ASTM_E_2160_-_04_2012.pdf

Designation:E216004(Reapproved 2012)Standard Test Method forHeat of Reaction of Thermally Reactive Materials byDifferential Scanning Calorimetry1This standard is issued under the fixed designation E2160;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.Scope1.1 This test method determines the exothermic heat ofreaction of thermally reactive chemicals or chemical mixtures,using milligram specimen sizes,by differential scanning calo-rimetry.Such reactive materials may include thermally un-stable or thermoset materials.1.2 This test method also determines the extrapolated onsettemperature and peak heat flow temperature for the exothermicreaction.1.3 This test method may be performed on solids,liquids orslurries.1.4 The applicable temperature range of this method is 25 to600C.1.5 The values stated in SI units are to be regarded asstandard.No other units of measurement are included in thisstandard.1.6 There is no ISO method equivalent to this standard.1.7 This standard is related to Test Method E537 and toNAS 1613,but provides additional information.1.8 This standard may involve hazardous materials,operations,and equipment.This standard does not purport toaddress all of the safety concerns,if any,associated with itsuse.It is the responsibility of the user of this standard toestablish appropriate safety and health practices and deter-mine the applicability of regulatory limitations prior to use.2.Referenced Documents2.1 ASTM Standards:2E473 Terminology Relating to Thermal Analysis and Rhe-ologyE537 Test Method for The Thermal Stability of Chemicalsby Differential Scanning CalorimetryE967 Test Method for Temperature Calibration of Differen-tial Scanning Calorimeters and Differential Thermal Ana-lyzersE968 Practice for Heat Flow Calibration of DifferentialScanning CalorimetersE1142 Terminology Relating to Thermophysical PropertiesE1231 Practice for Calculation of Hazard Potential Figures-of-Merit for Thermally Unstable MaterialsE1860 Test Method for Elapsed Time Calibration of Ther-mal Analyzers2.2 Other Standard:NAS 1613 Seal Element,Packing,Preformed,EthylenePropylene Rubber,National Aerospace Standard,Aero-space Industries Association of America,1725 DeSalesSt.,NM,Washington,DC 200363.Terminology3.1 Specific technical terms used in this standard are definedin Terminologies E473 and E1142.4.Summary of Test Method4.1 A small(milligram)quantity of the reactive material isheated at 10C/min through a temperature region where achemical reaction takes place.The exothermic heat flowproduced by the reaction is recorded as a function of tempera-ture and time by a differential scanning calorimeter.Integrationof the exothermic heat flow over time yields the heat ofreaction.If the heat flow is endothermic,then this test methodis not to be used.4.2 The test method can be used to determine the fraction ofa reaction that has occurred in a partially reacted sample.Theheat of reaction is determined for a specimen that is known tobe 100%unreacted and is compared to the heat of reactiondetermined for the partially reacted sample.Appropriate cal-culation yields the fraction of the latter sample that wasunreacted.4.3 Subtracting the reaction fraction remaining from unity(1)yields the fraction reacted.The fraction reacted may beexpressed as percent.If the sample tested is a thermoset resin,the percent reacted is often called the percent of cure.1This test method is under the jurisdiction ofASTM Committee E37 on ThermalMeasurements and is the direct responsibility of Subcommittee E37.01 on Calo-rimetry and Mass Loss.Current edition approved Sept.1,2012.Published September 2012.Originallyapproved in 2001.Last previous edition approved in 2004 as E2160 04.DOI:10.1520/E2160-04R12.2For 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.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 4.4 The extrapolated onset temperature and peak heat flowtemperature are determined for the exothermic heat flowthermal curve from 4.1.5.Significance and Use5.1 This method is useful in determining the extrapolatedonset temperature,the peak heat flow temperature and the heatof reaction of a material.Any onset temperature determined bythis method is not valid for use as the sole information used fordetermination of storage or processing conditions.5.2 This test method is useful in determining the fraction ofa reaction that has been completed in a sample prior to testing.This fraction of reaction that has been completed can be ameasure of the degree of cure of a thermally reactive polyme