27 research outputs found

    Extending the functionalities of shear-driven chromatography nano-channels using high aspect ratio etching

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    An new injection system is presented for shear-driven chromatography. The device has been fabricated by high aspect ratio etching of silicon. The performance of the injection slit is studied through the aid of computational fluid dynamics, and the first experimental results are presented

    3D-Printed Stationary Phases with Ordered Morphology: State of the Art and Future Development in Liquid Chromatography Chromatographia

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    Stabilization of Scandium Terephthalate MOFs against Reversible Amorphization and Structural Phase Transition by Guest Uptake at Extreme Pressure

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    Previous high-pressure experiments have shown that pressure-transmitting fluids composed of small molecules can be forced inside the pores of metal organic framework materials, where they can cause phase transitions and amorphization and can even induce porosity in conventionally nonporous materials. Here we report a combined high-pressure diffraction and computational study of the structural response to methanol uptake at high pressure on a scandium terephthalate MOF (Sc2BDC3, BDC = 1,4-benzenedicarboxylate) and its nitro-functionalized derivative (Sc2(NO2–BDC)3) and compare it to direct compression behavior in a nonpenetrative hydrostatic fluid, Fluorinert-77. In Fluorinert-77, Sc2BDC3 displays amorphization above 0.1 GPa, reversible upon pressure release, whereas Sc2(NO2–BDC)3 undergoes a phase transition (C2/c to Fdd2) to a denser but topologically identical polymorph. In the presence of methanol, the reversible amorphization of Sc2BDC3 and the displacive phase transition of the nitro-form are completely inhibited (at least up to 3 GPa). Upon uptake of methanol on Sc2BDC3, the methanol molecules are found by diffraction to occupy two sites, with preferential relative filling of one site compared to the other: grand canonical Monte Carlo simulations support these experimental observations, and molecular dynamics simulations reveal the likely orientations of the methanol molecules, which are controlled at least in part by H-bonding interactions between guests. As well as revealing the atomistic origin of the stabilization of these MOFs against nonpenetrative hydrostatic fluids at high pressure, this study demonstrates a novel high-pressure approach to study adsorption within a porous framework as a function of increasing guest content, and so to determine the most energetically favorable adsorption sites

    Gradient-temperature hot-embossing for dense micropillar array fabrication on thick cyclo-olefin polymeric plates: An example of a microfluidic chromatography column fabrication

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    The fabrication of dense and high aspect ratio pillar arrays is important for several applications. In particular polymeric microfluidic chromatography columns are of high importance for various biological, pharmaceutical and chemical separations. Here, a cyclo‐olefin polymeric (COP) microcolumn fabrication process is developed using hot embossing with a temperature gradient for replication of a fine and highly dense array of micropillars on the surface of a 2 mm thick polymer plate without chip deformation. The design consists of an array of ordered cylindrical pillars with 15 μm diameter, 4 μm interpillar, and 2 μm pillar-wall distance with 20 μm height. The produced microcolumn is subsequently sealed with thermal bonding in a laminator and tested for liquid pressure operation up to 20 bar. Since COPs are hydrophobic by nature and have been used for reversed-phase liquid chromatographic (RPLC) separations in the past, preliminary separation experiments are also demonstrated in the fabricated column. © 201
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