Temperature and Heat Flow Calibration of A DSC-instrument in the Temperature Range Between −100 and 160°C
Temperature and Heat Flow Calibration of A DSC-instrument in the Temperature Range Between −100 and 160°C
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-100 至 160°C 温度范围内 DSC 仪器的温度和热流校准
DOI：
10.1023/a:1010156407261
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发表时间：
2000
影响因子：
4.4
通讯作者：
M. Schubnell
中科院分区：
文献类型：
--
作者：
M. Schubnell
热分析仪器广泛用于研发和工业质量控制。热分析测量数据的定量分析需要仔细校准仪器。在差示扫描量热法（DSC）中，必须校准的量是温度和热流。这两个量通常是通过评估一些参考材料的熔化或固-固转变来校准的，这些参考材料具有众所周知的转变谱和温度。在这篇文章中，我们研究了−100和160°C之间温度范围内的温度和热流校准。我们包括9种不同的样品进行分析，并建立了一些校准过程的一般规则。因此，我们发现，使用校准良好的仪器，在此温度范围内可以以90%的置信度测量热流，精度约为± 3%。关于温度校准，我们发现可以预期±0.8°C（90%置信度）的精度。这些值表示由于样品内不同的传热条件而导致的DSC的一般精度限制。
Thermoanalytical instruments are extensively used in R&D as well as in industrial quality control. A quantitative analysis of the data of a thermoanalytical measurement requires a careful calibration of the instrument. In differential scanning calorimetry (DSC) the quantities that have to be calibrated are the temperature and the heat flow. These two quantities are usually calibrated by evaluating melting or solid-solid transitions of some reference materials with well known transition enthalpies and temperatures. In this contribution we investigate temperature and heat flow calibration in the temperature range between −100 and 160°C. We included 9 different samples for the analysis and established some general rules for the calibration process. As a result we found that with a well calibrated instrument the heat flow can be measured with 90% confidence to about ± 3% accuracy in this temperature range. With respect to temperature calibration we find that accuracies of ±0.8°C (90% confidence) may be expected. These values represent general accuracy limitations of DSC’s due to varying heat transfer conditions within the samples.