Development and validation of a magnetic solid‐phase extraction with high‐performance liquid chromatography method for the simultaneous determination of amphetamine and methadone in urine

The simultaneous determination of amphetamine and methadone was carried out by magnetic graphene oxide nanoparticles, a magnetic solid‐phase extraction adsorbent, as a new sample treatment technique. The main factors (the amounts of sample volume, amount of adsorbent, type and amount of extraction organic solvent, time of extraction and desorption, pH, the ionic strength of extraction medium, and agitation rate) influencing the extraction efficiency were investigated and optimized. Under the optimized conditions, good linearity was observed in the range of 100–1500 ng/mL for amphetamine and 100–1000 ng/mL for methadone. The method was evaluated for determination of AM and methadone in positive urine samples, satisfactory results were obtained, therefore magnetic solid‐phase extraction can be applied as a novel method for the determination of drugs of abuse in forensic laboratories.     

Piston scuffing fault and its identification in an IC engine by vibration analysis

In this paper, the effects of piston scuffing fault on engine performance and vibrations are investigated. A procedure based on vibration analysis is also presented to identify piston scuffing fault. To this end, an internal combustion (IC) engine ran under a specific test procedure. The engine parameters and vibration signals were measured during the experiments. To produce piston scuffing fault, three-body abrasive wear mechanism was employed. The experimental results showed that piston scuffing fault caused the engine performance to reduce significantly. The vibration signals were analyzed in time-domain, frequency-domain and time–frequency domain. Continuous wavelet transform (CWT) was used to obtain time–frequency representations. “dmey” wavelet was selected as the optimum wavelet type for this research among different wavelet types using the three criteria of energy, Shannon entropy and energy to Shannon entropy ratio. The results of CWT analysis by “dmey” wavelet showed that piston scuffing fault excited the frequency band of 2.4–4.7 kHz in which the frequency of 3.7 kHz was affected more. Finally, seven different features were extracted from the engine vibration signals related to the frequency band of 2.4–4.7 kHz. The results indicated that maximum, mean, RMS, skewness, kurtosis and impulse factor of the engine vibration related to the found frequency band increased significantly due to piston scuffing fault. The obtained results showed that the proposed method identified piston scuffing fault and discovered the vibration characteristics of this fault like frequency band. The results also demonstrated the possibility of using engine vibrations in piston scuffing fault identification.     

Fast Quantitation of Target Analytes in Small Volumes of Complex Samples by Matrix‐Compatible Solid‐Phase Microextraction Devices

Herein we report the development of solid‐phase microextraction (SPME) devices designed to perform fast extraction/enrichment of target analytes present in small volumes of complex matrices (i.e. V≤10 μL). Micro‐sampling was performed with the use of etched metal tips coated with a thin layer of biocompatible nano‐structured polypyrrole (PPy), or by using coated blade spray (CBS) devices. These devices can be coupled either to liquid chromatography (LC), or directly to mass spectrometry (MS) via dedicated interfaces. The reported results demonstrated that the whole analytical procedure can be carried out within a few minutes with high sensitivity and quantitation precision, and can be used to sample from various biological matrices such as blood, urine, or Allium cepa L single‐cells.     

A multi‐MHz single‐shot data acquisition scheme with high dynamic range: pump–probe X‐ray experiments at synchrotrons

The technical implementation of a multi‐MHz data acquisition scheme for laser–X‐ray pump–probe experiments with pulse limited temporal resolution (100 ps) is presented. Such techniques are very attractive to benefit from the high‐repetition rates of X‐ray pulses delivered from advanced synchrotron radiation sources. Exploiting a synchronized 3.9 MHz laser excitation source, experiments in 60‐bunch mode (7.8 MHz) at beamline P01 of the PETRA III storage ring are performed. Hereby molecular systems in liquid solutions are excited by the pulsed laser source and the total X‐ray fluorescence yield (TFY) from the sample is recorded using silicon avalanche photodiode detectors (APDs). The subsequent digitizer card samples the APD signal traces in 0.5 ns steps with 12‐bit resolution. These traces are then processed to deliver an integrated value for each recorded single X‐ray pulse intensity and sorted into bins according to whether the laser excited the sample or not. For each subgroup the recorded single‐shot values are averaged over ～10⁷ pulses to deliver a mean TFY value with its standard error for each data point, e.g. at a given X‐ray probe energy. The sensitivity reaches down to the shot‐noise limit, and signal‐to‐noise ratios approaching 1000 are achievable in only a few seconds collection time per data point. The dynamic range covers 100 photons pulse^?1 and is only technically limited by the utilized APD.     

Assessing silicon deposits in Zilfi province,Saudi Arabia,using XRF and XRD techniques

The aim of this project is to create a geochemical database of the Nafud Desert in Zilfi Province, which lies 260 km northwest of Riyadh, capital of Saudi Arabia, and assess its potential as a silicon mine. The area of study was surveyed during December 2012 collecting 21 geological samples from 7 places (Alsabla, Almatal, Shlwan, Alaaga, Jaway, Magra and Althuare). Elemental composition was determined using X‐ray fluorescence spectrometry, while mineral content and crystallography analysis was performed using X‐ray diffraction. Analysis results revealed that silicon was abundant in the area, in fairly homogeneous amounts. Silica was found in concentrations of around 93% per sampled mass, and silicon concentrations were around 42%, in the surface layers down to the depth of 40 cm. Other elements (Al, K, Ca, Ti, Cr, Mn, Fe, Sr, Zr and Pd ) were present in very low concentrations, except for aluminium oxide, which was present in three areas (Jaway, Magra and Althuare) at concentrations around 5%, while Alsabla samples showed higher concentrations of CaO. Thus, according to the results, the Nafud Desert is a rich source of silicon that can be exploited very cheaply because of the presence of the raw material on the surface. Copyright © 2016 John Wiley & Sons, Ltd.     

Metal- and Catalyst-Free Synthesis of 2-Substituted-Phthalimides Using 2-(Arenesulfonyl)Phthalimide as Key Reagents

Phthalimide derivatives are important in medicinal chemistry, several phthalimidation methodologies have been developed. Here, we report a facile, metal-free, and catalyst-free method for the preparation of N-phthalimides in good to excellent yield by reacting 2-(arenesulfonyl)phthalimides with various amine substrates.     

A Targeted Review of Current Progress,Challenges and Future Perspective of g-C3N4 based Hybrid Photocatalyst Toward Multidimensional Applications

The increasing demand for searching highly efficient and robust technologies in the context of sustainable energy production totally rely onto the cost-effective energy efficient production technologies. Solar power technology in this regard will perceived to be extensively employed in a variety of ways in the future ahead, in terms of the combustion of petroleum-based pollutants, CO₂ reduction, heterogeneous photocatalysis, as well as the formation of unlimited and sustainable hydrogen gas production. Semiconductor-based photocatalysis is regarded as potentially sustainable solution in this context. g-C₃N₄ is classified as non-metallic semiconductor to overcome this energy demand and enviromental challenges, because of its superior electronic configuration, which has a median band energy of around 2.7 eV, strong photocatalytic stability, and higher light performance. The photocatalytic performance of g-C₃N₄ is perceived to be inadequate, owing to its small surface area along with high rate of charge recombination. However, various synthetic strategies were applied in order to incorporate g-C₃N₄ with different guest materials to increase photocatalytic performance. After these fabrication approaches, the photocatalytic activity was enhanced owing to generation of photoinduced electrons and holes, by improving light absorption ability, and boosting surface area, which provides more space for photocatalytic reaction. In this review, various metals, non-metals, metals oxide, sulfides, and ferrites have been integrated with g-C₃N₄ to form mono, bimetallic, heterojunction, Z-scheme, and S-scheme-based materials for boosting performance. Also, different varieties of g-C₃N₄ were utilized for different aspects of photocatalytic application i. e., water reduction, water oxidation, CO₂ reduction, and photodegradation of dye pollutants, etc. As a consequence, we have assembled a summary of the latest g-C₃N₄ based materials, their uses in solar energy adaption, and proper management of the environment. This research will further well explain the detail of the mechanism of all these photocatalytic processes for the next steps, as well as the age number of new insights in order to overcome the current challenges.     

Polycarbonate-coated magnetic nanoparticles for the extraction of imipramine and its primary metabolite from urine

This study introduces a reliable and inexpensive magnetic dispersive solid phase extraction to extract imipramine and its primary metabolite (desipramine) from urine samples. To accomplish this aim, Fe₃O₄ magnetic nanoparticles were synthesized by sonication, subsequently, polycarbonate was precipitated gradually onto the surface of them to form the adsorbent. Extraction recoveries of 85% and 76%, enrichment factors of 57 and 51, limits of detection of 2.5 and 2.8 μg/L, and limits of quantification of 8.3 and 9.3 μg/L were obtained for imipramine and desipramine under the optimal conditions, respectively. In addition, relative standard deviations for intra- (n = 6) and inter-day (n = 5) precisions at two concentrations (50 and 100 μg/L of each analyte) were less than or equal to 4%. Short extraction time, good repeatability, high enrichment factors, and simplicity are the main advantages of the proposed method.     

N-Chloro-2,2-dimethyltaurines: a new class of remarkably stable N-chlorotaurines

The preparation of novel N-chloro-2,2-dimethyltaurine (4) and N,N-dichloro-2,2-dimethyltaurine (5) is described. These 2,2-dimethyltaurines were strategically designed to avoid the hydrolytic dehydrochlorination of N-chlorotaurines. Thus, they possess long-term stability in contrast to the parent N-chlorotaurines, which exhibit broad-spectrum antimicrobial activities.     

Optimum kinetic performance of open-tubular separations in microfluidic devices

A survey is made of the different factors contributing to the kinetic performance of open-tubular separation channels. Being representative for most of the channels used in microfluidic devices, the main focus is on channels with a rectangular format. Kinetic plots of t(0)/N(2 )versus N are established to allow for a visual selection of the ideal channel format and dimensions. These plots for example show that in the pressure-driven mode a channel with a flat-rectangular crosssection (top and bottom wall covered by a retentive layer) can always yield slightly faster (some 15%) separations than a cylindrical capillary, provided the channel depth is optimized. If the channel depth is fixed, the optimal w/d-ratio depends on the required plate number. In electrically driven flows, the situation is reversed and rectangular channels with a small width are to be preferred, and the cylindrical capillary format becomes the best format.