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.     

Voltammetric determination of hafnium with calconcarboxylic acid

The interaction of Hf(IV) with calconcarboxylic acid (1-(2-hydroxy-4-sulfo-1-naphtylazo)-3-naphtolic acid) was investigated by cyclic voltammetry varying various factors (pH, ionic strength, contents of ethanol and scan rate). Optimal conditions of Hf(IV) determination in the presence of calconcarboxylic acid were found: acetic buffer solution pH 2.6, scan rate 0.5 Vs⁻¹. The detection limit of Hf(IV) concentration was 2.46 × 10⁻⁷ mol L⁻¹. The influence of foreign ions on the Hf(IV) determination was studied. It was established that some metals like cadmium, nickel, zinc, copper and titanium could be determined with Hf(IV) simultaneously. The method of voltammetric determination of hafnium was tested on model solutions and used in the determination of Hf(IV) in terbium-base alloy.     

Complexation of Ni (II) and Zn(II) ions by 3-(1-naphthyI)-2-mercaptopropenoic acid

The complexation equilibria between Ni(II) and Zn(II) metal ions with 3-(1-naphthyl)-2-mercaptopropenoic acid (H₂NMP) were studied by glass electrode potentiometry, at 25 °C and 1.0 mol·dm^–3 in NaClO₄ as constant ionic medium in 50% (v/v) water-ethanol solutions. Formation constants for the complexes Ni(NMP), Ni(NMP) ₂ ^2– , Zn(NMP) and Zn(NMP) ₂ ^2– , refined by the MINIGLASS program, are reported.     

Mono- and diboronates derived from tridentate ONO ligands and arylboronic acids

The syntheses of eight [4.3.0] heterobicyclic boronates containing a N → B coordinative bond are described. The monomeric compounds were prepared by reaction of arylboronic acids with a tridentate ligand having the ONO donor set of atoms. It was shown that substituents at the para-position of the B-phenyl moiety transmit electronic effects to the CN bond which in turn is polarized by formation of the N → B coordination bond. At the same time, related tridentate ligands were also reacted with 1,4-benzenediboronic acid in order to prepare benzene diboron complexes. The structure of this type of compounds was confirmed by X-ray analysis for one of the derivatives.     

过渡金属酞菁配合物化学修饰电极的研究 Ⅰ.对草酸的电催化氧化

用不可逆吸附法首次制备了Co(Ⅱ)的3,3′,3″,3′″—四硝基酞菁配合物化学修饰电极(CoL CME),用循环伏安法研究了它的电化学性质和电催化功能,与未修饰玻碳电极相比,草酸在CoL CME上的氧化峰电位至少负移300mV,峰电流显著增大,表现出对草酸氧化具有明显的电催化作用,并发现草酸的电催化氧化峰电流与其浓度之间有很好的线性关系。     

铬（Ⅲ）—尼克酸配合物合成方法的改进及其与酸反应特性的研究

为了避免Ｃｒ（ＯＨ）３引起的污染,本文用改进的方法合成了配合物Ｃｒ（ｎｉｃ）２（Ｈ２Ｏ）３ＯＨ,这里ｎｉｃ表示尼克酸根。通过红外光谱、热分析对其结构进行了表征。结果表明,尼克酸以羧基氧与铬（Ⅲ）配位。对该配合物与酸的反应特性和可能的机理进行了研究讨论。     

稀土与对-茴香酸配合物的合成与性质

本文合成了通式为ＲＥＬ３（ＲＥ３＋＝Ｐｒ３＋、Ｓｍ３＋、Ｔｂ３＋,,Ｌ＝对茴香酸根）的二元配合物．用元素分析、电导、ＩＲ、ＵＶ、ＴＧＤＴＡ等对其结构和性质进行了表征．该类配合物属桥式双齿配位     

采用NP催化剂的芥酸氢化制备山嵛酸工艺研究

本文制备了高效加氢ＮＰ催化剂,并讨论了芥酸采用该催化剂加氢制备山嵛酸时,催化剂浓度、氢气压力、反应温度、搅拌速度等因素对反应的影响。试验结果表明其适宜的工艺条件为：催化剂浓度０．６％,氢气压力８．１１×１０５Ｐａ,反应温度４１３Ｋ,脉冲式搅拌速度８０次／ｍｉｎ。     

SAG法合成钛酸铅纳米晶粒的工艺和结构研究

ＳＡＧ法合成钛酸铅纳米晶粒的工艺和结构研究李永祥刘泽吴冲若（东南大学电子工程系,南京２１００９６）ＰｂＴｉＯ３是应用广泛的铁电和光电材料之－,研究ＰｂＴｉＯ３纳米晶粒的合成技术和电学性能对基础研究和新型复合功能材料研究都有重要意义．作者曾采用Ｓｏｌ...     

对巯基苯甲酸的合成

目的寻找简便经济地合成对巯基苯甲酸的方法．方法在常压条件下,将对氨基苯甲酸重氮化处理后,在多硫化钠的作用下,形成４,４′－二硫代二苯甲酸钠,经浓盐酸酸化后成４,４′－二硫代二苯甲酸．除去多余的硫后,用锌粉与冰醋酸还原,用碱液除去过量的锌,然后经酸化、洗涤、烘干成对巯基苯甲酸．结果经元素分析符合对巯基苯甲酸的化学式Ｃ７Ｈ６Ｏ２Ｓ,红外光谱及熔点测定证明为本产品．结论本方法原料易得,成本低,合成周期短,辅料可回收利用,得率较高,而且对环境无污染．