1、Designation: D4493 12D4493 16Standard Test Method forSolidification Point of Bisphenol A(4,4-Isopropylidenediphenol)1This standard is issued under the fixed designation D4493; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the yea
2、r of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope*1.1 This test method describes the procedure for determination of the solidification point of bisphenol A (4,4-isopr
3、opylidenediphenol).1.2 The test method has been found applicable for determination of the solidification point between 150 and 157C.1.3 In determining conformance of the test results using this method to applicable specifications, results shall be rounded offin accordance with the rounding-off metho
4、d 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 the responsibilityof the user of this stand
5、ard to establish appropriate safety and health practices and determine the applicability of regulatorylimitations prior to use. For specific hazard statements, see Section 9.2. Referenced Documents2.1 ASTM Standards:2D1493 Test Method for Solidification Point of Industrial Organic Chemicals (Withdra
6、wn 2004)3D4297 Practice for Sampling and Handling Bisphenol A(4,4 -Isopropylidinediphenol)D6809 Guide for Quality Control and Quality Assurance Procedures for Aromatic Hydrocarbons and Related MaterialsE1 Specification for ASTM Liquid-in-Glass ThermometersE29 Practice for Using Significant Digits in
7、 Test Data to Determine Conformance with SpecificationsE77 Test Method for Inspection and Verification of ThermometersE691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method2.2 Other Documents:OSHA Regulations, 29 CFR paragraphs 1910.1000 and 1910.1200 43. T
8、erminology3.1 Definitions:3.1.1 solidification point, nthe temperature at which the liquid phase of a substance is in approximate equilibrium with arelatively small amount of the same substance in its solid phase.4. Summary of Test Method4.1 Bisphenol A is melted, and then cooled slowly with constan
9、t agitation. When crystallization begins, and super-coolingoccurs, the temperature falls to a minimum, rises to a maximum, and then falls again. The maximum temperature attained aftercrystallization begins is the solidification point of bisphenol A.1 This test method is under the jurisdiction of AST
10、M Committee D16 on Aromatic Hydrocarbons and Related Chemicals and is the direct responsibility of SubcommitteeD16.02 on Oxygenated Aromatics.Current edition approved June 1, 2012June 1, 2016. Published June 2012June 2016. Originally approved in 1985. Last previous edition approved in 20082012 asD44
11、93 08.D4493 12. DOI: 10.1520/D4493-12.10.1520/D4493-16.2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM website.3 The
12、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 an ASTM standard and is intended o
13、nly to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Becauseit may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current ver
14、sionof the standard as published by ASTM is to be considered the official document.*A Summary of Changes section appears at the end of this standardCopyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States15. Significance and Use5.1 The solidif
15、ication point of bisphenol A is a direct indication of its purity, although it gives no information as to the natureof any impurities present.5.2 High purity bisphenol A has a solidification point of approximately 157C.5.3 This test method can be used for internal quality control or for setting spec
16、ifications.6. Interference6.1 BisphenolAthat is not stored or packaged properly may adsorbabsorb moisture.AdsorbedAbsorbed moisture will lower thesolidification point.7. Apparatus7.1 Nessler Tubes, borosilicate, 100 mL, short form, 32-mm diameter.7.2 Electric Heat Block, thermostatically controlled,
17、 capable of reaching 170C; having flat-bottom holes 34 mm in diameterby 172 mm deep. A suitable block is 100 by 110 by 175 mm high, and made of aluminum. Alternatively, a thermostaticallycontrolled hot oil bath may be used.7.3 ThermometerASTM 102C, having a range from 123 to 177C and conforming to t
18、he requirements for thermometer 102Cas prescribed in Specification E1. Thermometers should be calibrated in accordance with Test Method E77 or calibrated from 154to 157C versus an NBS thermometer or platinum resistance thermometer. Preferably, thermometers should be calibrated andcertified by a ther
19、mometer 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 Magnetic Spinner, starhead. A wire stirrer, as specified in Test Method D1493, may be used as well.7.6 Chloroprene Rubber Stopper,
20、 number 6, with hole to fit 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 Materials8.1 Methyl Silicone Oil, suitable for continuous use at 200C.9. Hazards9.1 Consult current OSHA Regulations, suppliers M
21、aterial Safety Data Sheets, and local regulations for all materials used inthis test method.9.2 When handling molten solids in open tubes, adequate ventilation must be provided and proper protection should be usedto prevent thermal burns. It is preferable to perform this test in a fume hood.10. Samp
22、ling10.1 Sample the material in accordance with Practice D4297.11. Procedure11.1 Place a Nessler tube, filled with bisphenol A, and containing the magnetic spinner, the stopper, and thermometer, in anelectric heat block, preheated to 170 6 5C, to melt bisphenol A. The solidification point is determi
23、ned on the specimen asreceived, with no drying procedure.11.2 As the bisphenolAmelts, add more to the Nessler tube, if necessary, so that the immersion requirement of the thermometerwill be met. It takes approximately 30 to 45 min to melt enough bisphenolAto run the test. In order to minimize the lo
24、ss of volatilecomponents, it is advisable to begin the solidification point determination within 5 min after the bisphenol A is molten.11.3 After the bisphenol A has melted, remove the Nessler tube from the heat block and place in a 500 mL Erlenmeyer flask,which has been clamped to a ring stand (see
25、 Fig. 1). It may be necessary to wrap aluminum foil around the top portion of theNessler tube before placing in the Erlenmeyer flask to prevent the tube from turning in the flask. The flask contains 400 mL ofsilicone oil that has been preheated to 140 6 2C, and is on a heater-stir plate. It is advis
26、able to set the flask in a small aluminumfoil pan to catch the oil in the event of a flask failure.Alternatively, the melted sample may be cooled in an air jacket-cooling bath,as specified in Test Method D1493.11.4 Submerge the thermometer to the immersion mark and ensure that the bulb of the thermo
27、meter is approximately 20 mmabove 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 enoughto prevent the spinner from stirring. The cooling rate should be adjusted
28、to maintain a constant temperature for about 3 min. Thecooling rate may or may not be critical, depending upon the product purity.D4493 16211.6 Observe and record the thermometer readings at 30-s intervals to the nearest 0.1C until the temperature rises from theminimum, due to super cooling, to a ma
29、ximum, and finally begins to drop. Taking temperature readings 30 s apart will ensureagainst mistaking a temporary plateau for the maximum temperature. Plotting the temperature readings against time will also helpto identify a temporary plateau. Further stirring will be impossible at this point. The
30、 maximum temperature after crystallizationbegins is the solidification point.11.7 Correct the observed solidification point for the calibration of the thermometer.12. Report12.1 Report the solidification point as the maximum temperature attained after crystallization begins. Report to the nearest0.1
31、C.13. Precision and Bias513.1 PrecisionThe following criteria should be used to judge the acceptability at the 95 % probability level of the resultsobtained by this test method. The criteria were derived from an interlaboratory study conducted by four laboratories to determinesolidification points o
32、n three separate materials. Duplicates were run by each laboratory on two different days. The details are givenin ASTM Research Report RR:D16-1008. Results of the interlaboratory study were calculated using Practice E691, although itshould be noted the size of the sample set did not meet the minimum
33、 requirements of Practice E691.13.1.1 RepeatabilityResults should not be suspect unless they differ by more than 0.5C. Results differing by less than 0.5Chave a 95 % probability of being correct.13.1.2 ReproducibilityResults submitted by each of two laboratories should not be considered suspect unle
34、ss they differ bymore than 1.8C. Results differing by less than 1.8C have a 95 % probability of being correct.13.2 BiasSince there is no accepted reference material or alternate test method suitable for determining the bias in this testmethod, bias has not been determined.14. Quality Guidelines14.1
35、Laboratories shall have a quality control system in place.5 Supporting data have been filed at ASTM International Headquarters and may be obtained by requesting Research Report RR:D16-1008. Contact ASTM CustomerService at serviceastm.org.FIG. 1 Bisphenol A Solidification Point ApparatusD4493 16314.1
36、.1 Confirm the performance of the test instrument or test method by analyzing a quality control sample following theguidelines of standard statistical quality control practices.14.1.2 Aquality control sample is a stable material isolated from the production process and representative of the sample b
37、einganalyzed.14.1.3 When QA/QC protocols are already established in the testing facility, these protocols are acceptable when they confirmthe 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 orsimilar s
38、tatistical quality control practices.15. Keywords15.1 bisphenol-A; 4,4-isopropylidenediphenol; solidification pointSUMMARY OF CHANGESCommittee D16 has identified the location of selected changes to this standard since the last issue (D4493 08) 12) that may impact the use of this standard. (Approved
39、June 1, 2012.)2016.)(1) Sections 1, 13, and 14 were updated to current editorial guideline verbiage and format.Section 6: Used absorb instead of adsorb.(2) Section 9: Changed MSDS to SDS.ASTM International takes no position respecting the validity of any patent rights asserted in connection with any
40、 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
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42、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 Dr
43、ive, 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). Permission rights to photocopy the standard may also be secured from the Copyright Clearance Center, 222Rosewood Drive, Danvers, MA 01923, Tel: (978) 646-2600; http:/ 164
