Improved methodology for the microwave digestion of carbonate-rich environmental samples

Microwave-assisted digestion permits a rapid and total dissolution of sediments and various other sample types, allowing easier and more accurate multi-element determinations. In this study, we present an optimised microwave digestion method for the complete digestion of 200 mg of carbonate-rich sediments. The optimised method prevents the formation of precipitates and assures a complete dissolution of the material. The optimised method involves treatment with concentrated hydrochloric acid (HCl) prior to microwave digestion, which prevents the formation of an insoluble calcium fluoride precipitate associated with the use of hydrofluoric acid (HF). Three different certified reference samples along with a pure calcium carbonate standard and a carbonate-rich in-house marine sediment sample were considered. Sediments were found to only be partially digested if insufficient HF was present, while a noticeable fluoride-based precipitate was found if excess HF was present. Twenty elements were analysed using sector field inductively coupled plasma mass spectrometry (ICP-MS) (Al, Ag, Ba, Ca, Cd, Co, Cr, Cu, Fe, Mg, Mn, Mo, Na, Ni, Sr, Th, Ti, U, V and Zn). A total sample digestion with average elemental recoveries above 90% was obtained by reacting carbonate-rich samples with HCl on a hotplate at 150°C for 2 h (time for the total release of generated CO₂), prior to any microwave digestion step. This extra step prevented the accumulation of gas in the sealed vessels during digestion, which would otherwise influence the carbonate chemical equilibria and make insoluble calcium available for precipitation. After this initial treatment, the improved digestion method consisted of microwave attack employing a mix of concentrated HCl, nitric acid (HNO₃) and HF (4 mL/10 mL/2 mL), followed by evaporation on a hotplate. The limits of detection (LOD) obtained using the optimised microwave protocol and ICP-MS measurements were below 0.1 µg/kg for the trace elements and below 0.2 mg/kg for major elements.     

Synthetische anthracyclinone XVI synthese hydroxylierter anthrachinone durch regioselektive Diels-Alder-reaktion

Naturally occurring quinones such as 7-methyljuglone, chrysophanol, emodin, helminthosporin, phomarin and physcion were prepared via Diels-Alder reaction and PCC-oxidation of the allylic alkohols obtained from the adducts.     

Herstellung und Umsetzungen von β-Lactamen

The cycloaddition of N-chlorosulfonyl-isocyanate with isoprene, butadiene and a polyolefin as well as the reaction of ketenes with some bis-azomethines were investigated. Suitably substituted bis-azomethines could be separated in the rac. and the meso-form. The reactivity of the azetidinones towards hydrolysis and hydrogenation was tested. Attempts to polymerise 4-vinyl-azetidin-2-one, polyazetidinone and N-substituted bis-azetidinones to give cross-linked poly-β-amides were not successful.     

Über endlich erzeugte Fittingklassen

Ohne Zusammenfassung     

Sub-Stonean spaces and corona sets

A self-contained account of the theory of sub-Stonean spaces, and their relations to Stonean spaces and Rickart spaces is given. Of particular interest are the corona sets (of the form β(X) for locally compact, σ-compact spaces, because these highly nontrivial sub-Stonean spaces lend themselves to C?ech-cohomological considerations. The theory of sub-Stonean spaces is essential for our solution of the diagonalization problem for C(X)? M_n, found in K. Grove and G. K. Pedersen, Diagonalizing matrices over C(X), submitted for publication.     

A note on the stability theory of buoyancy-driven ocean currents over a sloping bottom

In a previous paper, a new model was derived describing the baroclinic dynamics of buoyancy-driven ocean currents over a sloping bottom. In particular, a normal mode stability analysis and a general stability analysis based on an appropriately constrained energy invariant were presented. However, these two sets of stability results were not identical to each other. Here, we show that the normal-mode stability results previously described may be derived from a general stability analysis based on an appropriately constrained linear momentum invariant. In addition, we establish conditions for the nonlinear stability in the sense of Liapunov of these flows. The analysis presented here eliminates the need to introduce a Poincare inequality between the perturbation energy and the enstrophy which the previous analysis was forced to assume. Relaxing this assumption means the present analysis is applicable to a much larger range of flow geometries and is therefore a substantially stronger result.