JP5721953B2 - 熱分析装置 - Google Patents
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N25/00—Investigating or analyzing materials by the use of thermal means
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N25/00—Investigating or analyzing materials by the use of thermal means
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- G01N25/48—Investigating or analyzing materials by the use of thermal means by investigating the development of heat, i.e. calorimetry, e.g. by measuring specific heat, by measuring thermal conductivity on solution, sorption, or a chemical reaction not involving combustion or catalytic oxidation
- G01N25/4846—Investigating or analyzing materials by the use of thermal means by investigating the development of heat, i.e. calorimetry, e.g. by measuring specific heat, by measuring thermal conductivity on solution, sorption, or a chemical reaction not involving combustion or catalytic oxidation for a motionless, e.g. solid sample
- G01N25/4866—Investigating or analyzing materials by the use of thermal means by investigating the development of heat, i.e. calorimetry, e.g. by measuring specific heat, by measuring thermal conductivity on solution, sorption, or a chemical reaction not involving combustion or catalytic oxidation for a motionless, e.g. solid sample by using a differential method
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N25/00—Investigating or analyzing materials by the use of thermal means
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N25/00—Investigating or analyzing materials by the use of thermal means
- G01N25/20—Investigating or analyzing materials by the use of thermal means by investigating the development of heat, i.e. calorimetry, e.g. by measuring specific heat, by measuring thermal conductivity
- G01N25/48—Investigating or analyzing materials by the use of thermal means by investigating the development of heat, i.e. calorimetry, e.g. by measuring specific heat, by measuring thermal conductivity on solution, sorption, or a chemical reaction not involving combustion or catalytic oxidation
- G01N25/4806—Details not adapted to a particular type of sample
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- G01N25/00—Investigating or analyzing materials by the use of thermal means
- G01N25/20—Investigating or analyzing materials by the use of thermal means by investigating the development of heat, i.e. calorimetry, e.g. by measuring specific heat, by measuring thermal conductivity
- G01N25/48—Investigating or analyzing materials by the use of thermal means by investigating the development of heat, i.e. calorimetry, e.g. by measuring specific heat, by measuring thermal conductivity on solution, sorption, or a chemical reaction not involving combustion or catalytic oxidation
- G01N25/4806—Details not adapted to a particular type of sample
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Description
これは、具体的に熱抵抗Zに対して重要である。熱抵抗Zは、直接に決定され得ないが、装置の較正中に決定される特性から算定される必要がある。特に、等周温条件化の熱量計において、例えば、チップタイプ熱量計においては、試料位置に配置される任意の試料は、周囲の環境に考慮されなければならない試料位置の熱抵抗ZSEに影響を与える。更に、特にもっと程度の進んだシステムは理想的状態からかけ離れていて、ある程度すべてが利用できない仮定及び簡素化のいくつかが標準的熱流動に関する算定に関連し、実行されている。例えば、熱容量CPに関する一定値を含むこれら仮定は、空の測定位置の熱容量及びチップタイプ熱量計の場合は、試料の幾何学的安定性と等価である。実験条件が実質上、理想的な状態と大幅に異なり得るので、結果となる描画は、基線変動及び湾曲を示し、実証的な手段によってのみ修正され得る。
2 基準位置
6 試料
13 加熱器
201 試料位置
202 基準位置
203 試料加熱器
204 基準加熱器
205 周囲の環境/熱分析装置
206 試料
301 試料位置
302 基準位置
303 試料加熱器
304 基準加熱器
307 第1のサーモパイル
308 第2のサーモパイル
309 コントロール・ループ
310 PIDコントローラー
311 測定回路
323 メインコントローラー
401 試料位置
402 基準位置
403 試料加熱器
404 基準加熱器
407 第1のサーモパイル
408 第2のサーモパイル
410 PIDコントローラー
411 測定回路
412 コントロール・ループ
423 メインコントローラー
720 電力補償
721 エンハンス熱流量
722 標準的熱流量
Claims (11)
- 試料(206)を受容するための試料位置(201,401)と、基準位置(202,402)と、
前記試料位置(201,401)及び前記基準位置(202,402)の各々を直接加熱する手段と、
時間対温度の名目値の所定の温度プログラムを設定する手段と、
前記試料位置(201,401)における試料温度(TS)を測定するための第1のセンサー(407)と、
前記基準位置(202,402)における基準温度(TR)を測定するための第2のセンサー(408)と、
更に、前記加熱手段の加熱電力を制御するコントローラー(423)を含んでいて、
前記加熱手段の加熱電力が、前記試料の測定温度(TS)を前記所定の温度プログラムに実質上、従わせるように制御されていることと、
前記試料(206)への正味の熱流量が、前記試料位置(201,401)と前記基準位置(202,402)との間に生じる差温及び/又は前記試料位置における温度測定(TS)から導き出されること、
を特徴とする熱流束型示差走査熱量計。 - センサー(407,408)それぞれが、少なくとも1つの熱電対、抵抗温度センサー又は半導体ベース温度センサーを有する少なくとも1つのサーモパイル配置を含むことを特徴とする請求項1記載の熱流束型示差走査熱量計。
- 基準物質が、前記基準位置(202,402)に関連付けられていることを特徴とする請求項1又は2記載の熱流束型示差走査熱量計。
- 前記加熱手段が、前記試料位置及び前記基準位置に関連付けられている共通の加熱器を含むことを特徴とする請求項1〜3記載のいずれかの熱流束型示差走査熱量計。
- 前記加熱手段が、前記基準位置(202,402)に関連付けられている基準加熱器(204、404)及び前記試料位置(201,401)に関連付けられている試料加熱器(203,403)を含むことを特徴とする請求項1〜4記載のいずれかの熱流束型示差走査熱量計。
- 前記試料位置(201,401)及び前記基準位置(202,402)が、共通ホルダー又は個別ホルダーに配置されていることを特徴とする請求項1〜5記載のいずれかの熱流束型示差走査熱量計。
- 前記試料位置(201,401)及び基準位置(202,402)が、本質上、対称を示していることを特徴とする請求項1〜6記載のいずれかの熱流束型示差走査熱量計。
- 前記熱流束型示差走査熱量計が、等周温条件下で作動されることを特徴とする請求項1〜7記載のいずれかの熱流束型示差走査熱量計。
- 前記熱流束型示差走査熱量計が、チップタイプ示差走査熱量計であることを特徴とする請求項1〜8記載のいずれかの熱流束型示差走査熱量計。
- 熱流束型示差走査熱量計を制御するための方法であって、
前記熱流束型示差走査熱量計が、
試料(206)を受容するための試料位置(201,401)と、基準位置(202,402)と、
前記試料位置(201,401)及び前記基準位置(202,402)の各々を直接加熱する手段と、
時間対温度の名目値の所定の温度プログラムを設定する手段と、
前記試料位置(201,401)における試料温度(TS)を測定するための第1のセンサー(407)と、
前記基準位置(202,402)における基準温度(TR)を測定するための第2のセンサー(408)と、
前記加熱手段の加熱電力を制御するコントローラー(423)と、を含んでいて、
前記試料位置(201,401)に試料(206)を配置するステップと、
前記加熱手段の加熱電力を制御することによって前記所定の温度プログラムを前記試料位置(201,401)及び前記基準位置(202,402)に適用するステップと、
前記試料温度(TS)を時間関数として決定するステップと、
を含む方法であって、
前記加熱手段の加熱電力が、前記試料の測定温度(TS)を実質上、前記所定の温度プログラムに従わせるように制御されていることと、
前記試料(206)への正味の熱流量が、前記試料位置(201,401)と前記基準位置(202,402)との間に生じる差温及び/又は前記試料位置における温度測定(TS)から導き出されること、
を特徴とする方法。 - 前記試料(206)の熱量が、基準位置(202,402)と前記試料位置(201,401)との間の熱量における不均衡と比較して常に大きいことを特徴とする請求項12記載の方法。
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EP09151986.8A EP2214005B1 (en) | 2009-02-03 | 2009-02-03 | Thermo-Analytical Instrument |
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ATE501433T1 (de) * | 2008-06-13 | 2011-03-15 | Mettler Toledo Ag | Wärmeanalyseinstrument mit dynamischer leistungskompensation |
US8926172B2 (en) * | 2009-07-07 | 2015-01-06 | Frank Leu Wu | Differential adiabatic compensation calorimeter and methods of operation |
JP5642525B2 (ja) * | 2010-02-02 | 2014-12-17 | 株式会社日立ハイテクサイエンス | 示差走査熱量計 |
CN101915774B (zh) * | 2010-08-09 | 2012-08-22 | 中国计量科学研究院 | 使用差示扫描量热仪测定有机物熔点的方法 |
US8836925B2 (en) * | 2011-05-06 | 2014-09-16 | Purdue Research Foundation | Imaging crystalline domains of small molecules |
JP5466333B1 (ja) * | 2013-11-25 | 2014-04-09 | 株式会社パルメトリクス | 熱測定装置 |
GB2532746B (en) * | 2014-11-26 | 2017-03-29 | Ibm | Temperature sensing |
EP3106851B1 (en) * | 2015-06-19 | 2019-01-02 | Endress + Hauser Flowtec AG | Process of determining at least one thermal property of a fluid under investigation with a thermal sensor |
CN105588854B (zh) * | 2016-02-26 | 2018-12-07 | 中国计量学院 | 快速温度扫描筛选量热仪 |
CN107228789B (zh) * | 2017-07-31 | 2023-09-08 | 郝东辉 | 一种具有温度测量功能的热裂解器及一种汞分析仪 |
JP6682485B2 (ja) * | 2017-09-12 | 2020-04-15 | エスペック株式会社 | 熱容量測定装置及び熱容量測定方法 |
CN108088871B (zh) * | 2018-01-10 | 2024-03-08 | 上海工程技术大学 | 一种纤维集合体蓄热性能的测试装置及其测试方法 |
CN108459046B (zh) * | 2018-05-09 | 2020-10-09 | 哈尔滨工业大学 | 薄膜型热电材料塞贝克系数及电导率的测试装置 |
CN108844993A (zh) * | 2018-06-28 | 2018-11-20 | 广州市建筑科学研究院有限公司 | 一种用于修正围护结构传热系数现场检测结果的方法 |
JP2020060522A (ja) * | 2018-10-12 | 2020-04-16 | 株式会社島津製作所 | 熱分析装置 |
CN109556987B (zh) * | 2018-11-27 | 2021-04-13 | 西安近代化学研究所 | 火炸药样品热分析过程中量热曲线基线位移的处理方法 |
JP7250268B2 (ja) * | 2018-12-21 | 2023-04-03 | 国立研究開発法人産業技術総合研究所 | 比熱とエンタルピー変化の測定方法 |
CN113640343B (zh) * | 2021-08-13 | 2023-04-25 | 中国计量大学 | 基于激光功率激励的差式扫描量热仪温度标定与重构方法 |
EP4350312A1 (en) * | 2022-10-04 | 2024-04-10 | Mettler-Toledo GmbH | Calibration method for a differential scanning calorimeter |
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JP2001305086A (ja) * | 2000-04-26 | 2001-10-31 | Seiko Instruments Inc | 熱分析装置 |
JP2003014674A (ja) * | 2001-07-03 | 2003-01-15 | Sumitomo Chem Co Ltd | 熱量計設置雰囲気の制御方法 |
EP1371973B1 (en) * | 2002-06-10 | 2011-08-24 | Mettler-Toledo AG | Method and apparatus for thermally investigating a material |
EP1494126B1 (de) * | 2003-07-04 | 2007-08-29 | Mettler-Toledo AG | Verfahren und Vorrichtung zur Stoffuntersuchung |
US7021820B2 (en) * | 2003-07-10 | 2006-04-04 | Simon Chippett | Low thermal inertia scanning adiabatic calorimeter |
US7371006B2 (en) * | 2004-02-10 | 2008-05-13 | Perkinelmer Las, Inc. | Differential scanning calorimeter (DSC) with temperature controlled furnace |
JP2006105935A (ja) * | 2004-10-08 | 2006-04-20 | Tokyo Institute Of Technology | 微小熱分析用プローブおよび微小熱分析装置ならびに微小熱分析方法 |
JP4849961B2 (ja) * | 2006-06-05 | 2012-01-11 | エスアイアイ・ナノテクノロジー株式会社 | 熱分析装置 |
DE202007002324U1 (de) * | 2007-02-13 | 2007-05-16 | Mettler-Toledo Ag | Vorrichtung für thermoanalytische Messungen |
CN100559175C (zh) | 2007-08-09 | 2009-11-11 | 同济大学 | 帕尔帖低温微分热分析仪 |
FR2925163B1 (fr) * | 2007-12-12 | 2010-02-26 | Centre Nat Rech Scient | Procede et appareil d'analyse thermique |
CN202267663U (zh) * | 2008-06-06 | 2012-06-06 | 魄金莱默保健科学有限公司 | 量热计及其控制系统 |
ATE501433T1 (de) * | 2008-06-13 | 2011-03-15 | Mettler Toledo Ag | Wärmeanalyseinstrument mit dynamischer leistungskompensation |
-
2009
- 2009-02-03 EP EP09151986.8A patent/EP2214005B1/en active Active
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2010
- 2010-01-27 US US12/694,464 patent/US20100195695A1/en not_active Abandoned
- 2010-02-02 JP JP2010020885A patent/JP5721953B2/ja active Active
- 2010-02-03 CN CN201611050822.6A patent/CN107014859B/zh active Active
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CN101799439A (zh) | 2010-08-11 |
US20100195695A1 (en) | 2010-08-05 |
US20140146847A1 (en) | 2014-05-29 |
JP2010181408A (ja) | 2010-08-19 |
US9528953B2 (en) | 2016-12-27 |
EP2214005B1 (en) | 2019-09-18 |
EP2214005A1 (en) | 2010-08-04 |
CN107014859B (zh) | 2020-12-11 |
CN107014859A (zh) | 2017-08-04 |
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