激光诱导击穿光谱法对钢中夹杂物类型的表征

激光诱导击穿光谱( LIBS)不仅可以对材料整体成分进行分析,还可进行微区及成分分布分析。本实验采用激光诱导击穿光谱对两牌号钢铁样品进行扫描分析,尝试对34CrNiMo6钢中的MnS夹杂物和重轨钢中的Si-Al-Ca-Mg复合夹杂物进行表征。结果表明,34CrNiMo6钢中元素信号的二维强度分布及元素通道合成后,个别位置Mn及S两元素的信号强度同时异常高,可确定试样中存在较多MnS夹杂物;重轨钢中元素的二维强度分布及元素通道合成后,个别位置Si、Ca、Mg及Al元素的信号同时异常高,可确定试样中存在Si-Al-Ca-Mg复合夹杂物。采用扫描电子显微镜/能谱法( SEM/EDS)对上述样品中夹杂物的对比分析结果表明,两种方法对夹杂物类型的判定结果一致。     

Classification of the distribution of trace impurities by spark source mass spectrometry analysis

Spark source mass spectrometry in combination with principal component analysis and clustering analysis was used to investigate the trace element distributions in metallic samples. The analysis of Zn and Cu samples and a comparison with direct imaging secondary ion microscopy demonstrated the consistency of the approach.On leave from Department of Chemistry, Nanjing Normal University, Nanjing, People's Republic of China.     

Hard X-ray micro-spectroscopy at Berliner Elektronenspeicherring für Synchrotronstrahlung II

The capabilities of the X-ray beamlines at Berliner Elektronenspeicherring für Synchrotronstrahlung II (BESSY II) for hard X-ray measurements with micro- and nanometer spatial resolution are reviewed. The micro-X-ray fluorescence analysis (micro-XRF), micro-extended X-ray absorption fine structure (micro-EXAFS), micro-X-ray absorption near-edge structure (micro-XANES) as well as X-ray standing wave technique (XSW), X-ray beam induced current (XBIC) in combination with micro-XRF and micro-diffraction as powerful methods for organic and inorganic sample characterization with synchrotron radiation are discussed. Mono and polycapillary optical systems were used for fine X-ray focusing down to 1 µm spot size with monochromatic and white synchrotron radiation. Polycapillary based confocal detection was applied for depth-resolved micro-XRF analysis with a volume resolution down to 3.4 · 10^− 6 mm³. Standing wave excitation in waveguides was also applied to nano-EXAFS measurements with depth resolution on the order of 1 nm. Several examples of the methods and its applications in material research, biological investigations and metal-semiconductor interfaces analysis are given.     

Image processing in secondary ion mass spectrometry

The application of image processing in secondary ion mass spectrometry is discussed. The Cameca 4f SIMS uses a single microchannel plate and a highly sensitive camera in combination with an image processor with real time capabilities (Kontron IBAS). An automation procedure with image integration, extended dynamic range image acquisition and retro depth profiling is presented and illustrated with practical applications.     

青铜生锈过程中铜元素的扩散—CuCl的作用

采用扫描电镜、电子探针微区分析、微区Ｘ射线衍射及Ｘ光荧光光谱等仪器分析手段，对一块被粉状锈（主要成分为Ｃｕ２（ＯＨ）３Ｃｌ）严重腐蚀的东汉青铜镜残片进行元素和结构的分区分析。剖面分析表明，青铜合金在浇铸过程中的偏析作用是造成其电化学腐蚀的内在因素；铜锈的生成是分步进行的；氯元素对合金的侵蚀由表面直至基体深部；生锈过程中铜元素从合金内部向表面外扩散。运用相平衡理论、电化学腐蚀原理及化学热力学对青铜器     

Quantitative microbeam analysis of particles

The ability to characterize individual microscopic particles is important in many areas of science and technology. A variety of microbeam analysis methods are capable of providing information on microscopic particles. With electron probe X-ray microanalysis quantitative analysis is possible under well controlled conditions. Using computer controlled electron microscopes it is feasible to characterize a large number of individual particles. The application of this technique requires the use of multivariate data analysis procedures for the interpretation of the large amount of data obtained.     

微量法测定有机锡化合物中锡的含量

随着金属有机化学的不断发展,金属有机化合物中金属元素的分析显得日益重要。本微量法是用混合酸快速分解有机锡化合物,以EDTA络合剂和四价锡离子所生成的稳定的Sn~(+4)-EDTA络合物为依据,其过量的EDTA,用Pb(NO_3)_2、CuSO_4、ZnAc_2或La(NO_3)_3为滴定剂进行回滴,均得到准确的分析结果。此方法简单、快速、极易掌握操作技术;滴定     

激光扫描成像的纳米分辨技术

阐述一种新型激光近场扫成像系统──光子扫描隧道显微镜的实验成像显示技术。利用本系统对多种光学表面、聚合物、生物病毒等透光样品进行三维显微成像分析，获得了样品表面结构的纳米级空间化辨。     

单柱离子色谱的研究-有机化合物中氯,溴元素的微量分析

本文介绍用单柱离子色谱法对有机化合物中氯和溴进行微量分析。样品经氧瓶法燃烧分解,被吸收于含双氧水的苯二甲酸氢钾溶液中的Cl-和Br-,可在单柱离子色谱的分离柱上得到分离,然后用电导检测器检测,用峰面积积分进行定量。本法简便、快速,可同时测定氯、溴两种元素。分析标准偏差分别为±0.39%和±0.59%。