In situ non-invasive Raman spectroscopic characterisation of succinic acid polymorphism during segmented flow crystallisation
In situ non-invasive Raman spectroscopic characterisation of succinic acid polymorphism during segmented flow crystallisation
复制标题
DOI：
10.1039/c9me00103d
复制
发表时间：
2020-01-01
影响因子：
3.6
通讯作者：
Robertson, Karen
中科院分区：
文献类型：
--
作者：
Pallipurath, Anuradha R.;Flandrin, Pierre-Baptiste;Robertson, Karen
动力学调节的拉曼光谱自动输入结晶器（KRAIC-R）结合了高度控制的结晶环境，通过三段流，与非侵入性共聚焦拉曼光谱。利用分段流动结晶器内高度可重现的结晶环境和共聚焦光谱的非侵入性，我们能够通过我们的分析技术在拉曼活性多晶材料的成核和生长上发光，而不会引起不具代表性的结晶事件。利用KRAIC-R对琥珀酸的成核和后续生长进行了研究。琥珀酸通常在溶液结晶中结晶为β - sa，尽管在β - sa产物中有一小部分α - sa的报道。在这里，我们发现α - sa和β - sa同时成核，但经过奥斯特瓦尔德成熟，主要形成β - sa产物。
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 beta-SA from solution-based crystallisation although some examples of a small proportion of alpha-SA have been reported in the beta-SA product. Here we show that alpha-SA and beta-SA nucleate concomitantly but undergo Ostwald ripening to a predominantly beta-SA product.