Publications by authors named "Douglas Hausner"

While macromixing (gross uniformity) has received a lot of attention in pharmaceutical powder blending, micromixing (particularly, particle-level aggregation) has been significantly less studied. This study investigated the impact of active pharmaceutical ingredient (API) particle size (D: 11, 28, and 70 µm) and blending shear rate (low and high) that was caused by tumbling blending (specifically, a V-blender) on micro-mixing. The effect on micro-mixing (API domain sizes) was assessed in direct compression tablets using high-resolution Raman chemical mapping.

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Raman chemical mapping is an inherently slow analysis tool. Accurate and robust multivariate analysis algorithms, which require least amount of time and effort in method development are desirable. Calibration-free regression and resolution approaches such as classical least squares (CLS) and multivariate curve resolution using alternating least squares (MCR-ALS), respectively, help in reducing the resources required for method development.

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In-line measurements of low dose blends in the feed frame of a tablet press were performed for API concentration levels as low as 0.10% w/w. The proposed methodology utilizes the advanced sampling capabilities of a Spatially Resolved Near-Infrared (SR-NIR) probe to develop Partial Least-Squares calibration models.

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The structure and reactivity of 0-70mol% Al/Fe iron oxyhydroxides (ferrihydrite in the absence and presence of Al) toward gaseous CO2 were investigated with X-ray photoelectron spectroscopy (XPS), atomic absorption (AA), scanning transmission electron microscopy with electron dispersive X-ray spectroscopy (STEM/EDS), X-ray diffraction (XRD), and attenuated total reflectance Fourier transform Infrared spectroscopy (ATR-FTIR) combined with density functional theory (DFT) calculations. Results showed that Al/Fe oxyhydroxide particles containing more than 20 mol% Al consisted at least in part of Fe-oxyhydroxide with incorporated Al and a discrete AlOOH phase. Results from ATR-FTIR experiments and DFT calculations suggested that the bicarbonate complex formed by passing CO2 over the particles was accommodated on at least three distinct binding sites.

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Pair distribution function (PDF) analysis of neutron total scattering data from deuterated two-line ferrihydrite is consistent with the Keggin-related structural model for ferrihydrite published by Michel et al. (2007). Other models proposed in the literature, such as that of Drits et al.

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The photodissolution of the iron oxyhydroxide, ferrihydrite, in the presence of oxalic acid was investigated with vibrational spectroscopy, density functional theory (DFT) calculations, and batch geochemical techniques that determined the composition of the solution phase during the dissolution process. Specifically, in situ attenuated total reflection Fourier transform infrared spectroscopy (ATR- FTIR) was used to determine the structure of the adsorbed layer during the dissolution process at a solution pH of 4.5.

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Background: In nature or in the laboratory, the roughly spherical interior of the ferritin protein is well suited for the formation and storage of a variety of nanosized metal oxy-hydroxide compounds which hold promise for a range of applications. However, the linkages between ferritin reactivity and the structure and physicochemical properties of the nanoparticle core, either native or reconstituted, remain only partly understood.

Scope Of Review: Here we review studies, including those from our laboratory, which have investigated the structure of ferritin-derived ferrihydrite and reactivity of ferritin, both native and reconstituted.

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Differential pair distribution function (d-PDF) analysis of high energy powder X-ray diffraction data was carried out on 2-line ferrihydrite nanoparticles with arsenate oxyanions adsorbed on the surface to investigate the binding mechanism. In this analysis, a PDF of ferrihydrite is subtracted from a PDF of ferrihydrite with arsenate sorbed on the surface, leaving only correlations from within the surface layer and between the surface and the particle. As-O and As-Fe correlations were observed at 1.

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The interaction of ascorbic acid with ferrihydrite nanoparticles with and without adsorbed phospholipid has been investigated with atomic force microscopy (AFM), attenuated total reflection Fourier transform infrared spectroscopy (ATR-FTIR), density functional theory (DFT) cluster calculations, and batch geochemical methods. Both batch geochemical rate measurements and in situ AFM showed that ferrihydrite particles dissolved in the presence of ascorbic acid over a period of hours. The area-normalized dissolution rate derived from AFM measurements of isolated ferrihydrite particles was relatively constant over the period of dissolution and was faster than the dissolution rate derived from batch reaction methods.

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The reaction of ferrihydrite with gaseous CO(2) was investigated with attenuated total reflection Fourier transform infrared spectroscopy (ATR-FTIR) and density functional theory (DFT) calculations. ATR-FTIR results show that CO(2) reacts with ferrihydrite resulting in surface adsorbed carbonate species. The carbonate species experimentally observed in view of theoretical calculations are shown to be in large part monodentate binuclear complexes.

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Experiments with dinitrogen-, nitrite-, nitrate-containing solutions were conducted without headspace in Ti reactors (200 degrees C), borosilicate septum bottles (70 degrees C) and HDPE tubes (22 degrees C) in the presence of Fe and Ni metal, awaruite (Ni80Fe20) and tetrataenite (Ni50Fe50). In general, metals used in this investigation were more reactive than alloys toward all investigated nitrogen species. Nitrite and nitrate were converted to ammonium more rapidly than dinitrogen, and the reduction process had a strong temperature dependence.

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The composition and topography of calcite 10114 cleavage surfaces, with and without exposure to divalent metals, have been investigated as a function of relative humidity. Atomic force microscopy (AFM) was used to understand topographical changes on the calcite surface due to the presence of divalent metal and exposure to different humid environments. Ion scattering spectroscopy (ISS) was used to determine the composition of the near and outermost surface of the calcite after exposure to Cd and Pb and before exposure to the varying humidity conditions.

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Ferrihydrite nanoparticles with nominal sizes of 3 and 6 nm were assembled within ferritin, an iron storage protein. The crystallinity and structure of the nanoparticles (after removal of the protein shell) were evaluated by high-resolution transmission electron microscopy (HRTEM), atomic force microscopy (AFM), and scanning tunneling microscopy (STM). HRTEM showed that amorphous and crystalline nanoparticles were copresent, and the degree of crystallinity improved with increasing size of the particles.

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New applications in regenerative biotechnology require the ability to understand and control protein-surface interactions on micrometer and submicrometer length scales. Evidence presented here shows that micropatterned amphiphilic comb polymer films exhibit a pretreatment-dependent behavior with respect to protein adsorption for the proteins fibronectin, laminin, and for serum. A micropatterned surface, consisting of protein-reactive regions, separated by comb polymer, was created and tested for protein adsorption using the surface-sensitive imaging tool TOF-SIMS.

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The interaction of divalent Cd and Pb with the {101 4} cleavage faces of calcite has been investigated with X-ray photoelectron spectroscopy (XPS) and atomic force microscopy (AFM). Analysis of the {101 4} cleavage planes of calcite was carried out with X-ray photoelectron spectroscopy (XPS) after exposure to divalent metal-bearing solutions in the 0.1-100 microM concentration range for times ranging from 1 to 24 h.

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