Sébastien Clercq , Jérôme Vicente , Philippe Moulin
{"title":"用于三维结晶监测的 X 射线计算机断层扫描:扑热息痛应用案例","authors":"Sébastien Clercq , Jérôme Vicente , Philippe Moulin","doi":"10.1016/j.jcrysgro.2024.127794","DOIUrl":null,"url":null,"abstract":"<div><p>This work highlights the capabilities and limits of X-ray computed tomography in crystallization monitoring through a use case involving paracetamol as the solute, recrystallized from ethanol, methanol, or a mixture of both. The cooling crystallization operation was set up in two different containers, prepared with cotton yarns stretched vertically, acting as linear nucleation sites that immobilize the grown crystals in the recording area. The largest container (10 mL test tubes) allowed the acquisition of a larger number of crystals (up to 300 particles) for a more appropriate bulk analysis. The smallest container (5 mL pipette tips) allowed for a finer resolution of the recorded solid phase at the expense of a reduced recording volume. Crystallization was monitored in terms of the number of individual crystals, their size, and the overall volume, thus leading to the nucleation and growth rates, and solid-phase production rate. The main benefit of X-ray computed tomography is in the 3D analysis of the reconstructed solid phase. The crystal habit of paracetamol form I was predicted using force-field modeling. The predicted habit was in great accordance with the reconstructed solids, confirming the polymorphic form. Furthermore, face-specific growth rates of reconstructed crystals were measured, paving the way for a novel approach to the investigation of crystal-solvent interactions.</p></div>","PeriodicalId":353,"journal":{"name":"Journal of Crystal Growth","volume":null,"pages":null},"PeriodicalIF":1.7000,"publicationDate":"2024-06-13","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.sciencedirect.com/science/article/pii/S002202482400229X/pdfft?md5=3f4fc51795fac1d329ec849f55893371&pid=1-s2.0-S002202482400229X-main.pdf","citationCount":"0","resultStr":"{\"title\":\"X-ray computed tomography for 3D crystallization monitoring: A use case with paracetamol\",\"authors\":\"Sébastien Clercq , Jérôme Vicente , Philippe Moulin\",\"doi\":\"10.1016/j.jcrysgro.2024.127794\",\"DOIUrl\":null,\"url\":null,\"abstract\":\"<div><p>This work highlights the capabilities and limits of X-ray computed tomography in crystallization monitoring through a use case involving paracetamol as the solute, recrystallized from ethanol, methanol, or a mixture of both. The cooling crystallization operation was set up in two different containers, prepared with cotton yarns stretched vertically, acting as linear nucleation sites that immobilize the grown crystals in the recording area. The largest container (10 mL test tubes) allowed the acquisition of a larger number of crystals (up to 300 particles) for a more appropriate bulk analysis. The smallest container (5 mL pipette tips) allowed for a finer resolution of the recorded solid phase at the expense of a reduced recording volume. Crystallization was monitored in terms of the number of individual crystals, their size, and the overall volume, thus leading to the nucleation and growth rates, and solid-phase production rate. The main benefit of X-ray computed tomography is in the 3D analysis of the reconstructed solid phase. The crystal habit of paracetamol form I was predicted using force-field modeling. The predicted habit was in great accordance with the reconstructed solids, confirming the polymorphic form. Furthermore, face-specific growth rates of reconstructed crystals were measured, paving the way for a novel approach to the investigation of crystal-solvent interactions.</p></div>\",\"PeriodicalId\":353,\"journal\":{\"name\":\"Journal of Crystal Growth\",\"volume\":null,\"pages\":null},\"PeriodicalIF\":1.7000,\"publicationDate\":\"2024-06-13\",\"publicationTypes\":\"Journal Article\",\"fieldsOfStudy\":null,\"isOpenAccess\":false,\"openAccessPdf\":\"https://www.sciencedirect.com/science/article/pii/S002202482400229X/pdfft?md5=3f4fc51795fac1d329ec849f55893371&pid=1-s2.0-S002202482400229X-main.pdf\",\"citationCount\":\"0\",\"resultStr\":null,\"platform\":\"Semanticscholar\",\"paperid\":null,\"PeriodicalName\":\"Journal of Crystal Growth\",\"FirstCategoryId\":\"88\",\"ListUrlMain\":\"https://www.sciencedirect.com/science/article/pii/S002202482400229X\",\"RegionNum\":4,\"RegionCategory\":\"材料科学\",\"ArticlePicture\":[],\"TitleCN\":null,\"AbstractTextCN\":null,\"PMCID\":null,\"EPubDate\":\"\",\"PubModel\":\"\",\"JCR\":\"Q3\",\"JCRName\":\"CRYSTALLOGRAPHY\",\"Score\":null,\"Total\":0}","platform":"Semanticscholar","paperid":null,"PeriodicalName":"Journal of Crystal Growth","FirstCategoryId":"88","ListUrlMain":"https://www.sciencedirect.com/science/article/pii/S002202482400229X","RegionNum":4,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"Q3","JCRName":"CRYSTALLOGRAPHY","Score":null,"Total":0}
引用次数: 0
摘要
这项研究通过一个以扑热息痛为溶质,从乙醇、甲醇或两者的混合物中重结晶的应用案例,强调了 X 射线计算机断层扫描技术在结晶监测方面的能力和局限性。冷却结晶操作在两个不同的容器中进行,容器中的棉纱垂直拉伸,作为线性成核点,将生长的晶体固定在记录区域。最大的容器(10 mL 试管)可以采集更多的晶体(多达 300 个颗粒),以便进行更适当的批量分析。使用最小的容器(5 mL 移液器吸头)可获得更精细的固相记录分辨率,但记录体积有所减少。根据单个晶体的数量、大小和总体积监测结晶情况,从而得出成核率、生长率和固相生成率。X 射线计算机断层扫描的主要优势在于对重建的固相进行三维分析。利用力场模型预测了扑热息痛 I 型的晶体习性。预测的习性与重建的固相非常吻合,证实了其多晶形态。此外,还测量了重建晶体的特定面生长率,为研究晶体与溶剂的相互作用铺平了道路。
X-ray computed tomography for 3D crystallization monitoring: A use case with paracetamol
This work highlights the capabilities and limits of X-ray computed tomography in crystallization monitoring through a use case involving paracetamol as the solute, recrystallized from ethanol, methanol, or a mixture of both. The cooling crystallization operation was set up in two different containers, prepared with cotton yarns stretched vertically, acting as linear nucleation sites that immobilize the grown crystals in the recording area. The largest container (10 mL test tubes) allowed the acquisition of a larger number of crystals (up to 300 particles) for a more appropriate bulk analysis. The smallest container (5 mL pipette tips) allowed for a finer resolution of the recorded solid phase at the expense of a reduced recording volume. Crystallization was monitored in terms of the number of individual crystals, their size, and the overall volume, thus leading to the nucleation and growth rates, and solid-phase production rate. The main benefit of X-ray computed tomography is in the 3D analysis of the reconstructed solid phase. The crystal habit of paracetamol form I was predicted using force-field modeling. The predicted habit was in great accordance with the reconstructed solids, confirming the polymorphic form. Furthermore, face-specific growth rates of reconstructed crystals were measured, paving the way for a novel approach to the investigation of crystal-solvent interactions.
期刊介绍:
The journal offers a common reference and publication source for workers engaged in research on the experimental and theoretical aspects of crystal growth and its applications, e.g. in devices. Experimental and theoretical contributions are published in the following fields: theory of nucleation and growth, molecular kinetics and transport phenomena, crystallization in viscous media such as polymers and glasses; crystal growth of metals, minerals, semiconductors, superconductors, magnetics, inorganic, organic and biological substances in bulk or as thin films; molecular beam epitaxy, chemical vapor deposition, growth of III-V and II-VI and other semiconductors; characterization of single crystals by physical and chemical methods; apparatus, instrumentation and techniques for crystal growth, and purification methods; multilayer heterostructures and their characterisation with an emphasis on crystal growth and epitaxial aspects of electronic materials. A special feature of the journal is the periodic inclusion of proceedings of symposia and conferences on relevant aspects of crystal growth.