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In situ non-invasive Raman spectroscopic characterisation of succinic acid polymorphism during segmented flow crystallisation
Molecular Systems Design & Engineering ( IF 3.6 ) Pub Date : 2019/10/18 , DOI: 10.1039/c9me00103d
Anuradha R. Pallipurath 1, 2, 3 , Pierre-Baptiste Flandrin 1, 2, 3 , Lois E. Wayment 1, 2, 2, 3, 4 , Chick C. Wilson 1, 2, 2, 3, 4 , Karen Robertson 1, 2, 3
Affiliation  

The kinetically regulated automated input crystalliser for Raman spectroscopy (KRAIC-R) combines highly controlled crystallisation environments, via tri segmented flow, with non-invasive confocal Raman spectroscopy. Taking advantage of the highly reproducible crystallisation environment within a segmented flow crystalliser and the non-invasive nature of confocal spectroscopy, we are able to shine light on the nucleation and growth of Raman active polymorphic materials without inducing unrepresentative crystallisation events through our analysis technique. Using the KRAIC-R we have probed the nucleation and subsequent growth of succinic acid. Succinic acid typically crystallises as β-SA from solution-based crystallisation although some examples of a small proportion of α-SA have been reported in the β-SA product. Here we show that α-SA and β-SA nucleate concomitantly but undergo Ostwald ripening to a predominantly β-SA product.

中文翻译:

分段流结晶过程中琥珀酸多态性的原位非侵入性拉曼光谱表征

用于拉曼光谱的动力学调节自动输入结晶器(KRAIC-R)结合了高度受控的结晶环境,通过三段流,无创共聚焦拉曼光谱。利用分段流动结晶器中高度可再现的结晶环境和共聚焦光谱法的非侵入性,我们能够通过我们的分析技术将光照射到拉曼活性多晶型材料的形核和生长上,而不会引起代表性结晶事件。使用KRAIC-R,我们探查了琥珀酸的成核及其随后的生长。琥珀酸通常从溶液基结晶中结晶为β-SA,尽管在β-SA产品中已报道了少量α-SA的一些例子。在这里,我们显示α-SA和β-SA伴随有核,但经历了奥斯特瓦尔德熟化,成为主要的β-SA产物。
更新日期:2020-02-13
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