示波极谱滴定的研究(ⅩⅩⅧ)——单微铂电极上的示波极谱络合滴定法

示波极谱滴定中使用一个微铂电极和一个大面积电极者称为单微铂电极示波极谱滴定法,本文研究了单微铂电极示波极谱络合滴定法,取得了较好的结果。     

普鲁士蓝纳米修饰电极的制备及表征

采用激光加热拉伸的方法制备铂纳米电极,并通过交流电刻蚀的方法制备纳米孔电极,在这两种电极上可通过电化学方法原位合成单颗普鲁士蓝微晶. 结果表明,普鲁士蓝微晶在纳米微孔电极上的机械附着强度增强. 这种方法可用于制备纳米修饰电极或研究功能微晶体材料的电化学性质.     

新型光化学电池高活性铂电极的研究

应用循环伏安法，在导电玻璃表面沉积微量铂，制备新型光电化学电池的高比表面高洁性对电极所获得的电极比表面最高达371m2·g-1;同时发现，该电极对的质量交换电流密度随铂沉积量的增加而减小，而相对于宏观面积的交换电流密度几乎没有变化，因此，在实验可控制的限度内，用微色的铂就可以获得高活性的对电极     

铂电极在碱性含氧溶液中的预还原处理对鲁米诺电 致化学发光的影响

研究了铂电极的不同预极化处理过程对碱性鲁米诺阳极电致化学发光(ECL)和阳极极化曲线的影响,发现在碱性含氧溶液中预还原处理的铂电极可增强0.22V(vs.SCE)处发光峰强度,且催化产生1.07V(vs.SCE)附近氧气析出过程并伴随产生明显的ECL发光峰;在酸性溶液中预处理电极可抑制这些活性。给出了催化氧气析出的可能作用机理：在碱性溶液中溶解氧还原生成了吸附在铂电极表面的(OH^-)~a~d~s,从而回忆了氧气的析出过程。同时给出了在碱性含氧溶液中预还原的铂电极上两个可能的ECL反应通道：(1)在0.22V鲁米诺阴离子氧化为鲁米诺自由基,然后与溶解氧反应而发光;(2)1.07V处析出的新鲜氧与鲁米诺阴离子反应而发光。     

铅在铂电极上的还原电位溶出分析法

研究了以亚铁氰化钾为还原剂铅在铂电极上的还原电位溶出法；讨论了电极的预处理、阳极富集和随后的还原电位溶出及铅测定的干扰。     

固定有四硫富瓦烯.四氰基奎诺二甲烷的杂聚吡咯膜微葡萄糖电极

铂比互铂化处理后，形成疏松，粗糙的表面，将四硫富瓦烯－四氰基奎诺二甲烷导电有机盐入到铂化的铂黑微粒中。将３－羰基丁酸吡咯与吡咯按适当的比例在其表面用电化学聚合方法，将葡萄糖氧化酶固定于聚合形成的杂聚膜中制成微酶电极。该微酶电极测定时几乎不受氧分压影响，灵敏度高，响应快。     

扫描电化学显微镜直接电沉积法构建葡萄糖氧化酶微米点

利用自制的凹形电极在铂基底电极上直接构建了葡萄糖氧化酶微米点. 首先, 将电聚合和电化学刻蚀法相结合制备了凹形铂微米电极. 然后将此种电极作为参比及辅助电极, 基底铂电极作为工作电极, 利用葡萄糖氧化酶在合适的条件下(浓度、一定量Triton X-100存在、电极电位等)由于电极表面pH的降低可以在铂电极上电沉积这一特性, 将酶固定在铂基底电极上, 微修饰得到了具有活性的葡萄糖氧化酶微米点. 最终用扫描电子显微镜和扫描电化学显微镜对所得微米点进行了表征. 所得微米点直径约20 μm, 且具有催化活性. 该方法简便, 干扰因素较少.     

乙醇氧化酶电极的研究

1 引言 本文在Clark 1972年工作基础上,以自制的铂电极为工作电报,采用简单的预处理方法,并且调整乙醇氧化酶(AOD),牛血清白蛋白,缓冲液的比例,以戊二醛为交联剂,将(AOD)固定在铂电极上,制成AOD电极,并且研究了该电极的性能,用于测定啤酒,白酒中乙醇含量,结果证明此电极具有响应快,灵敏度高,稳定性好,测试方便等优点。     

基于微腔型电极的半乳糖生物传感器

采用微机械加工技术制作了具有三维结构的微腔型传感器芯片（腔深３００μｍ,铂工作电极１．２＊１．２＾ｍｍ＾－２。作者对微腔型电极进行了电化学特征的表征。并通过明胶包埋法将半乳糖氧化酶固定在电极中,构成微腔型半乳糖传感器。     

示波极谱滴定的研究 ⅩⅩⅩⅡ.金电极上的示波极谱滴定法

本文研究了用微金电极为工作电极的示波极谱滴定法。在同样的条件下,用金电极时某些离子如Co~(2+)和Ni~(2+)能产生敏锐的切口,而用铂电极时无切口。用两个相同的微铂电极时,EDTA和某些有机物质可以有灵敏的切口,但用金电极时无切口。微金电极能用于络合、沉淀和氧化还原滴定。这时Mn~(2+),Fe~(2+),Co~(2+),Ni~(2+),Hg~(2+),和Cu~(2+)有灵敏的切口,能用于示波极谱滴定。滴定结果较好,标准偏差不大于0.12％。     

微波加热快速测定腐植酸总量

利用微波加热技术，在密闭容器内通过压力浸提、消解试样、能大大加快分析速度，本实验测定了不同煤样中的腐植酸总量，讨论了功率、时间、酸度等因素对分析结果的影响，并与标准方法相对照，用ｔ－检验法及Ｆ－检验法检验，没有明显差异，结果令人满意，该法具有省时、省力、经济、不污染环境，宜于批量分析，便于普及推广等优点。     

多组分体系同时定性定量测定的逐步回归分析法

阐述了逐步回归分析法用于多组分体系同时定性定量分析的原理、实验及数据处理方法。分析了硝基酚类人工样、未知样及合成样。该法可用于仅知可能含有的组分范围的样品分析。     

计算原子吸收分光光度法多元素同时测定

本文研究了用计算原子吸收分光光度法进行多元素同时测定的方法：利用火焰原子吸收法中的化学干扰效应．建立相应的关系函数，以标准增量法测定，非线性最小二乘法迭代求解，同时计算出主测素和干扰元素的含量，从而实现了多元素的同时测定。     

稀土元素示踪技术及其在土壤侵蚀研究中的应用

稀土元素示踪技术作为一种研究土壤侵蚀的新方法,被广泛应用于土壤坡面侵蚀和泥沙来源等方面的研究.在对稀土元素布设方法、含量测定方法和精度分析方法进行分析的基础上,对稀土元素示踪技术作了总结.对其在坡面侵蚀以及泥沙运移过程中的研究进行了评述,并在此基础上对稀土元素示踪技术的相关问题进行了探讨,指出了目前这些研究中存在的不足,以便为后期稀土元素示踪技术的改进及其在土壤侵蚀研究中的应用提供一定参考.     

New background correction method for liquid chromatography with diode array detection, infrared spectroscopic detection and Raman spectroscopic detection

A new method to eliminate the background spectrum (EBS) during analyte elution in column liquid chromatography (LC) coupled to spectroscopic techniques is proposed. This method takes into account the shape and also intensity differences of the background eluent spectrum. This allows the EBS method to make a better estimation of the background eluent spectrum during analyte elution. This is an advantage for quantification as well as for identification of analytes. The EBS method uses a two-step procedure. First, the baseline spectra are modeled using a limited number of principal components (PCs). Subsequently, an asymmetric least squares (asLS) regression method is applied using these principal components to correct the measured spectra during elution for the background contribution. The asymmetric least squares regression needs one parameter, the asymmetry factor p. This asymmetry factor determines relative weight of positive and negative residuals. Simulations are performed to test the EBS method in well-defined situations. The effect of spectral noise on the performance and the sensitivity of the EBS method for the value of the asymmetry factorp is tested. Two applications of the EBS method are discussed. In the first application, the goal is to extract the analyte spectrum from an LC-Raman analysis. In this case, the EBS method facilitates easy identification of unknown analytes using spectral libraries. In a second application, the EBS method is used for baseline correction in LC-diode array detection (DAD) analysis of polymeric standards during a gradient elution separation. It is shown that the EBS method yields a good baseline correction, without the need to perform a blank chromatographic run.     

Method for constructing isomerization reactions

A method is formulated for enumerating and constructing isomerization reactions of molecules exhibiting large amplitude nonrigid motions. This method not only enumerates the isomers of nonrigid molecules and the corresponding rigid molecules but also the symmetry species spanned by the equivalent structures whose representative is an isomer. Consequently, using the method of correlating the symmetry species of a group to the symmetry species of its subgroup the splitting patterns of isomers of nonrigid molecule to those of rigid molecule are obtained. This provides an elegant method for both enumerating and constructing reaction graphs. The method is illustrated with examples.     

电解还原法生产的对氨基苯酚纯度及杂质4，4＇－二氨基二苯醚的高效液相色谱分析

电解还原法生产的对氨基苯酚纯度及杂质４，４＇－二氨基二苯醚的高效液相色谱分析尤进茂，孙学军，李怀娜，周连君（曲阜师范大学化学系曲阜２７３１６５）１前言对氨基苯酚（ＰＡＰ）是制造显影剂、药物扑热息痛和偶氮染料的重要中间体［１～３］，用途十分广泛。虽然工...     

New applications of integral equations methods for solvation continuum models: ionic solutions and liquid crystals

We present a new method for solving numerically the equations associated with solvation continuum models, which also works when the solvent is an anisotropic dielectric or an ionic solution. This method is based on the integral equation formalism. Its theoretical background is set up and some numerical results for simple systems are given. This method is much more effective than three‐dimensional methods used so far, like finite elements or finite differences, in terms of both numerical accuracy and computational costs. This revised version was published online in July 2006 with corrections to the Cover Date.     

用模糊数学评价中成药质量的方法研究

本研究应用模糊数学中ISODATA(Interactive Self-Organizing Data Analysis Technique A)聚类分析法,把不同厂家的同一品种中成药分成五个等级,即Ⅰ、Ⅱ、Ⅲ、Ⅳ、Ⅴ级品。并根据此分级结果构造一个多元隶属函数,提出一种模糊模型的等级识别法,为制定各类中成药质量判别标准提供了依据。本文用十个厂家共三十个批号的冠心苏合丸验证,效果满意。     

Method for the detection of diethylamine, a metabolite of disulfiram, in urine.

Disulfiram is a drug used in the treatment of chronic alcoholism in man. Accurate assessment of patient compliance is important in this treatment. This paper describes a method for the detection and quantitative analysis of diethylamine, a metabolite of disulfiram, in urine. The method involves conversion of the water-soluble diethylamine in the urine to a derivative, N,N-diethyl-3,5-dinitrobenzamide, that is soluble in an organic solvent. This derivative is extracted from urine with diethyl ether and then subjected to thin-layer chromatography. A spectrophotometric procedure is used for quantification. This method provides a means of determining whether or not a patient is taking his prescribed disulfiram.