Trace anion determination in concentrated hydrofluoric acid solutions by two-dimensional ion chromatography II. Method performance study with a hydroxide eluent and a low noise suppressor

The two-dimensional ion exclusion chromatography/ion chromatography (ICE-IC) approach is considered to be the method of choice for the determination of trace anions in concentrated hydrofluoric acid (48-50%, w/w). In order to achieve lower detection limits, this method was for the first time used with electrolytically generated and purified hydroxide eluents in combination with a low noise electrochemical suppressor. Compared to carbonate based eluents, the achieved gain in peak height sensitivity for chloride, sulfate, nitrate and phosphate is a factor of 6, 7, 16 and 13, respectively. The instrumental detection limits, based on the background noise, are 2, 0.2, 0.4 and 1.4 microg/kg HF 50% (w/w) for the same anions. Their method detection limits, calculated according to SEMI, are all within the 6-10microg/kg HF 50% (w/w) range and thus at least 10 times lower than the current Tier C grade requirements. The chromatographic run time could be shortened with some 10 min by the use of a relatively fast high-capacity hydroxide selective anion exchange column.     

Quantitation in capillary electrophoresis-mass spectrometry

CE-MS has evolved into a strong alternative to LC-MS. Most of CE-MS applications deal with characterization and identification. However, quantitative aspects have gained importance in, e.g., pharmaceutical and biotechnological applications. Here we summarize and evaluate various methodological aspects in order to achieve sensitive and reproducible results. Similar to LC-MS, aspects of matrix influence on the electrospray process need to be carefully addressed when quantitative results are intended by CE-MS. Due to a more complicated coupling special emphasis needs to be put on the CE-MS interface. Generally linearity over more than three orders of magnitude can be achieved by CE-ESI-MS. Furthermore, a literature survey has been performed in order to give an overview over quantitative measurements performed by CE-MS. The precision can be doubled when changing from a structural related to an isotopically labeled internal standard. Thus a level of precision better than 5% RSD can be achieved.     

对固体圆二色光谱测试方法的再认识——兼谈“浓度效应”

对近期发展的固体圆二色(CD)光谱测试方法进行了概述、评价和比较, 着重探讨了“浓度效应”的存在使固体CD光谱失真的原因. 通过对本课题组和其他作者已报道的四种化合物的固体CD谱再测试的反思, 强调了依手性化合物的手性光谱学性质不同, 根据浓度梯度实验选择其合适测试浓度的必要性. 对固有手性的阻转异构化合物(S)-1,1'-联二萘酚(S-BINOL)进行了成膜法固体CD谱浓度梯度测试, 发现所得固体薄膜CD谱中也存在着“浓度效应”     

材料断口中的分形(英文)

分形几何(Fractal geometry)是近年来出现的一门应用数学分支。本文简要介绍了分形在材料断裂表面分析中的应用概况,并叙述了本文作者关于“延性断裂韧性与断裂表面的分形”研究工作。如果继续深入研究,将可从材料破坏的断口上直接分析并推知其断裂特性,从而为材料的失效分析提供一种简便而实用的新方法。     

棉纺厂管理信息系统的研制

本文根据开发CTU-JMS管理信息系统已取得的成功经验,介绍CTU—JMS管理信息系统的运行环境;总体规划中运用的两种设计策略——“由顶向下”分析法和“由下至上”分析法;MIS中建立大型基础数据库采用的主要技术;MIS决策管理层的形成以及生产经营决策子系统的技术特点。为推进我国的纺织企业管理信息系统的开发和实现现代化管理作了探索。     

偏最小二乘法在原子吸收光谱分析中的应用——钴和铟的同时测定

本文用偏最小二乘法（ＰＬＳ）校正了火焰原子吸收分析Ｉｎ２５２．１３７ｎｍ对Ｃｏ２５２．１３６ｎｍ的吸收线重叠干扰,对混合样中Ｃｏ和Ｉｎ的含量进行了测定,结果令人满意。     

基于密码学的通信安全性——语音的数字加密方法

基于密码学的通信安全性思考,提出了语音的数字加密方法,设计了一种加密体制及两部密钥的模型。     

热电偶测温结果的校准

本文介绍了用高精度的水银温度计测得的温度作为标准温度,来校准热电偶的测温结果,并用最小二乘法来拟合其修正公式的方法。     

《初等几何研究》教法改革的尝试

该文分析了《初等几何研究》课的特点和学生学习该课程存在的问题,阐述了实施“单元循环教学法”的教改实验过程及所取得的效果。     

Evaluation of measurement uncertainty for analytical procedures using a linear calibration function

In the EURACHEM/CITAC draft ”Quantifying uncertainty in analytical measurement” estimations of measurement uncertainty in analytical results for linear calibration are given. In this work these estimations are compared, i.e. the uncertainty deduced from repeated observations of the sample vs. the uncertainty deduced from the standard residual deviation of the regression. As a result of this study it is shown that an uncertainty estimation based on repeated observations can give more realistic values if the condition of variance homogeneity is not correctly fulfilled in the calibration range. The complete calculation of measurement uncertainty including assessment of trueness is represented by an example concerning the determination of zinc in sediment samples using ICP-atomic emission spectrometry. Received: 9 February 2002 Accepted: 17 April 2002