A review is given dealing with commonly used adsorbent materials in ambient air analysis of volatile organic compounds (VOCs). The adsorbents covered in the paper are selected in consideration of their compatibility with thermal desorption. Initially, we discuss the requirements that an adsorbent should fulfill, and useful parameters for the selection and evaluation of an appropriate material. Then, the most important materials are presented considering their properties, advantages, and drawbacks. A few applications are given, but a complete review of sampling techniques and applications dealing with adsorptive enrichment and thermal desorption is beyond the scope of this paper.

Systematic investigations were performed to study the dependence of the extraction efficiency of persistent organic pollutants (POPs), including chlorobenzenes, HCH isomers, DDX, PCB congeners, and PAHs, on the accelerated solvent extraction (ASE) operating variables solvent and temperature. Mixed soil samples from two locations with considerable differences in soil properties and contamination in the Leipzig-Halle region (Germany) were used. The objective was to optimize ASE for the extraction of POPs from real soil samples and to improve on the results achieved with Soxhlet extraction (SOX). Solvents with differing polarities were tested. Quadruple and triple determinations were performed on the two soils, respectively, between 20 and 180 degrees C in 20 degrees C steps. All the results were compared with those obtained by SOX, as well as, in some cases during preliminary studies, by ultrasonic extraction (USE). In ASE, the optimum conditions proved to be two extraction steps at 80 and 140 degrees C (average RSD 10.7%) with three static cycles (extraction time 35 min) using toluene as solvent and at a pressure of 15 MPa. Owing to the superior analyte/matrix separation by ASE, in many cases for real soil samples analytical values better by up to 1 order of magnitude or even more were obtained compared to SOX results.

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In order to develop a liquid chromatography/electrospray ionisation tandem mass spectrometry (LC/ESI-MS/MS) method for identification and quantification of polar metabolites of explosives using a triple quadrupole system, the mass spectrometric ionisation and fragmentation behaviour of different nitrophenols, nitro- and aminonitrobenzoic acids, nitrotoluenesulfonic acids, and aminonitrotoluenes was investigated. Due to their different molecular structures, the substances concerned showed a very different ionisation efficiency in the ESI process. Interestingly, 2,4-dinitrobenzoic acid yielded no mass signals in the Q1 scan suggesting a thermal decarboxylation in the ion source, whereas the corresponding 3,5-isomer showed a high ionisation yield. Using negative ionisation polarity, carboxylic, phenolic, and sulfonic acid groups were deprotonated resulting in molecular anions, which could be fragmented in a collision cell. A pronounced dependency of the produced fragment ion series on the kind and position of substituents at the nitrobenzene ring (ortho effects) was observed and exploited for the development of substance-specific detection methods in the multiple reaction monitoring mode. In case of benzoic and sulfonic acids, decarboxylation and desulfonation, respectively, were observed as the most frequent fragmentation reactions. Furthermore, besides loss of NO(2), NO fragmentation occurred and preceded a decarbonylation of the benzene ring. The expulsion of the open-shell molecules NO and NO(2) led to a variety of distonic radical anions.