Gas chromatographic determination of aromatic amines in water samples after solid-phase extraction and derivatization with iodine: I. Derivatization

A new method for the selective determination of aromatic amines is presented, which is based on the solid-phase extraction at pH 9 and subsequent derivatization of the analytes to the corresponding iodobenzenes. These can selectively and sensitively be determined with gas chromatography and electron-capture detection. Separation of at least 30 compounds in a single chromatographic run in 30 min is possible. With this method, 56 aromatic amines were investigated, and only in six cases no derivatives were obtained. Limits of quantitation were between 0.5 and 8 μg l⁻¹, but may still be lowered with higher sample volumes or different injection techniques. The application to water samples revealed the suitability for the investigation of ground, leachate and wastewater.     

The numerical solution of an inverse periodic transmission problem

We consider the inverse problem of recovering a 2D periodic structure from scattered waves measured above and below the structure. We discuss convergence and implementation of an optimization method for solving the inverse TE transmission problem, following an approach first developed by Kirsch and Kress for acoustic obstacle scattering. The convergence analysis includes the case of Lipschitz grating profiles and relies on variational methods and solvability properties of periodic boundary integral equations. Numerical results for exact and noisy data demonstrate the practicability of the inversion algorithm. Copyright © 2004 John Wiley & Sons, Ltd.     

Stereoselective Ring Opening of Electronically Excited Cyclohexa-2, 4-dienones: Cause and effect

The two conformers of a cyclohexa-2, 4-dienone with different substituents at C(6) on irradiation are believed to undergo ring opening stereospecifically affording a mixture of two configurationally isomeric diene-ketenes (and descendents thereof)- Exceptions are generally found for those dienones with one C and one O substituent or even with two C substituents, if one of them carries a polar group at a site able to interact through space with the ring C?O group. In these cases, only one of the two anticipated diene-ketenes (and descendents thereof) is produced. A thorough investigation of the photochemistry of a series of structurally different cyclohexa-2, 4-dienones on analytical as well as on preparative scale extends our mechanistic knowledge of the various routes from diene-ketenes into a variety of compound classes. Novel compound classes accessible to diene-ketenes are seven-membered carbocycles (by intramolecular aldolization of the zwitterion of appropriately substituted, transiently formed diene-(N, O)-ketene acetals) and β-lactams (by Staudinger reaction).     

The analysis of synthetic organic materials—A review

Synthetic organic materials consist of polymers, low-molecular-weight additives, and fillers. The review deals with the characterization of the polymer portion in the solid state by inelastic interactions with X-rays and by mass spectrometry (MS). Field desorption MS, secondary ion MS, fast atom bombardment MS, and plasma desorption MS have been used in a molar mass range up to 50000 g/mol. Electrospray or laser desorption MS enable samples of even higher molar mass to be investigated.     

Die Quotientenräume eines linearen vollkommenen Raumes

Ohne Zusammenfassung     

Stereoisomers of perhydrophenanthrene. The synthesis and crystal structure of a derivative of the trans-syn-trans isomer

The trans-syn-trans isomer of perhydrohenanthrene has the central ring in a boat conformation. A crystalline derivative (the dibenzoate of the cis 9,10-diol) was prepared, and the crystal structure was determined. The boat conformation is slightly twisted, as predicted by molecular mechanics.