非完全消化-火焰原子吸收光谱法测定杜仲叶中的微量元素

用非完全消化法处理杜仲叶,在低温下用浓硝酸消解样品,加入乳化剂Triton X-100(OP)溶解消化过程中所产生的油脂,获得均匀的样品乳浊液,取适量的乳浊液制成试液,用火焰原子吸收光谱法快速测定了样品中的微量元素,并对检出限、加标回收率进行了测定。结果表明,相对标准偏差小于2.1%,测定结果与灰化法一致,且相对误差小于±1.8%。用非完全消化法结合火焰原子吸收光谱法对杜仲叶进行预处理取代灰化法是可行的,且方法简便、准确。     

非完全消化悬浮液进样火焰原子光谱法测定木耳中钾铜锌

将非完全消化法与悬浮液进样技术相结合处理木耳样品 ,即在加热下用浓硝酸消解样品 ,使绝大部分样品组分进入溶液 ,再加入乳化剂OP溶液及琼脂溶液将极小部分的不溶物悬浮成悬浮液 ,用吸收法测定铜、锌 ,以发射法测定钾。建立了测定木耳中钾、铜和锌的快速火焰原子光谱法。工作曲线法的测定结果与灰化法一致 ,相对误差小于± 2 .6% ,t检验表明此法与灰化法之间无显著性差异。方法简便、快速、准确     

非完全消化—悬浮液进样—火焰原子光谱法测定蘑菇中钾、镁、锌

将非完全消化法与悬浮液进样技术相合处理蘑菇样品，即先用浓HNO3低温消解样品至溶液呈透明，再用琼脂溶液悬浮极少量不溶物，制成样品溶液。分别以Sr^2 溶液和NaCl溶液作为测定镁、钾的释放剂和消电离剂。以原子吸收光谱法测定镁、锌，以原子发射光谱法测定钾。对样品处理方法、干扰、线性范围及检出限进行了考察。建立了快速测定蘑菇中钾、镁、锌的火焰原子光谱法。相对标准偏差小于2.8%，加标回收率为97.9%-101.6%。     

非完全消化-悬浮液进样-火焰原子光谱法测定蘑菇中的钾、镁、锌

将非完全消化法与悬浮液进样技术相组合处理蘑菇样品 ,即先用浓HNO3低温消解样品至溶液呈透明 ,再用琼脂溶液悬浮极少量不溶物 ,制成样品溶液。分别以Sr2 +溶液和NaCl溶液作为测定镁、钾的释放剂和消电离剂。以原子吸收光谱法测定镁、锌 ,以原子发射光谱法测定钾。对样品处理方法、干扰、线性范围及检出限进行了考察。建立了快速测定蘑菇中钾、镁、锌的火焰原子光谱法。相对标准偏差小于 2 8% ,加标回收率为 97 9%～ 1 0 1 6%。     

悬浮液进样-火焰原子光谱法测定烟叶中的钾锰

用悬浮液技术处理烟叶样品 ,即将样品烘干、粉碎、过筛 ,并悬浮在 1 .5g L琼脂溶液中制成均匀的悬浮液。以钙作为锰的释放剂和以钡作为钾的消电离剂。用工作曲线法测定 ,以火焰原子发射法 (FAES)测定钾 ,以火焰原子吸收法 (FAAS)测定锰。建立了快速测定烟叶中钾、锰的FAS法。对化学干扰、介质的影响及检出限进行了考察。测定结果的相对标准偏差 <2 .4% ,测定结果与灰化法一致 ,相对误差 <± 2 .5 %。     

悬浮液技术-火焰原子吸收光谱法测定明胶中钙镁

用悬浮液技术处理明胶样品。将样品烘干、粉碎、过筛,制备成琼脂悬浮液。取适量样品悬浮液加入释放剂Sr2+配制成试剂,喷入空气-乙炔火焰进行测定,建立了悬浮液技术-火焰原子吸收光谱法快速测定明胶中钙、镁的分析方法。以空白溶液为参比,用工作曲线法测定。对琼脂溶液用量、化学干扰、试液与空白溶液粘度一致性、背景吸收干扰及检出限进行了考察。测定结果与灰化法一致,相对误差小于±0．9％,相对标准偏差小于5．2％。方法简便、准确。     

非完全消化-火焰原子吸收光谱法测定鸡蛋中钙和镁

用非完全消化法处理鸡蛋样，即在80～130℃的低温下用浓硝酸及过氧化氢消化，直至消化液呈透明淡黄色，再加入乳化剂OP溶解消化过程中所产生的油脂，可获得均匀的样品乳浊液。取适量乳浊液制成试液，喷入空气-乙炔火焰，以氘灯扣除背景吸收，用工作曲线法测定。建立了用火焰原予吸收光谱法测定鸡蛋中钙和镁的快速分析方法。对样品处理条件、干扰的消除进行了考察，测定结果与灰化法一致，相对误差小于±2．5％，方法简便。     

非完全消化-火焰原子吸收光谱法测定人发中的钾和锌

1　引　　言用非完全消化法处理人发样 ,即在低温下用浓硝酸及过氧化氢消化人发至溶液呈透明黄棕色 ,再加乳化剂ＯＰ溶解消化化过程中所产生的油脂 ,制得一均匀的样品乳浊液。取适量乳浊液配制成试液 ,喷入空气 乙炔火焰 ,用工作曲线法测定。建立了火焰原子吸收光谱法测定人发中钾、锌的快速分析方法。测定结果与灰化法一致 ,相对误差小于± 0 .8%。方法简便、快速、准确。目前 ,人发样品的预处理方法通常是传统的灰化法及消化法 ,其缺点是耗时长 ,一般需要 3～ 6ｈ ,不能满足快速分析的要求。我们在 80～ 130℃以浓硝酸及过氧化氢处理发样…     

非完全消化-分光光度法测定环烷酸钴中钴

用非完全消化法处理环烷酸钴样品，即先用(1 3)HClO4-HNO3混合酸及H2O2消解破坏样品，使Co^2 游离出来，再用乳化剂Triton X-100溶解残存的环烷酸根而配制成透明的样品溶液。采用Co^2 -5-Br-PADAP-OP显色体系测定钴，在硫磷混合酸介质中共存元素与5-Br-PADAP形成的有色络合物被分解破坏，从而达到消除干扰的目的。建立了非完全消化-分光光度法测定环烷酸钴中钴的分析方法。对测定条件、线性范围进行了考察。测定结果与灰化法-分光光度法一致，相对标准偏差小于0．7％，加标回收率97．4％～103．0％。     

中草药中铁锌钙的悬浮液进样-火焰原子吸收光谱法测定

将悬浮液进样技术应用于火焰原子吸收光谱法, 建立了中草药中微量元素的快速分析新方法。将样品粉碎、悬浮在琼脂胶体中制成悬浮液; 取适量样品悬浮液配制成试液, 喷入空气－ 乙炔火焰, 用标准加入法测定。 用该法成功地测定了当归、川芎及川乌中的铁、锌、钙, 测定结果与灰化法一致, 方法简便、快速、准确。     

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.