DDT-related compounds bound to the nonextractable particulate matter in sediments of the Teltow Canal,Germany

Sediment samples of the Teltow Canal (Berlin, Germany) were analyzed with respect to extractable and nonextractable organic compounds. The study focused on the identification and quantitation of bound 2,2-bis(chlorophenyl)-1,1,1-trichlorethane (DDT) residues in order to obtain further information about the fate of DDT-derived compounds within the particulate matter of the aquatic environment. Various chemical degradation techniques and a complementary online pyrolysis-GC/MS method were applied to the pre-extracted sediment residues. Generally, the distribution of the bound DDT-related compounds was found to differ distinctly from the substances distribution within the extractable fraction. The main metabolite of the anaerobic degradation pathway (2,2-bis(chlorophenyl)-1,1-dichlorethane, DDD) is most abundant in the sediment extracts but occurred only in insignificant concentrations in the degradation products of all procedures applied. The most abundant DDT-metabolites released after the degradation procedures were 4,4'-DBP, 4,4'-DDA, and 4,4'-DDM. In addition, 4,4'-DDM was detected at rather high concentrations by pyrolytic analysis. The results imply a weak association to the nonextractable particulate matter based on noncovalent interactions for the observed DDT-related contaminants. The release of these compounds was initiated by the modification and degradation of the organic macromolecular matrix as well as of the inorganic material. Furthermore, numerous methoxychlor-related compounds were detected not only in the extracts but also in parts of the hydrolysis products.     

Synthesis of cubic zirconium and hafnium nitride having Th3P4 structure

High-pressure synthesis is a powerful method for the preparation of novel materials with high elastic moduli and hardness. Additionally, such materials may exhibit interesting thermal, optoelectronic, semiconductuing, magnetic or superconducting properties. Here, we report on the high-pressure synthesis of zirconium and hafnium nitrides with the stoichiometry M3N4, where M = Zr, Hf. Synthesis experiments were performed in a laser-heated diamond anvil cell at pressures up to 18 GPa and temperatures up to 3,000 K. We observed formation of cubic Zr3N4 and Hf3N4 (c-M3N4) with a Th3P4-structure, where M-cations are eightfold coordinated by N anions. The c-M3N4 phases are the first binary nitrides with such a high coordination number. Both compounds exhibit high bulk moduli around 250 GPa, which indicates high hardness. Moreover, the new nitrides, c-Zr3N4 and c-Hf3N4, may be the first members of a larger group of transition metal and/or lanthanide nitrides with interesting ferromagnetic or superconducting behaviour.     

Kinetic studies of the pyrolysis of sewage sludge by tga and comparison with fluidized beds

The pyrolysis of sewage sludge was examined by thermogravimetric analysis using different heating rates, particle sizes and final temperatures. A semi-empirical model was developed with four global consecutive/competitive reactions to volatile and solid products including also a heat balance. This model was extrapolated to isothermal reactor conditions and compared to experimental data on fluidized bed pyrolysis. Depending on the particle size and reactor temperature, about 90% of the maximum conversion in a fluidized bed takes place under external heat transfer control, the rest under kinetic control. Incomplete conversion occurs at short particle residence times, which were calculated approximately by the model.     

Polyimine Container Molecules and Nanocapsules

The field of dynamic covalent nanocapsule synthesis is very young, and most contributions to the development of reliable approaches for the assembly of dynamic covalent capsules have been made during the past five years. In 1991, Quan and Cram published the first Schiff base molecular container compound. Over the past six years, a large number of multi-component polyimine hemicarcerand and polyhedron syntheses have been developed. This review will focus primarily on recent achievements in the area of pure Schiff base nanocapsules and highlight different synthetic approaches and design strategies, as well as first applications of these capsules in molecular recognition, gas storage, and gas separation.     

Probing the pore space of geothermal reservoir sandstones by Nuclear Magnetic Resonance

Pulsed-Field-Gradient–Nuclear Magnetic Resonance (PFG–NMR) is an interesting method to determine microscopic but volumetrically averaged properties of pore space. In the present paper a number of sandstone samples, taken from drill cores of geothermal wells in North Germany, have been investigated. The time-dependent self-diffusion of water molecules in their confined geometry is used to probe the pore space. The short-time behaviour of the self-diffusion coefficient (anomalous diffusion) in the porous matrix allows the determination of the surface-to-pore volume ratio S/V_p. At long diffusion times, molecules scout the tortuosity of the interconnected pore space of the sandstones. The NMR results were compared with data from petrographic image analysis (PIA), adsorption experiments and electric conductivity measurements. The PFG–NMR measurements give surface-to-pore volume ratios S/V_p that are comparable to those estimated with the petrographic image analysis. The tortuosities match in most cases data from conductivity measurements, so the PFG–NMR is regarded as an appropriate tool to determine this quantity. The results are not influenced by the adherence of ‘scout-molecules’ to the pore walls. The surface-to-pore volume ratios and tortuosities were used to calculate permeabilities of the systems of interest, which were in good agreement with measured core-plug permeabilities. Results of additional NMR relaxation experiments are used to obtain adsorption isotherms for cations at active surface sites.     

Improved signal-to-noise ratio in EPI sequences with highly asymmetric spin echo and highly asymmetric STEAM preparations (HASE-EPI and HASTEAM-EPI)

Magnetic Resonance Materials in Physics, Biology and Medicine - Alternative versions of echo-planar imaging (EPI) sequences with standard spin echo (SE) or stimulated echo acquisition mode (STEAM)...