新型酸碱通用滴定器研制成功

西南石油学院化工系陈集等人研制了一种新型的酸碱通用滴定器。这种通用滴定器能迅速准确地加液调零,灵活自如地控制滴定过程,具有较高的精密度和准确度,克服了老式滴定管漏液、沾污、堵塞、终点液滴难以控制、加液调零     

一种新型气压式滴定仪的研制

介绍一种新型气压式滴定仪的结构、性能、特点及使用方法。该仪器能迅速、准确地加液调零,使用方便,克服了旧式滴定管漏液、取液时易玷污、加液调零较麻烦等缺点,在适当的情况下还可以作为移液管使用。     

微型滴定分析装置的研究

微型滴定分析装置的研究朱兵吴倩（华东师范大学化学系上海２０００６２）一、微型滴定装置的设计制作和特点在设计制作微型试剂滴瓶、电解装置、焰色反应器、固液分离器和定量加液管等多种微型器件的基础上［１，２］，设计制作能规范操作的微型滴定分析装置，其主要部件...     

零流电位法在酸碱滴定中的应用研究

探讨了零流电位法在酸碱滴定中的检测原理及应用,通过考察强碱滴定弱酸、强碱滴定强酸、强酸滴定弱碱以及强酸滴定强碱四种滴定体系,探明了零流电位法在酸碱滴定中的适用性。通过氢氧化钠滴定醋酸对本方法进行评价,实验结果表明:本法的相对误差为-0.4%,同一根电极的滴定值的相对标准偏差(RSD)为0.4%(n=5),同一根电极五天滴定值的RSD为0.6%,五根电极滴定值的RSD为0.5%。本方法具有较高的准确性、稳定性和重现性。     

氧化还原滴定理论处理的一种通用方法

氧化还原滴定理论处理的一种通用方法魏永巨，李克安，童沈阳（北京大学化学系，１００８７１）氧化还原滴定的计量关系远比酸碱与络合摘定复杂，因而，严格的理论处理比较困难￣［１］。特别是涉及到不对称电对的氧化还原滴定，通常难以对滴定过程中各组分的平衡浓度及相...     

广义氧化还原滴定

根据广义氧化还原新概念 ,提出了广义氧化还原滴定。广义氧化还原滴定包括酸碱滴定、沉淀滴定、配位滴定和氧化还原滴定。它们的滴定曲线可以由相同的原理绘出     

微型滴定在定量化学分析中的应用

本文在讨论微型滴定装置和滴定误差的基础上，探索了微型滴定在酸碱、络合、氧化还原和沉淀滴定中应用的可能性。结果表明，效果良好     

滴定分析

本文是《分析试验室》定期评述中“滴定分析”课题的第三篇文章,前两篇为“络合滴定”,本文扩大了内容,故改题为“滴定分析”,它述评了1987～1990年6月间国内滴定分析的进展。内容包括新方法和新技术、酸碱滴定法、络合滴定法(1988.7～1990.6)、氧化还原滴定法以及沉淀滴定法等。     

谈谈酸碱滴定教学中新知识的引进

对分析化学酸碱滴定教学中引进酸碱滴定通式的问题进行了讨论。通过实例表明,将酸碱滴定通式引入到教学中,有助于学生更完整正确地把握酸碱滴定的理论。     

质子平衡思想用于酸碱滴定终点误差的计算

现有的酸碱滴定终点误差计算方法归为两类,一类是针对不同滴定体系提出不同的计算公式;另一类是仿造林邦误差公式,但不同体系的终点误差计算公式形式上仍不相同。至今未有简明且通用的计算方法。本文从酸碱滴定反应的本质出发,首次明确提出了适用于所有酸碱滴定体系的终点误差计算方法,并做了深入的论证。即只需写出化学计量点时滴定产物的质子平衡式,左右两式之差即为滴定终点误差。简明通用,可大大简化相应的教学内容。     

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%.     

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.     

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.     

A general and convenient synthesis of 4-(tosylmethyl)semicarbazones and their use in amidoalkylation of hydrogen,heteroatom, and carbon nucleophiles

A general synthesis of previously unknown semicarbazone-based α-amidoalkylating reagents, 4-(tosylmethyl)semicarbazones, has been developed. The synthesis involved three-component condensation of semicarbazones of aliphatic or aromatic aldehydes with the same or other aldehydes and p-toluenesulfinic acid. The scope and limitations of this reaction were investigated. The compounds obtained were demonstrated to be an efficient α-(4-semicarbazono)alkylating agents. They were reacted with H- (sodium borohydride), O- (sodium methylate), S- (sodium phenylthiolate), N- (pyrrolidine, sodium succinimide), P- (trialkyl phosphites), and C-nucleophiles (sodium diethyl malonate) to give the corresponding products of the tosyl group substitution, 4-substituted semicarbazones, including analogues of nitrofurazone. Among the prepared compounds tested in vitro for antibacterial and antifungal activity, three nitrofuryl-containing semicarbazones exhibited high biological activities with minimum inhibitory concentration (MIC) values of 8–32 μg/mL.     

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.     

Synthesis of novel chiral bidentate hydroxyalkyl-N-heterocyclic carbene ligands and their application in palladium-catalyzed Mizoroki–Heck couplings and asymmetric addition of diethylzinc to benzaldehyde

A small library of new chiral bidentate hydroxyalkyl-imidazolium salts 1 is conveniently synthesized on multi-gram scale from inexpensive and commercially available chiral pool amino acids. The corresponding carbenes, generated by deprotonation of imidazolium salts 1, in combination with palladium(II) chloride were tested in the Mizoroki–Heck coupling reaction. The most significant results in terms of yields and reactivities were achieved with low catalyst loading. The catalytic activities of these imidazolium salts were also investigated in the asymmetric addition of diethylzinc to benzaldehyde. The use of MgO nanoparticles as an additive in conjunction with these ligands played a crucial role in increasing the efficiency of these reactions.