Catalytic destruction of brominated aromatic compounds studied in a catalyst microbed coupled to gas chromatography/mass spectrometry

The capability of solid porous catalysts has been studied for the destruction or modification of halogenated aromatic compounds contaminating the pyrolysis oil of recycled plastics from electronic waste. A fast and simple experimental procedure is carried out using a micropyrolyser coupled to GC-MS in such a way that catalyst microbed was placed in the sample tube of the pyrolyser. The pyrolysis products of polycarbonate blended with a frequently applied flame retardant tetrabromobisphenol A (TBBPA) and epoxy resin containing TBBPA monomer units have been analysed, and the brominated components were compared with the thermal decomposition products of TBBPA and its diallyl ether. When TBBPA vapour passes through molecular sieve 4A a slight debromination and a partial cleavage of bisphenol A into phenols occur. Over molecular sieves of larger pore size (13X and NaY zeolite) an important decrease of TBBPA amount is observed indicating effective trapping ability of these catalysts of basic character for brominated aromatic compounds. A total chemical modification of the vapour was achieved by Al-MCM-41 catalyst that split TBBPA into bromophenols. Analogous results were obtained by carrying out similar experiments on diallyl ether of TBBPA. Moreover, it was revealed that brominated bisphenol A compounds are modified essentially the same way, either evaporated or evolved from a polycarbonate blend or produced by pyrolysis from an epoxy resin.     

A new approach for development of rugged sample preparation of metabolites of albendazole in cow milk

Sample preparation is the critical step in analysis of residues in biological samples. The development of a ragged method is time-consuming, because a huge number of parameters must be checked. To reduce the number of experiments Taguchi's method was applied in the sample preparation of metabolites of albendazole. During the experiments 11 controllable and 7 noise factors were investigated. From the influence of controllable and noise factors on recovery and standard deviation, conditions for the sample preparation and recovery could be concluded with high accuracy and reliability.     

Trace level triacetone-triperoxide identification with SPME–GC-MS in model systems

Triacetone-triperoxide is a high explosive mainly used by terrorist groups. With the spreading of the recipe on the Internet, increasing number of bomb attacks are being reported worldwide using triacetone-triperoxide. A simple identification method is described using 100 μm polydimethyl siloxane fibre solid phase microextraction and gas chromatography combined with spectrometry. The method was tested on various pre- and post-explosion models that can be collected in a house search or after a bomb attack. Sample preservation and stability was also examined. Identification of triacetone-triperoxide residues in post-explosion models was feasible 24 h after ignition, the detection limit being 5 ng.     

Simulations of petawatt-class few-cycle optical-parametric chirped-pulse amplification, including nonlinear refractive index effects

We present three-dimensional simulations of optical-parametric chirped-pulse amplification stages for a few-cycle petawatt-class laser. The simulations take into account the effects of depletion, diffraction, walk-off, quantum noise, and the nonlinear refractive index (n(2)). In the absence of n(2) effects, we show these stages can generate 3.67J pulses supporting 4fs transform-limited pulse durations. Adding the nonlinear refractive index to the simulation, the energy output is reduced by ~11% and the bandwidth narrows by ~129nm, increasing the Fourier limit by ~17.5%.     

New facile tandem route to oxo- and thioxo[1,2,4]triazolo[1,5-a]pyridinium salts

2-Arylsulfanyl- and benzylsulfanylpyridinium N-arylimides (2), easily available from tetrazolo[1,5-b]pyridinium salts (1), participate in 1,3-dipolar cycloaddition with aryl isothiocyanates and aryl isocyanates to result in formation of fused thioxo- and oxo[1,2,4]triazolium salts (5 and 12), respectively. This transformation is interpreted as a regular 1,3-cycloaddition followed by spontaneous elimination of the aryl- or benzylsulfanyl group. Formation of these triazolium salts can be followed--under appropriate reaction conditions--by ring-opening reactions to afford some new triazolyldienes (6). Recognition of the intermediate participation of the thiolate anion along the pathway 1 --> 5 allowed elaboration of a simple procedure to 5 implying a tandem reaction sequence.