM standard and
13、is intended only to provide the user of anASTM standard an indication of what changes have been made to the previous version. Because it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only th
14、e current version of the standard as published by ASTM is to be considered the official document. *ASummary 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 15. Signicance and Use
15、5.1 The solidication point of bisphenolAis 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 solidication point of approximately 157C. 5.3 This test method can be used for internal quality control or for
16、setting specications. 6. Interference 6.1 BisphenolAthat is not stored or packaged properly may adsorb moisture.Adsorbed moisture will lower the solidication point. 6. Interference 6.1 BisphenolAthat is not stored or packaged properly may adsorb moisture.Adsorbed moisture will lower the solidication
17、 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 170C; having at-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. Alte
18、rnatively, a thermostatically controlled hot oil bath may be used. 7.3 ThermometerASTM102C,havingarangefrom123to177Candconformingtotherequirementsforthermometer102C as prescribed in Specication E1.Thermometers should be calibrated in accordance withTest Method E77 or calibrated from 154 to 157C vers
19、us an NBS thermometer or platinum resistance thermometer. Preferably, thermometers should be calibrated and certied 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 150C. 7.5 Magn
20、etic Spinner, starhead. A wire stirrer, as specied in Test Method D1493, may be used as well. 7.6 Chloroprene Rubber Stopper, number 6, with hole to t 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 Mate
21、rials 8.1 Methyl Silicone Oil, suitable for continuous use at 200C. 9. Hazards 9.1 Consult current OSHARegulations, suppliers Material 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 pro
22、vided and proper protection should be used to prevent thermal burns. It is preferable to perform this test in a fume hood. 10. Sampling 10.1 Sample the material in accordance with Practice D4297. 11. Procedure 11.1 Place a Nessler tube, lled with bisphenol A, and containing the magnetic spinner, the
23、 stopper, and thermometer, in an electric heat block, preheated to 170 6 5C, to melt bisphenol A. The solidication point is determined on the specimen as received, with no drying procedure. 11.2 AsthebisphenolAmelts,addmoretotheNesslertube,ifnecessary,sothattheimmersionrequirementofthethermometer wi
24、llbemet.Ittakesapproximately30to45mintomeltenoughbisphenolAtorunthetest.Inordertominimizethelossofvolatile components, it is advisable to begin the solidication point determination within 5 min after the bisphenol A is molten. 11.3 After the bisphenolAhas melted, remove the Nessler tube from the hea
25、t block and place in a 500 mL Erlenmeyer ask, which has been clamped to a ring stand (see Fig. 1). It may be necessary to wrap aluminum foil around the top portion of the Nessler tube before placing in the Erlenmeyer ask to prevent the tube from turning in the ask. The ask contains 400 mL of silicon
26、e oil that has been preheated to 1406 2C, and is on a heater-stir plate. It is advisable to set the ask in a small aluminum foilpantocatchtheoilintheeventofaaskfailure.Alternatively,themeltedsamplemaybecooledinanairjacket-coolingbath, as specied in Test Method D1493. D4493 12 211.4 Submerge the ther
27、mometer to the immersion mark and ensure that the bulb of the thermometer is approximately 20 mm above the bottom of the Nessler tube, clearing the magnetic spinner. 11.5 Start the magnetic spinner stirring at a rate to create a vortex, and continue stirring until the liquid becomes solid enough to
28、prevent the spinner from stirring. The cooling rate should be adjusted to maintain a constant temperature for about 3 min. The cooling rate may or may not be critical, depending upon the product purity. 11.6 Observe and record the thermometer readings at 30-s intervals to the nearest 0.1C until the
29、temperature rises from the minimum, due to super cooling, to a maximum, and nally begins to drop. Taking temperature readings 30 s apart will ensure against mistaking a temporary plateau for the maximum temperature. Plotting the temperature readings against time will also help to identify a temporar
30、y plateau. Further stirring will be impossible at this point. The maximum temperature after crystallization begins is the solidication point. 11.7 Correct the observed solidication point for the calibration of the thermometer. 12. Report 12.1 Report the solidication point as the maximum temperature
31、attained after crystallization begins. Report to the nearest 0.1C. 13. Precision and Bias 5 13.1 PrecisionThe following criteria should be used to judge the acceptability at the 95% probability level of the results obtained by this test method. The criteria were derived from an interlaboratory study
32、 conducted by four laboratories to determine solidicationpointsonthreeseparatematerials.Duplicateswererunbyeachlaboratoryontwodifferentdays.Thedetailsaregiven in ASTM Research Report RR:D16-1008. Results of the interlaboratory study were calculated using Practice E691, although it should be noted th
33、e size of the sample set did not meet the minimum requirements of Practice E691. 13.1.1 IntermediatePrecision(formerlycalledRepeatability)RepeatabilityResultssubmittedbythesamelaboratoryshould not be considered suspect unless they differ by more than 0.5C. On the basis of test error alone, the diffe
34、rence between two test results obtained in the same laboratory on the same material on the same day will be expected to exceed this value only 5% of the time.Results differing by less than 0.5C have a 95 % probability of being correct. 5 Supporting data have been led at ASTM International Headquarte
35、rs and may be obtained by requesting Research Report RR:D16-1008. FIG. 1 Bisphenol A Solidication Point Apparatus D4493 12 313.1.2 ReproducibilityResults submitted by each of two laboratories should not be considered suspect unless they differ by more than 1.8C. On the basis of test error alone, the
36、 difference between two test results obtained in different laboratories on the same material will be expected to exceed this value only 5% of the time. Results differing by less than 1.8C have a 95% probability of being correct. 13.2 BiasNo statement is made about bias of the test method since Since
37、 there is no absolute method available as a referee method.acceptedreferencematerialoralternatetestmethodsuitablefordeterminingthebiasinthistestmethod,biashasnotbeen determined. 14. Quality Guidelines 14.1 RefertoGuideLaboratoriesshallhaveD6809forsuggestedQA/QCactivitiesthatcanbeusedasapartofthistes
38、tmethod. It is recommended that the operator of this test method select and perform relevant QA/QC activities like the ones in Guide a D6809 to help ensure the quality of the data generated by this test method.quality control system in place. 14.1.1 Conrm the performance of the test instrument or te
39、st method by analyzing a quality control sample following the guidelines of standard statistical quality control practices. 14.1.2 Aqualitycontrolsampleisastablematerialisolatedfromtheproductionprocessandrepresentativeofthesamplebeing analyzed. 14.1.3 When QA/QC protocols are already established in
40、the testing facility, these protocols are acceptable when they conrm the validity of test results. 14.1.4 When there are no QA/QC protocols established in the testing facility, use the guidelines described in Guide D6809 or similar statistical quality control practices. 15. Keywords 15.1 bisphenol-A
41、; isopropylidenediphenol;4,4-isopropylidenediphenol; solidication point SUMMARY OF CHANGES Committee D16 has identied the location of selected changes to this standard since the last issue (D4493-03D4493) 08) that may impact the use of this standard. (Approved JanuaryJune 1, 2008.)2012.) (1)Section
42、1 Former 1.1 divided into 1.1 and 1.2 per Editorial Guidelines and the rest renumbered. (2)Section 2 Reference to Guide D6809 was added. (3)Sections 7, 8, and 11 The liberal use of notes was removed and the text incorporated in the appropriate subsection. (4)Section 13 Numbering and some verbiage wa
43、s changed per Editorial Guidelines. (1)Section 14 was added and the following renumbered accordingly.Sections 1, 13, and 14 were updated to current editorial guideline verbiage and format. ASTM International takes no position respecting the validity of any patent rights asserted in connection with a
44、ny item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. Thisstandardissubjecttorevisionatanytimebytheresponsibletechnicalcommitte
45、eandmustbereviewedeveryveyearsand ifnotrevised,eitherreapprovedorwithdrawn.Yourcommentsareinvitedeitherforrevisionofthisstandardorforadditionalstandards and should be addressed toASTM International Headquarters.Your comments will receive careful consideration at a meeting of the responsible technica
46、l committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, at the address shown below. This standard is copyrighted byASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken
47、, PA19428-2959, United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the above address or at 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website (www.astm.org). Permission rights to photocopy the standard may also be secured from the ASTM website (www.astm.org/ COPYRIGHT/). D4493 12 4
