1、Designation: D 4493 08Standard 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. Scope*1.1 This test method describes the procedure for determina-tion of the solidification point of bisphenol A (4,48-isoprop
3、ylidene diphenol).1.2 The method is applicable for determination of thesolidification point between 150 and 157C.1.3 In determining conformance of the test results using thismethod to applicable specifications, results shall be rounded offin accordance with the rounding-off method of Practice E29.1.
4、4 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 standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use. For specific haz
5、ardstatements, see Section 9.2. Referenced Documents2.1 ASTM Standards:2D 1493 Test Method for Solidification Point of IndustrialOrganic Chemicals3D 4297 Practice for Sampling and Handling Bisphenol A(4,48 -Isopropylidinediphenol)D 6809 Guide for Quality Control and Quality AssuranceProcedures for A
6、romatic Hydrocarbons and Related Ma-terialsE1 Specification for ASTM Liquid-in-Glass ThermometersE29 Practice for Using Significant Digits in Test Data toDetermine Conformance with SpecificationsE77 Test Method for Inspection and Verification of Ther-mometersE 691 Practice for Conducting an Interlab
7、oratory Study toDetermine the Precision of a Test Method2.2 Other Documents:OSHA Regulations, 29 CFR, paragraphs 1910.1000 and1910.120043. Terminology3.1 Definitions:3.1.1 solidification pointthe temperature at which theliquid phase of a substance is in approximate equilibrium witha relatively small
8、 amount of the same substance in its solidphase.4. Summary of Test Method4.1 Bisphenol A is melted, and then cooled slowly withconstant agitation. When crystallization begins, and super-cooling occurs, the temperature falls to a minimum, rises to amaximum, and then falls again. The maximum temperatu
9、reattained after crystallization begins is the solidification point ofbisphenol A.5. Significance and Use5.1 The solidification point of bisphenol A 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 solid
10、ification point ofapproximately 157C.5.3 This test method can be used for internal quality controlor for setting specifications.6. Interference6.1 Bisphenol A that is not stored or packaged properly mayadsorb moisture. Adsorbed moisture will lower the solidifica-tion point.7. Apparatus7.1 Nessler Tu
11、bes, borosilicate, 100 mL, short form, 32-mmdiameter.7.2 Electric Heat Block, thermostatically controlled, ca-pable of reaching 170C; having flat-bottom holes 34 mm in1This test method is under the jurisdiction of ASTM Committee D16 onAromatic Hydrocarbons and Related Chemicals and is the direct res
12、ponsibility ofSubcommittee D16.02 on Oxygenated Aromatics.Current edition approved Jan. 1, 2008. Published January 2008. Originallyapproved in 1985. Last previous edition approved in 2003 as D 4493 03.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Servi
13、ce at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3Withdrawn.4Available from U.S. Government Printing Office Superintendent of Documents,732 N. Capitol St., NW, Mail Stop: SDE, Washington, DC 20401, http:/www.a
14、ccess.gpo.gov.1*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.diameter by 172 mm deep. A suitable block is 100 by 110 by175 mm high, and made of aluminum. Alternativel
15、y, a ther-mostatically controlled hot oil bath may be used.7.3 ThermometerASTM 102C, having a range from 123to 177C and conforming to the requirements for thermometer102C as prescribed in Specification E1. Thermometers shouldbe calibrated in accordance with Test Method E77 or cali-brated from 154 to
16、 157C versus an NBS thermometer orplatinum resistance thermometer. Preferably, thermometersshould be calibrated and certified by a thermometer manufac-turer. An alternative thermometer is a platinum resistancethermometer with digital read-out.7.4 Electric Heater, stir plate, capable of reaching 150C
17、.7.5 Magnetic Spinner, starhead. A wire stirrer, as specifiedin Test Method D 1493, may be used as well.7.6 Chloroprene Rubber Stopper, number 6, with hole to fitthermometer. If wire stirrer is used, an additional hole isneeded. Stoppers made of cork or other materials should not beused.8. Reagents
18、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 molten solids in open tubes, adequateventilation must be pr
19、ovided 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 with bisphenol A, andcontaining the magnetic spinner, the sto
20、pper, and thermometer,in an electric heat block, preheated to 170 6 5C, to meltbisphenol A. The solidification point is determined on thespecimen as received, with no drying procedure.11.2 As the bisphenolAmelts, add more to the Nessler tube,if necessary, so that the immersion requirement of the the
21、r-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 after the bisphe-nol A is molten.11.3 After the bisphenol A has melte
22、d, remove the Nesslertube from the heat block and place in a 500 mL Erlenmeyerflask, which has been clamped to a ring stand (see Fig. 1). Itmay be necessary to wrap aluminum foil around the top portionof the Nessler tube before placing in the Erlenmeyer flask toprevent the tube from turning in the f
23、lask. The flask contains400 mL of silicone oil that has been preheated to 140 6 2C,and is on a heater-stir plate. It is advisable to set the flask in aFIG. 1 Bisphenol A Solidification Point ApparatusD4493082small aluminum foil pan to catch the oil in the event of a flaskfailure. Alternatively, the
24、melted sample may be cooled in anair jacket-cooling bath, as specified in Test Method D 1493.11.4 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
25、 spinner stirring at a rate to create avortex, and 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
26、 purity.11.6 Observe and record the thermometer 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. Taking temperature readings 30 s apart willensure against mistaking a temporary plateau for the ma
27、ximumtemperature. Plotting the temperature readings against timewill also help to identify a temporary plateau. Further stirringwill be impossible at this point. The maximum temperatureafter crystallization begins is the solidification point.11.7 Correct the observed solidification point for the cal
28、i-bration of the thermometer.12. Report12.1 Report the solidification point as the maximum tem-perature attained after crystallization begins. Report to thenearest 0.1C.13. Precision and Bias513.1 PrecisionThe following criteria should be used tojudge the acceptability at the 95 % probability level
29、of theresults obtained by this test method. The criteria were derivedfrom an interlaboratory study conducted by four laboratories todetermine solidification points on three separate materials.Duplicates were run by each laboratory on two different days.Results of the interlaboratory study were calcu
30、lated usingPractice E 691.13.1.1 Intermediate Precision (formerly calledRepeatability)Results submitted by the same laboratoryshould not be considered suspect unless they differ by morethan 0.5C. On the basis of test error alone, the differencebetween two test results obtained in the same laboratory
31、 on thesame material on the same day will be expected to exceed thisvalue only 5 % of the time.13.1.2 ReproducibilityResults 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 res
32、ults obtained in different labo-ratories on the same material will be expected to exceed thisvalue only 5 % of the time.13.2 BiasNo statement is made about bias of the testmethod since there is no absolute method available as a refereemethod.14. Quality Guidelines14.1 Refer to Guide D 6809 for sugge
33、sted QA/QC activitiesthat can be used as a part of this test method. It is recom-mended that the operator of this test method select and performrelevant QA/QC activities like the ones in Guide D 6809 tohelp ensure the quality of the data generated by this testmethod.15. Keywords15.1 bisphenol-A; iso
34、propylidenediphenol; solidificationpointSUMMARY OF CHANGESCommittee D16 has identified the location of selected changes to this standard since the last issue(D 4493 - 03) that may impact the use of this standard. (Approved January 1, 2008.)(1) Section 1 Former 1.1 divided into 1.1 and 1.2 perEditori
35、al Guidelines and the rest renumbered.(2) Section 2 Reference to Guide D 6809 was added.(3) Sections 7, 8, and 11 The liberal use of notes wasremoved and the text incorporated in the appropriate subsec-tion.(4) Section 13 Numbering and some verbiage was changedper Editorial Guidelines.(5) Section 14
36、 was added and the following renumberedaccordingly.5Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR:D16-1008.D4493083ASTM International takes no position respecting the validity of any patent rights asserted in connection with an
37、y 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 technical
38、 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 consideration a
39、t 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 Barr Harbor
40、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).D4493084
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