Determination of pentachlorophenol residues in wine and corks by solvent extraction methodology and specific gas chromatography detection

Summary A gas chromatographic methodology with selective detection is presented for the analysis in wines and corks of pentachlorophenol residues, which are suspected to be the most likely precursors of some off-flavours described in several wine samples. After derivatisation, pentachlorophenol acetate residues were monitored by electrolytic conductivity detection and/or mass spectrometric detection in the selective ion mode at m/z 264 and 266. Recoveries varied from 80 to 96% for wine samples fortified with 5 to 100 g l^–1 and from 83 to 91% for corks (fortified at 25 to 100 g kg^–1). The proposed methodology allowed for a determination limit of g l^–1 for wine and 10 g kg^–1 for corks.     

Application of HPLC to measure vanadium in environmental,biological and clinical matrices

Vanadate and vanadium compounds exist in many environmental, biological and clinical matrices, and despite the need only limited progress has been made on the analysis of vanadium compounds. The vanadium coordination chemistry of different oxidation states is known, and the result of the characterization and speciation analysis depends on the subsequent chemistry and the methods of analysis. Many studies have used a range of methods for the characterization and determination of metal ions in a variety of materials. One successful technique is high performance liquid chromatography (HPLC) that has been used mainly for measuring total vanadium level and metal speciation. Some cases have been reported where complexes of different oxidation states of vanadium have been separated by HPLC. Specifically reversed phase (RP) HPLC has frequently been used for the measurement of vanadium. Other HPLC methods such as normal phase, anion-exchange, cation-exchange, size exclusion and other RP-HPLC modes such as, ion-pair and micellar have been used to separate selected vanadium compounds. We will present a review that summarizes and critically analyzes the reported methods for analysis of vanadium salts and vanadium compounds in different sample matrices. We will compare various HPLC methods and modes including sample preparation, chelating reagents, mobile phase and detection methods. The comparison will allow us to identify the best analytical HPLC method and mode for measuring vanadium levels and what information such methods provide with regard to speciation and quantitation of the vanadium compounds.     

Simultaneous acquisition of X-ray spectra using a multi-wire, position-sensitive gas flow detector

A multi-wire, gas-filled position-sensitive detector has been developed for the simultaneous recording of wavelength-dispersed X-ray signals that enables X-ray fluorescence spectrometry with a limited multi-element capability in the low Z element range. Details of the modular construction of the detector are given. The detector performance was characterized using Al–K radiation and a variable slit system. The detector has been applied in a laboratory spectrometer equipped with an electron source and a double multilayer mirror device as the wavelength-dispersing element. Spectra from Al and Si obtained in the simultaneous acquisition mode show good agreement with calculations performed using a ray-tracing model.     

基于循环平稳的复调频信号检测性能研究

针对加性色噪声和乘性色噪声联合干扰下的雷达运动目标检测问题进行了研究.首先利用循环平稳信号处理原理,分析了加性噪声和乘性噪声联合干扰下的复调频信号的循环统计特性,在此基础上构造了基于二阶循环矩的检测统计量,推导了检测统计量的输出信噪比与观测噪声统计特性的关系.最后利用Monte-Carlo仿真试验得到检测性能的曲线,并与基于时频分布的Wigner-Hough检测器做了比较,仿真试验进一步验证了本文提出的二阶循环矩检测器性能要优于Wigner-Hough检测器.     

高速数字化三维集成式CCD-CMOS图像传感器

为了解决CCD与CMOS工艺兼容性低、互连集成制作难度大,以及芯片间接口匹配和高性能兼备等问题,对CCD器件拓扑结构与像元、CMOS读出电路、三维异质互连集成及高密度引脚封装等技术进行研究,提出了一种1024×256阵列规模的集成式CCD-CMOS图像传感器。该器件实现了CCD信号的高精度数字化处理、高速输出及多芯粒的技术融合,填补了国内CCD-CMOS三维集成技术空白。测试结果表明:集成CCD-CMOS器件的光响应和成像功能正常,双边成像效果良好,图像无黑条和坏列,互连连通率(99.9%)满足三维集成要求,实现了集成式探测器件的大满阱高灵敏度成像(满阱电子数达165.28ke-、峰值量子效率达86.1%)、高精度数字化(12bit)和高速输出(行频率达100.85kHz),满足集成化、数字化、小型化的多光谱探测成像系统要求。     

单边凹槽电极结构MSM型蓝光探测器的研究

为提升InGaN基可见光探测器性能,制作并测试了基于GaN/InGaN MQWs外延材料的单边凹槽叉指电极MSM结构蓝光光电二极管。凹槽电极器件的I-V特性测试结果显示,相较于传统平面电极器件,随着偏压增加,器件暗电流越小且越趋于平缓,而光电流越大;光谱响应率测试显示,器件截止带边都位于490nm附近,凹槽电极器件带边处拒绝比高于平面电极器件1个量级。当偏压为5V时,凹槽电极器件响应率为0.0346A/W@480nm,对应外量子效率为8.94%,高于平面电极器件。器件性能提升的原因是单边凹槽电极结构有效改善了内建电场的分布,从而抑制了表面传导漏电流,使得器件暗电流更小且更有利于电极收集光生载流子,提升了响应率。     

潜望式红外夜视瞄准镜的研制

介绍了潜望式红外夜视瞄准系统的工作原理和研制方案.该系统兼具了潜望瞄准镜和红外热像仪的功能.从探测器外围电路,信号处理系统、潜望式红外光学系统的设计以及移动焦平面整体电动调焦技术等几个方面分析了潜望式红外夜视瞄准系统研制过程中存在的关键技术.最后对基于此方案所研制出的海军红外夜视瞄准镜应用情况做了简要报告.     

化学发光技术在色谱柱后检测中的应用

化学发光与色谱联用具有选择性好、灵敏度高等优点,应用广泛.本文主要介绍近三年来化学发光包括鲁米诺、过氧草酸酯、Ru(bipy)33 、无机等体系作为液相色谱柱后检测及含氮、含硫化合物气相化学发光等体系作为气相色谱柱后检测的现状.     

低耦合损耗的光电混合光纤旋转连接器

设计了一种光电混合光纤旋转连接器,能实现相对旋转的光信号在较大对准误差范围内低损耗连接.旋转状态下的自聚焦透镜准直光纤输出的光信号,并由PIN光电探测器将其转换为电信号,冉由激光器根据电信号再生出原始光信号继续在光纤通讯系统中传输.该光电混合光纤旋转连接器在离轴偏移量至520μm或对准倾斜角至0.5°时的附加耦合损耗为0.3 dB,而采用双自聚焦透镜的光纤旋转连接器要获得小于3 dB的插入损耗,其离轴偏移或倾斜角度必须小于100 μm和0.10°相比之下,本文设计的光纤旋转连接器能降低系统对机械加上及装配精度的要求,具有较高的实用价值.