ASTM_D_4493_-_12.pdf

Designation:D449312Standard 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 year 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 determina-tion of the solidification point of bisphenol A(4,4-isopropylidene diphenol).1.2 The test method has been found applicable for determi-nation of the solidification 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 The values stated in SI units are to be regarded asstandard.No other units of measurement are included in thisstandard.1.5 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 hazardstatements,see Section 9.2.Referenced Documents2.1 ASTM Standards:2D1493 Test Method for Solidification Point of IndustrialOrganic Chemicals(Withdrawn 2004)3D4297 Practice for Sampling and Handling Bisphenol A(4,4-Isopropylidinediphenol)D6809 Guide for Quality Control and Quality AssuranceProcedures for Aromatic 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-mometersE691 Practice for Conducting an Interlaboratory 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 point,nthe 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.When 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 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 BisphenolAthat is not stored or packaged properly mayadsorb moisture.Adsorbed moisture will lower the solidifica-tion point.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 June 1,2012.Published June 2012.Originallyapproved in 1985.Last previous edition approved in 2008 as D4493 08.DOI:10.1520/D4493-12.2For referenced ASTM standards,visit the ASTM website,www.astm.org,orcontact ASTM Customer Service at serviceastm.org.For Annual Book of ASTMStandards volume information,refer to the standards Document Summary page onthe ASTM website.3The last approved version of this historical standard is referenced onwww.astm.org.4Available 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.*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 States1 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-bottom holes 34 mm indiameter by 172 mm deep.A suitable block is 100 by 110 by175 mm high,and made of aluminum.Alternatively,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 calibratedfrom 154 to 157C versus an NBS thermometer or platinumresistance thermometer.Preferably,thermometers should becalibrated and certified by a thermometer manufacturer.Analternative thermometer is a platinum resistance thermometerwith digital read-out.7.4 Electric Heater,stir plate,capable of reaching 150C.7.5 Magnetic Spinner,starhead.A wire stir