The adsorption of proteins by a smectitic clay mineral was investigated. The clay used in this study is a mixture of montmorillonite and amorphous SiO(2). Due to the high porosity the montmorillonite units are accessible for protein adsorption. The amorphous silica prevents the montmorillonite from swelling and allows column packing. Protein adsorption was performed at different pH under static conditions. Furthermore, static capacities were determined. The material reveals high adsorption capacities for proteins under static conditions (270-408 mg/g), whereby proteins are mainly adsorbed via electrostatic interactions. The Freundlich isotherm is suggested as an adsorption model. For desorption a pH shift was found to be most effective. Binding and elution of human serum albumin and ovalbumin were tested under dynamic conditions. Dynamic capacities of about 40 mg/g for ovalbumin at 764 cm/h were found. The clay mineral provides suitable properties for the application as cost-efficient, alternative separation material.
The distribution of unpaired electron spin over all regions of the organic ligands was extracted from the large positive and negative 1H and 13C NMR paramagnetic shifts of the title complexes. Owing to benevolent line broadening and to very high sensitivities of approximately 254,000 and approximately 201,000 ppm/(unpaired electron spin) for Co(II) and Ni(II), respectively, at 298 K in these pseudotetrahedral bis(N,N'-chelates), spin transmission through the sigma- (and orthogonal pi)-bonding system of the ligands could be traced from the chelate ring over five to nine sigma bonds. Most of those "experimental" spin densities DeltarhoN (situated at the observed nuclei) agree reasonably well with quantum chemical DeltarhoDFT (DFT = density functional theory) values and provide an unsurpassed number of benchmark values for the quality of certain types of modern density functionals. The extraction of DeltarhoN became possible through the unequivocal separation of the nuclear Fermi contact shift components from the metal-centered pseudocontact shifts, which are proportional to the anisotropy Deltachi of the magnetic susceptibility: Experimental Deltachi values were obtained in solution from measured deuterium quadrupole splittings in the 2H NMR spectra of two deuterated model complexes and were found to be nonlinear functions of the reciprocal temperature. This provided the reliable basis for predicting metal-centered pseudocontact shifts for any position of a topologically well-defined ligand at varying temperatures. The related ligand-centered pseudocontact shifts were sought by using the criterion of their expected nonlinear dependence on the reciprocal temperature. However, their contributions could not be differentiated from other small effects close to the metal center; otherwise, they appeared to be smaller than the experimental uncertainties. The free activation energy of N-aryl rotation past a vicinal tert-butyl substituent in the Ni(II) vinamidine bis(N,N'-chelates) is DeltaG++(+74 degrees C) approximately 17.0 kcal/mol and past a vicinal methyl group DeltaG++(-6 degrees C) approximately 13.1 kcal/mol.
Abstract:Interstratifications of talc and trioctahedral smectites from different provenances are used as indicators for geological environments and for geotechnical and technical applications. However, comprehensive layer characterization of these interstratifications is rare. Sample EX M 1694, a clay with red-beige appearance from the Madrid basin was studied by X-ray diffraction analysis, X-ray fluorescence analysis, Fourier transformation infrared spectroscopy, simultaneous thermal analysis, gas adsorption measurements, cation exchange capacity, and environmental scanning electron microscopy. More than 95% of particles in EX M 1964 belong to the clay fraction <2 µm. It contains 75% interstratification of 30% turbostratic talc, and 70% saponite type III and 25% turbostratic talc. The turbostratic talc(0.3)/saponite interstratification is characterized by a low number of layers per stack (3), small lateral dimension of layers (60-80 nm) and, accordingly, a high specific surface area (283 m 2 /g) with nearly equal surface area of micro-and mesopores. Thus, the studied material can be used as mined for adsorption, in contrast to acid-treated clays that produce hazardous waste during production. Low particle size of the interstratification drastically reduced thermal stability and dehydroxylation was superimposed by recrystallization of high temperature phases already at 816 • C, which is low for trioctahedral 2:1 layer minerals.
The main physico-chemical properties of a new smectitic clay containing large amounts of amorphous material are reviewed and potential industrial applications of this type of clay are discussed. Due to a 34% amorphous material content (natural silica gel), the investigated clay has very high porosity and can be used as it is or in acid-impregnated form for oil bleaching or phosphate reduction in edible oil. In the field of biodiesel purification, the new clay can be used to remove, in particular, mono-, diglycerides and glycerol. The natural silica-smectite mixture is also suitable as a carrier for liquid ingredients, for example in animal feeds, and might serve as a partial or complete substitute for synthetic precipitated silicas. In the field of bioseparation processes, the clay can be used as an adsorbent for protein separation by means of cation exchange. Due to the suppressed swelling (compared with smectite alone), it can be packed in columns which can be regenerated.
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