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Instruments / Technical Area	Publication Details	Published	Actions
I11-High Resolution Powder Diffraction	Evaluation of microflow configurations for scale inhibition and serial X-ray diffraction analysis of crystallization processes Mark A. Levenstein , Yi-Yeoun Kim , Liam Hunter , Clara Anduix-Canto , Carlos Gonzalez Nino , Sarah J. Day , Shunbo Li , William J. Marchant , Phillip A. Lee , Chiu C. Tang , Manfred Burghammer , Fiona C. Meldrum , Nikil Kapur Lab On A Chip 57 DOI: 10.1039/D0LC00239A Diamond Proposal Number(s): [10425, 12352] Open Access Show Abstract ▼ Abstract: The clean and reproducible conditions provided by microfluidic devices are ideal sample environments for in situ analyses of chemical and biochemical reactions and assembly processes. However, the small size of microchannels makes investigating the crystallization of poorly soluble materials on-chip challenging due to crystal nucleation and growth that result in channel fouling and blockage. Here, we demonstrate a reusable insert-based microfluidic platform for serial X-ray diffraction analysis and examine scale formation in response to continuous and segmented flow configurations across a range of temperatures. Under continuous flow, scale formation on the reactor walls begins almost immediately on mixing of the crystallizing species, which over time results in occlusion of the channel. Depletion of ions at the start of the channel results in reduced crystallization towards the end of the channel. Conversely, segmented flow can control crystallization, so it occurs entirely within the droplet. Consequently, the spatial location within the channel represents a temporal point in the crystallization process. Whilst each method can provide useful crystallographic information, time-resolved information is lost when reactor fouling occurs and changes the solution conditions with time. The flow within a single device can be manipulated to give a broad range of information addressing surface interaction or solution crystallization.	Jul 2020
B22-Multimode InfraRed imaging And Microspectroscopy	Synchrotron FTIR mapping of mineralization in a microfluidic device Shunbo Li , Johannes Ihli , William Marchant , Muling Zeng , Li Chen , Katia Wehbe , Gianfelice Cinque , Oscar Cespedes , Nikil Kapur , Fiona Meldrum Lab On A Chip DOI: 10.1039/C6LC01393G Diamond Proposal Number(s): [12717] Show Abstract ▼ Abstract: Fourier transform infrared micro-spectroscopy provides an effective means of performing rapid, non-destructive, and label-free analysis of specimens according to their vibrational modes. However, as water absorbs very strongly in the infrared region, analysis of aqueous solutions in transmission mode can suffer from problems with signal saturation. We here describe the fabrication of a novel microfluidic device that overcomes this problem. Devices with channel depths of just 3 µm were constructed from calcium fluoride using photolithography and hot embossing bonding, where calcium fluoride was selected due to its transparency in the IR region. The utility of this device was then demonstrated by employing it to follow the precipitation pathways of calcium sulfate and calcium carbonate using synchrotron FTIR micro-spectroscopy. Importantly, due to the high brightness provided by synchrotron radiation, and the fact that the reacting ions (HCO3- , CO32- and SO42-) and the different mineral polymorphs all have finger print spectra in the measured IR range, this method can be used to acquire time-resolved, hyperspectral maps of the mineral particles formed within the sample cell, and then study the interaction and evolution of particles. The data provide new insight into the formation pathway of a population of crystals in confined volumes, and demonstrate that this in situ, real-time detection system provides a powerful tool for studying crystallization processes.	Mar 2017

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