毛细管气相色谱法同时测定水产品中的多氯联苯和有机氯农药残留量

建立了毛细管气相色谱法同时测定水产品中多氯联苯和有机氯农药的方法，用高氯酸与冰乙酸的混合溶液消化样品，以石油醚提取，浓硫酸净化后，用毛细管气相色谱法测定，方法的回收法为88％－110％，相对标准偏差为8％－19％（n=6)，检出限为0．08－0．60ug/kg，方法简便，快速，结果准确。     

示波极谱同时测定金属锌中铜和镉

本文提出了在ＨＣｌ－Ｈ３ＰＯ４－ＫＣｌ底液中示波极谱同时测定金属锌中铅，镉含量的方法，检测下限铅为０．１ｍｇ／Ｌ，镉为０．０１ｍｇ／Ｌ，铅、锡波形清晰，重现性好，试样中回标准回收，铅回收率为９９．２％～１００％，镉回收率为９５％～９８％，与标准方法比较，相对误差〈５％，方法准确，简便，快速，适用于金属锌中铅，镉的常规分析。     

ICPMS测定高纯氧化钇中痕量稀土杂质的研究

研究了直接电感耦合等离子质谱（ＩＣＰＭＳ）测定９９．９９９％纯度氧化钇中稀土杂质的方法，详细探讨了仪器工作参数对稀土元素的测定的影响，对各种干扰现象进行了研究，并提出定量校正方法，实验表明，加入内标元素可有效地克服基体效应、接口效应和仪器工作参数漂移的影响。方法的检出限为０．００３～０．０２ｎｇ／ｍｌ，变异系数（ＣＶ％）为０．２％～５．４％，回收率为９０％～１１５％。适合９９．０％～９９．９９９％     

氢化物—原子吸收光谱法测定六味地黄丸中砷和锑

本文建立了氢化物原子吸收光谱法测定六味地黄丸中砷和锑的方法。方法的相对标准偏差砷为１．３％，锑为１．６％，回收率在９０％－１１０％之间，检出限分别为砷０．０６ｎｇ／ｍＬ，锑０．１ｎｇ／ｍＬ，本方法可用于中成药中砷和锑的测定。     

示波极谱同时测定金属锌中铅和镉

本文提出了在ＨＣｌ－Ｈ＿３ＰＯ＿４－ＫＣｌ底液中示波极谱同时测定金属锌中铅、镉含量的方法，检测下限铅为０．１ｍｇ／Ｌ，镉为０．０１ｍｇ／Ｌ铅、锡波形清晰，重视性好。试样中加标准回收，铅回收率为９９．２％～１００％，镉回收率为９５％～９８％，与标准方法比较，相对误差＜５％。方法准确、简便、快速，适用于金属锌中铅、镉的常规分析。     

氢化物发生-原子荧光光谱法测定中草药中的微量砷

研究了氢化物发生-原子荧光光谱法测定中草药中微量砷的方法的最佳条件，以50g／L硫脲 50g／L抗坏血酸为预还原抗干扰剂，测定了10种中草药药品中的砷，方法检出限(3σ)为0．103μg/L，相对标准偏差为1．6％-3.2％，回收率为89．2％-112％。     

火焰原子吸收光谱法间接测定饲料预混硒中硒

研究了用火焰原子吸收光谱法间接测定饲料预混硒中硒，与其它方法比较，简单、快速，测定的相对标准偏差小于5．0％，回收率为96．3％-104．0％，检出限为0．0005％。     

流动注射在线萃取色谱分离原子吸收光谱法测定痕量铂

研究了流动注射在线分离富集原子吸收光谱法测定痕量铂的方法。以自制的GDX501-TBP萃取树脂为微型分离柱，在优化后的分离富集条件下，进样时间为60s，洗脱时间为45s。在线分离测定时间为3min，方法检出限为0．25μg/L，线性范围10—600μg/L，加标回收率为97．8％-103．6％，相对标准偏差3．49％-4．25％。方法已用于矿物管理样中铂的测定。     

氯化亚锡还原-硫氰酸铵快速光度法测定合金钢中的钨

建立了氯化亚锡还原－硫氰酸铵快速光度法测定合金钢中钨的方法，方法的线性范围为2－400μg/50mL，相对标准偏差为0．24％－1．22％，方法简便，快速，测定结果准确。     

火焰原子吸收光谱法间接测定非金属材料中氯

报道了火焰原子吸收光谱法（ＦＡＡＳ）间接测定非金属材料中氯的方法，采用ＡｇＣｌ沉淀，测定剩余Ａｇ~＋间接求出氯含量。方法的特征浓度为０．０１４ｍｇ／Ｌ（１％吸收），检出限为０．０３２ｍｇ／Ｌ（３），测定下限为０．１１ｍｇ／Ｌ，相对标准偏差（ＲＳＤ）为１．５％～１０％，样品加标准回收率在９１．４％－１０５％之间。     

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.