Prediction of analyte retention for ion chromatography separations performed using elution profiles comprising multiple isocratic and gradient steps

This study addresses the simulation of ion chromatographic (IC) separations performed under conditions where the elution profile consists of a sequence of isocratic and gradient elution steps (referred to as "complex elution profiles"). First, models for prediction of retention under gradient elution conditions in IC were evaluated using an extensive database of gradient elution retention data. It is shown that one such model is preferred on the basis that it can be used to predict gradient retention times on the basis of isocratic input data. A method is then proposed for using this model for complex elution profiles whereby each step of the elution profile is treated separately and analyte movement through the column is mapped. An empirically based algorithm for predicting peak width under complex elution conditions is also proposed. Evaluation of the suggested approaches was undertaken on a set of 24 analyte anions and 13 analyte cations on 5 different Dionex columns using a range of 5-step complex elution profiles that gave R2 values for correlations between predicted and observed retention times of 0.987 for anions and 0.997 for cations. The simulation of separations of anions and cations using a 3-step complex elution profile is demonstrated, with good correlation between observed and predicted chromatograms. The proposed approach is useful for the rapid development of separations when complex elution profiles are used in IC.     

Linear velocity surge caused by mobile-phase compression as a source of band broadening in isocratic ultrahigh-pressure liquid chromatography

A linear velocity surge caused by mobile-phase compression was investigated as a source of band broadening for ultrahigh-pressure liquid chromatography (UHPLC). To measure the effect of compression on mobile-phase velocity, ionic sample fronts were monitored using a contactless conductivity detector, as they migrated through long packed capillaries. Mobile-phase compression was found to cause an abnormally high linear velocity surge as the pressure was applied to the inlet of the column. An empirical equation was developed to describe the mobile-phase flow velocity during and after compression. Data fits to this equation were then used to determine the amount of additional variance caused by mobile-phase compression. For a 10/90 v/v acetonitrile/water mobile phase, the velocity surge occurred over roughly 10-15% of the column length. In addition, the velocity surge caused by mobile-phase compression was found to be capable of causing a 50% increase in the measured van Deemter C-terms for reversed-phase UHPLC.     

First demonstration of neutron resonance absorption imaging using a high-speed video camera in J-PARC

The neutron resonance absorption imaging technique with a high-speed video camera was successfully demonstrated at the beam line NOBORU, J-PARC. Pulsed neutrons were observed through several kinds of metal foils as a function of neutron time-of-flight by utilizing a high-speed neutron radiography system. A set of time-dependent images was obtained for each neutron pulse, and more than a thousand sets of images were recorded in total. The images with the same time frame were summed after the measurement. Then the authors obtained a set of images having enhanced contrast of sample foils around the resonance absorption energies of cobalt (132 eV), cadmium (28 eV), tantalum (4.3 and 10 eV), gold (4.9 eV) and indium (1.5 eV).     

Microfluidic device for the detection of glucose using a micro direct methanol fuel cell as an amperometric detection power source

We designed and prepared a novel microbiosensing system consisting of a microbioreactor fabricated using photosensitive sheets intercalated between Pyrex wafers as a dam structure, together with a micro fuel cell as a power source device between the electrodes for amperometric detection. The dam structure retains enzyme (glucose oxidase, GOx)-immobilized microbeads in a microchannel. Microelectrodes are used as an integrated detector within a microchannel located downstream of the dam structure, and these are used to detect the oxidation current of hydrogen peroxide produced from a glucose sample and GOx. A micro direct methanol fuel cell (mu-DMFC, i.d. 500 microm) was fabricated on a polymeric substrate and was used to supply a potential for the electrochemical detector. In this case, two mu-DMFCs were stacked on one substrate to increase the voltage for the oxidation of hydrogen peroxide. A linear response curve was obtained in range from 0.1 to 10 mM glucose for the designed microbiosensing system. These results show that a microfluidic biosensing system designed with a mu-DMFC device is useful and has the potential to assist minuaturization and simplification of the sensing system, in addition to increasing disposability of the device.     

Localisation of a neutron source using measurements and calculation of the neutron flux and its gradient

We have performed laboratory measurements of the neutron flux and its gradient in a static model experiment, similar to a model problem proposed in Pázsit (Ann. Nucl. Energy 24 (1997) 1257). The experimental system consists of a radioactive neutron source located in a water tank. The measurements are performed using a recently developed very small optical fibre detector. The measured values of the flux and its gradient are then used to test the possibility of localising the source. The results show that it is possible to measure the flux on the circumference of a circle and from this calculate the flux gradient vector. Then, by comparison of the measured quantities with corresponding MCNP calculations, both the direction and the distance to the source are found and thus the position of the source can be determined.     

Signal detection and noise suppression using a wavelet transform signal processor: application to ultrasonic flaw detection

The utilization of signal processing techniques in nondestructive testing, especially in ultrasonics, is widespread. Signal averaging, matched filtering, frequency spectrum analysis, neural nets, and autoregressive analysis have all been used to analyze ultrasonic signals. The Wavelet Transform (WT) is the most recent technique for processing signals with time-varying spectra. Interest in wavelets and their potential applications has resulted in an explosion of papers; some have called the wavelets the most significant mathematical event of the past decade. In this work, the Wavelet Transform is utilized to improve ultrasonic flaw detection in noisy signals as an alternative to the Split-Spectrum Processing (SSP) technique. In SSP, the frequency spectrum of the signal is split using overlapping Gaussian passband filters with different central frequencies and fixed absolute bandwidth. A similar approach is utilized in the WT, but in this case the relative bandwidth is constant, resulting in a filter bank with a self-adjusting window structure that can display the temporal variation of the signal's spectral components with varying resolutions. This property of the WT is extremely useful for detecting flaw echoes embedded in background noise. The detection of ultrasonic pulses using the wavelet transform is described and numerical results show good detection even for signal-to-noise ratios (SNR) of -15 dB. The improvement in detection was experimentally verified using steel samples with simulated flaws.     

基于心理声学参数的燃料电池轿车车内噪声评价及噪声源识别

燃料电池汽车是采用燃料电池动力系统的新型零排放环保汽车,其噪声源是分布式的,车内噪声组成比较复杂,噪声的线性度没有传统汽车好,因此亟需改善其车内声音品质,使人们在享受能源环保的同时也能有舒适的乘坐环境。论文测试某型燃料电池轿车怠速工况车内噪声,进行车内噪声的频谱分析。以响度作为声品质评价指标,提出了改善车内声品质应着重考虑的频率范围,同时结合噪声频谱分析,采用参数化滤波方法对主要峰值频率进行处理,找出对人耳主观感觉影响较大的频率或频段。为了降噪和改善车内声品质,采取分别运行法进行物理问题识别,找出对乘员主观感觉影响较大的频率和频段产生的声振部件,实现从声品质问题到物理问题的转换,研究发现车内噪声上述频率和频段主要是由燃料电池辅助系统（氢泵和风机）产生的。     

白噪声激励下的复合材料层合结构损伤检测的内积向量法

利用白噪声激励下结构各测点的动力学响应之间的互相关函数,引入了内积向量（Inner Product Vector,IPV）的概念,提出了应用内积向量进行结构损伤检测的方法,并分析了测试噪声对基于内积向量的损伤检测方法的影响。通过对复合材料层合梁的分层损伤检测仿真算例,验证了该方法检测损伤的有效性以及较高的抗噪能力。     

Damage detection in beams from modal and wavelet analysis using a stationary roving mass and noise estimation

This paper uses the Continuous Wavelet Transform Analysis on mode shapes for damage identification. The wavelet analysis is applied to the difference in the mode shapes between a healthy and a damaged state. The paper also includes a novel methodology for estimating the level of noise of the experimental mode shapes based on a standard Signal to Noise Ratio (SNR). The estimated SNRs are used for identifying and making emphasis on the less noisy data. Moreover, a mass attached to the structure is considered to enhance the sensitivity of the structure to damage. Modal analysis is performed for different positions of the mass along the beam. The results obtained for all the positions of the mass are combined so an averaging process is implicitly applied. The paper presents the results from an experimental test of a cantilever steel beam with different severity levels of damage at the same location. The results show that the use of the attached mass reduces the effect of noise and increases the sensitivity to damage. Little damage can be identified with the proposed methodology even using a small number of sensors and only the first five bending modes.     

Two-point maximum entropy noise discrimination in spectra over a range of baseline offsets and signal-to-noise ratios

The two-point maximum entropy method (TPMEM) is a useful method for signal-to-noise ratio enhancement and deconvolution of spectra, but its efficacy is limited under conditions of high background offsets. This means that spectra with high average background levels, regions with high background in spectra with varying background levels, and regions of high signal-to-noise ratios are smoothed less effectively than spectra or spectral regions without these conditions. We report here on the cause of this TPMEM limitation and on appropriate baseline estimation and removal procedures that effectively minimize the effects on regularization. We also present a comparative analysis of TPMEM and Savitzky-Golay filtering to facilitate selection of the best technique under a given range of conditions.     

Quenched phosphorescence as a detection method in capillary electrophoretic chiral separations. Monitoring the stereoselective biodegradation of camphorquinone by yeast

Quenched phosphorescence detection of camphorquinone in cyclodextrin-based electrokinetic chromatography provides very favorable detection limits, i.e., 7 x 10(-)(7) M, 3 orders of magnitude lower than conventional UV absorption detection at 200 nm. The detection is based on the dynamic quenching by the analyte of the strong phosphorescence emission of brominated naphthalenesulfonate, under deoxygenated buffer solution conditions. This approach has been used to detect (1S)-(+)- and (1R)-(-)-camphorquinone after enantiomeric separation by CE. Although the use of the negatively charged carboxymethyl beta-cyclodextrin (CM-beta-CD) alone was not successful, the addition of a second, neutral cyclodextrin, alpha-CD, provided an adequate enantiomeric separation of camphorquinone. Using 25 mM borate buffer (pH 8.5) with 10 mM CM-beta-CD and 20 mM alpha-CD (applied voltage 20 kV, ambient temperature), the enantiomeric separation was performed in approximately 14 min. The chiral method was applied to monitor the stereoselectivity of the biotransformation of a racemic mixture of camphorquinone by yeast. It was found that the enantiomeric ratio calculated from the peak areas in the electropherogram (RSD = 5%) after 24 h of incubation decreased from 0.92 for the control solution (culture medium without yeast) to 0.24 for the culture medium; a similar ratio of 0.25 was observed for cell extract solutions. Therefore, racemic camphorquinone is enantioselectively degraded by yeast, the biodegradation of (1S)-(+)-camphorquinone being faster than that of the (1R)-(-)-enantiomer.     

High-speed, whole-column fluorescence imaging detection for isoelectric focusing on a microchip using an organic light emitting diode as light source

An integrated and simplified microfluidic device using a 250 microm x 1-4 cm of organic light emitting diode (OLED) array as a two-dimensional light source for single-channel and multichannel whole-column imaging detection was developed. This fluorescence detection system was used for isoelectric focusing (IEF) of R-phycoerythrin in a microchip. The IEF conditions were optimized, and the total analysis time was extremely reduced to 30 s for 2-cm-long microchannels at 700 V/cm of electric field strength without the presence of electroosmotic flow. The compression of pH gradient caused by electrolytes drawing into the microchannels was efficiently restrained when 1% hydroxylpropylmethyl cellulose in 2% ampholyte was used as the carrier for IEF. Under optimized IEF conditions, the detection limit of this system was approximately 0.6 microg/mL or 45 pg at 75 nL/column injection of R-phycoerythrin. This OLED-induced fluorescence detection system for WCID provides a high-speed IEF technique with quantitative ability and the potential for high integration and throughput microchip systems.     

MBE of InGaN/GaN heterostructures using ammonia as a source of nitrogen

Technical Physics Letters - InGaN/GaN heterostructures have been grown by molecular beam epitaxy (MBE) using ammonia as a source of nitrogen. The influence of the growth temperature and rate on the...     

Stand-off detection of solid targets with diffuse reflection spectroscopy using a high-power mid-infrared supercontinuum source

We measure the diffuse reflection spectrum of solid samples such as explosives (TNT, RDX, PETN), fertilizers (ammonium nitrate, urea), and paints (automotive and military grade) at a stand-off distance of 5 m using a mid-infrared supercontinuum light source with 3.9 W average output power. The output spectrum extends from 750-4300 nm, and it is generated by nonlinear spectral broadening in a 9 m long fluoride fiber pumped by high peak power pulses from a dual-stage erbium-ytterbium fiber amplifier operating at 1543 nm. The samples are distinguished using unique spectral signatures that are attributed to the molecular vibrations of the constituents. Signal-to-noise ratio (SNR) calculations demonstrate the feasibility of increasing the stand-off distance from 5 to ~150 m, with a corresponding drop in SNR from 28 to 10 dB.     

Self-assembled films containing crude extract of avocado as a source of tyrosinase for monophenol detection

This paper reports on the use of the crude extract of avocado (CEA) fruit (Persea americana) as a source of tyrosinase enzyme. CEA was immobilized via layer by layer (LbL) technique onto indium tin oxide (ITO) substrates and applied in the detection of monophenol using a potentiometric biosensor. Poly(propylene imine) dendrimer of generation 3 (PPI-G3) was used as a counter ion in the layer by layer process due to its highly porous structure and functional groups suitable for enzyme linkage. After the immobilization of the crude CEA as multilayered films, standard samples of monophenol were detected in the 0.25–4.00 mM linear range with approximately 28 mV mM^? 1 of sensitivity. This sensitivity is 14 times higher than the values found in the literature for a similar system. The results show that it is possible to obtain efficient and low-cost biosensors for monophenol detection using potentiometric transducers and alternative sources of enzymes without purification.     

Photoluminescence optimization of BCNO phosphors synthesized using citric acid as a carbon source

Citric acid was used as carbon source for the optimization of the photoluminescence (PL) performance of boron carbon oxynitride (BCNO) phosphor. Citric acid was chosen as an alternative carbon source because of its simple molecular structure, low decomposition temperature, relative inexpensiveness, and environmental friendliness. The prepared sample exhibited a single, homogeneous, and broad photoluminescence emission band whose peak varied from near-UV (400 nm) to yellow-visible (500 nm) upon excitation at 365 nm. The effects of varying the synthesis temperature, molar ratio of the carbon/boron and nitrogen/boron sources, and addition of SiO₂ nanoparticles on the PL properties were also studied. The optimized BCNO phosphors may find potential use in white LED applications.     

Facile synthesis of fluorescent carbon dots using watermelon peel as a carbon source

The synthesis of water-soluble fluorescent carbon dots (C-dots) has received much attention recently. Here, high quality fluorescent C-dots have been synthesized through low-temperature carbonization and simple filtration using watermelon peel, a waste and reproducible raw resource, as a novel carbon resource. This facile approach allows large-scale production of aqueous C-dots dispersions without any post-treatment process. The as-prepared C-dots possess small particle sizes (~ 2.0 nm), strong blue luminescence, acceptable fluorescence lifetime and good stability in a wide range of pH values (pH 2.0-11.0) and at a high salt concentration. Besides, the obtained C-dots have been successfully applied in live cell imaging, indicating these carbon nanoparticles can serve as high-performance optical imaging probes.