邻苯三酚红修饰碳糊电极吸附伏安法测定痕量铋

报道了采用邻苯三酚红修饰碳糊电极测定痕量铋的方法。在０．３０ｍｏｌ／Ｌ的ＨＣｌ溶液中,于－０．１０Ｖ搅拌富集３ｍｉｎ,然后在－０．３５Ｖ静止还原６０ｓ,再进行阳极化扫描,在－０．１０Ｖ左右获得灵敏的铋溶出峰,二次导数民流与铋浓度在１．０＊１０＾－９－６．０＊１０＾－７ｍｏｌ／Ｌ范围内呈线性关系,同限为５＊１０＾－１０ｍｏｌ／Ｌ。对电极反应机理进行了讨论。     

KBrO3—KBr紫外分光光度法测定痕量水杨酸

研究了ＨＣｌ溶液中ＫＢｒＯ３－ＫＢｒ紫外分光光度法测定水杨酸的条件,建立了测定痕量水杨酸的新方法。结果表明,在０．６ｍｏｌ／ＬＨＣｌ,３＊１０＾－５ｍｏｌ／ＬＫＢｒＯ３,５＊１０＾－４ｍｏｌ／ＬＫＢｒ,６＊１０＾－４ｍｏｌ／ｌＫＩ溶中测定水杨酸,其线性范围为０．２－４．０ｍｇ／Ｌ,表观摩尔吸光系数为１．９＊１０＾－４Ｌ．ｍｏｌ＾－１．ｃｍ＾－１,Ｓａｎｄｅｌｌ为７．３μｇ／ｃｍ＾２。ｓｇ ｉｆ ｅ     

依诺沙星在混合粘合剂碳糊电极上的电化学特性

制备了混合粘合剂碳糊电极。在０．０１５ｍｏｌ／Ｌ，磷酸－０．１０ｍｏｌ／ＬＫＣｌ溶液中，依诺沙星在该电极上于－１．２６Ｖ处产生一灵敏的阴极溶出伏安峰。在－０．９０Ｖ富集９０ｓ后，依诺沙星的线性范围为３．１×１０＾－７－１．２×１０＾－５ｍｏｌ／Ｌ，检测下限为９．４２×１０＾－８ｍｏｌ／Ｌ，所提出的方法用于尿液和血清中依诺沙星测定，回收率在９６％－１０３％之间。     

碳糊电极测定甲硝唑的研究

报道了用碳糊电极测定甲硝唑的方法。在ｐＨ３．２的ＬｉＣｌ－ＨＣｌ电解溶液中，用二次导数阴极溶出伏安法测定甲硝唑。在碳糊电极上开路富集甲硝唑６０ｓ，然后记录其在－０．５８Ｖ的二次导数阴极溶出峰。溶出峰电流ｉｐ与甲硝唑浓度在３．０×１０－７～３．０×１０－６ｍｏｌ／Ｌ和３．０×１０－６～１．０×１０－４ｍｏｌ／Ｌ范围内呈良好的线性关系，相关系数分别为０．９９８６和０．９９９７，检出限为１．７×１０－７ｍｏｌ／Ｌ，相对标准偏差为６．０％（ｎ＝１０）。本方法直接用于甲硝唑片剂的测定，并用多种方法对甲硝唑在碳糊电极表面的反应机理进行了探讨。     

博莱霉素A5的示波极谱行为及测定

在０．０５ｍｏｌ／Ｌ Ｈ２ＳＯ４支持电解质中，博莱霉素Ａ５出现二个示波极谱导数还原峰，峰电位Ｅｐ１＝－０．８２Ｖ和Ｅｐ２＝－１．０８Ｖ（ｖｓ．ＳＣＥ）。峰电流ｉｐ１比峰电流ｉｐ２小得多。ｉｐ２与博莱霉素Ａ５的浓度在５．０＊１０＾－８－４．０＊１０＾－６ｍｏｌ／Ｌ范围内呈线性关系；检出限为１．０＊１０＾－８用于老鼠血样中博莱霉素Ａ５含量的测定，得到满意的结果，对第二个峰的电化学行为作了初步探讨。     

痕量多巴酚丁胺在碳糊电极上的吸附伏安行为及其痕量？…

在０．１ｍｏｌ／Ｌ Ｈ２ＳＯ４底液中，用碳糊电极吸附伏安法测定多巴酚丁胺，阳极峰电位为０．４６Ｖ，峰电流与多巴酚丁胺的浓度在３．０×１０＾－９－１．０×１０＾－６ｍｏｌ／Ｌ范围内呈良好的线性关系。     

PVC膜修饰粉末微电极溶出伏安法测定水中铅(Ⅱ)

介绍一种ＰＶＣ膜修饰粉末微电有的溶出伏地。该法不需镀汞,不需搅拌,且可在浓度很稀的支持电南中富集。在浓度为０．０２ｍｏｌ／ＬＨＡｃ介质中,进行阳极溶出伏安扫描,有一灵敏Ｐｂ氧化出现,峰电位为－０．４５３Ｖ,溶出峰电流Ｐｂ＾２＋的质量浓度在５．０×１０＾８￣５．０×１０＾－６ｇ／ｍＬ,范围内有很好的线性关系,检出限为２．０×１０＾－８ｇ／ｍＬ。该法应用于逢来水和湖水中微量Ｐｂ＾２＋的直接测定,测定结     

单扫描极谱法连续测定人发中的微量元素锌铁锰铜

本提出在０．１５ｍｏｌ／Ｌ乙二胺－７．５×１０＾－３ｍｏｌ／Ｌ三乙醇胺－２．５×１０＾－２ｍｏｌ／Ｌ硫氰酸钾底液中单扫描极谱法测定锌、铁、锰，续加硫酸（０．３ｍｏｌ／Ｌ）测定铜的方法，峰电位分别为－１．４２Ｖ，－１．６３Ｖ，－１．７１Ｖ，－０．４８Ｖ（ｖｓ．ＳＣＥ），线性范围：０．０５～１．４μｇ／ｍＬＭｎ，０．０４～１μｇ／ｍＬＣｕ，最低检出浓度．０３，０．０５，０．０２，０．０４μｇ／ｍＬＭ     

阴极溶出伏安法测定异烟肼的研究

报道了吸附阴极溶出伏安法测定异烟肼。探讨了电极反应机理。在０．０１ｍｇｏｌ／Ｌ硼砂底液中，峰电位为－１．４０Ｖ。峰电流与异烟肼浓度在４．０＊１０＾－７－１．５＊１０＾－５ｍｏｌ／Ｌ范围内呈良好的线性关系，相关系为０．９９１３。该方法用于异烟肼片剂的测定，获得满意结果。     

α—苯偶酰二肟修饰碳湖电极的制备及对合成水样中铜的测定

报道了α－苯偶酰二肟修饰碳湖电极的制 及对合成水样中铜的测定,在ＰＨ４．１的Ｂ－Ｒ缓冲溶液中通过在－１．２０Ｖ电位下富集Ｃｕ＾２＋后,在－０．２￣＋０．２电位一范围内作阳极溶出伏安法测定。在＋０．０４８Ｖ处有一灵敏的氧化峰,峰电流与Ｃｕ＾２＋浓度在１×１０＾－７￣１×１０＾ｍｏｌ／Ｌ范围内成良好的线性关系,检出限为５×＾－８ｍｏｌ／Ｌ。     

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.