Summary of ISO/TC 201 standard: XXI. ISO 21270:2004—Surface chemical analysis—X‐ray photoelectron and Auger electron spectrometers—Linearity of intensity scale

This International Standard specifies two methods for determining the maximum count rate for an acceptable limit of divergence from linearity of the intensity scale of Auger and x‐ray photoelectron spectrometers. It also includes methods to correct for intensity non‐linearities so that a higher maximum count rate can be employed for those spectrometers for which the relevant correction equations have been shown to be valid. Copyright © 2004 John Wiley & Sons, Ltd.     

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。     

原油饱和烃指纹的内标法分析

采用内标法建立了原油中正构烷烃、生物标志物(甾、萜烷类)的分析方法。确定了样品前处理方法和组分定性定量方法。讨论了柱层析分离能力。结果表明,所有饱和烃组分均流入第一部分流出液F1中,分离能力较为满意。对48种甾、萜烷类生物标志物组分以及姥鲛烷、植烷和正构烷烃等进行了定性确认,定性化合物数量多,信息量大,易于据此进行可靠的油指纹分析鉴别。32个正构烷烃组分相对标准差为1.2%～7.4%;45个生物标志物组分相对标准偏差为2.5%～9.2%。分析精密度较好,满足油指纹鉴别需要。正构烷烃回收率为73%～116%;生物标志物为84%～106%;回收率结果较为满意。正构烷烃方法检出限为7.0μg/g;生物标志物为0.65μg/g,满足原油样品分析要求。通过本方法对自不同和相同平台的原油样品进行饱和烃浓度分析,并采用浓度数据进行鉴别,结果与实际情况相符。     

中学生营养平衡米膳食最佳模式评价

根据中国营养学会推荐的热量标准,研制了中学生营养平衡米膳食最佳模式。按该模式,中学生每日应摄入的膳食品种及其数量如下:主食:营养平衡米,初中男生510~597g,女生468~510g;高中男生618~683g,女生532~575g;副食相同:青菜或水果500g或600g,鱼或肉100g或50g,蛋类40g,大豆制品30g,花生油12.5g,盐6g。调查结果表明,蛋白质、脂肪、碳水化合物,热量摄入量全部达标准要求。Q(蛋白质)∶Q(脂肪)∶Q(碳水化合物):高中男女生为16∶20∶64,初中男、女生分别为17∶20∶63。提示中学生营养平衡米膳食最佳模式使中学生达到营养平衡,建议推广食用。     

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.     

Solid sampling Fourier transform infrared determination of Mancozeb in pesticide formulations

A series of approaches have been assayed for FTIR determination of Mancozeb in several solid commercial fungicides using different calibration strategies. The simplest procedure was based on the use of the ratio between the absorbance of a characteristic band of Mancozeb and that of a KSCN internal standard measured in the FTIR spectra obtained from KBr pellets. It was employed the quotient between peak height absorbance values at 1525 cm⁻¹ for Mancozeb and 2070 cm⁻¹ for KSCN. In these conditions a precision as relative standard deviation (RSD) of 0.6% and a relative accuracy error of 0.8% (w/w) were found. For complex formulations, containing other compounds with characteristic absorption bands at different wavenumbers than Mancozeb, one of them was used as internal reference being employed the standard addition approach. In this case, the Mancozeb bands at 1525 cm⁻¹ or at 1289 cm⁻¹ were employed, being used the ferrocyanide band at 2075 cm⁻¹ as internal reference. RSD values between 0.7-1.4% and a relative accuracy error of 3% (w/w) were found. A third strategy was based on the use of partial least squares (PLS) calibration. A reference set was prepared mixing Mancozeb, Kaolin, Cymoxanil and KBr, being predicted the Mancozeb concentration in pesticide formulations by using the quotient between absorbance bands of Mancozeb and those of Cymoxanil. In these conditions a relative accuracy error of 0.6% (w/w) and a relative standard deviation of 1.3% were found.     

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。     

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.