ASTM_D_1493_-_97.pdf

Designation:D 1493 97Standard Test Method forSolidification Point of Industrial Organic Chemicals1This standard is issued under the fixed designation D 1493;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(e)indicates an editorial change since the last revision or reapproval.1.Scope1.1 This test method covers a general procedure for deter-mining the solidification point of most organic chemicalshaving appreciable heats of fusion and solidification pointsbetween 20 and+150C.1.2 This test method is applicable only to relatively purecompounds.Values obtained for grossly impure compoundscan be low because of the freezing out of one componentduring the determination.1.3 In order that the test method may be used on manymaterials,a choice of certain alternatives and a selection ofapparatus are permitted.The report(Section 12)requires thatthe selected alternatives must be stated.Materials to which thetest method is applicable in particular detail include phenol,naphthalene,phthalic anhydride,and maleic anhydride.1.4 The following applies to all specified limits in this testmethod:for purposes of determining conformance with thistest method,an observed value or a calculated value shall berounded off“to the nearest unit”in the right-hand digit used inexpressing the specification limit,in accordance with therounding-off method of Practice E 29.NOTE1A companion test method is Test Method D 852.1.5 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 8.2.Referenced Documents2.1 ASTM Standards:D 850 Test Method for Distillation of Industrial AromaticHydrocarbons and Related Materials2D 852 Test Method for Solidification Point of Benzene2D 1015 Test Method for Freezing Points of High PurityHydrocarbons3D 1016 Test Method for Purity of Hydrocarbons fromFreezing Points3D 3437 Practice for Sampling and Handling Liquid CyclicProducts2D 3438 Practice for Sampling and Handling Naphthalene,Maleic Anhydride,and Phthalic Anhydride2D 3852 Practice for Sampling and Handling Phenol andCresyl Acid2E 1 Specification for ASTM Thermometers4E 29 Practice for Using Significant Digit in Test Data toDetermine Conformance with Specifications5E 77 Test Method for Inspection and Verification of Ther-mometers42.2Other Document:OSHA Regulations,29 CFR,paragraphs 1910.1000 and1910.120063.Terminology3.1 Definitions:3.1.1 solidification pointan empirical constant defined asthe temperature at which the liquid phase of a substance is inapproximate equilibrium with a relatively small amount of thesame substance in its solid phase.3.1.1.1 DiscussionSolidification point is distinguishedfrom freezing point,which is described in Test Method D 1015.An interpretation of mole percent purity in terms of freezingpoint is given in Test Method D 1016.4.Summary of Test Method4.1 Solidification point is measured by noting the maximumtemperature reached during a controlled cooling cycle after theappearance of a solid phase in a liquid sample.5.Significance and Use5.1 This test method is suitable for setting specifications on1This test method is under the jurisdiction of ASTM Committee D16 onAromatic Hydrocarbons and Related Chemicals and is the direct responsibility ofSubcommittee D16.04 on Instrumental Analysis.Current edition approved Feb.10,1997.Published September 1997.Originallypublished as D 1493 57 T.Last previous edition D 1493 92.2Annual Book of ASTM Standards,Vol 06.04.3Annual Book of ASTM Standards,Vol 05.01.4Annual Book of ASTM Standards,Vol 14.03.5Annual Book of ASTM Standards,Vol 14.02.6Available from Superintendent of Documents,U.S.Government PrintingOffice,Washington,DC 20402.1Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959,United Spounds of the type described in Section 1.It is also suitablefor use as an intense quality-control tool and in developmentand research work involving these compounds.6.Apparatus6.1 ThermometerAn etched-stem liquid-in-glass ther-mometer having a range of no more than 30C shall be used.Itshall be graduated in subdivisions no greater than 0.1C.Unless otherwise specified,it shall be calibrated,for 76-mmimmersion,at no fewer than three points.These shall includethe approximate solidification point of the material being testedand two other points,respectively,about 5C above and belowthe solidification point.A total immersion thermometer can beused if it is specified for testing a particular material,as,forexample,benzene.(See Test Method D 852.)The thermometershall conform to Specification E 1.It should be so chosen thatthe graduation at which the s