矿物药蒙脱石散EDS指纹图谱双指标等级序列个性化模式识别分析及快速质量评价

矿物药中的多种金属和非金属元素及其含量决定了其功效。目前亟待建立普遍适用的、非化学分析的、以元素种类及其含量信息为基础的多种矿物药快速鉴别及定量质量评价方法。EDS元素指纹图谱可以快速测定各类矿物药的元素种类及含量。双指标等级序列个性化模式识别法则通过比较计算任意两个样品的共有(量)指标率及变异(量)指标率,建立以各个样品为参考的个性化双指标序列,然后再计算每个序列中所有样品的平均共有指标率及其标准偏差S,构造相似尺度函数P≥+xS。确定适合于所有样品最优分类的x和每个样品的个性化的显著相似样品特征序列,将其作为分类标准实现最佳分类。该法不仅适用于仅有共有峰,同时也适用于既存共有峰又有变异峰的指纹图谱的量化分析。测定了七种不同公司生产的蒙脱石散的EDS指纹图谱,计算了不同样品指纹图谱之间峰面积(或主要活性元素Fe,Al,Ca,Mg,Si的含量)的双指标率,当相似尺度x=0.5,可对七种蒙脱石散产品进行高分辨鉴别及准确质量评价。该法为矿物药的快速高分辨鉴别及定量质量评价提供了一种新途径。     

Combined analysis methods for investigating titanium and nickel surface contamination after plasma deep etching

Plasma etching techniques can result in damage and contamination of materials, which, if not removed, can interfere with further processing. Therefore, characterisation of the etched surface is necessary to understand the basic mechanisms involved in the etching process and enable process control and cleaning procedures to be developed. A detailed investigation by means of the combined use of scanning electron microscopy coupled with energy-dispersive X-ray spectrometry (SEM/EDS), X-ray photoelectron spectroscopy (XPS) and optical microscopy (OM) has been carried out on deep titanium trenches etched by plasma. This innovative approach has provided a further insight into the microchemical structure of the surface contamination layer on both the titanium and the nickel hard mask surfaces. The described experiments were conducted on 25 to 100-μm wide trenches, first etched in bulk titanium by an optimised Cl₂/SF₆/O₂-based inductively coupled plasma process, through an electroplated nickel hard mask. The results allow to identify chlorine, fluorine and carbon as the main contaminating agents of the nickel mask and to associate three oxidation states around the etched trenches highlighting certain specific aspects related to the passivation mechanism. These observations reinforce the scientific relevance of the combined use of complementary optical and imaging analytical techniques.     

Characterization of carbon nanotubes and analytical methods for their determination in environmental and biological samples: A review

In the present paper, a critical overview of the most commonly used techniques for the characterization and the determination of carbon nanotubes (CNTs) is given on the basis of 170 references (2000–2014). The analytical techniques used for CNT characterization (including microscopic and diffraction, spectroscopic, thermal and separation techniques) are classified, described, and illustrated with applied examples. Furthermore, the performance of sampling procedures as well as the available methods for the determination of CNTs in real biological and environmental samples are reviewed and discussed according to their analytical characteristics. In addition, future trends and perspectives in this field of work are critically presented.     

Multiple Electron Beam Analyses Applied to Eclogite from the Western Alps

 The occurrence of compositional and microtextural relics within metamorphic rocks can provide useful information on the pressure-temperature history of the host rock. The grain-size of these microstructures, such as coronitic reaction microtextures, is mostly too fine to be detected by optical microscopy. Therefore, a more detailed analytical approach is needed. In this paper multiple electron beam techniques including the acquisition of X-ray multi-element maps, micro and nano-analysis performed by SEM/EDS and TEM/STEM-EDX systems were applied to a specific petrological problem related to metamorphism. Fine-grained decompressional reaction microtextures of an eclogitic sample (Mt. Rosa Nappe, Western Alps) are described and discussed.     

SEM/EDS investigation of one-step flame sprayed and fused Ni-based self-fluxing alloy coatings on steel substrates

Abstract

This study presents the results of light optical and scanning electron microscopy as well as energy dispersive spectroscopy investigation of the Ni-based self-fluxing alloys (NiCrBSi, NiCrWBSi and NiCrBSi + WC) deposited on steel substrates (heat treated carbon steel C45, heat treated low-alloyed steel 42CrMo4 and austenitic stainless steel X6CrNiMo18-10-2) by one-step flame spraying and fusing process. The microstructure of coatings and coating/substrate interface but also the effects of deposition technology on the heat-treated steel substrates which have frequently been used in practice were investigated. The influence of the sample size on the microstructure was also discussed. A proof is given of the change in the structure of coating, coating/substrate interface and substrate due to high fusing temperature, depending on type of steel substrate (and relating thermal properties), coating thickness but also on dimensions of the sample.     

A comparative study on the effects of Co-60 gamma radiation on polypropylene and polyimide

Polypropylene (PP) and polyimide (PI), which belong to entirely different classes of polymers, are irradiated by Co-60 gamma radiation under similar doses and similar conditions in the dose range varying from 57.6 to 230.4 kGy. The radiation responses of these two polymers are analyzed by various characterizations such as Fourier transform infrared, UV–visible, energy-dispersive spectroscopy, X-ray diffraction, scanning electron microscopy and contact angle. PP shows substantial modifications in its structure and properties while in the same dose range, PI shows remarkable stability. These two different responses are interpreted in terms of physicochemical structure and properties of these polymers.     

梧桐木与烟煤混烧的灰分特性分析

通过SEM/EDS分析、X射线衍射分析和灰熔融性实验对梧桐木与烟煤混烧适宜的灰化温度、灰化时间以及混煤灰的灰分特性进行了研究。研究表明,适宜的灰化时间为2 h,灰化温度则根据不同的梧桐木配比分别选取650、700和800 ℃。随着梧桐木配比的升高,混烧灰中SiO₂和Al₂O₃的含量逐渐降低,而K₂O、CaO和MgO的含量逐渐升高,Na₂O和Fe₂O₃含量的变化,整体维持在较低的水平。当梧桐木配比为30%时,混烧灰中出现钙长石的晶相;当配比为50%时,混烧灰中出现钠长石的晶相,同时莫来石晶相消失,且随着温度的升高混煤灰中结晶相的强度减弱。梧桐木灰中高含量的碱性氧化物与硅铝氧化物所生成的低熔点硅铝酸盐是导致梧桐木混煤灰熔点降低的直接原因。     

提高能谱无标样定量分析准确度的参数选择

针对如何提高X射线能谱仪(EDS)无标样定量分析的准确度,进行了一系列实验研究和理论分析.讨论了样品制样的基本要求,能谱分析过程中加速电压、收集时间和分析区域等方面对能谱分析结果的影响及其最佳的选择参数,如对于轻元素分析应采用较低电压、分析时间过长可能导致样品在电子束轰击下引起更大碳沉积等,通过合理的参数选择均能得到较为满意的分析结果,提高了定量测试的准确度.     

Spectroscopic study of decontaminated corroded carbon steel surfaces

Removal of uranium from contaminated carbon steel surfaces by chelation with hydroxycarboxylic acid has been tested as a cleaning process for decommissioning and decontaminating contaminated surfaces. Comparison of contaminated surfaces prior to decontamination with subsequently cleaned surfaces was done in order to study the effectiveness of this cleaning technique. This was accomplished using various spectroscopic techniques, including x‐ray photoelectron spectroscopy, synchrotron infrared microspectroscopy, Rutherford backscattering spectroscopy and scanning electron microscopy/energy‐dispersive spectroscopy. Mild carbon steel (1010) coupons were exposed to uranyl nitrate solution, which led to the formation of a lightly corroded surface. Some contaminated samples underwent further cyclic humidity treatment, during which additional corrosion took place. In this study, it was found that a citric acid–hydrogen peroxide–citric acid cleaning method successfully removed uranium in lightly corroded areas. However, the method but incompletely decontaminated some heavily corroded areas where more highly crystallized corrosion products are found or where complex surface structure can occlude contaminants. Use of complementary analytical techniques is essential to provide an accurate model of surface chemistry before and after decontamination. Copyright © 2004 John Wiley & Sons, Ltd.     

Effect of annealing temperature on photoelectrochemical properties of nanocrystalline MoBi2(Se0.5Te0.5)5 thin films

Nanocrystalline MoBi₂(Se_0.5Te_0.5)₅ thermoelectric thin films have been deposited on ultrasonically cleaned glass and FTO-coated glass substrates by Arrested Precipitation Technique. The change in properties of MoBi₂(Se_0.5Te_0.5)₅ thin films were examined after annealing at the temperature 473 K for 3 h. The structural, morphological, compositional and electrical properties of thin films were characterized by X-ray Diffraction, Scanning Electron Microscopy, Energy Dispersive Spectroscopy, etc. Thermoelectric properties of the thin films have been evaluated by measurements of electrical conductivity and Seebeck coefficient in the temperature range 300–500 K. Our aim is to investigate the effect of annealing on behaviour of MoBi₂(Se_0.5Te_0.5)₅ thin films along with photoelectrochemical properties.