State-of-the-art in analytical characterization of high purity solid samples by different spectroscopic methods

Facilities and some results of several spectroscopic methods which have potential applications in the field of analysis of solid high purity substances and which have been elaborated in Russia, will be discussed in this paper. Laser nondispersive atomic fluorescence method with glow discharge cathode sputtering atomiser, may be used for trace element determination as well as a tool for the investigation of technological processes, viz. deposition of thin films. Investigations on reduction of a background level in the new hollow cathode ion source for mass-spectrometry have been carried out. Laser mass spectrometry with tandem laser mass reflectron is successfully designed and applied for gaseous impurities determination in high pure silicon with limit of detection of 10⁻³–10⁻⁵ ppm wt. Several results of the layer-by-layer and bulk trace analysis of solids by high resolution mass spectrometry with radio frequency powered glow discharge ion source with the limits of detection at 10⁻¹–10⁻³ ppm wt will be presented here. The traditional arc and spark emission technique still finds considerable use. One of the examples considered in the paper is the analysis of metalfullerenes. To overcome the calibration problem the fluorination process inside the electrode crater using zinc fluoride has been investigated.     

A characterization of stiffly stable linear multistep methods

A theorem expressing geometric conditions necessary and sufficient for the stiff stability of a linear multistep method is obtained. A corollary to this theorem provides sufficient conditions for stiff stability, for the class of algorithms characterized by a single essential root. By applying the Schur-Cohn criterion and employing a computerized algebraic manipulation program, the result provides a first step towards an exhaustive search technique for determining a continuum of members of this class.     

Field screening test methods: performance criteria and performance characteristics

Field-portable test methods may be quantitative, semi-quantitative, or qualitative and screening methods are often used in the field to determine if the concentration of a toxic substance exceeds regulatory or recommended standards or action levels. For on-site analysis, accurate quantitative tests for field measurements may not be available, depending on the analyte(s) or specific field situation. Thus, in lieu of more definitive test methods, screening tests which are based on qualitative or semi-quantitative methods are often used for making immediate decisions in the field, e.g. for compliance or risk assessment. Also, quantitative methods may be used for screening purposes in many instances. To ensure the quality of these screening tests and the decisions that are made based upon their results, screening methods need to be evaluated with sufficient data and should meet basic performance criteria prior to their being employed for decision-making purposes. Although quantitative, semi-quantitative and qualitative methods demonstrate different characteristics, it is desired that the performance criteria for all three method categories be consistent. If there is consistency, then one can have a sound basis for selecting the most appropriate test(s) for a given application. In order to unify the performance criteria for the different types of methods, a performance function is used to characterise both qualitative and semi-quantitative methods; in turn, this performance function is related to that for quantitative methods. False negative rates, false positive rates, sensitivity and specificity are key characteristics of screening methods that can be determined from the pertinent performance curves. The performance characteristics of each method are related to the uncertainty region that is associated with each method and the applicable uncertainty regions can be gleaned from the performance curves. Also, various options for using multiple test results to improve decisions based on test results are provided.     

Raman spectra of biological samples: A study of preprocessing methods

In this study preprocessing of Raman spectra of different biological samples has been studied, and their effect on the ability to extract robust and quantitative information has been evaluated. Four data sets of Raman spectra were chosen in order to cover different aspects of biological Raman spectra, and the samples constituted salmon oils, juice samples, salmon meat, and mixtures of fat, protein, and water. A range of frequently used preprocessing methods, as well as combinations of different methods, was evaluated. Different aspects of regression results obtained from partial least squares regression (PLSR) were used as indicators for comparing the effect of different preprocessing methods. The results, as expected, suggest that baseline correction methods should be performed in advance of normalization methods. By performing total intensity normalization after adequate baseline correction, robust calibration models were obtained for all data sets. Combination methods like standard normal variate (SNV), multiplicative signal correction (MSC), and extended multiplicative signal correction (EMSC) in their basic form were not able to handle the baseline features present in several of the data sets, and these methods thus provide no additional benefits compared to the approach of baseline correction in advance of total intensity normalization. EMSC provides additional possibilities that require further investigation.     

Validation of analytical methods using a regression procedure

The evaluation and validation of analytical methods and instruments require comparison studies using sample material for testing accuracy and precision. In analytical chemistry, the commonly accepted means of analyzing data from method comparison studies is least-squares regression analysis, a model which has limitations. In this paper, the results from ordinary least-squares and many other regression approaches recommended in the literature were compared with a new regression procedure that takes into account the errors in both variables (methods). After a discussion of the properties of the regression procedure, recommendations are given for carrying out a method comparison study using informational analysis of variance. The efficiency of the regression procedure proposed is demonstrated by applying it to different data sets from published literature.     

Evaluation of WEDM performance characteristics of Inconel 706 for turbine disk application

Inconel 706 is a newly developed superalloy, which offers high mechanical strength alongwith easy fabricability thus making it suitable for turbine disk applications. Although Inconel 706 exhibits a substantial increase in stress rupture and tensile yield strength compared to other superalloys, its conventional machining yields poor surface finish and low dimensional accuracy of the machined components. Hence, wire electrical discharge machining (WEDM) of Inconel 706 has been performed and various performance attributes such as material removal rate (MRR), surface roughness (SR), recast surface, topography, microhardness, microstructural and metallurgical changes of the machined components have been evaluated. The experimental results revealed that servo voltage, pulse on time, and pulse off time greatly influence the MRR and SR. Due to high toughness of Inconel 706, no micro cracks were observed on the machined surface. Micro voids and micro globules are significantly reduced at low pulse on time and high servo voltage. But, there is a propensity of thick recast layer formation at high pulse on time and low servo voltage. EDAX analysis of recast surface exposed the existence of Cu and Zn which have migrated from the brass wire. The subsurface microhardness was changed to 80 μm due to significant thermal degradation.     

橡胶防老剂RD不同分析方法的比较

为比较橡胶防老剂RD(TMQ 2,2,4-三甲基-1,2-二氢化喹啉聚合体(C12H15N)n(n=2～4))高效液相色溶剂梯度洗脱的方法和GC-Ms高温裂解方法测定聚合物的含量,采用高效液相色谱法,以水-甲醇作为流动相,检测波长254nm,流速为1mL/min,C18 4.6mm×150mm/5μm色谱柱;GC-Ms法的热分解温度590℃,分解时间6s,热分解室温度为320℃,注射温度250℃,色谱柱DB-1 30mm×0.32mm×0.25μm,升温速度10℃/min,终温为120℃。载气N2流速为1mL/min,FID检测温度280℃,H2流速为30mL/min,空气流速为300mL/min;面积归一法计算含量。结果表明,高效液相色谱法比气相色谱法稳定、可靠,高效液相色谱法测定橡胶防老剂RD的含量优于气相色谱法。     

Evaluation of specific absorbed fractions from internal photon sources in ORNL analytical adult phantom

To design a diagnostic or therapeutic irradiation programme, there is a need to estimate the absorbed dose. In this investigation, specific absorbed fractions (SAFs) were calculated based on Cristy and Eckerman's analytical adult phantom, by MCNP4C Monte Carlo code. SAFs were estimated with uncertainty <3%, for about 600 source organ-target organ pairs at 12 photon energies (these data are available at http://www.um.ac.ir/~mirihakim). Then these results were compared with Cristy and Eckerman's, which were based on direct Monte Carlo, reciprocity principle and point source kernel methods. Also, agreements and disagreements between them for different states were discussed.     

Knowledge representation for the selection of methods in analytical chemistry

Expert systems are gaining rapidly in importance in several areas of science, and in chemistry in particular. One of the most important factors that determines the success of an expert system is the representation of the knowledge. To understand better the suitability of the different knowledge representation techniques for the selection of methods in analytical chemistry, a test knowledge base was developed for the high-performance liquid chromatographic analysis of pharmaceutical compounds. This knowledge base has been used to study which features of knowledge representation are necessary to describe analytical chemical knowledge in a natural and efficient way. It is concluded that no single representation method is optimal. A combination of production rules and frame structures seems to be much more suitable. The possibility of consulting external databases and programs is also a very important aspect.     

Study of composite patch repair by analytical and numerical methods

A combined analytical and numerical study of an isotropic cracked plate that was repaired by using a bonded composite patch was conducted. The analytical work was based on Rose's equations, whereas for the numerical investigation a three-dimensional finite element analysis was implemented. A number of cracked plates with different crack lengths and overall dimensions of the composite repair were considered. The composite patch was made of unidirectional laminates with different stacking sequences. Both, one- and two-sided patches were analysed. Results are presented for the stress intensity factor in the patched crack and the maximum stress reinforcement stress and adhesive strain. It was found that for the case of a two-sided reinforcement the results obtained by both methods were in good agreement. However, for the case of a single reinforcement the accuracy of the analytical method decreased due to the tendency to out-of-plane bending as a result of bonding a reinforcing patch to only one face of a plate, which is ignored in the analysis.     

A study on the performance of natural neighbour‐based Galerkin methods

In this paper we address the problem of improving natural element simulations in terms of computational cost. Several problems are discussed, that include an efficient natural neighbour search algorithm and a comparison of different natural neighbour‐based interpolation algorithms. In particular, we review the so‐called pseudo‐NEM, a moving least squares‐like approximation scheme that employs natural neighbours, and compare it with traditional Sibson and Laplace interpolation schemes in terms of both accuracy and computational cost. Some examples in linear Elasticity and visco‐plasticity are analysed in order to test the proposed schemes in engineering problems. Copyright © 2007 John Wiley & Sons, Ltd.     

BJMOSFET 静态特性的解析模型及模拟分析

建立了新型半导体功率器件－双极型压控晶体管（BJMOSFET）的直流解析模型,通过提取模型参数,运用电路模拟软件PSPICE的多瞬态分析法对BJMOSFET的直流特性进行了模拟,分析得出这种新型器件在相同结构参数和同等外界条件下与传统MOSFET相比,电流密度提高30％－40％。     

Evaluation of activation energy in sintered samples

The neck curvature obtained in sintering two spherical particles is related to the neck radius of the contact area and the radius of the particles. The radius of the neck curvature, when expressed in terms of the fractional shrinkage, leads to an elegant method of evaluating the activation energy corresponding to the operating mechanism at different stages of sintering. The calculated values of activation energy confirm the diffusion mechanisms operative at different temperatures and different sintering durations.     

Evaluation and optimization of the optical performance of low-concentrating dielectric compound parabolic concentrator using ray-tracing methods

We present a detailed design concept and optical performance evaluation of stationary dielectric asymmetric compound parabolic concentrators (DiACPCs) using ray-tracing methods. Three DiACPC designs, DiACPC-55, DiACPC-66, and DiACPC-77, of acceptance half-angles (0° and 55°), (0° and 66°), and (0° and 77°), respectively, are designed in order to optimize the concentrator for building fa?ade photovoltaic applications in northern latitudes (>55 °N). The dielectric concentrator profiles have been realized via truncation of the complete compound parabolic concentrator profiles to achieve a geometric concentration ratio of 2.82. Ray-tracing simulation results show that all rays entering the designed concentrators within the acceptance half-angle range can be collected without escaping from the parabolic sides and aperture. The maximum optical efficiency of the designed concentrators is found to be 83%, which tends to decrease with the increase in incidence angle. The intensity is found to be distributed at the receiver (solar cell) area in an inhomogeneous pattern for a wide range of incident angles of direct solar irradiance with high-intensity peaks at certain points of the receiver. However, peaks become more intense for the irradiation incident close to the extreme acceptance angles, shifting the peaks to the edge of the receiver. Energy flux distribution at the receiver for diffuse radiation is found to be homogeneous within ±12% with an average intensity of 520 W/m2.