Over 30 years, portable systems for fast and reliable gas analysis are at the core of both academic and industrial research. Miniaturized systems can be helpful in several domains. The way to make it possible is to miniaturize the whole gas chromatograph. Micro-system conception by etching silicon channel is well known. The main objective is to obtain similar or superior efficiencies to those obtained from laboratory chromatographs. However, stationary phase coatings on silicon surface and micro-detector conception with a low limit of detection remain a challenge. Developments are still in progress to offer a large range of stationary phases and detectors to meet the needs of analytical scientists. This review covers the recent development of micro-gas analyzers. It focuses on injectors, stationary phases, column designs and detectors reported in the literature during the last three decades. A list of commercially available micro-systems and their performances will also be presented.
A partial chiral discrimination of racemic p-halogenated derivatives of phenylethanol is observed during the crystallization in water of host-guest supramolecular compounds with permethylated b-cyclodextrin. Enantioenrichment with this chiral host is however highly sensitive to crystallization durations and to the chemical nature of the halogenated substituent of the guest. Structural determinations performed for the complexes formed with (R) and (S) p-bromo-phenylethanol indicate that stereodifferenciation for this guest is associated to distinct inclusion features. The understanding of the underlying chiral recognition mechanisms, the careful design of suitable crystallization conditions, and the use of a procedure involving successive crystallizations allows to envisage a complete resolution of racemic mixtures by means of supramolecular complexations.
The static headspace technique is the most common approach to residual solvent analysis in pharmaceutical and environmental matrices. This paper presents an alternative tool where the volatile impurities are released from the matrix by working directly on a small amount of sample at a high equilibration temperature: the so-called Full Evaporation Technique (FET). The capability of this method was evaluated on a mixture of nine solvents, which belong to Class 3 in the classification of the European Pharmacopoeia Agency for residual solvents, at various levels of concentration: ethanol, acetone, 2-propanol, methyl acetate, 2-butanone, ethyl acetate, tetrahydrofuran, 2-methyl-1-propanol, 1-butanol. Data on linearity, accuracy, precision and sensitivity are reported. Use of an internal standard proved to be necessary when using such a method. The method is then successfully applied to the analysis of solvent traces in permethylated beta-cyclodextrin.
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