8－羟基喹啉纤维微柱分离富集ICP－AES测定多种痕量元素

制备了８－羟基喹啉纤维滤纸片，作为微柱填充物，同时富集了九种痕量元素，并分离了样品中的高盐组分。富集后的痕量组分采用电感耦合等离子体原子发射光谱法（ＩＣＰ－ＡＥＳ）测定，回收率为９０％～１０２％。     

ICP-AES法测定矿石中的BeO

报道了采用ICP－AES法测定矿石中的BeO。对试样的溶解进行了选择；考察了其体和无机酸对测定的影响。采用基体匹配法进行测定。在优化条件下，对三个试样进行测定，其相对标准偏差（n=9）为0.28%；回收率为97％－103％。     

ICP-AES法直接测定金属钕、氧化钕中的稀土和非稀土杂质元素

建立了金属钕和氧化钕中24个杂质元素的高频感耦等离子体原子发射光谱直接测定的方法。配制了3组可混听多元素标准溶液，采用基体匹配法和多组分光谱拟合（MSF）技术以消除基体光谱干扰。测定元素的回收率为96．8％－104．0％，精密度为0．92（Ti)%-6.9(Ca)%.     

银杏叶中聚异戊烯醇化合物的分光光度法测定

基于秋加耶夫（Chugaev）反应，采用分光光度法测定银杏叶中聚异戊烯醇化合物含量；以ZnCl2的CH3COOH溶液－CH3COCl（体积比10：1）为显色剂，通过在388nm处测定溶液的吸光度确定聚异戊烯醇化合物的含量；聚异戊烯醇化合物在0．103－2．060mg范围内与吸光度值有良好线性关系；方法的回收率为97％－103％，相对标准偏差（RSD）为5．7％；方法简便、快速。     

饮料食品中Ge－132和Ge~（4＋）含量测定研究

本文报告了在０．０１ｍｏｌ／ＬＣＴＡＢ体系中，以Ｆ－为掩蔽剂、苯芴酮显色、用分光光度法测定饮料食品中Ｇｅ－１３２含量，最低检测限０．０５４μｇ／ｍＬ；线性范围０．５４～２７．１４μｇ／ｍＬ；回收率９６．３％～１０１．５％，并确定了Ｇｅ－１３２摩尔吸收系数（ε）３．３９×１０４。用本法测定了康寿茶、矿泉水和博士奶中Ｇｅ－１３２含量，灵敏度高、重现性和准确度好。用盐酸化本体系，研究了二氧化锗（Ｇｅ~（４＋））的含量测定，其最低检测限０．０２１μｇ／ｍＬ；线性范围１．０～２１．０μｇ／ｍｌ；回收率９５．８％～１０２．８％，Ｇｅ－１３２不干扰。饮料食品中同时存在Ｇｅ－１３２和Ｇｅ（４＋）时，本体系可分别测定两者含量。     

锆存在时铀中杂质元素的化学分离-ICP-AES法

采用磷酸三丁酯（TBP）－氢化煤油萃取油、过氧化氢掩蔽钛、磷酸氢二铵沉淀锆的方法，用ICP－AES法同时测定了锆存在在时铀中的铁、锰、铜、硅、铝、镍和钛7种杂质元素的含量。当测定范围在100μg/g-1000μg/g时，相对标准偏差＜9．0％，回收率为96％－109％。     

甘薯中微量钙铁的原子吸收分光光度法测定

研究了用原子吸收分光光度法测定甘薯中的微量钙、铁的含量；采用高温灰化法对样品进行处理，并对40多种不同品种和不同种植地区的甘薯进行了实样测定和含量差异比较；对9个样品进行钙和铁的加标回收试验，测定的回收率在91％－107％之间，相对标准偏差RSD（n=9)分别为4．6％、5．4％，结果令人满意。     

微分电位溶出法测定人发中铜铅镉锌的研究

本文报道了０．００２５ｍｏｌ·Ｌ￣（－１）ＨＣｌ－０．２ｍｏｌ·Ｌ￣（－１）ＮＨ＿（４）Ｃｌ底液中连续测定人发中铜、铅、镉、锌的微分电位溶出法。四元素峰电位分别为－０．２０Ｖ，－０．４６Ｖ，－０．６７Ｖ，一１．０２Ｖ（ＳＣＥ），峰形好，灵敏度高，干扰少，测定发样相对标准偏差≤４．３％，回收率为９７．６％～１０４．６％。并对ＨＮＯ＿３－ＨＣｌＯ＿４和ＨＮＯ＿（３）Ｈ＿（２）Ｏ＿２消化发样进行了比较。     

ICP-AES法同时测定石英砂中的痕量元素

采用微波溶样，并通过条件试验，建立了微波溶样ICP－AES法同时测定石英砂中13种痕量元素的分析方法并已应用于实际样品的分析，方法的相对标准偏差≤10％，加标回收率为90％－107％。     

氢化物发生-冷阱捕获-色谱分离-原子吸收法测定天然水中砷的形态

研究建立了氢化物发生－冷阱捕获－色谱分离－原子吸收方法测定天然水中四种主要砷形态。测试系统自行组装，色谱住填料采用ChromosorbGAW－DMCS（粒径0．3～0．45mm），其上涂布3％OV－101。方法的检出限以砷计分别为：As（V）0．51ng，As（Ⅲ）0．43ng，MMA0．38ng，DMA067ng；12ng砷标准偏差As（Ⅴ）4．21％，As（Ⅲ）3．56％，MMA3．23％，DMA5．46％。在0～50ng砷量范围标准曲线线性关系良好。该法适用性广，已用于湖水、河水、海水和地下水等不同水样神形态测定，加标回收率93．5％～104．9％。给出了上述水样四种砷形态的分析结果。     

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.