1、 Bereich InnovationDIN Deutsches Institut fr Normung e. V. Jede Art der Vervielfltigung, auch auszugsweise, nur mit Genehmigung des DIN Deutsches Institut fr Normung e. V., Berlin, gestattet. !$p“1772995Alleinverkauf der Spezifikationen durch Beuth Verlag GmbH, 10772 BerlinRecommendation for Tempera
2、ture Calibration of Fast Scanning Calorimeters (FSCs) for Sample Mass and Scan Rate; Text in English Empfehlung fr die Temperaturkalibrierung von Fast Scanning Calorimeters (FSCs) fr Probenmasse und Scanrate; Text in Englisch Recommandations pour ltalonnage de la temprature des Calorimtres Balayage
3、Rapide de la masse de lchantillon et la vitesse de balayage; Texte en anglais Zur Erstellung einer DIN SPEC knnen verschiedene Verfahrensweisen herangezogen werden: Das vorliegende Dokument wurde nach den Verfahrensregeln einer PAS erstellt. Juni 2011Preisgruppe 16ICS 17.200.10www.din.dewww.beuth.de
4、Gesamtumfang 37 SeitenDIN SPEC 91127B55EB1B3E14C22109E918E8EA43EDB30F09DCCB7EF8DD9NormCD - Stand 2012-03 Contents Page Foreword. 3 Introduction 4 1 Scope 4 2 References . 4 3 Abbreviations and Units . 5 3.1 Abbreviations 5 3.2 Units . 5 3.3 Convention. 6 4 Fast Scanning Calorimetry (FSC) 6 4.1 Gener
5、al . 6 4.2 DSCs. 7 4.3 Chip Calorimeters 7 5 Temperature Calibration Protocol . 8 5.1 FSC Performance (Annex A) 8 5.2 Primary Temperature Calibration (Annex B). 8 5.3 Check of the Primary Temperature Calibration 9 5.4 Temperature Calibration with Respect to Sample Mass and Scan Rate (Annex C) 9 5.5
6、Check of the Temperature Calibration for Sample Mass and Scan Rate (Annex C) . 10 5.6 Symmetry (Annex D) . 10 6 Calibration Protocol Flow Chart. 12 Annex A (informative) Examples of Performance 13 A.1 HyperDSCs PerkinElmer. 13 A.2 RHC TA Instruments . 16 A.3 FSC Universitt Rostock. 17 A.4 Flash DSC
7、1 Mettler-Toledo 18 Annex B (informative) Primary Temperature Calibration 19 B.1 HyperDSCs PerkinElmer. 19 B.2 RHC TA Instruments . 20 Annex C (informative) Temperature Calibration with Respect to Sample Mass and Scan Rate 21 C.0 Suitable sample masses for various FSCs . 21 C.1 HyperDSCs PerkinElmer
8、. 22 C.2 RHC TA Instruments . 25 C.3 FSC Universitt Rostock. 27 C.4 Flash DSC 1 Mettler-Toledo 28 Annex D (informative) Symmetry. 29 D.1 HyperDSCs PerkinElmer. 29 D.2 RHC TA Instruments . 32 D.3 FSC Universitt Rostock. 33 D.4 Flash DSC 1 Mettler-Toledo 34 Bibliography . 36 2 DIN SPEC 91127:2011-06 B
9、55EB1B3E14C22109E918E8EA43EDB30F09DCCB7EF8DD9NormCD - Stand 2012-03 Foreword This DIN Specification on differential scanning calorimetry, which has been developed by a standardization group using the PAS procedure, deals with high to very high scan rates and low to very low sample masses respectivel
10、y, and is complementary to the International Standard ISO 11357 which is dealing with low scan rates. It was elaborated by the following authors, members of the Standardization group1) Dr Geert Vanden Poel, DSM Resolve, Geleen, The Netherlands; Dr Albert Sargsyan, DSM Resolve, Geleen, The Netherland
11、s; Prof. Vincent Mathot, SciTe, the Netherlands and Ka tholieke Universiteit Leuven, Belgium, Chairman; Prof. Guy Van Assche, Vrije Universiteit Brussel, Belgium; Dr Andreas Wurm, Universitt Rostock, Germany; Prof. Christoph Schick, Universitt Rostock, Germany; Prof. Andres Krumme, Tallinn Universit
12、y of Technology, Estonia Prof. Dongshan Zhou, Nanjing University, Peoples Republic of China. The following persons also contributed to the document: Dr Sander van Herwaarden, Xensor Integration, Delfgauw, The Netherlands; Elina Iervolino, Xensor Integr ation, Delfgauw, The Netherlands; Gunnar Schulz
13、, Universitt Rostock, Germany; Davit Zohrabyan, Universitt Rostock, Germany; Evgeny Zhuravlev, Universitt Rostock, Germany. The work is an outcome of the NaPolyNet project of the 7thFramework Programme of the European Commission and was partially financed by NaPolyNet funds (EU-FP7 CSA NMP-2007-2.1-
14、3). DIN Deutsches Institut fr Normung e.V., Berlin March 21st, 2011 1) Although the authors strived to ensure that the information in this report is up-to-date and accurate as possible, they do not accept liability with regard to problems incurred as a result of using this report and/or any linked r
15、eports. The authors cannot be held liable for faults due to incorrectness, incompleteness and/or inaccuracy of the information in this report. In no event will the authors be liable for any damages whatsoever directly or indirectly arising out of or in connection with the use of the information in t
16、his report. The authors may revise the information in this report without notice. This disclaimer and report are construed under and shall be governed by the laws of Germany. 3 DIN SPEC 91127:2011-06 B55EB1B3E14C22109E918E8EA43EDB30F09DCCB7EF8DD9NormCD - Stand 2012-03 Introduction Thermal history es
17、pecially cooling and heating in combination with isothermal stays and sample/product treatment can change the behavior of materials drastically, influencing end properties. Experimentally it has been a challenging and very demanding job to realize fast, controlled cooling and heating at constant rat
18、es higher than the typical rates of Standard DSC, which are centred on approximately 10 C/min. In the past decade this challenge has been met through instrumental breakthroughs resulting in various Fast Scanning Calorimeters (FSCs), including commercial ones. This progress necessitates a dedicated p
19、rotocol for temperature calibration of FSCs. To address this need for extending existing temperature calibration protocols, the present Recommendation is firstly intended to inform the user about various types of FSCs and to compare their performances. To the opinion of the authors, FSC opens a new
20、world with respect to the analysis of substances, materials and products thereof. Undoubtedly it will lead to new concepts in domains like metastability, kinetics, reorganization, crystallization, melting, real-life conditions, and processing conditions. Secondly, one should be aware that instrument
21、ation facilitating different scan rates has consequences with respect to the way of performing measurements, especially because of the influence of scan rate and sample mass on sensitivity, resolution, thermal lag etc. Thirdly, because the impact is different for different FSCs, a need arises of a g
22、eneral applicable temperature calibration protocol, covering the issues mentioned and supporting measurements of good quality resulting in trustable and comparable results. In order to meet the abovementioned requirements an international standardization group has been formed with the aim to provide
23、 the users of FSCs with a recommendation covering: Temperature Calibration of FSCs for Sample Mass and Scan Rate. 1 Scope This specification describes a protocol of temperature calibration procedures for Fast Scanning Calorimeters for high to very high scan rates and low to very low sample masses, r
24、espectively, thus complementing ISO 11357. Procedures are given for both an extensive temperature calibration as well as a rather quick temperature calibration of FSCs in the heating and the cooling modes for various scan rates and concomitant adjusted sample masses. Thus, the specification also fac
25、ilitates making the right choices to minimize the thermal lag arising at increasing scan rates before performing a measurement. 2 References ISO 11357-1, Plastics Differential scanning calorimetry (DSC) Part 1: General principles (2009); in the present specification, terms and definitions used in IS
26、O 11357-1 are accounted for. 4 DIN SPEC 91127:2011-06 The following referenced documents are indispensable for the application of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) appl
27、ies. B55EB1B3E14C22109E918E8EA43EDB30F09DCCB7EF8DD9NormCD - Stand 2012-03 3 Abbreviations and Units 3.1 Abbreviations FSC Fast Scanning Calorimetry/- Calorimeter DSC Differential Scanning Calorimetry/- Calorimeter HPer DSC/ HyperDSC High Performance Differential Scanning Calorimetry/- Calorimeter RH
28、C Rapid Heat Cool differential scanning calorimeter UFSC Ultra Fast Scanning Calorimetry/- Calorimeter MEMS Micro-Electro-Mechanical Systems ICTAC International Confederation for Thermal Analysis and Calorimetry GEFTA Gesellschaft fr Thermische Analyse e. V. NIST National Institute of Standards and
29、Technology, Gaithersburg and Boulder, USA PTB Physikalisch-Technische Bundesanstalt, Braunschweig, Germany In indium Ad adamantane Sn tin Pb lead HP-53 4-(4-pentyl cyclohexyl)-benzoicacid-4-propyl-phenylester BCH-52 4-ethyl-4(4propylcyclohexyl)-biphenyl M-24 4-cyano-4-octyloxybiphenyl m sample mass
30、T temperature Teiextrapolated onset temperature Tei,refextrapolated onset temperature for reference value of primary standards t time scan rate minminimal scan rate maxmaximal scan rate SD standard deviation CF Correction Factor CFTeiCorrection Factor for the extrapolated onset temperature 3.2 Units
31、 Scan rate: C/min or K/min; C/s or K/s Heat flow rate: mW Specific heat flow: J/gC and J/gK T/C = T/K 273.15 5 DIN SPEC 91127:2011-06 B55EB1B3E14C22109E918E8EA43EDB30F09DCCB7EF8DD9NormCD - Stand 2012-03 3.3 Convention Heating and cooling curves are plotted upwards and downwards respectively. 4 Fast
32、Scanning Calorimetry (FSC) 4.1 General FSCs have received a great deal of attention in recent years. The reason that FSC is becoming increasingly popular is because, firstly, in practice, some physical and chemical processes occur at much higher scan rates than realizable using Standard DSC; and, se
33、condly, most nano-structures in materials and substances, including polymers and pharmaceuticals, are in metastable states. Thermal history specifically cooling and heating rates and sample/product treatment can change their behavior drastically, leading to deviating end properties. Phenomena relate
34、d to metastability of nano-structured crystallites and superstructures (if present) are well known to polymer scientists; daily they encounter supercooling, amorphization, hot crystallization, cold crystallization, recrystallization (after melting), annealing, reorganization etc. One of the breakthr
35、oughs in the past decennium with respect to the development of FSC was the realization of High Performance DSC 1, 2, 3, 4. (HPer; the term High Performance was meant as a general name for DSCs that realize higher scan rates than those attainable by Standard DSC, and show quantitative operation). It
36、has been promoted commercially since then by PerkinElmer (coining the name HyperDSC, operating at scan rates up to 750 C/min 5) and recently also by TA Instruments (project RHC, a rapid-scanning DSC operating at scan rates up to 2 000 C/min 6). One of the great benefits of these calorimeters based o
37、n DSC technology, see Table 1, is that they can mimic temperature-time ramps as occurring in practice, and specifically most of the cooling rates used in processing. A further advantage is the increased sensitivity, enabling measurement of low heat flow rate signals as related to small transitions a
38、nd to minute amounts of material. Another break-through was the (further) development of extremely fast-operating chip-calorimeters, see Table 1, based on MEMS technology, as described in various publications (see e.g. 7, 8 and references therein). So far the results by the chip calorimeter have bee
39、n obtained by specific equipment located at universities, like the instruments of the Polymer Physics Group at the Universitt Rostock 9. Continuous development and fine-tuning in this exciting field of research has been taken place over the years and with it the interest and demand with respect to F
40、SC increased within and outside the thermal analysis community. This is confirmed by the recent development of a commercially available FSC: the Mettler-Toledo Flash DSC 1 10, 11. To avoid the concomitantly strong increase of the thermal lag with increasing scan rate, the sample mass is decreased ac
41、cordingly. Due to these developments, the scan rate operating window of existing commercial DSCs is extended to more than 8 orders in magnitude in total, and even 12 orders with specialized instrumentation 12. In this way research groups have access to a huge range of scan rates as constituted by (f
42、or example) Calvet calorimetry, Standard DSC, HPer DSC and (Ultra-)FSC. In order to support this rapidly-growing field, and to facilitate a trouble-free utilization, an adequate and quick temperature calibration of FSCs in the heating and cooling mode should be possible. In addition, the symmetry of
43、 an instrument used with respect to the cooling and the heating modes has to be checked. 6 DIN SPEC 91127:2011-06 B55EB1B3E14C22109E918E8EA43EDB30F09DCCB7EF8DD9NormCD - Stand 2012-03 4.2 DSCs Table 1 Representation of some characteristics of calorimeters based on DSC technology discussed in this spe
44、cification, for empty cells, high scan rates and at the conditions given scan rate achievable temperature at constant rate purge gas Sourcein C/min in C in ml/min Figure DSC heating cooling* heating up to cooling down to* 350 200 350 75 He-Ne 25 * 350 200 350 0 He 25 * HyperDSC Pyris 1 350 200 350 1
45、25 N2 25 * 350 200 350 50 He-Ne 25 A1 300 200 300 20 He 25 A3 HyperDSC Diamond 300 200 300 185 N2 25 A2/A3 1 500/1 000 240/350 Ne 10 A4 RHC 1 500/1 000 1 000/500 175/275 100/-20 He 10 A4 * Cooling rate is determined by the cooling device, type of heat flow and rate, environmental conditions etc. * T
46、he graph is not included in this document. 4.3 Chip Calorimeters Table 2a Representation of some characteristics of calorimeters based on MEMS technology discussed in this specification, for empty cells, high scan rates and at the conditions given scan rate achievable temperature at constant rate purge gas Sourcein C/s in C in ml/min Figure FSC heating cooling* heating up to cooling down to* 20 000 5 000 410 40 N2 20 A6
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