Determination of Pb,Zr, Ti,Sr, Cr,Nb and La in lead zirconate titanate ceramics by particle‐induced X‐ray emission

A particle‐induced X‐ray emission (PIXE) technique has been used in the determination of the principal components Pb, Zr and Ti and the substituting elements Sr, Cr, Nb and La in lead zirconate titanate ceramics. In general, precision of analysis was concentration dependent from each element under study. For Pb, precision varied between 0.13% and 0.16%, at higher concentration of 59.32–64.5%. It was around 6–9% for Sr, Cr and Nb at concentrations of 1% or lower. Particular attention was devoted to the estimation of the analysis trueness. With this purpose, three methods were applied: (1) comparison of PIXE and inductively coupled plasma optical emission spectrometry concentrations, (2) recovery study and (3) comparison with a laboratory standard. Trueness of analysis was around 100 ± 10% for the evaluated elements Pb, Zr, Ti, Sr and Cr. The expected stoichiometry and elemental composition homogeneity of a wide group of produced ceramics were confirmed by the PIXE technique. Copyright © 2012 John Wiley & Sons, Ltd.     

在不同空间高度下遥感FTIR定量测定大气中的某些VOCs

应用遥感FTIR在不同高度下,测定大气中的有毒易挥发有机化合物(VOCs)——甲苯,正己烷和丙酮的浓度。并对相同的高度下,测量的精度做了研究。当高度为0.61 m时,所测得的气体的浓度值最大,而当仪器高度为0.36和0.86 m时,测得的浓度则较低。实验结果表明,在不同的高度下VOCs的挥发是不同的。     

原子吸收硫化锌法间接测定精氨酸络合反应的机理研究

通过编程计算精氨酸和锌离子在不同pH条件下的各种存在形式,通过分析拟合分布图,研究了在硫化锌法原子吸收间接测定精氨酸时的pH对原子吸收响应的影响及络合反应的机理.经对不同形态的精氨酸与金属锌离子的共存区域的各种组合探讨,指出在pH 9.0左右最佳测定条件下的pH响应峰是由于精氨酸和锌离子的两种不同存在形式的变化所引起的左右峰边缘,精氨酸是以正一价荷电形态的精氨酸基Arg -与Zn(OH)2形成了可溶性络合离子[HN=CH(NH 3)-NH-(CH2)3-CH(NH 3)-COO]2Zn(OH)2.结果表明,理论分析计算的结果与实验数据得到了基本吻合,确定了硫化锌法原子吸收间接测定精氨酸时的络合物反应机理及络合物的组成结构.     

Analysis of the Structure of the Bands in the IR Spectrum of β-D Glucose by the Regularized Method of Deconvolution

Deconvolution of the IR absorption spectrum of -D glucose in the spectral range 1500–450 cm^–1 has been carried out. The results of the deconvolution were compared with the IR and Raman spectra recorded at room and low temperatures and with the data obtained by theoretical calculations for the frequencies of the normal vibrations of the -D glucose molecule in the crystalline state. It is shown that deconvolution of the IR spectra recorded at room temperature makes it possible to separate the bands observed experimentally only at a very low temperature of the sample and a number of components that were not resolved earlier. The number of bands separated on deconvolution of the IR spectra of -D glucose in the spectral range 1500–450 cm^–1 is more than twice the number of visible absorption maxima in the usual spectrum. The results of deconvolution of the IR spectrum of -D glucose are in good agreement with the data of theoretical calculations for the frequencies of the normal vibrations of the -D glucose molecule in the crystalline state. The existence of the factor-group (Davydov) splitting of a number of frequencies of the nondegenerate fundamental vibrations of molecules in a crystal cell has been revealed in the IR spectrum of -D glucose. It was concluded that the model of an isolated molecule is insufficient for detailed theoretical interpretation of the vibrational spectra of carbohydrates.     

对地观测平台恒星敏感器离焦成像折中设计分析

从对地观测平台角秒量级姿态确定需求出发,在构建星敏感器惯性系成像模型的基础上指出,恒星在成像面上的定位误差是星敏感器姿态确定误差的主要来源。同时,结合理想光学系统离焦模型,分析了星敏感器主要性能指标间的量化关系,并给出了成像面定位误差最低限。仿真结果表明,从优化系统性能考虑,成像模糊区直径为2~3个像元的配置是利用星敏感器焦平面的“轻微离焦”来实现亚像元定位的最佳方案,定位误差可达0.2个像元,能够满足星敏感器惯性姿态确定精度4″~5″的要求。理论分析和数值仿真结果可为后续星敏感器指标的提出及仪器设计提供技术参考。     

Laser-phase determination methods and transfer equations for direct temporal structure measure- ments of atto- and femtosecond XUV pulses

In this paper the laser-phase determination methods and transfer equations are presented to directly reconstruct the detailed temporal structures of ultra-short extreme ultraviolet (xuv) pulses from the measured photoelectron energy spectra (PES). Each transfer equation includes one of PID (proportional-integral-differential) terms of PES. The intensity and instantaneous frequency of attosecond xuv can be retrieved from the integral term of PES. The intensity profiles of narrow bandwidth atto- and femtosecond xuvs can be rebuilt from the proportional and differential terms of PES respectively. The methods and equations may be used to improve time resolutions in measuring ultrashort pulses.     

中红外光谱法在无创血糖检测技术中的应用

构建了中红外无创血糖检测的实验方案,利用傅里叶红外光谱仪对葡萄糖溶液及手指进行了中红外光谱检测并进行分析,得到葡萄糖的中红外特征吸收峰在1000cm^-1附近,证实了中红外光谱在无创血糖检测中的可实现性,选择激光器和光导探测器进行特征峰处的光电检测实验,并得到了有效信号。     

液相阴极辉光放电原子发射光谱法高灵敏测定精铜矿中的铅和锌

由于重金属毒性大,且在环境、动物和人体器官中易积聚,因而在矿石开采、冶炼和加工之前,监测其中的微量重金属显得尤为重要。著名的原子光谱仪器,如原子荧光光谱(AFS)、原子吸收光谱(AAS)、电感耦合等离子体(ICP)等已广泛用于各种样品中元素的检测,但它们体积大、能耗高、价格昂贵、气体消耗大,这些缺点严重阻碍了野外现场的连续监测。为了满足分析仪器的微型化趋势,1993年Cserfalvi开发了一种电解液阴极放电原子发射光谱(ELCAD-AES)技术并将其用于分析检测中。该装置中,待测溶液以8～10 mL·min-1的流速从细管顶端溢出,然后沿管壁流入装满电解液的35 mL储液池中,以溢出溶液的液面作为放电阴极,在和流动液体电极相距2～4 mm处放一金属W(Ti)棒为阳极,细管浸入电解液并尖端向上弯曲超出储液池液面1～3 mm,细管顶端溢出的液体流入储液池并通过其中的碳棒与电源负极相连,从而构建放电系统。从那时起,为了提高激发效率和放电稳定性,人们对ELCAD进行了大量改进。基于ELCAD的特点,通过改进放电装置,建立了一种新的液相阴极辉光放电(LCGD)分析系统。该系统中,放电在直径0.5 mm的铂针阳极和内径1 mm的毛细管顶端溢出的溶液阴极之间的间隙中产生。毛细管上端和铂丝之间的间隙为2 mm,毛细管插入石墨管且露出石墨管的距离为2.5 mm。样品溶液以4.5 mL·min-1从毛细管顶端溢出流经石墨管上的凹槽,石墨管和电源负极连接。与ELCAD相比,LCGD的优点在于：Pt针做阳极,可形成尖端放电,从而降低能耗(<60 W),提高激发效率;蠕动泵管上打结,可降低泵的脉动性,提高放电的稳定性;石墨管链接电源负极,删除ELCAD中的储液池,使样品消耗更少。为了评估方法的分析性能,用LCGD测定了HNO₃-HCl消化的精铜矿样品中的铅和锌。系统研究了放电稳定性以及放电电压、溶液流速、支持电解质和溶液pH对发射强度的影响,并将LCGD与其他ELCAD的分析性能进行比较。此外,用ICP对LCGD的测试结果进行验证,t检验分析两种结果的差异性。结果表明,当电压从620升高到680 V,发射强度逐渐增大,这是因为电压升高,激发能量增大,单位体积内激发的金属原子增多,激发效率提高。考虑到放电稳定性,选择650 V为最佳放电电压。当流速从2.5增加到4.5 mL·min-1时,发射强度增加,这是由于流速增加导致进入放电区的样品量增加,发射强度增强;流速高于4.5 mL·min-1后,发射强度有下降的趋势,这是由于水荷载的增加引起放电区能量密度降低以及过量水加热消耗了用于激发样品的能量,导致激发能量降低。因此,选择最佳流速为4.5 mL·min-1。pH=1的HNO₃具有较高的激发强度,因而选择pH=1为最佳pH。最佳条件下,Pb和Zn的检出限分别为0.38和0.59 mg·L-1,相对标准偏差分别为0.9%和1.2%,功率低于60 W。实验中的检出限与其他类似方法所测结果有一定差距,这可能与所选谱仪有关。固定激发波长下研究发现,放电过程有较好的稳定性。矿石样品中Pb和Zn的回收率在87.6%~107.4％,LCGD测试结果与ICP基本一致,两种方法基本无显著性差异。与ICP相比,LCGD具有低能耗、高激发效率、小型便携等优点。随着进一步改进,有望开发出可用于实时、在线检测金属元素的微型化仪器。     

Self‐Assembly of Ag6 Clusters into Nanowires for Nonenzymatic Electrochemical Sensing of Glucose

Self‐assembly of metal nanoclusters into 3D ordered superstructures and the exploration of their electrochemical properties are highly significant for fundamental research and practical application. In this study, atomically precise Ag₆(NALC)₅ nanoclusters are successfully synthesized and their structure is determined carefully. It is interesting that the prepared Ag₆(NALC)₅ nanoclusters can be self‐assembled into ultrafine nanowires, long ribbons, and finally 3D porous network in the mixed solution of water and ethanol, which can be attributed to the solvent polarity, static electricity interaction between ligands, and the possible Van der Waals attractions. Such assembly phenomenon lays a foundation for the future fabrication of silver clusters‐based nanodevices. In addition, the synthesized silver nanoclusters can be used for electrochemical sensing of glucose with high detection sensitivity, selectivity, and low limit of detection. This work is expected to be helpful for the synthesis of atomically precise metal nanoclusters and their applications in fabrication of nanodevices for chemical sensors.     

变延迟进动定制激发(DANTE)序列在工程中的优化设计

变延迟进动定制激发（Delays Alternating with Nutation for Tailored Excitation,DANTE）序列作为一种黑血预脉冲序列,通过连续施加小角度激发脉冲,以及结合散相梯度,使得流动物质和静态物质达到不同的稳态,从而抑制流动的血液.对于静态物质而言,施加DANTE序列后在图像等间隔的位置会出现暗条纹,暗条纹的宽度与梯度幅值和小单元持续时间乘积相关：乘积越大,暗纹宽度越小.对于动态物质而言,为达到较好的抑制效果,需要增加整个DANTE序列模块的准备时间,并且增大梯度幅值和小单元持续时间的乘积.因此,该方法对于梯度系统的要求较高,而实际梯度放大器（Gradient Amplifier,GPA）有一定的限额.在有限的GPA条件下,为使得DANTE序列具有更好抑制流动信号效果,本文在读出方向以及片层旋转两个方面进行了梯度优化,实现了更好的黑血效果.