Hoeher, AlexandriaMergelsberg, Sebastian T.Borkiewicz, Olaf J.Dove, Patricia M.Michel, F. Marc2021-10-132021-10-132019-09-012053-2733S2053273319008623 (PII)http://hdl.handle.net/10919/105283Structural investigations of amorphous and nanocrystalline phases forming in solution are historically challenging. Few methods are capable of in situ atomic structural analysis and rigorous control of the system. A mixed-flow reactor (MFR) is used for total X-ray scattering experiments to examine the short- and long-range structure of phases in situ with pair distribution function (PDF) analysis. The adaptable experimental setup enables data collection for a range of different system chemistries, initial supersaturations and residence times. The age of the sample during analysis is controlled by adjusting the flow rate. Faster rates allow for younger samples to be examined, but if flow is too fast not enough data are acquired to average out excess signal noise. Slower flow rates form older samples, but at very slow speeds particles settle and block flow, clogging the system. Proper background collection and subtraction is critical for data optimization. Overall, this MFR method is an ideal scheme for analyzing the in situ structures of phases that form during crystal growth in solution. As a proof of concept, high-resolution total X-ray scattering data of amorphous and crystalline calcium phosphates and amorphous calcium carbonate were collected for PDF analysis.Pages 758-7658 page(s)application/pdfenCreative Commons Attribution 4.0 InternationalPhysical SciencesChemistry, MultidisciplinaryCrystallographyChemistryin situ X-ray total scatteringcrystallizationamorphous calcium phosphateamorphous calcium carbonatepair distribution function analysisPAIR DISTRIBUTION FUNCTIONCALCIUM-PHOSPHATEAREA DETECTORFLOW REACTORCARBONATECLUSTERSArticle - Refereed2021-10-13https://doi.org/10.1107/S205327331900862375Pt 5Michel, Frederick [0000-0003-2817-980X]314759192053-2733