碳糊电极阳极溶出法测定中药甘草中桑色素

用碳糊电极阳极溶出法测定桑色素的含量。在0.15mol·L-1NH4Cl 氨水缓冲溶液的介质中富集120s,桑色素在+0.10V(vs.SCE)左右出现阳极溶出峰。其峰电流的大小与桑色素的浓度呈线性关系。线性范围为4.00×10-6～1.40×10-5mol·L-1,相关系数为0.9996,检出限可达1.00×10-6mol·L-1,回收率为99.87%～102.01%。此法不用汞电极,灵敏度高,操作方便、快捷,成功地用于甘草提取物中桑色素的测定。     

Anodic Stripping Voltammetry of Heavy Metals at Nanocrystalline Boron‐Doped Diamond Electrode

Boron‐doped Diamond (BDD) electrode has become one of the important tools for heavy metal detection. By studying some analytical parameters of DPASV method, like deposition time and potential in different electrolyte concentrations (acetate buffer), the conditions for detecting very low metal ion levels (Zn, Cd, Pb, and Cu) could be chosen. Diluted electrolyte (0.01 M buffer) was one of the factors favoring low detection and quantification limits, but its quantification range is short in comparison to more concentrated media. For ?1.7 V deposition potential, the detection of single metal at ppb levels was reached in 60 s deposition time. Understanding different metal‐metal interactions shows the limits to the simultaneous determination of heavy metals at BDD. Quantification was possible for the simultaneous determination of Zn, Cd and Pb despite the overlapping of Zn and Cd peaks. The performance of the BDD was compared with that of another C‐based solid electrode: the glassy carbon electrode (without mercury plating). A lower base line current, wider potential range, higher sensitivity (3 to 5 times higher than GC) and longevity of the material were noticed for the BDD.     

香蕉组织膜草酸电极的研究

将香焦组织与氧电极偶合,制成了草酸生物组织电极。在静态和流动条件下,测得电极的线性响应范围分别为8.8×10~(-5)～6.3×10~(-4)mol/L和5.0×10~(-5)～1.8×10~(-3)mol/L,二者的相关系数均为0.9998。研究了介质条件、pH、温度、流速、取样量和固定化等条件的影响。测定了电极的选择性和使用寿命等性能。计算了该实验条件下酶反应的米氏常数。采用静态法和流动注射法测得7份草酸标液的平均回收率分别为98.4％和98.9％。电极已用于一些食品中草酸的测定,所得结果与文献报道基本一致。     

Ni,Pd／Al2O3对丙酮加氢一步合成甲基异丁基酮性能比较

研究了Ａｌ２Ｏ３负载Ｎｉ、Ｐｄ催化剂上丙酮加氢一步合成甲基异丁基酮的反应活性。考察了不同Ｎｉ含量和不同Ｐｄ含量对活性的影响。结果表明，在载体Ａｌ２Ｏ３中加入不同含量的ＳｉＯ２后，会改善载体的性能，Ｎｉ／Ａｌ２Ｏ３催化剂中添加稀土元素Ｌａ或Ｃｅ后可改善催化剂的稳定性。     

TZAAP-Nafion修饰电极溶出伏安法测定痕量铜

近年来,化学修饰电极以其独特的优越性,在分析测试中具有广阔的应用前景[1-6],因此对于新的修饰剂的研究,以及用修饰电极探讨灵敏度高,选择性好的测定方法具有重要的意义。2[2,3,5-三氮唑偶氮]-5-乙酰基氨基苯酚(2-(2,3,5-triazolylazo)-5-acetam idophenol,简称TZAAP)是一种新合成的有机化合物,其结构式为:由于TZAAP可以和金属离子形成稳定的配合物,在光谱法中可以作为显色剂用于环境及生物样品中微量元素的测定[7,8]。Nafion是一种优良的阳离子交换剂,用作电极修饰材料具有良好的离子交换特性[9]。本文作者制备了TZAAP-Nafion修饰…     

Re-Evaluation of the Activity Coefficients of Aqueous Hydrochloric Acid Solutions up to a Molality of 2.0 Using Two-Parameter Hückel and Pitzer Equations. Part I. Results at 25°C

Simple two-parameter Hückel and Pitzer equations were used for the calculation of the activity coefficients of aqueous hydrochloric acid at 25°C up to a molality of 2.0 mol-kg^–1. The data obtained by Harned and Ehlers^(12,13) from galvanic cells without liquid junction were used in the analysis and the parameters obtained were compared to those obtained from all reliable data presented in the literature for HCl at this temperature. A good agreement between the parameters was always observed. The activity coefficients obtained by the new equations were compared to those suggested by Robinson and Stokes,⁽⁸⁾ Hamer and Wu,⁽¹⁾ and Pitzer and Mayorga,⁽⁹⁾ and good agreement was also found. The data from the most important literature data sets for HCl were also predicted using the new activity coefficient equations, and the magnitude of the resulting errors was close to the precision of the measurements, the errors forming an almost random pattern for all data sets.     

Fabrication of Poly(allylamine)ferrocene Monolayer Based on Electrostatic Interaction and Its Electrocatalytic Oxidation of Ascorbic Acid

A poly(allylamine)ferrocene monolayer was built on the surface of gold electrode modified with negatively charged alkanethiol based on electrostatic interaction. The electrochemical behavior of the modified electrode was characterized by cyclic voltammetry in detail. The modified electrode was shown to exhibit excellent electrocatalytic response to the oxidation of ascorbic acid. The anodic overpotential was reduced by about 170 mV compared with that obtained at a bare gold electrode. The modified electrode possesses several attractive features, such as simple preparation, fast response and good chemical and mechanical stability.     

盐酸氨溴索在碳糊电极上阳极伏安法的研究

在０．５ ｍｏｌ／Ｌ Ｈ２ＳＯ４底液中，用碳糊电极阳极伏安法测定盐酸氨溴索，被测的阳极峰电位为１．１０Ｖ（ｖｓ．ＳＣＥ），另外，在０．４６Ｖ处还产生一对可逆的氧化还原峰。１．１０ Ｖ处的峰电流与盐酸氨溴索的浓度在３．９８×１０~（－７）～６．３４ × １０~（－５）ｍｏｌ／Ｌ范围内呈良好的线性关系，该方法的检出下限为３．０ × １０~（－８）ｍｏｌ／Ｌ。用标准加入法测得回收率范围为９２．８％～１０２％，ＲＳＤ为２．９％（ｎ＝１０）。对电极响应机理进行了初步探讨，氨溴索在１．１０ Ｖ处的氧化为不可逆过程，其氧化产物在０．４６０Ｖ处产生一对２电子２质子受扩散控制的可逆波，用该波也可进行定量测定并且干扰较少，但灵敏度略低。     

羧基化碳纳米管嵌入石墨修饰电极对多巴胺和抗坏血酸的电催化

采用涂层和嵌入修饰法 ,将羧基化多层碳纳米管制成两种修饰电极。以多巴胺 (DA)和抗坏血酸(AA)为模型化合物 ,研究了两种修饰电极对DA和AA共存时的电催化作用。结果表明 :嵌入的方式比涂层的方式显示了更多的优点。嵌入修饰电极不仅使峰电流增加 ,并且使两者共存时的氧化峰位分离达 16 0mV ,同时 ,该电极对DA的响应灵敏于AA ,这有利于在大量的AA存在下实现对DA的测定。在 1× 10 - 3 mol/L的AA的存在下 ,还原电流的一阶导数与DA浓度在 5× 10 - 7～ 1× 10 - 4 mol/L范围内呈良好的线性关系 ;检测下限达 1× 10 - 7mol L。     

A Magnesium-Selective Ionophore Containing Four Amide Carbonyl Ligands Derived from L-Tartaric Acid and Axial Furano Oxygen Binding Sites

Octahedrally converging hexadentate macrocyclic receptors 1 and 2, based on L-tartaric acid and furanmoieties, were synthesized andtheir complexation properties studied. In this paper,magnesium ion selectivitiesdetermined by ISE experiments, chiroptical changes observedby circular dichroism(CD) on complexation, and association constants measuredby NMR titration arediscussed.