Determination of trace hydrazine by differential pulse voltammetry using magnetic microspheres

A new type of magnetic polymer microspheres containing ketone groups on the surface was synthesized. It can be reacted with hydrazine to produce electroactive adduct. Reduction of this derivative that was aggregated on the magnetic electrode is possible and effective in indirect determination of hydrazine. The experimental conditions and electrode structure were discussed. Under optimum conditions, It was found that the peak potential (Ep) of hydrazine is -1.06 V (vs. Ag/AgCl). Hydrazine in the range 0.3-500 mug l(-1) can be determined. The detection limits for hydrazine is 0.1 mug l(-1). The relative standard deviation for determination of 100 mug l(-1) hydrazine was 2.43 %. The method was applied to the determination of hydrazine in water samples with satisfactory results.     

The tautomerism of Omeprazole in solution: a 1H and 13C NMR study

The tautomerism of 5(6)-methoxy-2-([(4-methoxy-3,5-dimethyl-2-pyridinyl)methyl] sulfinyl)-1H-benzimidazole (omeprazole) was determined in solution, K(T) = 0.59 in THF at 195 K, in favor of the 6-methoxy tautomer. The assignment of the signals was made by comparison with its two N-methyl derivatives in acetone-d6 and through theoretical calculations of the absolute shieldings (GIAO/DFT/6-311++G**).     

立方介孔相含钕氧化硅的合成与表征

以十六烷基三甲基溴化铵为结构导向剂，通过水热法合成了具有立方结构的含钕Nd-MCM-48介孔分子筛材料。XRD和TEM测试表明当n_Nd/n_Si<0.05时可以获得典型的长程有序介孔立方结构相，随n_Nd/n_Si比的增加，晶胞参数的增大和红外吸收光谱(FT-IR)的变化为Nd进入介孔分子筛骨架中提供了有力证据。N₂吸附-脱附实验给出了其BET表面积为1 195 m²·g^-1，BJH平均孔径为3.6 nm。紫外-可见漫反射光谱(UV-Vis)证明钕氧形成一种八面体结构。X射线光电子能谱(XPS)进一步证明钕主要以三价形式存在于立方介孔分子筛骨架中。     

负载型非晶态Cu/SiO2催化剂的非晶性质

以超细ＳｉＯ２为载体，用ＫＢＨ４还原Ｃｕ＾２＋盐溶液制备了非负载型Ｃｕ和负载型Ｃｕ／ＳｉＯ２催化剂，ＸＲＤ，ＴＥＭ和电子衍射分析结果表明，负载型Ｃｕ／ＳｉＯ２为完全非晶态，而非负载型Ｃｕ中存在着少量晶态Ｃｕ，ＤＳＣ结果表明，非晶态Ｃｕ／ＳｉＯ２的热稳定性明显高于非负载型Ｃｕ，说明超细ＳｉＯ２具有稳定非晶结构的作用，ＸＰＳ结果表明，还原产物中的铜原子呈Ｃｕ状态，ＩＣＰ分析结果表明，样品中的Ｂ含量均低     

Electrochemical characterization of boron-doped polycrystalline diamond thin-film electrodes

The electrochemical characterization of boron-doped polycrystalline diamond thin-film (BDF) electrodes was studied using the anodic scan after concentrating lead in 0.1 mol/L KCl - 41 micromol/L Hg(NO(3))(2) and 0.1 mol/L KNO(3) - 0.01 mol/L HNO(3) - 41 micromol/L Hg(NO(3))(2); accumulation voltage was -0.90 V. The results obtained were compared with those given by glassy carbon (GC) electrodes and proved that the BDF electrodes offered high sensitivity, good precision and extreme stability over a 2-month period. These electrodes provided good resolving power for the determination of lead and cadmium and gave satisfactory results in the analysis of a pure water sample.     

用亚硝基R盐螯合树脂分离富集催化极谱法测定矿石中的铱

本文研究了利用亚硝基Ｒ盐螯合形成的树脂，分离富集试液中痕量贵金属元素铱的实验条件。并利用ＪＰ－１型示波极谱仪，在１．５０ｍｏｌ／Ｌ盐酸＋５．０×１０＾－５ｍｏｌ／Ｌ硫脲＋０．２ｍｏｌ／Ｌ盐酸＋５．０×１０＾－５ｍｏｌ／Ｌ硫脲＋０．２ｍｏｌ／Ｌ碘化钾＋碲（ρ（Ｂ）＝０．４ｍｇ／Ｌ）的混合底液中，对铱进行极谱催化波测定。在示波极谱仪上峰电位约－０．５５Ｖ（银汞齐为参比电极），可测定试液中５．０×１．０     

化学形态分析

本文综述了金属元素的化学形态分析,包括:形态分析的方法与技术,形态分析在水、土壤、空气和生物样品中的应用,样品的处理方法等。     

硝酸钬水合物热分解及配位性质的研究

文献报道了Ho(NO_3)_3·5H_2O和Ho(NO_3)_3·(?)H_2O的热分解行为,但Ho(NO_3)_3·5H_2O脱水机理不清,Ho(NO_3)_3·4H_2O按文献[1]不能制出。六水、三水合物的热分解及与DMF的配位作用未见报道。     

高抗冲聚苯乙烯的增韧机理

概述了以高抗冲聚苯乙烯（ＨＩＰＳ）为中心的有关橡胶增韧机理的理论，并且总结了界面，性能、粒子尺寸、粒 距及缠结密度等因素对橡胶／高分子共混体系性能的影响。     

氧缺位铁酸盐的制备及结构与还原行为的研究

在３５８Ｋ下用２００ｍｌ／ｍｉｎ的空气氧化碱性悬浮液合成了ＭＦｅ_２Ｏ_（４＋δ）（δ≥０，Ｍ＝Ｆｅ、Ｃｏ、Ｎｉ、Ｍｎ），并在５７３Ｋ下用４０ｍｌ／ｍｉｎ的Ｈ_２还原ＭＦｅ_２Ｏ_（４＋δ）制备了氧缺位铁酸盐ＭＦｅ_２Ｏ_（４－δ）（δ＞０）。用ＸＲＤ、Ｍｓｓｂａｕｅｒ谱等测试方法对铁酸盐的结构进行了表征，考察了铁酸盐的组成及第二金属组分（Ｃｏ、Ｎｉ、Ｍｎ）对铁酸盐还原性能的影响。在Ｈ_２还原３ｈ内，铁酸盐氧缺位程度随还原时间增加而增大，晶格常数也相应增大；５ｈ以上，铁酸盐将被还原为ＭＯ－ＦｅＯ或α－Ｆｅ，晶格常数几乎不变。按Ｆｅ、Ｃｏ、Ｎｉ、Ｍｎ顺序，ＭＯ与ＦｅＯ的相互作用能力、ＭＯ－ＦｅＯ固溶体的稳定性及铁酸盐还原为ＭＯ－ＦｅＯ的能力均增强，ＭＯ－ＦｅＯ进一步还原为α－Ｆｅ的能力却减弱。