钼的分析进展

评述了 1991～ 2 0 0 3年间国内有关钼的分析技术现状及进展概况。包括了化学分离和化学分析、光度分析、原子光谱分析、电化学分析等 ,引用文献 16 1篇     

Use of the ion microanalyzer for the characterization of bulk and epitaxial silicon and gallium arsenide

The ion microanalyzer permits a localized mass spectrometric analysis, i.e. the qualitative and quantitative analysis of the impurities contained in a small selected volume. This procedure makes possible the analysis of very thin epitaxial layers (for example silicon and gallium arsenide). As regards qualitative analysis, the apparatus is designed for the selection of ions. After the recording and analysis of the ion spectrum, a large number of the impurities present in the sample are determined qualitatively. Quantitative analysis can be performed with the equipment, but this requires the analysis of a homogeneous standard sample previously dosed by spark-source mass spectrometry. The quantitative analysis of bulk and epitaxial silicon and gallium arsenide is described and the limits of detection of the principal impurities are given. It is also shown how the possibility of localized analysis was exploited. A correlation was established between the existing impurities and the chemically revealed crystal imperfections. A comparative analysis of the distribution of the impurities in the epitaxial layers was also carried out. The periodic analysis of epitaxial layers makes it possible to follow the deterioration by contamination, if any, under the epitaxial conditions, and to improve the sample quality.     

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.     

钛粉质量鉴定新方法试验研究

钛粉质量鉴定一直是用化学分析测定全钛含量，而不能确定单质态的钛含量，实验表明用Ｘ射线衍射分析鉴定钛粉质量效果较好，避名了化学分析的缺点，是一种值得推广的鉴定方法。     

Effects of molecular structure parameters on ring-opening reaction of benzoxazines

A colorless monoclinic crystal of dichloro-benzoxazine was obtained and examined by single crystal X-ray diffraction analysis. At the same time, molecular modeling analysis of nine benzoxazine compounds with different substituting groups was performed. Both single crystal X-ray diffraction analysis and molecular modeling analysis provide a detailed picture of molecular structure on molecular level and show good consistence with each other. On the basis of structural analysis, the effects of molecular structure parameters on ring-opening polymerization of ben-zoxazines have been explored.     

Application of comprehensive two-dimensional gas chromatography mass spectrometry and different types of data analysis for the investigation of cigarette particulate matter

In tobacco research, the comparison of different tobacco blends as well as the puff-dependent behaviour of cigarettes is a matter of particular interest. For the investigation of smoke characteristics, GC x GC offers different ways for data analysis, namely, compound target analysis, automated peak-based compound classification and comprehensive pixel-based data analysis. This study will show the application as well as the pros and cons of these types of data analysis for very complex matrices like cigarette particulate matter. In addition, new aspects about the recently discovered puff-dependent behaviour of compounds in cigarette smoke will be presented. Automated peak-based compound classification including mass spectrometric pattern recognition is used for the classification of tobacco particulate matter samples and the puff-dependent investigation of different compound classes. This compound group specific analysis is further reinforced by applying an even more comprehensive pixel-based analysis. This kind of analysis is used to generate fingerprints of different types of cigarettes. The combination of fast feature reduction methods like analysis of variance (ANOVA) and t-test with multivariate feature transformation methods like partial least squares discriminate analysis (PLSDA) for feature selection provides a powerful tool for a detailed inspection of different types of cigarettes.     

The use of micro-thermal analysis as a means of in situ characterisation of a pharmaceutical tablet coat

The technique of micro-thermal analysis (MTA) has been applied to a commercial sugar coated ibuprofen tablet in order to identify the ability of the method to differentiate between the coat and the tablet core and to characterise the thermal properties of both components using localised thermal analysis. Thermal conductivity measurements in conjunction with intensity histogram analysis indicated that differentiation across the coat/core interface was possible, with a bimodal distribution of pixel intensities corresponding to thermal conductivity noted. Localised thermal analysis studies indicated that the bulk response was dominated by the incorporated ibuprofen, with a discontinuity seen at ca. 70–80°C, corresponding to the published melting point of the drug. The coat showed a discontinuity at ca. 220°C that may be reasonably ascribed to the melting process. It was also noted that the coat showed a small discontinuity at a temperature corresponding to the melting of ibuprofen. In summary, the technique was shown to be capable of identifying the core/coat interface using thermal conductivity measurements, while localised thermal analysis experiments enable the operator to perform thermal analysis experiments on the individual components in situ.     

Electroanalytical study of fluvoxamine

Fluvoxamine (FVX) can be reduced at a mercury-drop electrode, with a maximum peak current intensity being obtained at a potential of –0.7 V vs. Ag/AgCl, in an aqueous electrolyte solution of pH 2. The compound was determined in a pharmaceutical product and in spiked human serum by square-wave adsorptive-stripping voltammetry (SWAdSV) after accumulation at the electrode surface, under batch conditions. Because the presence of dissolved oxygen did not interfere significantly with the analysis, it was also possible to determine FVX in the pharmaceutical product by use of a flow-injection analysis (FIA) system with SWAdSV detection. The methods developed were validated and successfully applied to the quantification of FVX in a pharmaceutical product. Recoveries between 76 and 89% were obtained in serum analysis. The FIA–SWAdSV method enabled analysis of up to 120 samples per hour at reduced cost, implying the possibility of competing with the chromatographic methods usually used for this analysis.     

Voltammetric analysis of drugs

A review on the voltammetric analysis of drugs is presented. The review includes a summary of the rules that must be considered for drug analysis and a survey of the use of voltammetry for drug analysis in the period from 1998 till 2002.     

Determination of wheat quality by mass spectrometry and multivariate data analysis

Multivariate analysis has been applied as support to proteome analysis in order to implement an easier and faster way of data handling based on separation by matrix-assisted laser desorption/ionisation time-of-flight mass spectrometry. The characterisation phase in proteome analysis by means of simple visual inspection is a demanding process and also insecure because subjectivity is the controlling element. Multivariate analysis offers, to a considerable extent, objectivity and must therefore be regarded as a neutral way to evaluate results obtained by proteome analysis.Proteome analysis of storage proteins from the wheat gluten complex based on two-dimensional electrophoresis and analysis of the N-terminal sequence has revealed a protein homologous to gamma-gliadins, tentatively associated with quality and within the molecular weight range 27-35 kDa. Further examinations of gliadin data based on mass spectrometry revealed that quality among wheat varieties could be determined by means of principal component analysis. Further examinations by interval partial least squares made it possible to encircle an overall optimal molecular weight interval from 31.5 to 33.7 kDa. The use of multivariate analysis on data from mass spectrometry has thus shown to be a promising technique to minimize the number of two-dimensional gels within the field of proteome analysis.     

Analysis of biological motors via multidimensional fractionation: a strategy

Past strategies for the analysis of ATP-fueled motors include single-motor analysis. Single-motor analysis bypasses limitations caused by motor asynchrony during the traditional ensemble averaging analysis. The present communication describes revised ensemble averaging analysis that also can bypass asynchrony-derived limitations. This revised analysis makes measurements of one motor variable dependent on the others. One example is nondenaturing gel electrophoresis with more than one dimension. Each dimension measures one of the motor variables. This multidimensional procedure is used to obtain the values of "conformational" motor variables as a function of a "clock" motor variable. In theory, the cycle of the motor can be analyzed from a single multidimensional analysis of a collection of asynchronous motors sampled at only one time. That is to say, motor asynchrony becomes an asset, rather than a liability.     

DNA片段的质谱试验中各相关因素的影响分析

利用DNA片断的质谱试验数据,通过分析各相关因素对质谱响应值的影响度,确定了灰色关联分析方法应用于本试验的可行性。并对灰色关联分析、相关分析和回归分析的结果做了比较。结果表明在DNA片段的质谱试验中,应用灰色关联分析能得到满意的分析结果,它克服了相关分析和回归分析等对数据量的要求,是在类似试验中最适合的分析方法。     

Historical review on research of kinetics in thermal analysis and thermal endurance of electrical insulating materials

Thermal analysis techniques, such as thermogravimetry, differential thermal analysis and evolved gas analysis, have been applied to thermal endurance evaluation of electrical insulating materials of high polymers, which are used for a long time at a relatively high operating temperature. Various attempts have been made to estimate the life time of the materials at the operating temperature by thermal analysis and a calorimetric method. These are critically described in this review paper.     

A review of the analysis and characterisation of polymeric glass fibre sizings

Glass fibre reinforcements form the backbone of a composites industry. Possibly the most critical component involved in the manufacture of glass fibres and their composites is the fibre sizing. Yet because of the intense level of secrecy surrounding size formulations there are few who have more than a superficial understanding of sizings. Composite developers and researchers have a growing need for practical tools which can assist with the understanding of the nature and role of sizings on the glass fibres which reinforce their composites. This work reviews some of the most relevant articles from the widely dispersed literature around the analysis and characterisation of these polymeric sizings. The review covers the analysis and characterisation of the polymeric sizing layer on the glass fibre surface using high vacuum surface analysis techniques, thermal analysis, atomic force microscopy based techniques, surface energy analysis, infrared methods, and combined multiple analysis techniques. The conclusions highlight the fragmented nature of the knowledge base on sizings and the lack of reliable and reproducible reference materials on which to build real progress in the understanding of this critical technology.     

Non-parametric multivariate analysis of variance in the proteomic response of potato to drought stress

Spot detection is a mandatory step in all available software packages dedicated to the analysis of 2D gel images. As the majority of spots do not represent individual proteins, spot detection can obscure the results of data analysis significantly. This problem can be overcome by a pixel-level analysis of 2D images.     

An improvement of window factor analysis for resolution of noisy HPLC-DAD data

Window factor analysis (WFA) is a powerful tool in analyzing evolutionary process. However, it was found that window factor analysis is much sensitive to the noise involved in original data matrix. An error analysis was done with the fact that the concentration profiles resolved by the conventional window factor analysis are easily distorted by the noise reserved by the abstract factor analysis (AFA), and a modified algorithm for window factor analysis was proposed. Both simulated and experimental HPLC-DAD data were investigated by the conventional and the improved methods. Results show that the improved method can yield less noise-distorted concentration profiles than the conventional method, and the ability for resolution of noisy data sets can be greatly enhanced.     

Application of Grey-correlated Spectral Region Selection in Analysis of Near-infrared Spectra

The optimal selection method of spectral region based on the grey correlation analysis was applied in the analysis of near-infrared(NIR) spectra. In order to compute “characteristic” spectral region, 160 samples of tobacco were surveyed by NIR. Next, the whole spectral region was randomly divided into six regions, and the values of association coefficients and correlation orders of different regions were computed for total sugar, reducing sugar and nicotine. Moreover, two regions that owned the largest value of association coefficient were regarded as “characteristic” spectral region of a model. Finally, the quantitative analysis models of different components were established via the partial least squares method, and the common selection methods of spectral region were compared. The simulation results indicate that the models to choose the spectral region based on grey correlation analysis are more effective than the common selection methods of spectral region, the optimized time of algorithm is shorter, the prediction precision of the models is higher and generalization ability for quantitative analysis results is stronger. This research can provide the support for the quantitative analysis models of NIR spectra and new idea for commercial analysis software of NIR. So, it has a high application value in the analysis of NIR spectra.     

Relaxation mode analysis of a peptide system: comparison with principal component analysis

This article reports the first attempt to apply the relaxation mode analysis method to a simulation of a biomolecular system. In biomolecular systems, the principal component analysis is a well-known method for analyzing the static properties of fluctuations of structures obtained by a simulation and classifying the structures into some groups. On the other hand, the relaxation mode analysis has been used to analyze the dynamic properties of homopolymer systems. In this article, a long Monte Carlo simulation of Met-enkephalin in gas phase has been performed. The results are analyzed by the principal component analysis and relaxation mode analysis methods. We compare the results of both methods and show the effectiveness of the relaxation mode analysis.     

毛细管电泳用于药物分析的研究进展

药物分析是毛细管电泳（CE）的重要应用领域,所有CE分离模式与检测方法都在各种药物及其不同形式样品的分离分析中显示出特色和应用能力。该文从药品分析领域中的小分子药物（包括手性药物）及其有关物质、中药与天然产物、体内药物分析、生物制品药物分析等几个方面,综述了近几年CE在这些传统药物分析领域应用的研究进展。限于篇幅,未包括现代药物分析研究比较活跃的理化常数测定、亲和毛细管电泳与结合常数研究（药物与受体间的相互作用等）、临床生物标志物分析、代谢组学和微流控芯片CE分析等方面的内容。根据目前传统药物分析领域的发展,该文关注到近期CE在顺应药物分析的法规需求、电容耦合非接触电导检测（CE-C⁴ D）、改进检测灵敏度与精密度、CE-十二烷基硫酸钠（SDS）毛细管电泳、全柱成像毛细管等电聚焦（icIEF）、抗体分析等方面的新进展。该文结合文献,讨论了目前传统药物分析领域的需求,以及CE在其中的地位、挑战和机遇。对目前CE主要作为互补分析方法在化学药和中药分析中的应用研究提出了一些针对性的建议,期待CE在生物制品分析中的特色和能力得到进一步的发挥,同时提出CE-MS和对CE分析重复性改进等新进展可能对未来CE应用领域的大幅度扩展。该综述主要涉及近3年（2017年1月到2020年2月）及部分2016年的相关文献。     

Determination of vanadium in high grade carbons by radioanalytical methods

The present work deals with the determination of vanadium in high grade carbons by three radioanalytical methods, viz. thermal neutron activation analysis with an accelerator, thermal neutron activation analysis with a reactor and proton induced X-ray emission analysis with an accelerator. It is cleared from this study that thermal neutron activation with an accelerator is more convenient for the rapid and non-destructive analysis of ppm-level vanadium in bulk carbons than thermal neutron activation analysis with a reactor. Proton induced X-ray emission is less useful for the analysis of bulk samples.