Some problems concerning the use of automated radiochemical separation systems in destructive neutron activation analysis

The present state of a long term program is reviewed. It was started to elaborate a remote controlled automated radiochemical processing system for the neutron activation analysis of biological materials. The system is based on wet ashing of the sample, followed by reactive desorption of some volatile components. The distillation residue is passed through a series of columns filled with selective ion screening materials to remove the matrix activity. The solution is thus “stripped” from the interfering radioions, and it is processed to single-elements through group separations using ion-exchange chromatographic techniques. Some special problems concerning this system are treated. (a) General aspects of the construction of a (semi)automated radiochemical processing system are discussed; (b) Comparison is made between various technical realizations of the same basic concept; (c) Some problems concerning the “reconstruction” of an already published processing system are outlined.     

Concentration and clean-up of trace hydrocarbons from atmospheric particulate matter

Summary The aim of this work is to establish the best conditions for concentration and purification steps in the trace analysis of aliphatic and polycyclic aromatic hydrocarbons (PAH) from atmospheric particulate matter by gas chromatography-flame ionisation detection (GC-FID) and high performance liquid chromatography with ultraviolet and fluorescence detection (HPLC-UV-FL). The best results for the more volatile compound were obtained with a combination of rotary evaporation and a stream of nitrogen (near to 100% for aliphatic hydrocarbons and from 70 to 105% for PAH). Two types of solid phase extraction (SPE)cartridges (Supelclean ^tm LC-Silica SPE tubes and Sep-Pak^? Plus silica cartridges) and glass column were examined for the purification and fractionation step. Blank chromatograms of both types of cartridges analysed by GC-FID made this study difficult, because a PSS (programmed split-splitless) injector was employed thereby increasing the sensitivity. This problem was not observed in the HPLC-UV-FL blank chromatograms of these cartridges. Glass columns filled with silica and alumina were chosen because no interference was found in the GC-FID blank chromatograms and the best recoveries in the fractionation of both aliphatic hydrocarbons and PAH were achieved. This is especially important when aliphatic hydrocarbons concentrations are lower than 1 μg mL⁻¹. Finally, the selected conditions were applied to the analysis of hydrocarbons in real atmospheric particulate samples.     

Self-assembled peptide tubelets with 7 A pores

Here we report the preparation and structural characteristics of self-assembling peptide tubelets composed of 32-membered rings formed of alternating alpha-amino acids and cis-3-aminocyclohexanecarboxylic acids. The tubelets possess a partial hydrophobic core environment, provided by the projection of the cyclohexane C2 methylene moiety into the lumen, and a Van der Waals pore diameter of about 7 A.     

Temperature Development of Homo- and Hetero-Clustering in Saturated Vapors

Computational findings of temperature increase of clustering degree in saturated vapors are analyzed. A thermodynamic proof is presented and a simple criterion derived. Illustrations are based on saturated steam, magnesium and carbon vapor. The results are applicable to synthesis of fullerenes, metallofullerenes, and heterofullerenes, chemical vapor deposition technique, or atmospheric chemistry.     

Semicarbazones and thiosemicarbazones,XII: Crystal structure of salicylaldehyde semicarbazone

Summary The crystal and molecular structure of salicylaldehyde semicarbazone was obtained by single crystal X-ray diffraction. The O atom of the semicarbazone fragment isanti to the N atom of the hydrazinic group. The distribution of bond lengths in the semicarbazone fragment indicates delocalization of the -electrons. The crystal structure is stabilized by intra- and intermolecular hydrogen bonds.

---

Semicarbazone und Thiosemicarbazone, 12. Mitt.: Die Kristallstruktur des Salicylaldehyd-Semicarbazons

Zusammenfassung Die Kristallstruktur und die molekulare Struktur des Salicylaldehyd-Semicarbazons wurde über Einkristall-Röntgenstreuung ermittelt. Das O-Atom des Semicarbazonteils stehtanti zum N-Atom der Hydrazin-Gruppierung. Die Bindungslängen in der Semicarbazoneinheit zeigen eine Delokalisierung der -Elektronen an. Die Geometrie der Verbindung wird durch stabilisierende intra- und intermolekulare Wasserstoffbrückenbindungen bestimmt.

     

Structural study of copper-nickel aluminate (CuxNi1−xAl2O4) spinels

CuAl₂O₄, NiAl₂O₄, and three ternary spinels Cu_xNi_1?xAl₂O₃ have been prepared, in polycrystalline form, by solid-state reaction of mixtures of CuO, NiO, and Al₂O₃ at 1223 K. X-Ray powder diffractometry, coupled with adequate computational methods, allowed determination of the unit-cell length, oxygen positional parameter, and cation distribution for each compound. Interdependence of these structural parameters is closely analyzed on the ternary oxide spinels. The one-electron difference between the Cu²⁺ and Ni²⁺ ions was found to be enough to render them distinguishable by X-ray powder diffraction.     

Emanation Thermal Analysis of SiC Based Materials

Results of emanation thermal analysis (ETA) characterizing microstructure changes of SiC based materials during heat treatment in argon are demonstrated. This method made it possible to reveal fine changes of the texture of SiC nano-sized powders, SiC micro-sized powders and SiC whiskers under in situconditions of the heating. ETA curves can serve as fingerprints of the respective samples.This revised version was published online in November 2005 with corrections to the Cover Date.     

X-ray investigation of the role of the mixed emulsifier in the structure formation in o/w creams

The aim of this research work was to clarify the role of the mixed emulsifier in the structure formation and water binding mode in the case of o/w creams prepared with different surfactants. The swelling behavior of mixed emulsifiers was examined by means of direct investigation methods such as transmission electron microscopy (TEM) and X-ray diffraction. The detailed structure image of the creams was created with the help of the latter. The influence of the structure of the hydrophilic gel phase, and the structural changes during storage were studied with rheological methods. On the basis of the results, it can be stated that the investigated creams had different structures from those mentioned in the literature: surfactant did not create a mixed bilayer with the structure to furnish fatty amphiphile; instead, micelles were formed. These results correlated well with the results of the rheological tests.