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Investigation of the effect of temperature cycling on surface features of sulfathiazole crystals during seeded batch cooling crystallization

机译:种子分批冷却结晶过程中温度循环对磺胺噻唑晶体表面特征影响的研究

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摘要

The effect of temperature cycling on the surface features of sulfathiazole crystals was investigated using focused beam reflectance measurement (FBRM) and ex situ optical microscopy, scanning electron microscopy (SEM), and atomic forced microscopy (AFM). Smoothing of the crystal surface was observed during heating, while during cooling the smooth crystals showed features growing on their surfaces. These changes on the crystal surface were detected by the FBRM as an increase in the number of coarse counts during heating phases and a drop during cooling phases. Laser beam spreading caused by the surface changes and signal/chord splitting due to the formation of sharp edges are suggested as explanations for the FBRM results. The study shows the capability of FBRM to provide useful information with regard to the changes on the surface of the crystalline products, which could be linked to possible growth mechanisms. The information can be used to avoid problems in the downstream processing or in the final product property due to variations in flowability and friability, which are related to the crystal surface property.
机译:使用聚焦束反射率测量(FBRM)和非原位光学显微镜,扫描电子显微镜(SEM)和原子强迫显微镜(AFM)研究了温度循环对磺胺噻唑晶体表面特征的影响。在加热期间观察到晶体表面的光滑,而在冷却期间观察到光滑的晶体显示出在其表面上生长的特征。 FBRM检测到晶体表面的这些变化是在加热阶段增加了粗粒数量,而在冷却阶段减少了数量。建议将由表面变化引起的激光束散布以及由于形成尖锐边缘而导致的信号/弦分裂作为FBRM结果的解释。研究表明,FBRM能够提供有关晶体产品表面变化的有用信息,这可能与可能的生长机制有关。该信息可用于避免由于与晶体表面特性有关的流动性和脆性变化而导致的下游加工或最终产品特性方面的问题。

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