Summary of ISO/TC 201 Standard XI. ISO 17974:2002—Surface chemical analysis—High‐resolution Auger electron spectrometers—Calibration of energy scales for elemental and chemical‐state analysis

This International Standard specifies a method for calibrating the kinetic energy scales of Auger electron spectrometers for elemental and chemical‐state analysis at surfaces. It is only applicable to instruments that incorporate an ion gun for sputter cleaning. This International Standard further specifies a method to establish a calibration schedule, to test for the kinetic energy scale linearity at one intermediate energy, to confirm the uncertainty of the scale calibration at one low and one high kinetic energy value, to correct for small drifts of that scale and to define the expanded uncertainty of the calibration of the kinetic energy scale for a confidence level of 95%. This uncertainty includes contributions for behaviours observed in interlaboratory studies but does not cover all of the defects that could occur. This International Standard is not applicable to instruments with kinetic energy scale errors that are significantly non‐linear with energy, to instruments operated at relative resolutions poorer than 0.2% in the constant ΔE/E mode or poorer than 1.5 eV in the constant ΔE mode, to instruments requiring tolerance limits of ±0.05 eV or less or to instruments equipped with an electron gun that cannot be operated in the energy range 5–10 keV. This standard does not provide a full calibration check, which would confirm the energy measured at each addressable point on the energy scale and should be performed according to the manufacturer's recommended procedures. Crown Copyright © 2003. Published by John Wiley & Sons, Ltd.     

锌盐及其化验研究

介绍了锌盐对人体的作用，对锌盐的化验方法进行了研究，包括锌的定性分析和定量分析。锌的定量分析又包括：EDTA滴定法和萃取吸光光度法。     

The interface of the Ising model and the Brownian sheet

We study the limit theorem related to the interface of the three-dimensional Ising model. Dobrushin proved that the interface does not fluctuate and becomes rigid for sufficiently large. We define the random fieldX ^L (t, s), 0t, s1, on the interface, and prove that X^L(t, s) converges to the Brownian sheet as L for sufficiently large, whereL denotes the size of the system. This result does not mean that the interface itself converges to the Brownian sheet.     

Infrared spectra of M+NO 3 − contact ion pairs in aprotic solvents and matrix isolated in the corresponding glasses

Studies of the vibrational spectra of matrix-isolated M⁺NO ₃ ^– ion pairs have been extended to glassy aprotic solvents. The deuterated form of the solvents DMSO, THF, and ACN have windows through the 7- nitrate ionv ₃(e) mode infrared region, so it was possible to clearly observe the splitting of the degeneracy of this mode,v ₃, produced by the contacting, but solvated, alkali metal cation. Primary attention has been directed to the extent to which this splitting is reduced relative to the argon matrix values. This reduction, which reflects electron-density transfer from the solvating molecules to the ion pairs, is comparable to that observed for H₂O and NH₃ matrices as the splitting is reduced to 20–35% of the argon-matrix values. The extent of reduction ofv ₃ for the different solvents has been related to Gutmann's donicity number scale with the correlation holding well for solvent molecules of comparable size, DMSO, THF and DMF, but breaking down for the smaller linear ACN, apparently because of more molecules in the cation solvation sphere. The matrix data have also been used, through comparison with spectra for saturated liquid solutions of Li⁺NO ₃ ^– , to show that the contact ion pair is the dominant species in liquid THF and ACN, whereas the ions are largely solvent separated in DMSO.     

Analytical procedures for quantification of peptides in pharmaceutical research by liquid chromatography–mass spectrometry

Peptide quantification by liquid chromatography–mass spectrometry (LC–MS) combines the high resolving power of reversed-phase (RP) chromatography with the excellent selectivity and sensitivity of mass spectrometric detection. On the basis of comprehensive practical experience in the analysis of small molecules, pharmaceutical research is developing technologies for analysis of a growing number of peptidic drug candidates. This article is a detailed review of procedures based on LC–MS techniques for quantitative determination of peptides. With the focus on pharmaceutical applications several technologies for sample preparation, various aspects of peptide chromatography, important characteristics of ESI–MS, selectivity of MS-detection modes, the large variability of internal standards, and modern instrumentation are discussed. The demand for reliable, robust, sensitive, and accurate methods is discussed using numerous examples from the literature, complemented by experiments and results from our laboratory.     

气相色谱叠加定量方法的研究

叠加法是由内标法衍生而来的一种气相色谱定量方法。对于较复杂混合物的分析,当选择内标物困难时,用叠加法定量更为方便。本文在大量实验的基础上,提出了叠加法定量过程中应注意的一些问题。     

Inductively coupled plasma atomic emission spectrometry — Optimization of the operating conditions in the determination of trace of elements in line-rich emission matrices

Radial viewing 40.68 MHz inductively coupled plasma atomic emission spectrometer was used in the determination of Y, Sc and rare earth elements in Eu₂O₃ or Lu₂O₃ as pure rare earth matrices. The Mg II 280.270 nm/Mg I 285.213 nm line intensity ratio was measured to evaluate the robustness of the operating conditions. The operating conditions were affected by varying the incident power and sheathing gas flow rate. The carrier gas flow rate remained a constant value. The relationship between the Mg II 280.270 nm/Mg I 285.213 nm ratio and the excitation temperature was obtained. A dependence of the magnesium ratio in the pure solvent and the corresponding values in the presence of the above matrices was established.     

Estimation of the size of liposomes by modified HDC

Internal calibration in modified hydrodynamic chromatography has been realized by the approach of Prieve and Hoysan, i.e. the use of polystyrene monodisperse latexes to evaluate the equivalent capillary radius, R. The value obtained has been used to estimate the average sizes of a variety of liposome samples from egg yolk lecithin.     

Rare earth tungsten bronzes: a new method of synthesis. Perspectives for their application as inert matrices for transmutation of long-life actinide elements

A new method of synthesis of oxide tungsten bronzes containing lanthanide (Ln) Nd and Eu, based on thermal degradation of polyoxotungstate compounds, is proposed. The simplicity of the method allows to consider this class of compounds with chemical formula, Ln_xWO₃, as potential inert target for incineration or transmutation of minor actinides, Am and Cm, in neutron reactors. Nd and Eu were used as analogues of transplutonium elements. Powder X-ray diffraction patterns of compounds synthesized reveal a cubic perovskite structure. The lanthanide content in bronzes was determined by optical spectroscopy analysis. The experimental density of the pressed bronze samples was estimated at 6.58 g cm⁻³, i.e., 89% of the crystallographic value. The thermal stability of the bronzes synthesized was checked up to 900°C in an inert atmosphere. Leaching tests were performed for europium bronzes in nitric acid solutions using luminescence technique.