Determination of the electrical properties of 2.5 nm thick silicon-based dielectric films: thermally grown SiOx

Ultra-thin (<5 nm thick) thermal oxide and oxynitride films with different compositions are candidates for complementary metal/oxide/semiconductor technology in ultra-large-scale integration (ULSI) applications. The latter are expected to offer the best compromise between nitrides and oxides. The aim of this work is to measure the electrical properties of a leaky 2.5 nm thick thermally grown oxide film using the high frequency capacitance–voltage (HF C(V)) measurements. The cleanliness and the surface roughness of the Si(1 0 0) surface were measured prior to in situ oxidation by means of, respectively, Auger electron spectroscopy (AES) and atomic force microscopy (AFM). The physical–chemical properties of the thermal oxide film were measured by AES (film thickness, composition), Fourier transform infrared spectroscopy (FTIR) (composition, vibration modes), cross-sectional transmission electron microscopy (TEM) (film thickness, homogeneity) and electron energy loss spectroscopy (EELS) (gap width determination). The results are compared to those obtained for the native oxide film and a chemical oxide film. The latter was first grown on the silicon substrate to prevent contamination and surface disorder after flash heating in vacuum prior to oxide growth. The substrate Si(1 0 0) surface cleaned in ultra-high vacuum (UHV) was then oxidized in a 10⁻³ mbar oxygen (O₂) gas pressure at 900°C to get the 2.5 nm thick oxide film. The grafting of a self-assembled insulating monolayer (SAM) of organic molecules on the grown oxide film permits us to obtain analysable capacitance as a function of voltage data. Indeed, this monolayer made up of octadecyltrichlorosilane molecules leads to a reduction of the leakage current through the aluminium/self-assembled monolayer/oxide/silicon heterostructure. The resulting current as a function of voltage data were compared to those of a standard 2.5 nm thick oxide film. The method proposed here to extract the electrical parameters of the thermal oxide film is demonstrated to be valid. We show mainly that the reduction of the leakage current through the aluminium/self-assembled monolayer/thermal oxide/silicon heterostructure is seven orders of magnitude bigger than in the case of the native oxide film.     

SPE and LC-MS/MS determination of 14 illicit drugs in surface waters from the Natural Park of L’Albufera (València, Spain)

A simple and robust method using solid-phase extraction (SPE) and liquid chromatography tandem mass spectrometry (LC-MS/MS) for the simultaneous determination of 14 drugs of abuse and their metabolites (cocainics, amphetamine-like compounds, cannabinoids, and opiates) in surface waters has been developed. Seven SPE adsorbents (Oasis HLB, Oasis MCX, Oasis Wax, Supelselect HLB, Strata-X, Strata-XCW), amount of sorbent bed, water volume, and pH were investigated. The highest recoveries, as well as the simplest protocol, were obtained for Oasis HLB cartridges (6 mL/200 mg) using 250 mL of water. The proposed method was linear in a concentration range from 0.03–6 to 300–60,000 ng/L depending on the compound, with correlation coefficients higher than 0.998. Matrix effects have been studied in surface water samples, and several isotope-labeled internal standards have been evaluated as a way to compensate the signal suppression observed. Limits of detection (LODs) and quantification (LOQs) ranged from 0.01 to 1.54 ng/L and from 0.03 to 5.13 ng/L, respectively. Recoveries were 71–102% at the LOQ level and 77–104 at 50 ng/L. The intra-day and intermediate precisions were from 1% to 8% and from 2% to 11%, respectively. The present work reports for the first time the occurrence of drugs of abuse residues in surface water samples from the Natural Park of L’Albufera (Valencia, Spain). Codeine, cocaine, benzoylecgonine, ecgonine methylester, amphetamine, 3,4-methylendioxy methamphetamine, morphine, and methadone were quantified with median values of 11.10, 0.02, 5.59, 0.08, 0.21, 0.75 and 0.14 ng/L respectively, and 11-nor-9-carboxy-Δ9-tetrahydrocannabinol was detected in one sample at levels <LOQ.     

Determination of multiresidue pesticides in green tea by using a modified QuEChERS extraction and ion-trap gas chromatography/mass spectrometry

The pesticide residues in exported and imported tea products must not exceed the maximum residue limits (MRLs) regulated by the import countries. Tea is a complex matrix that obfuscates the determination of pesticide residues. Many available methods for multiresidue pesticide analysis of tea are time-consuming and require many cleanup steps. The objective of this study was to develop a simple multiresidue method by using a modified quick, easy, cheap, effective, rugged, and safe (QuEChERS) extraction and ion-trap GC/MS/MS, which can identify, confirm, and quantify pesticides in complex matrixes. A tea product was homogenized with water, and the pesticides were extracted with acetonitrile containing 1% acetic acid. The extract was subjected to centrifugation, initial cleanup with dispersive SPE (dSPE), solvent exchange, and final cleanup with dSPE. Diethyl-d10-parathion and triphenyl phosphate were used as the internal standard and surrogate, respectively. The final extract was injected into an ITQ 700 gas chromatograph/mass spectrometer. Quantitation of individual pesticides was based on matrix-matched calibration curves with a correlation coefficient of > 0.9930 for the 22 pesticides selected for the study. The recoveries of the 22 pesticides ranged from 78 to 115%, except those for diazinon (130%) and malathion (122%), with an average RSD of 8.7%. The LOD values of all of the pesticides, except for terbufos, were below the MRLs set by the European Union and Japan.     

Evaluation of the performance of single‐walled carbon nanohorns in capillary electrophoresis

This paper describes for the first time the use of single‐walled carbon nanohorns (SWNHs) as pseudostationary and stationary phases for EKC and CEC, respectively, taking advantage of their characteristic features, such as conical‐end termination, formation of spherical assemblies dahlia‐flower like superstructure and easy functionalization. The use of SWNHs as pseudostationary phase for EKC required the study of their dispersion in different surfactants as well as their compatibility with the electrophoretic system. The carboxylation and subsequent immobilization of carboxylated SWNHs in fused‐silica capillary to obtain useful, reproducible and stable stationary phases for CEC has also been investigated, with promising results. The electrophoretic separations obtained for water‐soluble vitamins in both modalities (EKC and CEC) have been systematically compared with those obtained with single‐walled carbon nanotubes.     

Phase calibration of sonar systems using standard targets and dual-frequency transmission pulses

The phase angle component of the complex frequency response of a sonar system operating near transducer resonance is usually distorted. Interpretation and classification of the received sonar signal benefits from the preservation of waveform fidelity over the full bandwidth. A calibration process that measures the phase response in addition to the amplitude response is thus required. This paper describes an extension to the standard-target calibration method to include phase angle, without affecting the experimental apparatus, by using dual-frequency transmission pulses and frequency-domain data processing. This approach reduces the impact of unknown range and sound speed parameters upon phase calibration accuracy, as target phase is determined from the relationship of the two frequency components instead of relying on a local phase reference. Tungsten carbide spheres of various sizes were used to simultaneously calibrate the amplitude and phase response of an active sonar system in a laboratory tank. Experimental measurements of target phase spectra are in good agreement with values predicted from a theoretical model based upon full-wave analysis, over an operating frequency of 50-125 kHz.     

Candida rugosa lipase Lip1–polyethyleneglycol interaction and the relation with its partition in aqueous two-phase systems

The interaction between a lipase from Candida rugosa (Lip1) and polyethyleneglycols of different molecular masses was studied using fluorescence and circular dichroism approaches in order to be applied to the analysis of the enzyme partition mechanism in aqueous two-phase systems of polyethyleneglycol–potassium phosphate. The decrease of the partition coefficients with the polyethyleneglycol molecular mass showed that the enzyme partition is driven by the excluded volume effect and not by the enzyme–polymer interaction. The polymer did not affect the secondary and tertiary structure of the enzyme nor its biological activity. The lipase from Candida rugosa lyophilizate was partitioned in favour of the polyethyleneglycol rich phase; PEG 2000 being the system which showed the better enzyme recovery (78.26%) with a purification factor of 2.3. This method could be applied as a first step to isolate the enzyme from a culture medium with good recovery and without modifying the enzymatic capacity and the molecular structure.     

Reliability of calculating the cepstral peak without linear regression analysis

Measures of cepstral peak prominence, using the smoothing algorithm and linear regression analysis software developed by Hillenbrand, have been shown to be reliable predictors of dysphonia in voice samples.(1-4) Recently, the Computerized Speech Laboratory [(CSL) Kay Elemetrics, Pinebrook, New Jersey] has introduced cepstral analysis as a component of that software package. The cepstral peak, in this instance, is calculated by the voice clinician analyzing the phonatory sample by subtracting the value of the peak from the apparent baseline signal. This study compares the ability of cepstral peak values calculated from the CSL software to predict dysphonia reliably with that of the values produced by the smoothing algorithm and linear regression analysis of Hillenbrand. The results of this study show that linear regression analysis is an important step in calculating the cepstral peak prominence, thus limiting the usefulness of software programs that do not employ this step.     

Mild Vocal Fold Paresis: Understanding Clinical Presentation and Electromyographic Findings

The implications of mild vocal fold hypomobility are incompletely understood. This study describes the clinical, electromyographic, and probable etiologic findings in patients who presented with complaints of dysphonia and whose physical examination revealed vocal fold paresis as a factor possibly contributing to their voice complaints. A retrospective chart review of all patients who presented to a tertiary laryngology referral center over a 13-month period, who had a clinical diagnosis of mild vocal fold hypomobility and who underwent laryngeal electromyography, were included in the study. A total of 22 patients completed the medical evaluation of their voice complaint. Of these patients, 19 (86.4%) were found to have evidence of neuropathy on laryngeal electromyography. The clinical picture indicated the following probable origins for the vocal fold paresis: goiter/thyroiditis (7/22 or 31.8%), idiopathic (4/22 or 18.2%), viral neuritis (4/22 or 18.2%), trauma (3/22 or 13.6%), and Lyme's disease (1/22 or 4.5%). This article describes the clinical entity of mild vocal fold hypomobility and associated flexible laryngoscopic, rigid strobovideolaryngoscopic, and laryngeal electromyographic findings.