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21.
《Surface and interface analysis : SIA》2005,37(7):589-607
The accuracy of quantitative XPS analysis can be improved using predetermined transmission functions. Two different calibration methods are used for estimating the transmission function T(E) of a photoelectron spectrometer, applying a survey spectra approach (SSA) and a quantified peak‐area approach (QPA) to minimize the quantification error. For the SSA method, Au, Ag and Cu spectra measured with the Metrology Spectrometer II have been used. The new QPA method was built up from Au 4f, Au 4d, Au 4p3/2, Ag 3d, Ag 3p3/2, Cu 3p, Cu 2p3/2, Ge 3p and Ge 2p3/2 standard peak areas, applying adequate ionization cross‐sections and mean free path lengths for different pass energies (10 and 50 eV), lens modes (large area, large area XL, small area 150) and x‐ray sources (Al/Mg Twin and Al Mono). In the energy range 200–1500 eV a transmission function T(E) = a0 + b1E (where a0, b1 and b2 are variable parameters) was found to give an appropriate approximation for eight tested spectrometer settings, implementing the largest changes in the case of pass energy variations. Determination and application of the transmission functions were integrated in the XPS analysis software (UNIFIT 2004) and tested by means of an Ni90Cr10 alloy. The results demonstrate the practicability of the SSA and QPA methods, giving decreased errors of <8% in comparison with errors up to 38% obtained using Wagner's sensitivity factors. Copyright © 2005 John Wiley & Sons, Ltd. 相似文献
22.
Two different spectrofluorimetric methods for the determination of piroxicam (PX) in serum are presented and discussed. One of them is based on the use of three-way fluorescence data and multivariate calibration performed with parallel factor analysis (PARAFAC) and self-weighted alternating trilinear decomposition (SWATLD). This methodology exploits the so-called second-order advantage of the three-way data, allowing to obtain the concentration of the studied analyte in the presence of any number of uncalibrated (serum) components. The method was developed following two different procedures: internal standard addition and external calibration with standard solutions, which were compared and discussed. The second approach investigated is based on the combination of solid-phase extraction (SPE) and room temperature fluorimetry. Both methods here presented yield satisfactory results. The concentration range in which PX could be determined in serum was 1–10 μg ml−1. The limits of quantification for the experimental solutions using the chemometric approach were 0.09 μg ml−1 for the standard addition mode and 0.12 μg ml−1 using external calibration (both for PARAFAC and SWATLD algorithms). In the solid-surface fluorimetric method, the calibration graph was linear up to 0.22 μg ml−1 and the limit of quantification was 0.02 μg ml−1. 相似文献
23.
Martí MP Pino J Boqué R Busto O Guasch J 《Analytical and bioanalytical chemistry》2005,382(2):440-443
The aromatic composition of sugar cane spirits and, in general, of alcoholic beverages, is mainly influenced by the ageing process in wood barrels. There are several factors that affect the quality of the final aged product, but the time of the storage in the barrel is perhaps the most important one. Ageing time must therefore be controlled in order to detect counterfeits; however, this parameter is very difficult to control and, at present, there is no analytical method available to determine it. We propose a quantitative method for determining the ageing time of sugar cane spirits in oak barrels by using an electronic nose based on coupling directly a headspace sampler to a mass spectrometer (HS-MS), and multivariate calibration. The method developed is simple and provides, in 5 min, the ageing time of spirits with an accuracy of about 1 month. 相似文献
24.
A new approach to calculating the equilibrium characteristics of the adsorption of noble gases on the amorphous surfaces of
adsorbents was developed and applied to the Ar−TiO2(rutile) system. Intermolecular adsorbate-adsorbate interactions are taken into account for the nearest neighbors in the quasi-chemical
approximation. The lattice energy parameters of all interactions of the model are determined from the Lennard-Jones potential
(12-6). The formation of amorphous TiO2(rutile) surface includes completion of the surface layers and partial removal of the surface oxygen ions. The quality of
the amorphization procedure was confirmed by the experimentally measured heats and isotherms of adsorption of the system under
study.
Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 6, pp. 1109–1118, June, 1997. 相似文献
25.
Hydrolytic degradation of cellulose was shown to take place during the activation procedure in distilled water during the dissolution procedure of cellulose samples from papers for size-exclusion chromatography analyses in the lithium chloride-N,N-dimethylacetamide (DMAc) solution system. The use of dilute aqueous sodium hydroxide solution in the activation procedure prevents hydrolytic degradation of cellulose during the dissolution procedure, especially in the case of samples of aged papers with low pH. The use of the freeze-drying technique provides samples of cellulose ready-made for dissolution in lithium chloride-N,N-dimethylacetamide solution. 相似文献
26.
In this paper, a novel exact fixed-node quantum Monte Carlo (EFNQMC) algorithm was proposed, which is a self-optimizing and self-improving procedure. In contrast to the previous EFN-QMC method, the importance function of this method is optimized synchronistically in the diffusion procedure, but not be-fore beginning the EFNQMC computation. In order to optimize the importance function, the improved steepest descent tech-nique is used, in which the step size is automatically adjustable.The procedure is quasi-Newton type and converges super linear-ly. The present method also uses a novel trial function, which has correct electron-electron and electron-nucleus cusp condi-tious. The novel EFNQMC algorithm and the novel trial func-tion are employed to calculate the energies of 1 ^1A1 state of CH2, ^1Ag state of Cs and the ground-states of H2, LiH, Li2 and H2O. 相似文献
27.
28.
Summary A program is described which calculates the number of effective plates and the coating efficiency over the entire range of a test chromatogram. The peak widths at half height are derived by assuming a Gaussian peak shape. The interpolated peak width at k=4 is used for computing a standardized number of effective plates. Plate height, column permeability, overall performance and a novel parameter called sampling efficiency are calculated from 5 other figures — i. e. carrier gas code, pressure drop, column length, column temperature and particle size.Dedicated to Dr. Leslie S. Ettre for his 60th birthday. 相似文献
29.
一种基于流动注射梯度技术识别异常峰及校正的方法 总被引:1,自引:0,他引:1
基于流动注射梯度信息提出了一种利用梯度比均值进行定量的校正方法。方法具有在线自动判别和修复异常峰并自行校正的功能,和通用的标准系列定量方法相比,两者测定精度相当。但本文提出的方法抗干扰能力明显优于后者,可适用于在线过程监测。 相似文献
30.
以作者开发的从蛋白质结合部位推导出其界面所具有的疏水性质和氢键性质的计算程序PP_SITE为基础,利用蛋白质结构数据库(PDB),对蛋白质-蛋白质相互作用界面进行了统计分析.从PDB中挑出非冗余的链间相互作用对,计算出这个数据集中所有链间界面的疏水和氢键相互作用特征.对得到的界面特征进行统计分析,寻找能够明显聚类的界面特征.结果表明,界面大小、氢键和疏水相互作用在界面所占比例以及疏水相互作用的集中程度可以作为分类的依据. 相似文献