分散第二相ZrO2对PESC—NaSCN络合物导电性能的影响

在聚丁二酸乙二酯－硫氰化钠（ＰＥＳＣ－ＮａＳＮＣ）络合物中了掺入分散第二相ＺｒＯ２，而ＺｒＯ２的含量及颗粒度对络合物电导率的影响很大。当颗粒度为０．５３７μｍ左右时，电导率比较ＰＥＳＣ－ＮａＳＣＮ高两个数量级，颗粒度为１．４３５μｍ和２．４３７μｍ左右时，电导率均比纯ＰＥＳＣ－ＮａＳＣＮ低。ＺｒＯ２与络合物重量比为０．３０时，电导率最大。这种现象可用空间电荷层的高电层层理论的连续沟通模型来解释。     

不同组成的铕—噻吩甲酰基三氟丙酮络合物合成与荧光特性

本文合成与铕与ＴＴＡ及啉啡罗啉或表面活性剂Ｎ－氯代十六烷基吡啶两个三元络合物及铕－ＴＴＡ两元络合物。用元素分析，差热热重分析，红外与紫外光谱等方法表征了各化合物。测定了各络合物的固态及溶液荧光光谱，实验表明高对称八配位的Ｅｕ（ＴＴＡ）４ＣＰ络合物荧光强度最高。     

显色剂交换萃取光光度法测定微量铜

用三氯甲烷萃取Ｃｕ－ＤＤＴＣ络合物，然后在ｐＨ＝９．２三羟甲基氨基甲烷（Ｔｒｉｓ）缓冲液中用５－Ｂｒ－ＰＡＤＡＰ交换络合物中ＤＤＴＣ，形成了Ｃｕ－ＰＡＤＡＰ络合物。该络合物最大吸收波长λｍａｘ＝５２０ｎｍ，表观摩尔吸光系数ε５２０＝１．２２×１０＾５，铜量在０．２￣１０．０μｇ／１２ｍｌ范围内服从比耳定律。本法应用于食品、生物材料中微量铜测定，得到较为满意的结果。     

高分子因体电解质研究进展

评述了高分子固体电解质的形成，分类，应用及离子传输机理的研究，并结合有关ＳＰＥ新材料制备、ＰＥＯ／盐络合物晶体结合全测定，离子传输机理探索及电化学器件应用等方面的最新报道对ＳＰＥ未来研究方向进行展望。全文引用８４篇文献。     

偏最小二乘光度法同时测定铜和铁的研究及应用

７－（１－苯偶氮）－８－羟基喹啉－５－磺酸钠在ＰＨ＝４．７５ＨＡｃ－ＮａＡｃ缓冲溶液中能与Ｃｕ（Ⅱ）和ＦＥ（Ⅲ）形成稳定的络合物，本文研究了Ｃｕ（Ⅱ）－ＰＡＨＱＳ、Ｆｅ（Ⅲ）－ＰＡＨＱＳ体系的显色条件，以偏最小二乘法处理两者重叠吸收峰，建立了光度法同时测定铜和铁的方法。     

乙丙三元橡胶磺酸钴离聚体膜的富氧性能研究

通过磺化、中和反应制备了乙丙三元橡胶（ＥＰＤＭ）磺酸钴离聚体（Ｃｏ（Ⅱ） Ｓ ＥＰＤＭ）膜并研究了其富氧性能．结果发现，该膜对分子氧具有促进输送作用，其原因被认为是在离聚体中可能形成了一种高分子钴络合物结构．这种络合物在其空位上能够与分子氧进行快速可逆的结合．ＥＳＲ谱提供了钴氧结合的证据     

新型梳状高分子固体电解质的研究（Ⅱ）

新型梳状高分子固体电解质的研究（Ⅱ）丁黎明，林云青，梁洪泽，汪东梅，王佛松（中国科学院长春应用化学研究所长春１３００２２）关键词梳状高分子，ＮａＣＩＯ＿４络合物，固体电解质，离子电导率聚环氧乙烷（ＰＥＯ）可以溶解多种碱金属盐并形成络合物，这种络合物具...     

铜电解液中锑铋的测定

电解液中锑、铋通常以沉淀法富集分离后,用碘化钾光度法测定铋;用结晶紫萃取光度法测定锑,方法不甚简便。锑、铋与碘化钾和硫脲均能生成黄色络合物,可用作各自的光度法测定,但两元素相互干扰严重。我们考察了酸度对锑、铋与碘化钾和硫脲络合物显色的影响。试验结果如图所示,铋络合物显色不受酸度影响,而锑络合物显色则明显受酸度影响。在     

铂微粒修饰固体石蜡碳糊电极对过氧化氢的电催化及分析应用

1　引　　言碳糊电极 (ＣＰＥ)与金属电极相比具有电位窗较宽、残余电流小、表面易更新修饰、制备简便等优点。在ＣＰＥ表面修饰金属微粒作为氧化还原中心 ,既保持了金属电极特点又通常比一般金属电极更具催化活性 ,在物质的测定中具有较高的灵敏度。但常见的ＣＰＥ为液体石蜡作粘合剂的碳糊电极 (ＬＣＰＥ) ,在其表面沉积的金属微粒易随碳粒脱落而损失 ,导致测定的重现性变差。固体石蜡碳糊电极 (ＳＣＰＥ)相比于ＬＣＰＥ能降低过电位、表面光洁稳定、重现性好 ,因此ＳＣＰＥ的研究应用近来受到关注。我们曾利用ＳＣＰＥ制成了硅钼酸和磷钼…     

稀土三元络合物的极谱研究：II.Eu（Ⅲ）—Cit—Ap体系稳定常数的测定

本实验用直流极谱法研究了Ｅｕ（Ⅲ）－Ａｐ，Ｅｕ（Ⅲ）－Ｃｉｔ二元体系和Ｅｕ（Ⅲ）－Ｃｉｔ－Ａｐ三元体系的极谱行为，在μ＝０．１（ＮａＮＯ３），ｔ＝２５±０．２℃条件下，电极过程为准可逆；测定了该条件下二元及三元络合物的稳定常数，讨论了三元络合物的有关形成条件。     

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.