Preprocessing of ion mobility spectra by lognormal detailing and wavelet transform

This study has developed an efficient preprocessing strategy for ion mobility spectrometry (IMS) data allowing for improved peak clarity and comparability of different measurements. Using the discrete wavelet transform for data compression and denoising, and fitting a lognormal function to the strong tailing of the reactant ion peak (RIP), enables a data reduction to 25% or less, a significant increase of the signal-to-noise ratio, and the successful elimination of the RIP tailing. The preprocessing of breath measurements obtained by coupling an IMS to a gaschromatographic column, has resulted in the desired outcome of smooth peaks lying on a common base level. These results are transferable to other applications of one- and two-dimensional separations with IMS or instrumentations generating a similar data structure.     

Highly stereoselective De-Novo synthesis of protected 2-amino-3-C-methyl-2,3-dideoxy-d-altrose

A new strategy for the stereoselective synthesis of 2-amino-2-deoxy-aldoses is described. Therefore epoxy carbamates are reacted with isocyanates to furnish urethanes, which will form the title compounds with high diastereoselectivities under basic conditions and O,O-migration of the carbamoyl group.     

Distinction between surface hydroxyl and ether groups on boron-doped diamond electrodes using a chemical approach

While it is clearly established that oxidation of as-grown boron-doped diamond (BDD) interfaces results in the introduction of different surface oxygen functions such as ether, carbonyl and hydroxyl groups, there is no reported approach which can clearly distinguish between the different surface functions. For further surface functionalization, it is important to quantify the presence of each group on the diamond surface. In this paper, the presence and amount of surface hydroxyl groups is identified using esterification of the COH groups with trifluoroacetic acid. The presence of CF₃ group in the acid allowed the identification and estimation of the amount of surface hydroxyl groups using X-ray photoelectron spectroscopy (XPS).     

Synthesis and characterization of high surface area TiO2/SiO2 mesostructured nanocomposite

Recently titania synthesis was reported using various structuration procedures, leading to the production of solid presenting high surface area but exhibiting moderate thermal stability. The study presents the synthesis of TiO₂/SiO₂ nanocomposites, a solid that can advantageously replace bulk titania samples as catalyst support. The silica host support used for the synthesis of the nanocomposite is a SBA-15 type silica, having a well-defined 2D hexagonal pore structure and a large pore size. The control of the impregnation media is important to obtain dispersed titania crystals into the porosity, the best results have been obtained using an impregnation in an excess of solvent. After calcination at low temperature (400 °C), nanocomposites having titania nanodomains (～2–3 nm) located inside the pores and no external aggregates visible are obtained. This nanocomposite exhibits high specific surface area (close to that of the silica host support, even with a titania loading of 55 wt.%) and a narrow pore size distribution. Surprisingly, the increase in calcination temperature up to 800 °C does not allow to detect the anatase to rutile transition. Even at 800 °C, the hexagonal mesoporous structure of the silica support is maintained, and the anatase crystal domain size is evaluated at ～10 nm, a size close to that of the silica host support porosity (8.4 nm). Comparison of their physical properties with the results presented in literature for bulk samples evidenced that these TiO₂/SiO₂ solids are promising in term of thermal stability.     

Selection of suitable operating conditions to minimize the gradient equilibration time in the separation of drugs by Ultra-High-Pressure Liquid Chromatography with volatile (mass spectrometry-compatible) buffers

Reversed phase gradient elution is the method of choice for pharmaceuticals analysis since it allows reducing the analysis time while improving both the quality of the separation and the detection limits. The current trends are towards faster separations which can be achieved thanks to equipments withstanding ultra-high pressures and/or high temperatures. Under such conditions, gradient separations can be carried out within a few minutes or even a few tens of seconds. A long equilibration time in addition to the gradient time can be therefore very detrimental. In this work, we investigated the extent to which the gradient equilibration time can be reduced and which parameters mainly affect the retention variability of ionizable compounds when using volatile buffers. We first found out an excellent repeatability between run-to-run experiments whatever the equilibration time and the operating conditions. We then pointed out the key operating parameters which allow achieving reproducible runs when varying the equilibration time between runs. With a view of reducing the equilibration time, the effects of various conditions were examined. The latter include the type of additive for mobile phase pH adjustment, the initial eluent composition, the type of stationary phase, the temperature and the flow-rate. Although much remains to be understood about the equilibration process, our study allows making progress in the knowledge of this phenomenon. Based on the present results, a beneficial effect of both temperature and flow-rate was highlighted and operating conditions leading to faster column equilibration are suggested.     

Detection of multicomponent signals: effect of difference in level between components

The detection of multicomponent signals for which the components are not equidetectable is precisely investigated as a function of the level difference ΔL(i∕j) between components. The detection thresholds are determined for a seven-tone complex signal with random starting phases masked by white noise. Level differences between the components are examined. A model for non-equidetectable conditions based on the statistical summation model is described. The improvement in detection is calculated from the level difference between components that is related to the thresholds for single components. The model predictions are in accordance with the experimental results.     

Trends in aircraft noise annoyance: the role of study and sample characteristics

Recently, it has been suggested that the annoyance of residents at a given aircraft noise exposure level increases over the years. The objective of the present study was to verify the hypothesized trend and to identify its possible causes. To this end, the large database used to establish earlier exposure-response relationships on aircraft noise was updated with original data from several recent surveys, yielding a database with data from 34 separate airports. Multilevel grouped regression was used to determine the annoyance response per airport, after which meta-regression was used to investigate whether study characteristics could explain the heterogeneity in annoyance response between airports. A significant increase over the years was observed in annoyance at a given level of aircraft noise exposure. Furthermore, the type of annoyance scale, the type of contact, and the response percentage were found to be sources of heterogeneity. Of these, only the scale factor could statistically account for the trend, although other findings rule it out as a satisfactory explanation. No evidence was found for increased self-reported noise sensitivity. The results are of importance to the applicability of current exposure-annoyance relationships for aircraft noise and provide a basis for decisions on whether these need to be updated.