Determination of mercury in sludge and materials used for HG-eliminations from industrial waste waters by zeeman atomic absorption spectrometry after matrix modification with potassium bromide and bromine

Summary Mercury was determined by Zeeman Atomic Absorption Spectrometry after matrix modification of urine and waste water by addition of 0.1M HNO₃, 0.05M KBr, and 5l Br₂/ml, and after its extraction from sludge, iron sludge and ion exchanger by a mixture containing the same additives. The same samples were also analysed by the cold vapour method after wet oxidation of the samples in closed teflon bombs. The ratio of the corresponding concentrations was 1.21±0.39 (SD) and the concentration range covered 0.1–50000 mg Hg/kg. The analytical powers of both procedures are compared.

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Bestimmung von Quecksilber in Schlamm und in für die Reinigung industrieller Abwässer verwendeten Materialien mit der Zeeman-Atomab-sorptions-Spektrometrie nach Matrixmodifizierung durch Kaliumbromid und Brom

Zusammenfassung Quecksilber wurde mit der Zeeman-Atomabsorptions-Spektroskopie in Urin und Abwässern nach einer Matrixmodifizierung durch Zugabe von 0,1M HNO₃, 0,05M KBr und 5 l Br₂/ml sowie nach seiner Extraktion aus Schlamm, Eisenschlamm und Ionenaustauschern mit einer Mischung der gleichen Zusatzstoffe bestimmt. Die gleichen Proben wurden auch nach der Kalt-Dampf-Methode nach dem Naßaufschluß in geschlossenen Teflonbomben analysiert. Das Verhältnis der betreffenden Konzentrationen betrug 1,21±0,39 (Standardabweichung), wobei der Konzentrationsbereich 0,1–50000 mg Hg/kg umfaßte. Die analytischen Leistungsfähigkeiten der beiden Verfahren wurden verglichen.

     

Synthesis of Novel <Emphasis Type="Italic">D</Emphasis>-<Emphasis Type="Italic">Seco</Emphasis>-Pregnenes

Summary. A new synthetic route was developed for the preparation of trans-3-hydroxy-16,17-seco-pregna-5,17(20)-dien-16-al, using Grob fragmentation as the key step. This seco-steroid contains a formyl group and an unsaturated side-chain in a sterically favourable position, and is therefore a promising starting material for the synthesis of novel condensed steroid heterocycles.Received March 22, 2003; accepted April 22, 2003 Published online September 25, 2003     

Determination of drug-cyclodextrin binding constants by capillary zone electrophoresis

Binding constants of the optical isomers of Deprenyl® (selegiline) and its potential metabolites with (2,6-di-O-methyl)--cyclodextrin were determined using electrophoretic mobility data gained from separations performed by capillary electrophoresis, and absorbancies obtained from spectrophotometric experiments. To calculate equilibrium constants l: l complex formation have been assumed. The comparison of the equilibrium constants calculated from different methods shows similar values in their order of magnitude. Their difference may probably be explained by the different media of the measurements. The effect of the structure of compounds on chiral discrimination were also elucidated.     

Why not ICP as atom reservoir for AAS?

The sensitivity S_A of determination by inductively coupled plasma atomic absorption spectrometry (ICP—AAS) is discussed. All important factors influencing S_A are comprised in one single sensitivity formula, which allows an estimate to be made of the correct order of magnitude of S_A for both flame—AAS and ICP—AAS measurements. The most important analytical factors are the degree of dissociation and ionization (0≤f_C, and f_I≤1), the dilution factor f_D, which takes into account the dilution of the analysis element A by its transition from the solution to the ICP, and the absorption path length b. Like flame—AAS, an analytical approach using ICP—AAS has high selectivity and makes it possible to carry out determinations without chemical and ionization interferences. This important advantage of ICP—AAS in comparison to flame—AAS is based on the fact that the ideal condition f_C→1 and Δf→0 for the analysis and standard solutions can be much more easily realized in the ICP than in flames. Serious disadvantages of an ICP as an atomic reservoir for AAS are the reduced sensitivity and lower detection power compared to flame—AAS. The reduction of S_A is caused mainly by the reduction of b/f_D by a factor of about 0.1 and to a smaller degree by stronger broadening of the absorption line and the depopulation of the lower energy state of the atom A that absorbs the resonance radiation. The estimated S_A value for A = Ag, Al, Ca, Cd, Co, Cr, Cu, Pd and Pt agree with the corresponding experimental values to within a factor of about 3. No experimental values could be obtained for B and Si. An application field of ICP—AAS is the analysis of complex compounds that are difficult to dissociate into atoms using flames. In these determinations, a high sensitivity is generally not needed but a good selectivity is important. Some applications are shown.     

Noncovalent cross-links in context with other structural and functional elements of proteins

Proteins are heteropolymers with evolutionary selected native sequences of residues. These native sequences code for unique and stable 3D structures indispensable for biochemical activity and for proteolysis resistance, the latter which guarantees an appropriate lifetime for the protein in the protease rich cellular environment. Cross-links between residues close in space but far in the primary structure are required to maintain the folded structure of proteins. Some of these cross-links are covalent, most frequently disulfide bonds, but the majority of the cross-links are sets of cooperative noncovalent long-range interactions. In this paper we focus on special clusters of noncovalent long-range interactions: the Stabilization Centers (SCs). The relation between the SCs and secondary structural elements as well as the relation between SCs and functionally important regions of proteins are presented to show a detailed picture of these clusters, which are believed to be primarily responsible for major aspects of protein stability.