催化动力学光度法测定钌

在磷酸介质中,痕量钌（Ⅲ）对溴酸钾氧化二安替比林对氨基苯基甲烷（DApAM）的显色反应具有明显的催化作用,研究了反应的最佳条件,并测定了一些动力学参数,据此建立了一种测定痕量钌（Ⅲ）的新方法,其检测限为2．10×10－9g／mL,针含量在0－20μg／L内符合比尔定律,方法用于贵金属精矿中痕量钌的测定,结果满意。     

The Simultaneous Spectrophotometric Determination of Osmium and Ruthenium

Abstract

A spectrophotometric procedure is described for the simultaneous determination of osmium and ruthenium in the form of bromo complexes. It was found that a blue ruthenium-thiourea complex could be formed in 6.7 M HBr solutions while the osmium could be maintained as the hexabromoosmate complex. Absorption maxima were at 620 μ for the ruthenium complex and at 446 μ for the osmium complex. Molar absorptivities for the ruthenium complex were 2.47 × 10³ at 620 μ and 763 at 446 μ. For the osmium complex molar absorptivities were 328 at 620 μ and 6.81 × 10³ at 446 μ. The method is useable over the range of 5 to 30 ppm with an absolute error of = 1 ppm over the range. Other platinum metals interfere.     

Spectrophotometric Determination of Trace Ruthenium with Molybdate and Ethyl Rhodamine B

Spectrophotometric determination of trace Ru(Ⅲ) with molybdate had been reported by references. Its sensitivity is much better. However, the colour reaction of ion-association complex of Ru(Ⅲ)-molybdate-rhodamine B(ERB) system has not been reported till now.     

对碘偶氮氯膦-高碘酸钾-钌(Ⅲ)的褪色反应用于痕量钌的催化分光光度法测定

在Ｈ２ＳＯ４ 介质中对碘偶氮氯膦与高碘酸钾的褪色反应只有在痕量钌（Ⅲ）的存在下才能定量进行。本文研究了该褪色反应的最佳条件及用于痕量钌的测定方法, 其检出限为０．０２ μｇ·１０ ｍ Ｌ－ １, 钌含量在０．０２～０．３０ μｇ·１０ ｍ Ｌ－ １范围内符合比尔定律。该方法用于贵金属精矿中钌含量的测定, 获得满意结果。     

流动注射催化分光光度法测定钌的研究

利用钌（Ⅲ）对过氧化氢氧化还原型百里酚酞显色反应的显著催化作用，建立了钌的新流动注射催化分光光度分析法，该法快速灵敏、简便，用于实际样品分析，结果良好。     

Complexes of Ruthenium and Osmium with 4-Amino-2-Mercapto-5-Nitroso-6-Pyrimidinol

Ruthenium(III) and osmium(VIII) form coloured complexes with 4–amino ?2-mercapto-5-nitroso-6-pyrimidinol (ammonium salt). The complexes have been spectrophotometrically studied and made use of in determination of the two metals; the reaction with ruthenium is particularly sensitive (0.006 μg of ruthenium/cm²for 0.001 absorbance). Many ions do not interfere in the determination.     

二安替比林对二甲氨基苯基甲烷-高碘酸钾催化光度法测定痕量钌

在磷酸介质和加热条件下,钌（Ⅲ）对高碘酸钾氧化二安替比林对圩甲氨基苯基甲烷（ＤＡＭＡＭ）的显反色应脸强催化作用,建立了催化动力学光度法测定痕量钌的新。方法的线性范围为０－５．４μｇ／Ｌ;检出限为２．１６＊１０＾－８ｇ／Ｌ;对２μｇ／Ｌ的Ｒｕ（Ⅲ）测定的ＲＳＤ为２．２９％（ｎ＝１１）。催化反应的表观活能为９２．２３ｋＪ／ｍｏｌ。考察了４０多种共存离子的影响。大多数常见离子不干扰测定。本法已用于矿样中     

高碘酸盐氧化罗丹明B催化光度法测定钌

在０．７２ｍｏｌ／Ｌ磷酸和９０℃水浴条件下,钌催化高碘酸盐氧化罗丹明Ｂ（ＲＢ）,据此建立了高灵敏催化光度测定钌的方法。方法的检出限为８．０×１０＾－１２ｇ／ｍＬ,测定范围为０．２～１５ｎｇ／２５ｍＬ,对５、１０、１５ｎｇ／２５ｍＬＲｕ（Ⅲ）测定的相对标准偏差分别为８．６７％,５．９４％和１．８５％。本反应对Ｒｕ（Ⅲ）、ＲＢ、ＫＩＯ４和Ｈ３ＰＯ４均为一级反应,表观活化能为３６．０５ｋＪ／ｍｏｌ。１３     

Spectrophotometric Determination of Microamounts of Ruthenium Using 2-(3,5-Dichloro-2-Pyridylazo)-5-Dimethylaminophenol and its Application

Binary component colour systems of spectrophotometric determination of Ru using heterocyclic-azo reagents have been reported, but their apparent molar absorptivities are low.     

Spectrophotometric Determination of Ruthenium in Solutions of Nitroso and Sulfate Complexes Using Microwave Radiation

It has been shown that ruthenium can be determined in solutions of ammonium nitrosopentachlororuthenate (NH₄)₂[Ru(NO)Cl₅] with nitroso and aquachloro complexes present simultaneously by its reaction with 1,10-phenanthroline and in solutions of sulfate complexes using microwave radiation. It is found by molecular absorption and luminescence studies that the composition of the complex formed corresponds to ruthenium(II) tris-(1,10-phenanthrolinate) {[Ru(Phen)₃]²⁺}. The complexation time is decreased by several tens of times (down to 5 min) compared to conventional heating, and a 100% yield of the complex is achieved. In the presence of HCl, the conversion of nitroso species to aquachloro ruthenium complexes upon microwave irradiation is inefficient. It is found that, compared to [Ru₂OCl₁₀]^4–, [Ru(NO)Cl₅]^2– is more labile in the complexation reactions of ruthenium with 1,10-phenanthroline under microwave irradiation. Regardless of the concentration of H₂SO₄ (1.7–12 M) in the starting solutions, ruthenium sulfate complexes can be converted in a microwave field to more labile chloride complexes.     

Simple Selective Spectrophotometric Method for the Determination of Ruthenium in Carbon Supported Pt-Ru-Ge Catalyst

ABSTRACT

A simple spectrophotometric method for the determination of ruthenium in the presence of platinum in Pt-Ru-Ge catalyst applied in fuel cells has been developed. Platinum catalyst (20% Pt) with carbon support containing 0.5% Ru and 5% Ge was digested in the mixture of HCl+HNO₃ (6+1). Carbon was separated from the examined sample by filtration after dissolution of the metals. Ruthenium was converted into a complex with thiourea (λ_max=640 nm, ε = 2.9·10³ 1 mol^?1 cm^?1) in the medium of 5 M in HCl and 1% in thiourea after 15 min heating at 70 °C. Platinum does not interfere with the determination of ruthenium. Germanium is converted into volatile GeCl₄ and escapes from the examined sample during the digestion step. The content of ruthenium determined in the examined samples of catalyst amounted to 0.49% (RSD = 0.14%).     

Spectrophotometric and First Derivative Spectrophotometric Determination of Magnesium with 1-Hydroxy-2-Carboxyanthraquinone

Abstract

1-Hydroxy-2-carboxyanthraquinone reacts with magnesium in ethanol-water mixtures to form a red complex having an absorption maximum at 490 nm in alkaline medium. A detailed study of the characteristics of this complex has been carried out and a spectrophotometric method for the determination of magnesium at the 0.4–4.0 μg ml^?1 level is proposed. The method has been sensitized by employing first derivative spectrophotometry. By the use of the derivative approach magnesium can be determined between 0.08–0.40 μg ml^?1. Statistical analysis of the results is also described.     

Chemistry of 2-Amino-3-cyanopyridines

This review presents a systematic and comprehensive survey of the method of preparation and the chemical reactivity of 2-amino-3-cyanopyridines. The target compounds are important intermediates for the synthesis of a variety of synthetically useful and novel heterocyclic systems.     

3-氨基-2-烯亚胺化合物的合成

芳胺和芳酮所形成的希夫碱在无水三氯化铝或二异丙胺锂与氯化锌乙醚溶液存在下和腈类化合物加成,制备了一些文献中未报导过的3-氨基-2-烯亚胺,并经元素分析、1H NMR,13C NMR和MS确证.     

Reactions of 2-Monosubstituted 3-Amino-2H-azirines with NH-Acidic Heterocycles

2-Monosubstituted 3-amino-2H-azirines 2 react with several heterocycles containing acidic NH groups via ring expansions, leading to benzo[g][1,2,5]thiadiazocin 1,1-dioxide derivatives 6 and imidazoles 9, 10 , and 13 , respectively.     

耐尔蓝-高碘酸钾催化光度法测定痕量钌

在磷酸介质和加热条件下,钌（Ⅲ）对高碘酸钾氧化耐尔蓝（ＮＢ）有强催化作用,详细研究了动力学条件,建立了动力学光度测定钌的新方法,１g（Ａ０／Ａ）与ＣＲu（Ⅲ）呈线性关系的范围为０．００８～１．２ｕｇ／Ｌ,检出限为０．００８ｒｇ／Ｌ,对０．００８和０．８ｕｇ／ＬＲｕ（Ⅲ）测定的ＲＳＤ分别为１４．３０％６和１．７３（n＝１１ ）。本催化反应对Ｒu（Ⅲ）、ＮＢ和ＫＩＯ４为一级反应,表观活化能为７３．４３ＫＪ     

甲基绿褪色分光光度法测定维生素K3

在pH8.7~9.5的弱碱性介质中,维生素K3(VK3)能使甲基绿发生褪色反应,其最大褪色波长为630nm,并在紫外区出现两个新的吸收峰,其褪色程度(ΔA)与VK3浓度在0·11~2·40mg/L的范围呈正比,可用于VK3的分光光度测定。方法具有很高的灵敏度,其表观摩尔吸光系数ε630=2·13×105L·mol-1·cm-1;对VK3的检出限(3σ)为32·0μg/L。方法有较好的选择性,可用于某些药物制剂及血药中VK3含量的测定。     

Synthese von in 2-Stellung substituierten 2-Amino- und 3-Amino-1-indanonen

An examination has been made of the reaction of secondary amines with 2-bromo-1-indanones II substituted at position C-2, and with 2-substituted indenones III. 2-Bromo-2-methyl-1-indanone (IIa) and dimethylamine yielded a mixture of the corresponding 2- and 3-amino-methylindanones IVa and Va. 2-Bromo-2-methyl-6-chloro-1-indanone (II b) and morpholine gave a mixture of the 2- and 3-aminocompounds IVe and Ve.