ASTM E967-2008(2014) 4386 Standard Test Method for Temperature Calibration of Differential Scanning Calorimeters and Differential Thermal Analyzers《差分扫描量热仪和差分热分析仪温度校准的标准试验方法》.pdf
《ASTM E967-2008(2014) 4386 Standard Test Method for Temperature Calibration of Differential Scanning Calorimeters and Differential Thermal Analyzers《差分扫描量热仪和差分热分析仪温度校准的标准试验方法》.pdf》由会员分享,可在线阅读,更多相关《ASTM E967-2008(2014) 4386 Standard Test Method for Temperature Calibration of Differential Scanning Calorimeters and Differential Thermal Analyzers《差分扫描量热仪和差分热分析仪温度校准的标准试验方法》.pdf(4页珍藏版)》请在麦多课文档分享上搜索。
1、Designation: E967 08 (Reapproved 2014)Standard Test Method forTemperature Calibration of Differential ScanningCalorimeters and Differential Thermal Analyzers1This standard is issued under the fixed designation E967; the number immediately following the designation indicates the year oforiginal adopt
2、ion 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 describes the temperature calibrationof differential the
3、rmal analyzers and differential scanningcalorimeters over the temperature range from 40 to +2500C.1.2 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.3 This test method is similar to ISO standard 113571.1.4 This standard does
4、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. Specific precau-tionary statements ar
5、e given in Section 7.2. Referenced Documents2.1 ASTM Standards:2E473 Terminology Relating to Thermal Analysis and Rhe-ologyE1142 Terminology Relating to Thermophysical Properties2.2 ISO Standards:3113571 Plastics-Differential Scanning Calorimetry (DSC)-Part 1: General Principles3. Terminology3.1 Def
6、initionsSpecific technical terms used in this testmethod are defined in Terminologies E473 and E1142.4. Summary of Test Method4.1 This test method consists of heating the calibrationmaterials at a controlled rate in a controlled atmospherethrough a region of known thermal transition. The heat flowin
7、to the calibration material or the difference of temperaturebetween the calibration material and a reference sample and areference material is monitored and continuously recorded. Atransition is marked by the absorption of energy by thespecimen resulting in a corresponding endothermic peak in thehea
8、ting curve.NOTE 1Heat flow calibrations are sometimes determined in conjunc-tion with temperature calibration. Some differential scanning calorimeterspermit both heat flow and temperature calibrations to be obtained from thesame experimental procedure.5. Significance and Use5.1 Differential scanning
9、 calorimeters and differential ther-mal analyzers are used to determine the transition temperaturesof materials. For this information to be meaningful in anabsolute sense, temperature calibration of the apparatus orcomparison of the resulting data to that of known standardmaterials is required.5.2 T
10、his test method is useful in calibrating the temperatureaxis of differential scanning calorimeters and differential ther-mal analyzers.6. Apparatus6.1 Apparatus shall be of either type listed below:6.1.1 Differential Scanning Calorimeter (DSC), capable ofheating a test specimen and a reference mater
11、ial at a controlledrate and of automatically recording the differential heat flowbetween the sample and the reference material to the requiredsensitivity and precision.6.1.1.1 A Furnace(s), to provide uniform controlled heatingor cooling of a specimen and reference to a constant tempera-ture or at a
12、 constant rate within the applicable temperaturerange of this test method.6.1.1.2 A Temperature Sensor, to provide an indication ofthe specimen temperature.6.1.1.3 Differential sensors, to detect a heat flow (power)difference between the specimen and reference.6.1.1.4 Test Chamber Environment, a mea
13、ns of sustaining atest chamber environment of nitrogen or other inert purge gasat a purge rate of 10 to 50 mL/min.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 edit
14、ion approved March 15, 2014. Published April 2014. Originallyapproved in 1983. Last previous edition approved in 2008 as E967 08. DOI:10.1520/E0967-08R14.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMS
15、tandards volume information, refer to the standards Document Summary page onthe ASTM website.3Available from International Organization for Standardization (ISO), 1, ch. dela Voie-Creuse, CP 56, CH-1211 Geneva 20, Switzerland, http:/www.iso.org.Copyright ASTM International, 100 Barr Harbor Drive, PO
16、 Box C700, West Conshohocken, PA 19428-2959. United States16.1.1.5 A Temperature Controller, capable of executing aspecific temperature program by operating the furnace(s)between selected temperature limits at a rate of temperaturechange of 10K/min.6.1.1.6 Data Collection Device, to provide a means
17、ofacquiring, storing, and displaying measured or calculatedsignals, or both. The minimum output signals required for DSCare heat flow, temperature, and time.6.1.2 Differential Thermal Analyzer (DTA), capable of heat-ing a test specimen and reference material at a controlled rateand of automatically
18、recording the differential temperaturebetween sample and reference material both to the requiredsensitivity and precision.6.2 Containers (pans, crucibles, vials, lids, closures, seals,etc.), that are inert to the specimen and reference materials andthat are of suitable structural shape and integrity
19、 to contain thespecimen and reference in accordance with the specific require-ments of this test method.6.3 Nitrogen, or other inert purge gas supply.6.4 A Balance, to weigh specimens or containers (pans,crucibles, vials, etc.), or both to 60.1 mg. The balance shouldhave a capacity greater than 20 m
20、g.7. Precautions7.1 Toxic or corrosive effluents, or both, may be releasedwhen heating some material and could be harmful to personneland to apparatus.7.2 This test method assumes linear temperature indication.Care must be taken in the application of this test method toensure that calibration points
21、 are taken sufficiently closetogether so that linear temperature indication may be approxi-mated. Linear temperature indications means that there exists alinear, or first order, dependence on the temperature determinedby the instruments temperature sensor on the true temperatureof the sample materia
22、l in its container and that this relation isadequately expressed by Eq 1.8. Calibration Materials8.1 For the temperature range covered by manyapplications, the melting transition of 99.99 % pure materialsin Table 1 may be used for calibration.9. Procedure9.1 Two Point Calibration:9.1.1 Select two ca
23、libration materials from Table 1, withmelting temperatures one above and one below the temperaturerange of interest. The calibration materials should be as closeto the temperature range of interest as practical.9.1.2 Determine the apparent transition temperature foreach calibration material.9.1.2.1
24、Into a clean specimen holder, placea5to15-mgweighed amount of calibration material. Other specimenmasses may be used but must be indicated in the report.9.1.2.2 Load the specimen into the instrument chamber,purge the chamber with dry nitrogen (or other inert gas) at aflow rate of 10 to 50 cm3/min th
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