Physical properties and structure ofa-Si1−x C x : H alloy films

Summary Two sets ofa-SiC:H films were deposited by glow discharge in an Ar-SiH₄-CH₄ atmosphere to investigate the effect of a variable CH₄/SiH₄ ratio on the physical properties. The composition of the films was determined by resonant nuclear reaction and by Rutherford backscattering measurements, the optical gap and the index of refraction by transmissivity measurements in the visible-UV-NIR range, the bonding configuration by IR transmissivity measurements and the resistivity and the photo-conductivity by electrical measurements in the dark and under a 500 W/m² illumination. Results indicate that with increasing carbon content the refractive index decreases systematically over all wavelengths, the energy gap increases, the dark resistivity increases, the bonding configuration becomes dominated by carbon-containing chains and the structure more disordered.

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Riassunto Sono stati realizzati film dia-SiC:H mediante glow-discharge in atmosfera Ar-SiH₄-CH₄ con differenti rapporti CH₄/SiH₄. La concentrazione di H nei film è stata determinate usando la reazione di risonanza¹H(¹⁵N, αγ)¹²C ed il contenuto di carbonio mediante spettrometria Rutherford-backscattering. Da misure di trasmittanza e riflettanza nella zona UV-visibile-vicino IR sono state ricavate le costanti ottiche, l'indice di rifrazione, la costante dielettrica, il coefficiente di assorbimento e il gap ottico. Un esame delle bande degli spettri vibrazionali dei vari legami CH, CSi e SiH ottenuti mediante misure di trasmissione nell'IR ha fornito un'interpretazione sulla struttura dei film. Sono state anche realizzate misure di conduttività di buio e di fotoconduttività sotto illuminamento di 500 W/m². I risultati indicano che all'aumentare del contenuto di carbonio l'indice di rifrazione diminuisce sistematicamente per tutte le lunghezze d'onda, il gap ottico aumenta, la conduttività di buio diminuisce e nella configurazione strutturale tendono a prevalere le catene contenenti il carbonio.

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Резюме Ъыли осаждены две системы пленокa-SiC:H в атмосфере Ar-SiH₄-CH₄, чтобы исследовать переменного отношения CH₄/SiH₄ на физические свойства. Состав пленок определяется с помощью резонансных ядерных реакций и измерений обратного резерфордовского рассеяния. Также определяются оптичззкся щеяь и показатель преломления с помщяю иемерений пронисаемости в видимойультрафиолетовой-близкой инфракрасной области, конфигурацуя связи с помощью измерений инфракрасной проницаемости и удельное сопротивление и фотопроводимость с помошью єлектрических измерений в темноте м при освешении 500 Bt/M². Полученные результаты покасывают, что с увеличением содержания углерода показатель преомления систематически уменьшается для всех длин волн, єнергетическая щель увеличивается, темновое сопротивление увеличивается, конфигурация связи становится доминирующей за счет углерод-содержащих цепочек и структура становится более разориентировнной.

     

Saturation of the Shepard operators

We discuss the Shepard operators S_n (f; x) in this paper and establish the saturation of the sequence {S_n f} _n-1 ^∞ , as well as investigate some related questions. The research of this author was supported in part by the Hungarian Science Foundation for Research, Grant. N ^o . 1157.     

Liquid chromatography coupled to quadruple time‐of‐flight tandem mass spectrometry for microcystin analysis in freshwaters: method performances and characterisation of a novel variant of microcystin‐RR

Cyanobacteria, also called blue‐green algae, occur worldwide within water blooms in eutrophic lakes and drinking water reservoirs, producing several biotoxins (cyanotoxins). Among these, microcystins (MCs) are a group of cyclic heptapeptides showing potent hepatotoxicity and activity as tumour promoters. So far, at least 89 MCs from different cyanobacteria genera have been characterised. Herein, ion trap, matrix‐assisted laser desorption/ionisation time‐of‐flight (MALDI‐ToF) and quadruple time‐of‐flight (Q‐ToF) mass spectrometry (MS)‐based methods were tested and compared for analysing MCs in freshwaters. Method performances in terms of limit of detection, limit of quantification, mean recoveries, repeatability, and specificity were evaluated. In particular, a liquid chromatography/electrospray ionisation (LC/ESI)‐Q‐ToF‐MS/MS method was firstly described to analyse MCs in freshwaters; this technique is highly selective and sensitive, and allowed us to characterise the molecular structure of an unknown compound. Indeed, the full structural characterisation of a novel microcystin variant from a bloom of Planktothrix rubescens in the Lake Averno, near Naples, was attained by the study of the fragmentation pattern. The new cyanotoxin was identified as the 9‐acetyl‐Adda variant of microcystin‐RR. Copyright © 2009 John Wiley & Sons, Ltd.     

New insights into the seleniranium ion promoted cyclization of prenyl and propenylbenzene aryl ethers

The chromane core is widely represented in nature being part of a wide array of secondary metabolites of plant, fungal, and bacterial origin. In this paper an improved method for the chemical synthesis of differently substituted chromanes is described. Substituted 2H-1-benzopyrans have been synthesized in good to excellent yields (52–81%) by treatment of 3,3-dimethylallyl and propenylbenzene ethers of differently substituted phenols with phenylselenyl chloride.     

A new controlled release system of chlorhexidine and chlorhexidine:βcd inclusion compounds based on porous silica

The purpose of this study was to prepare and characterize a controlled release system based on porous silica loaded with chlorhexidine (Cx) and its inclusion compounds in β-cyclodextrin (βcd), and to evaluate its antimicrobial activity. Acetate chlorhexidine (CxA), gluconate chlorhexidine (CxG), βcd:chlorhexidine acetate 2:1 (βcd:CxA) and βcd:chlorhexidine gluconate 2:1 (βcd:CxG) were incorporated into porous silica. Drug loading was characterized by FTIR, powder X-ray diffraction, thermal analysis and BET, and was shown to be in an amorphous state and porous matrix. The kinetics release parameter of the drug was established, which showed that the Cx systems release profile followed zero order release until 400 h and Higuchi model release until 750 h, after the burst effect at the first 8 h. Chlorhexidine therapeutic range was reached near first hour for all systems. The chlorhexidine porous silica system was biologically active against Enterococcus faecalis and Candida albicans in vitro. The systems showed an efficient Cx controlled release modulated by the presence of the β-cyclodextrin and by the porous silica matrices, providing effective antimicrobial activity.     

Microemulsion electrokinetic chromatography: an application for the simultaneous determination of suspected fragrance allergens in rinse-off products

The feasibility of microwave-accelerated derivatization for capillary electrophoresis (CE) with laser-induced fluorescence (LIF) detection was evaluated. The derivatization reaction was performed in a domestic microwave oven. Histidine (His), 1-methylhistidine (1-MH) and 3-methylhistidine (3-MH) were selected as test analytes and fluorescein isothiocyanate (FITC) was chosen as a fluorescent derivatizing reagent. Parameters that may affect the derivatization reaction and/or subsequent CE separation were systematically investigated. Under optimized conditions, the microwave-accelerated derivatization reaction was successfully completed within 150 s, compared to 4-24 h in a conventional water-bath derivatization process. This will remarkably reduce the overall analysis time and increase sample throughput of CE-LIF. The detection limits of this method were found to be 0.023 ng/mL for His, 0.023 ng/mL for 1-MH, and 0.034 ng/mL for 3-MH, respectively, comparable to those obtained using traditional derivatization protocols. The proposed method was characterized in terms of precision, linearity, accuracy and successfully applied for rapid and sensitive determination of these analytes in human urine.     

Control of degradation of polypropylene during its radical functionalisation with furan and thiophene derivatives

The traditional melt radical functionalisation of isotactic polypropylene (iPP) with maleic anhydride (MAH) and peroxide affords functionalized samples with a severe decrease of the average molecular weight (MW) due to the β-scission reaction. In this work new push-pull unsaturated molecules were investigated, consisting of a heterocyclic ring conjugated with a double bond bearing an electron attracting group. These molecules were specifically designed as MAH substitute able to limit the iPP degradation, while providing functionalisation through grafting. Butyl 3-(2-furanyl) propenoate (BFA) and butyl 3-(2-thienyl) propenoate (BTA) were comparatively tested. The analysis of the reaction products indicated that both molecules are able to graft onto the iPP backbone by prompt reaction with the macro-radicals formed through H-abstraction from iPP chains, thereby significantly limiting the MW decrease, as the functionalized macro-radicals are stabilized by resonance. Nonetheless, some of iPP macro-radicals can give a parallel chain scission before reacting with the new molecules. In the case of BFA, coupling reactions of the formed macro-radicals can lead to the formation of branched high MW architectures, whereas in the case of the thiophene derivative (BTA) only a partial retaining of polymer chain fragmentation was observed due to the reduction of β-scission.