Application of In-Process X-ray Powder Diffraction for the Identification of Polymorphic Forms during Batch Crystallization Reactions

Robert B.Hammond; Xiaojun Lai; Kevin J.Roberts; Alistair Thomas; Graeme White

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Application of In-Process X-ray Powder Diffraction for the Identification of Polymorphic Forms during Batch Crystallization Reactions

机译：过程中X射线粉末衍射在间歇结晶反应过程中多晶型鉴定中的应用

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An on-line X-ray diffraction system capable of monitoring and identifying the polymorphic form of organic materials crystallized during batch crystallization processes is described.The overall system comprises a conventional X-ray source,monochromator,collimator,slits,curved position sensitive detector,and a flow-through analysis cell together with the electronics and the data acquisition software.The cell enables X-ray diffraction data to be recorded from crystals suspended within a slurry pumped to and from a batch crystallizer via an external temperature controlled sampling loop.The system is validated via benchmark crystallization studies of urea,L-glutamic acid and monosodium glutamate.The system was found to have a performance consistent with a lower detection limit of ca.1% wt % of crystals and to be able to follow polymorphic transformation during representative crystallization processes.A forward look to the further development of the system is provided.

机译：描述了一种能够监测和识别在批结晶过程中结晶的有机物的多晶型形式的在线X射线衍射系统。整个系统包括常规X射线源，单色仪，准直仪，狭缝，弯曲位置敏感探测器，该单元可以通过外部温度控制的采样环路记录从泵送至间歇结晶器的浆液中悬浮的浆料中悬浮的晶体中的X射线衍射数据。通过对尿素，L-谷氨酸和谷氨酸钠的基准结晶研究验证了该系统的有效性，发现该系统的性能与较低的检出限（约1％wt％的晶体）相一致，并且能够在检测过程中进行多晶型转变具有代表性的结晶过程。提供了对该系统进一步开发的前瞻性信息。

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《Crystal growth & design》 |2004年第5期|共6页
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Robert B.Hammond; Xiaojun Lai; Kevin J.Roberts; Alistair Thomas; Graeme White;
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1. Application of In-Process X-ray Powder Diffraction for the Identification of Polymorphic Forms during Batch Crystallization Reactions [J] . Robert B.Hammond, Xiaojun Lai, Kevin J.Roberts, Crystal growth & design . 2004,第5期

机译：过程中X射线粉末衍射在间歇结晶反应过程中多晶型鉴定中的应用
2. Dynamic Crystallization Pathways of Polymorphic Pharmaceuticals Revealed in Segmented Flow with Inline Powder X-ray Diffraction [J] . Levenstein Mark A., Wayment Lois E., Scott C. Daniel, Analytical chemistry . 2020,第11期

机译：具有内联粉末X射线衍射的分段流动揭示多态性药物的动态结晶途径
3. Crystallization of a Desired Metastable Polymorph by Pseudoseeding, Crystal Structure Solution from Its Powder X-ray Diffraction Data, and Confirmation of Polymorphic Transition [J] . Hidenori Miura, Takaniro Ushio, Keiko Nagai, Crystal growth & design . 2003,第6期

机译：拟亚晶型的拟晶种结晶，粉末X射线衍射数据的晶体结构溶液以及多晶型转变的确认
4. Decoupling Electrolyte and Electrode Reactions Using in-Operando Electrochemical X-Ray Powder Diffraction [C] . Oles Sendetskyi, Mark Salomons, Steve Launspach, Pacific Rim Meeting on Electrochemical and Solid-State Science . 2020

机译：使用Outmando电化学X射线粉衍射去耦电解质和电极反应
5. Development of multivariate powder X-ray diffraction techniques and total scattering analyses to enable informatic calibration of solid dispersion potential. [D] . Moore, Michael D. 2010

机译：多元粉末X射线衍射技术和总散射分析技术的发展，可以对固体分散电位进行信息校准。
6. Identification of Polymorphic Forms of Active Pharmaceutical Ingredient in Low-Concentration Dry Powder Formulations by Synchrotron X-Ray Powder Diffraction [O] . Kenji Egusa, Fumiaki Okazaki, Joerg Schiewe, 2017

机译：用同步辐射X射线粉末衍射法鉴定低浓度干粉制剂中活性药物成分的多晶型物
7. Application of X-Ray Powder Diffraction to Drug Information and Dispensing Services. II. Identification of Ingredients in Powder Preparations Containing Composite Powder Like Granules and Pulverized Tablets (or Capsules). [O] . KAZUYUKI SAITO, YOSHIFUMI MURATA, ETSUKO MIYAMOTO, 1992

机译：X射线粉衍射在药物信息和分配服务中的应用。 II。鉴别含有颗粒和粉碎片（或胶囊）的复合粉末的粉末制剂中成分。
8. CALGULATED X-RAY DIFFRACTION DATA FOR POLYMORPHIC FORMS OF CARBON [R] . C. E. Holcombe 1973

机译：用于碳的多晶形态的计算X射线衍射数据

Application of In-Process X-ray Powder Diffraction for the Identification of Polymorphic Forms during Batch Crystallization Reactions

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