响应面法优化超声辅助提取-原子荧光法快速测定茶叶痕量汞

研究了一种使用超声波辅助提取(UAE)-原子荧光法测定茶叶痕量汞的快速方法.采用Plackett-Burman设计从6个影响汞提取率的因素中筛选出3个显著因素—超声时间St,超声温度T和HNO3:H2O2(1:1,δ)体积A2,并采用中心组合设计和响应面法优化参数.结果表明,最优提取条件为,浸泡时间6 min,St 8...     

A sensitive fluorimetric method for determination of trace amounts of nitrite based on luminescence energy transfer

An efficient luminescence energy transfer (LET) system based on terbium(III)-sodium hexametaphosphate (Tb/SHMP) chelates as donor and 4-((4-(2-aminoethylamino)naphthalen-1-yl)diazenyl)benzenesulfonic acid dihydrochloride (ANDBS) as acceptor was developed for sensitive determination of trace nitrite. Stable and strong fluorescence Tb/SHMP chelates were prepared in aqueous solution. Based on Griess Reaction, ANDBS was generated by the quantitative reaction of nitrite, sulfanilamide and N-(1-naphtyl)-ethylenediamine dihydrochloride (N1NED). The degree of the overlap was effective for LET between the emission spectrum of Tb/SHMP chelates and the absorption spectrum of ANDBS. Based on the luminescence intensity quenching of Tb/SHMP chelates in proportion to the trace amounts of nitrite, a new assay for the selective and sensitive determination of nitrite was developed. Under the optimum conditions, the linear calibration graph was obtained with a linear range of 0.00040-0.20 μg mL⁻¹ (R=0.99657). The detection limit of was 0.00010 μg mL⁻¹ (R=0.99657). The method was applied successfully to the determination of nitrite for synthetic samples.     

Ultrasound irradiation effect on morphology and size of two new potassium coordination supramolecule compounds

Two new potassium coordination supramolecular compounds (2D and 1D), [K(H₃L)(H₂L)(H₂O)]_n·H₂O (1) and [K(H₂L′)(HL′)(H₂O)₂]·H₂O (2), (L = 1,3,5-tricarboxylic acid, L′ = 2,6-pyridinedicarboxylic acid), have been synthesized under different experimental conditions. Micrometric crystals (bulk) or nano-sized materials have been obtained depending on using the branch tube method or sonochemical irradiation. All materials have been characterized by field emission scanning electron microscopy (FE-SEM), scanning electron microscopy (SEM), powder X-ray diffraction (PXRD), FT-IR spectroscopy and elemental analyses. Single crystal X-ray analyses on compounds 1 and 2 show that K⁺ ions are 3- and 7-coordinated, respectively. Additionally, H-bonds incorporate the layers and chains in 1 and 2 into 3D and 2D (along (0,0,1) direction) frameworks. Topological analysis shows that the compound 1 and 2 are 3,6-coordinated kgd and 2,4-coordinated 2,4C4 net. The thermal stability of compounds 1 and 2 in bulk and nano-size has been studied by thermal gravimetric (TG) and differential thermal analyses (DTA) and compared each other. The role of different parameters like temperature, reaction time and ultrasound irradiation power on the growth and morphology of the nano-structures are studied. Results suggest that an increase of temperature, sonication power and reduction of reaction time led to a particle size decrease.     

Fabrication of electrochemical sensor based on molecularly imprinted polymer and nanoparticles for determination trace amounts of morphine

Ionics - A simple and rapid electrochemical method developed for the detection of trace amounts of morphine (MO) at the surface of modified pencil graphite electrode (PGE) with multiwall carbon...     

Search for a reliable methodology for PSD determination based on a combined molecular simulation-regularization-experimental approach: The case of PHTS materials

We present here a methodology for searching a robust pore size distribution (PSD) for adsorbent materials. The method is based on a combination of individual adsorption isotherms, obtained from Grand Canonical Monte Carlo simulations, a regularization procedure to invert the adsorption integral equation (Tikhonov regularization solved by singular value decomposition), and the needed experimental adsorption isotherm. The selection of several parameters from the available choices to start the procedure are discussed here: the size of the kernel (number of individual pores and number of experimental adsorption points to be included), the fulfillment of the Discrete Picard condition, and the L-curve criteria, all leading to find a reliable and robust PSD. The procedure is applied to plugged hexagonal templated silicas (PHTS), synthesized, and characterized in our laboratory.     

激光器特性在痕量气体检测中的影响

研究了激光器扫描步长和线宽两种特性对可调谐半导体激光吸收光谱检测系统的影响,理论上推导出激光与气体吸收谱线的作用原理,分析出扫描信号(锯齿波)的台阶间隔和高度影响激光器中心波长的扫描原理.设定了仿真参数,仿真出锯齿波台阶数与最大扫描误差关系曲线,得出扫描信号的一个周期内具有4000个台阶时,半高全宽(FWHM)大于0.01 cm-1,误差小于1‰;仿真出激光器线宽与最大幅值、线宽误差关系曲线,给出线宽误差最大为1%,0.5%时激光器线宽对应的最小FWHM.在温度系数n取0.9,大气展宽系数γair取0.005的条件下,给出温度T,压强P与FWHM关系图,推出了适用的压强与温度范围.为指导选取激光器与气体吸收谱线、提高系统检测限提供了相关理论依据.     

Pressure effect on the melting point of alkali metals

The mean-square displacement of alkali metals is studied theoretically using our local Heine-Abarenkov-type model potential in the perturbational scheme. The temperature-dependent mean-square displacement of alkali metals decreases as function of the compressed volume. Lindemann's criterion for melting x_m, which is defined as the ratio of two times the root-mean-square displacement to the nearest-neighbour distance, is found to be nearly constant for five alkali metals. The volume effect on the melting temperature of alkali metals is studied by keeping x_m constant. The obtained melting curve increases as function of the compressed volume and are qualitatively in good agreement with the observed tendency for alkali metals.     

Sensitive solid-state optical sensible materials for photothermal determination of trace metals

Methods of photothermal (thermal-lens) determination of iron and mercury on the basis of solid polymer matrices with immobilized reagents are developed. These methods combine selective and efficient preconcentration of trace elements to be analyzed on a transparent polymer matrix, the sensitivity of determination with the reliable and traceable photometric procedures and highly sensitive thermal-lens detection (enhanced in polymers compared to solutions). The advantage of this approach is in the use of sensitive organic reagents previously developed for spectrophotometry. In this study, transparent polymethacrylate matrices modified with copper dithizonate and 1,10-phenanthroline were applied to the determination of mercury(II) and iron(II), respectively.     

Hand vein recognition based on the connection lines of reference point and feature point

According to the essential characters of the image topology, a new hand vein recognition algorithm based on the connection lines of reference point and feature points is proposed. In this method, the intersection points and the endpoints of the vein image are used as feature points. After the intersection points and the endpoints selected as feature points, the reference point for image matching are extracted from these points. The relative distances between the reference point and the feature points and the angles between the adjacent connections of the reference point and feature points are calculated and used as recognition features. Finally these two features are combined for hand vein recognition. This method can effectively overcome the influence on the recognition results caused by image translation and rotation. Experimental results show that the proposed algorithm is able to achieve hand vein recognition reliably and quickly.     

Track infrared point targets based on projection coefficient templates and non-linear correlation combined with Kalman prediction

For a long time, tracking IR point targets is a great challenge task. We propose a tracking framework based on template matching combined with Kalman prediction. Firstly, a novel template matching method for detecting infrared point targets is presented. Different from the classic template matching, the projection coefficients obtained from principal component analysis are used as templates and the non-linear correlation coefficient is used to measure the matching degree. The non-linear correlation can capture the higher-order statistics. So the detection performance is improved greatly. Secondly, a framework of tracking point targets, based on the proposed detection method and Kalman prediction, is developed. Kalman prediction reduces the searching region for the detection method and, in turn, the detection method provides the more precise measurement for Kalman prediction. They bring out the best in each other. Results of experiments show that this framework is competent to track infrared point targets.     

基于灭点理论的目标姿态角单站测量

提出了一种基于灭点理论的目标姿态角单站测量方法,利用单台光测设备的参数信息和目标在图像上的灭点位置计算目标特征直线的方向,从而获得目标的姿态信息。同时给出了灭点精度评价指标,可作为姿态测量精度的评价标准和加权融合时的权重因子。通过模拟实验和实物实验验证了方法的可行性和准确性。该方法与中轴线法测量偏差均值为0.2,表明所给出的方法对类柱状目标的姿态测量具有精度高、易于实现的特点。     

用于快速定量塑料中微量元素的标准样品制备方法研究

采用色母粒法制备含重金属元素的电子信息产品(塑料)的标准样品,建立了标准样品制备的程序;利用X射线荧光光谱仪(XRF)定量分析方法,考察了标准样品测定重金属和溴元素含量的重复性以及不确定度,建立了标准样品工作曲线的测定程序及测定电子信息产品实际样品的方法和程序.结果表明,利用该方法制备的标准样品在200～2 000 mg·kg-1浓度范围内,测量有机物中微量Pb,Hg,Cr,Br元素及在20～200mg· kg-1浓度范围内测量Cd元素,均获得了非常好的线性关系,并经六次检测具有很好地重复性,并以日本三菱重工公司的电路板ICB288和ICB288G作为实际样品进行测试,其结果与推荐值一致.     

A new methodology for the determination of silicon in plants by wavelength dispersive X-ray fluorescence

Silicon is an important element for plants at their structure and physiology and plays an important role in bone mineralization and soft tissue development in human beings. Furthermore, its determination is being requested more frequently due to nutritional requirements. However, the methods found in the literature to determine silicon in this type of samples require a sample preparation step, which makes them time-consuming and provides high uncertainties. In this paper, a method for the determination of silicon in plants by wavelength dispersive X-ray fluorescence (WD-XRF) spectrometry has been developed. Horsetail (Equisetum arvense L.) and nettle leaf (Urtica dioica) have been used as a source of silicon due to its medical use. Sample preparation involved calcining the sample at 700°C and preparing fused beads from the calcined sample. Calibration standards for WD-XRF measurement were prepared by mixing certified reference materials and chemical products to reproduce the samples matrix. The linear range for silicon concentration ranges from 6 to 55 wt% SiO₂. The validation of the method was performed measuring a reference material (NCS DC73349 Bush branches and leaves) and comparing the results obtained by WD-XRF with those obtained by an independent method by atomic absorption spectrometry. The developed methodology is rapid and accurate, provides low uncertainties, and is environmentally friendly, as it does require the use of less hazardous reagents.     

A shock-capturing methodology based on adaptative spatial filtering for high-order non-linear computations

A shock-capturing methodology is developed for non-linear computations using low-dissipation schemes and centered finite differences. It consists in applying an adaptative second-order filtering to handle discontinuities in combination with a background selective filtering to remove grid-to-grid oscillations. The shock-capturing filtering is written in its conservative form, and its magnitude is determined dynamically from the flow solutions. A shock-detection procedure based on a Jameson-like shock sensor is derived so as to apply the shock-capturing filtering only around shocks. A second-order filter with reduced errors in the Fourier space with respect to the standard second-order filter is also designed. Linear and non-linear 1D and 2D problems are solved to show that the methodology is capable of capturing shocks without providing dissipation outside shocks. The shock detection allows in particular to distinguish shocks from linear waves, and from vortices when it is performed from dilatation rather than from pressure. Finally the methodology is simple to implement and reasonable in terms of computational cost.     

S+Au增感中心的电子陷阱效应对光电子行为的影响

利用微波吸收相敏检测技术，对AgBrI-T颗粒乳剂中自由光电子与浅束缚光电子时间行为进行了检测，结果表明在一级衰减曲线的不同区域中增感中心对光电子衰减的作用表现不同；S+Au增感中心的电子陷阱效应随浓度的增加发生了由浅电子陷阱到深电子陷阱的转变.根据增感浓度与光电子衰减时间的对应关系，获得了S+Au最佳增感浓度. 关键词： 微波相敏检测 光电子 增感 电子陷阱     

The effect of oxygen on sensitization of AgBrI crystals with anionic dye

A mechanism is suggested for the effect of oxygen on spectral sensitization of AgBrI microcrystals (MCs) with anionic dye adsorbed on the surface, which adequately describes the changes of both luminescent and spectral-sensitometric properties of this system. It is shown that the effect of oxygen on the spectral sensitization of AgBrI MC with anionic dye cannot be explained only by desensitization of the AgBrI MC sensitivity as has been suggested in the literature, but rather its effect on the spectral sensitization of AgBrI MC was not so unambiguous. In the framework of the suggested mechanism such ambiguity is due to the fact that the Ag⁺ and Ag₂⁺ silver centers that participate in the generation recombination processes and are different in structure, interact on the surface of the AgBrI MC with different aggregate forms of the dye, which are in turn differently affected by oxygen. Understanding physicochemical processes occurring in the considered system allows using the obtained results in holographic and spectrozonal photographic materials, gas-phase sensors, and in solar-energy systems.     

基于边缘特征的中值滤波的小目标检测法

提出了一种基于边缘特征调整滤波尺寸的中值滤波算法用于小目标的检测。以图像像素的四个方向的边缘分量确定阈值,以此阈值判断像素是否为小目标区域,在此基础上调整滤波尺寸,采用中值滤波方法检测出小目标。结果表明,该算法对于小目标检测有很好的效果。