氧化邻苯三酚红褪色光度法测定食盐中碘

１引言 碘是人体必需营养元素之一,成年人缺碘会导致甲状腺机能亢进,患大脖大病,小孩缺碘会导致甲状腺发育不良,生长发育迟缓,智力低下,甚至于痴呆。食盐中加碘是防止碘缺乏病最主要、最经济、最简单的方法。测定微量碘最常用的方法是重铬酸钾法,也有用催化光度法、离子色谱法、离子选择性电极法等。基于国家有关规定,碘盐中所加人的碘必须以碘酸钾形式,本文利用在酸性介质中,碘酸根能氧化邻苯三酚红使之褪色,且褪色的程度与碘酸根的存在量有关,从而建立了光度法测定碘的新方法。实验表明,在０．３６～０．９６ ’ｍｏｌ／ＬＨ…     

催化动力学光计法测定微量碘的研究

基于微量碘离子对高碘酸钠氧化甲基紫反应的催化作用，建立了测定微量碘的动力学光度法。方法检出限０．２２μｇ／ｍＬ线性范围０．３０－１．４０μｇ／ｍＬ，包括其它卤素在内的大多数阴离子、阳离子不干扰测定，用于食盐中微量碘的测定，有满意的结果。     

催化动力学光度法测定微量碘的研究

基于微量碘离子对高碘酸钠氧化甲基紫反应的催化作用，建立了测定微量碘的动力学光度法。方法检出限０．２２μｇ／ｍＬ，线性范围０．３０～１．４０μｇｍＬ，包括其它卤素在内的大多数阴离子、阳离子不干扰测定，用于食盐中微量碘的测定，有满意的结果。     

利用压电频移法测定水中的痕量亚硝酸盐

提出了利用压电频移法测定亚硝酸盐的方法。方法以碘离子与亚硝酸根之间的氧化还原反应为依据，通过测定由反应生成的碘所引起的压电晶体频率的变化，在被萃取水相中亚硝酸盐浓度为０．００９￣２．３ｍｇ／Ｌ范围内，频移值与浓度成正比：ΔＦ＝５．８＋２．５×１０＾３Ｃ（ｍｇ／Ｌ），ｒ＝０．９９０１。方法简便，用于天然水中亚硝酸盐的测定，结果令人满意。     

异硫氰酸荧光素荧光猝灭法测定痕量碘酸根

碘酸根与碘离子反应生成游离碘使异硫氰酸荧光素的荧光猝灭,λｅｘ为４８７ｎｍ,λｅｍ为５１７ｎｍ,碘酸根含量在２－８μｇ／Ｌ范围内与荧光猝灭程度有良好线性关系,检测限为０．７４μｇ／Ｌ,该法灵敏度高,操作简便,用于含碘含盐中微量碘酸根的测定,结果满意。     

二甲酚橙褪色光度法测定微量碘的研究

研究了在硫酸介质中,溴化钾催化下,碘酸根氧化二甲酚橙褪色的最佳条件。其最大吸收波长λmax为430nm,表观摩尔吸光系数为1．3×104L·mol-1·cm-1,碘浓度在0-30μg／25ml范围内呈线性关系。方法用于测定加碘食盐中碘,回收率可达98．0％-101．3％,结果满意。     

催化光度法测定痕量亚硝酸根的研究：溴酸钾—结晶紫体系

基于在稀磷酸介质中，亚硝酸根对溴酸钾氧化结晶紫的反应，具有催化作用，建立了测定痕量亚硝酸根的新催化光度法。方法检出限为８．０×１０－９ｍｇ／Ｌ，线性范围０．６～１２．０ｍｇ／２５Ｌ，回收率为９７％～１０２％。与其它方法相比，常见离子如Ｂｒ－、Ｉ－等的允许存在量大。用于地面水和地下水的测定结果满意。     

结晶紫选择电极的制备及催化电位法测定碘的研究

根据磷酸介质中碘离子催化高碘酸钠氧化结晶紫的氧化还原反应,应用自制的结晶紫选择电极跟踪紫的 度变化,对催化电位法测定碘进行了研究。测定碘离子 的线性范围为０．２０－５．５μｇ／２５ｍＬ,方法检出限为４．１＊１０＾－９ｇ／ｍＬ。该方法应用于测定食盐和饮用水中碘含量,ＲＳＤ〈４．１％,平均回收率为９５．１％。     

氯酸钾氧化鸡冠花红新催化光度法同时测定痕量钒（V）,铬（VI）

基于硫酸介质中，柠檬酸作活化剂，钒（Ⅴ）、铬（Ⅵ）催化氯酸钾氧化鸡冠花红褪色的反应，建立了催化光度同时测定痕量钒（Ｖ）、铬（Ⅵ）的新方法。研究了影响反应速率的最佳条件。本法测定钒（Ｖ）、铬（Ⅵ）的线性范围分别为０￣８μｇ／Ｌ和０￣０．６ｍｇ／Ｌ；检出限分别为１．７９×１０＾－７ｇ／Ｌ和２．３６×１０＾－５ｇ／Ｌ。用于测定环境水样、钢样及废水中的钒（Ⅴ）、铬（Ⅵ），结果令人满意。     

萃取催化光度法测定痕量铜

研究了在ｐＨ５．５的弱酸性介质中,利用邻菲罗啉活化铜（Ⅱ）催化过氧化氢氧化邻氨基酚显色的指示反应,用萃取平衡控制反应时间,水相中邻氨基酚的浓度和反应程度,建立了萃取催化光度法测定痕量铜的新方法。方法的线性范围为０．０００５０￣０．１０ｍｇ／Ｌ,检测限为５．０×１０＾－７ｇ／Ｌ。用于水和粮食中痕量铜的测定,结果满意。     

二氧化碳和丙烯直接合成甲基丙烯酸的NiPMo/TiO2催化剂的研究

用溶胶-凝胶法以磷钼酸(MPA)的镍盐溶液水解钛酸四丁酯制备了NiPMo/TiO2催化剂.使用ICP、 XRD、 TG-DTA、 IR、 TPD-MS和微反应技术研究了催化剂的化学组成、热稳定性、化学吸附性质和催化反应性能.杂多钼酸盐与TiO2通过O2-在TiO2表面发生了键合.在623 K下,杂多阴离子仍保持原有的Keggin结构.CO2在Lewis酸位Ni(Ⅱ)和Lewis碱位Ni-O-Mo的桥氧协同作用下生成CO2卧式吸附态Ni(Ⅱ)←O-(CO)←(O--Ni).丙烯有多种吸附态在催化剂上吸附.在563 K、 1 MPa和空速1500 h-1的反应条件下,丙烯的摩尔转化率为3.2%,产物MAA选择性为95%.     

Toward new camptothecins. Part 6: Synthesis of crucial ketones and their use in Friedländer reaction

In the context of the preparation of camptothecin and luotonin A analogs, the synthesis of some key keto-precursors and their use in Friedländer condensation are described. This paper also focuses on the stability of these keto intermediates and emphasizes the major differences between indolizinones and pyrroloquinazolinones series. Noteworthy is also the report of some original structures isolated as by-products of some experiments.     

CoFe2O4自形成磁性液体场致结构化对磁化的影响

The Langevin paramagnetic theory can’t describe the relation between magnetization of ferrofluids and applied magnetic field. The structuralization of ferrofluids, which is considered the main influence factor of the magnetization, is regarded. The part of magnetization works is deposited when the structure is forming. This action influences the magnetization of ferrofluids directly or indirectly. On the base of the “compressing” model, the Langevin function that usually describes the magnetization of ferrofluid is modified, and a well-fitted curve is obtained. An equation of the relation between the equivalent volume fraction after being “compressed” and the intensity of magnetic field is discovered, which approximately describes the process of magnetization. The relation between the approximate initial susceptibility and the volume fraction can be obtained from modified formula.     

Highly regioselective Buchwald–Hartwig amination at C-2 of 2,4-dichloropyridine enabling a novel approach to 2,4-bisanilinopyridine (BAPyd) libraries

The highly regioselective Buchwald–Hartwig amination at C-2 of the cheap and readily accessible reagent, 2,4-dichloropyridine with a range of anilines and heterocyclic amines is described. This new methodology is robust and provides a facile access to 4-chloro-N-phenylpyridin-2-amines on 0.25 mol scale. These intermediates undergo a further Buchwald–Hartwig amination at higher temperature to enable rapid exploration of the chemical space at C-4 and to provide a library of 2,4-bisaminopyridines.     

KMnO4-mediated oxidative CN bond cleavage of tertiary amines: Synthesis of amides and sulfonamides

KMnO₄-mediated oxidative CN bond cleavage of tertiary amines producing secondary amine was introduced, which was trapped by electrophiles (acyl chloride and sulfonyl chloride) to form amides and sulfonamides. The reaction could take place at mild condition, tolerating a wide range of function groups and affording products in moderate to excellent yields.     

Chemistry of heterocyclic compounds at the A. E. Favorsky Irkutsk Institute of Chemistry, Siberian Branch of the Russian Academy of Sciences, over 50 years (Review)

The review contains a concise historical account and information on the most significant researches undertaken by the staff at the A. E. Favorsky Irkutsk Institute of Chemistry, Siberian Branch of the Russian Academy of Sciences on the Chemistry of Heterocyclic Compounds. Dedicated to Academician of the Russian Academy of Sciences B. A. Trofimov on his 70th jubilee. Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 10, pp. 1443–1502, October, 2008.     

Sulfur-directed metal-free and regiospecific methyl C(sp3)–H imidation of thioanisoles

Regiospecific and direct imidation of the methyl C(sp³)–H bond of thioanisoles is realized under mild and metal-free conditions with N-fluorobis(benzenesulfonyl)imide as an oxidant and nitrogen source. Proposed mechanism suggests that thionium ion intermediates and a Pummerer-type reaction are involved. The imidation has advantages such as high step-economy, excellent functionality tolerance, and regiospecificity, giving structurally diverse imidation products.     

Selective syntheses of 2H-1,3-oxazines and 1H-pyrrol-3(2H)-ones via temperature-dependent Rh(II)-carbenoid-mediated 2H-azirine-ring expansion

The Rh(II)-catalyzed reaction of 2-carbonyl-substituted 2H-azirines with ethyl 2-cyano-2-diazoacetate or 2-diazo-3,3,3-trifluoropropionate provides an easy access to 2H-1,3-oxazines and 1H-pyrrol-3(2H)-ones. These compounds can be selectively prepared from the same starting material using temperature as the only varied parameter. The 2-azabuta-1,3-diene intermediate, a common precursor for both heterocyclic products, isomerizes into 2H-1,3-oxazine under kinetic control, while 1H-pyrrol-3(2H)-one is the sole product of the reaction at elevated temperatures. According to DFT-calculations a one-atom oxazine ring contraction involving ring-opening to a 2-azabuta-1,3-diene intermediate, followed by a 1,5- and 1,2-prototropic shift leads to the consecutive formation of imidoylketene and azomethine ylide, which then further undergo cyclization to the pyrrole derivative.     

Synthesis of 1-benzyloxypyrazin-2(1H)-one derivatives

Different approaches for the synthesis of 1-benzyloxypyrazin-2(1H)-one derivatives from simple amino acids have been investigated. A library of 33 precursors for the preparation of N-hydroxy pyrazinones was obtained in moderate to good yields.