T D Turner, C O'Shaughnessy, X He, M A Levenstein, L Hunter, J Wojciechowski, H Bristowe, R Stone, C C Wilson, A Florence, K Robertson, N Kapur, F C Meldrum
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引用次数: 0
Abstract
Characterization of crystallization processes in situ is of great importance to furthering knowledge of how nucleation and growth processes direct the assembly of organic and inorganic materials in solution and, critically, understanding the influence that these processes have on the final physico-chemical properties of the resulting solid form. With careful specification and design, as demonstrated here, it is now possible to bring combined X-ray diffraction and Raman spectroscopy, coupled to a range of fully integrated segmented and continuous flow platforms, to the laboratory environment for in situ data acquisition for timescales of the order of seconds. The facility used here (Flow-Xl) houses a diffractometer with a micro-focus Cu Kα rotating anode X-ray source and a 2D hybrid photon-counting detector, together with a Raman spectrometer with 532 and 785 nm lasers. An overview of the diffractometer and spectrometer setup is given, and current sample environments for flow crystallization are described. Commissioning experiments highlight the sensitivity of the two instruments for time-resolved in situ data collection of samples in flow. Finally, an example case study to monitor the batch crystallization of sodium sulfate from aqueous solution, by tracking both the solute and solution phase species as a function of time, highlights the applicability of such measurements in determining the kinetics associated with crystallization processes. This work illustrates that the Flow-Xl facility provides high-resolution time-resolved in situ structural phase information through diffraction data together with molecular-scale solution data through spectroscopy, which allows crystallization mechanisms and their associated kinetics to be analysed in a laboratory setting.
原位结晶过程的表征对于进一步了解成核和生长过程如何指导溶液中有机和无机材料的组装,以及对于了解这些过程对所形成的固体形式的最终物理化学性质的影响至关重要。正如本文所展示的,通过精心的规范和设计,现在可以将 X 射线衍射和拉曼光谱结合到一系列完全集成的分段和连续流动平台上,在实验室环境中以秒为单位进行现场数据采集。这里使用的设备(Flow-Xl)包括一台配有微焦点 Cu Kα 旋转阳极 X 射线源和二维混合光子计数探测器的衍射仪,以及一台配有 532 和 785 纳米激光器的拉曼光谱仪。报告概述了衍射仪和光谱仪的设置,并介绍了当前用于流动结晶的样品环境。调试实验强调了两台仪器在流动样品的时间分辨原位数据收集方面的灵敏度。最后,通过对溶质和溶液相物种随时间变化的跟踪,介绍了监测水溶液中硫酸钠批量结晶的案例研究,强调了此类测量在确定结晶过程相关动力学方面的适用性。这项工作表明,Flow-Xl 设备可通过衍射数据提供高分辨率的时间分辨原位结构相信息,并通过光谱学提供分子尺度的溶液数据,从而可在实验室环境中分析结晶机制及其相关动力学。
期刊介绍:
Many research topics in condensed matter research, materials science and the life sciences make use of crystallographic methods to study crystalline and non-crystalline matter with neutrons, X-rays and electrons. Articles published in the Journal of Applied Crystallography focus on these methods and their use in identifying structural and diffusion-controlled phase transformations, structure-property relationships, structural changes of defects, interfaces and surfaces, etc. Developments of instrumentation and crystallographic apparatus, theory and interpretation, numerical analysis and other related subjects are also covered. The journal is the primary place where crystallographic computer program information is published.