Differential Scanning Calorimetry Material Studies: Benzil Melting Point Method for Eliminating the Thermal History of DSC

How to eliminate the thermal history present in differential scanning calorimetry, this question has been widely concerned. Benzil has a serious thermal history that is not well eliminated by conventional thermal history methods. Herein, using benzil as a target, we developed a freeze-gradient tempe...

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Main Authors: Ziyang Zhu, Wei Li, Yilin Yin, Ruilin Cao, Zenghe Li
Format: Article
Language:English
Published: Wiley 2022-01-01
Series:Journal of Chemistry
Online Access:http://dx.doi.org/10.1155/2022/3423429
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author Ziyang Zhu
Wei Li
Yilin Yin
Ruilin Cao
Zenghe Li
author_facet Ziyang Zhu
Wei Li
Yilin Yin
Ruilin Cao
Zenghe Li
author_sort Ziyang Zhu
collection DOAJ
description How to eliminate the thermal history present in differential scanning calorimetry, this question has been widely concerned. Benzil has a serious thermal history that is not well eliminated by conventional thermal history methods. Herein, using benzil as a target, we developed a freeze-gradient temperature rate heating up method to eliminate the thermal history of DSC. Compared with the conventional method, this method avoids the introduction of new thermal histories by new crystalline forms that may appear during the cooling crystallization process. The results show that the peak shape of the melting peak is sharper and the peak emergence position is closer to the theoretical melting point after the elimination of the thermal history by the freeze-gradient heating up method. Based on this method, we optimized other factors to establish a complete method for the determination of melting point by DSC, analyzed the uncertainty of the method, and obtained an extended uncertainty of 0.19°C for DSC in this method. The validation results show that the p-nitrotoluene of the melting point reference substance was 52.64°C, which is within its reference value of (52.53 ± 0.20) °C, showing that this method is reliable. This study provides a reference for other thermal analysis methods to eliminate thermal history.
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issn 2090-9071
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publishDate 2022-01-01
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spelling doaj-art-cd3a11a17db748be9bdaa68b230229d92025-02-03T01:20:05ZengWileyJournal of Chemistry2090-90712022-01-01202210.1155/2022/3423429Differential Scanning Calorimetry Material Studies: Benzil Melting Point Method for Eliminating the Thermal History of DSCZiyang Zhu0Wei Li1Yilin Yin2Ruilin Cao3Zenghe Li4Calibration &Test CenterCalibration &Test CenterCollage of ChemistryCalibration &Test CenterCollage of ChemistryHow to eliminate the thermal history present in differential scanning calorimetry, this question has been widely concerned. Benzil has a serious thermal history that is not well eliminated by conventional thermal history methods. Herein, using benzil as a target, we developed a freeze-gradient temperature rate heating up method to eliminate the thermal history of DSC. Compared with the conventional method, this method avoids the introduction of new thermal histories by new crystalline forms that may appear during the cooling crystallization process. The results show that the peak shape of the melting peak is sharper and the peak emergence position is closer to the theoretical melting point after the elimination of the thermal history by the freeze-gradient heating up method. Based on this method, we optimized other factors to establish a complete method for the determination of melting point by DSC, analyzed the uncertainty of the method, and obtained an extended uncertainty of 0.19°C for DSC in this method. The validation results show that the p-nitrotoluene of the melting point reference substance was 52.64°C, which is within its reference value of (52.53 ± 0.20) °C, showing that this method is reliable. This study provides a reference for other thermal analysis methods to eliminate thermal history.http://dx.doi.org/10.1155/2022/3423429
spellingShingle Ziyang Zhu
Wei Li
Yilin Yin
Ruilin Cao
Zenghe Li
Differential Scanning Calorimetry Material Studies: Benzil Melting Point Method for Eliminating the Thermal History of DSC
Journal of Chemistry
title Differential Scanning Calorimetry Material Studies: Benzil Melting Point Method for Eliminating the Thermal History of DSC
title_full Differential Scanning Calorimetry Material Studies: Benzil Melting Point Method for Eliminating the Thermal History of DSC
title_fullStr Differential Scanning Calorimetry Material Studies: Benzil Melting Point Method for Eliminating the Thermal History of DSC
title_full_unstemmed Differential Scanning Calorimetry Material Studies: Benzil Melting Point Method for Eliminating the Thermal History of DSC
title_short Differential Scanning Calorimetry Material Studies: Benzil Melting Point Method for Eliminating the Thermal History of DSC
title_sort differential scanning calorimetry material studies benzil melting point method for eliminating the thermal history of dsc
url http://dx.doi.org/10.1155/2022/3423429
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AT yilinyin differentialscanningcalorimetrymaterialstudiesbenzilmeltingpointmethodforeliminatingthethermalhistoryofdsc
AT ruilincao differentialscanningcalorimetrymaterialstudiesbenzilmeltingpointmethodforeliminatingthethermalhistoryofdsc
AT zengheli differentialscanningcalorimetrymaterialstudiesbenzilmeltingpointmethodforeliminatingthethermalhistoryofdsc