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溶剂萃取中采用混合萃取剂所产生的协同效应,已获得了广泛的研究.特别是以螯合萃取剂与中性萃取剂组成的协同萃取体系,更引起人们的重视.Cvjeticanin将纸上反相分配色谱用于协萃效应的研究.选用螯合萃取剂噻吩甲酰三氟丙酮(TTA)与中性磷类萃取剂磷酸三丁酯(TBP)、三辛基氧化膦(TOPO)或磷酸三辛酯(TOP)组成的混合萃取剂作固定相,研究了对铀、钍和稀土元素的协萃效应,并探讨了有关的协萃机理. 相似文献
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泡腾辅助微萃取(EAM)技术是一种利用CO2供体和H+供体反应产生CO2气泡促进萃取剂快速分散、增大与目标物的接触面积,以实现高效萃取的新型样品预处理手段。该技术具有分散速率快、萃取效率高、使用成本低、应用范围广等优点。得益于萃取剂的快速发展,泡腾辅助微萃取方法的构建和应用范围研究日趋完善和多样,已广泛用于环境、食品、生物等样品的前处理领域。该前处理技术结合各类检测仪器构建新型快速的检测方法,成功实现了重金属离子、农药、内分泌干扰物、抗生素等污染物的检测。在EAM技术的构建中,常考查泡腾片剂的组成、溶液pH、萃取温度、萃取剂种类、萃取剂添加量、洗脱剂种类、洗脱剂体积、洗脱时间、循环使用次数等因素对方法的影响,重点依据线性范围、相关系数、富集因子、检出限、定量限等参数对方法进行评判,最后结合各类仪器检测方法,实现在实际样品检测中的应用。该文从EAM技术常用的萃取剂方面入手,综述了基于纳米材料、离子液体等新兴萃取剂的EAM方法的构建,以及与液相色谱、气相色谱、原子吸收光谱或质谱等大型仪器联用,用于复杂基质中有害物质检测的研究... 相似文献
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水中氯苯类污染物的顶空液相微萃取 GC-MS法测定 总被引:3,自引:0,他引:3
研究了用顶空液相微萃取GC-MS法测定水中的痕量氯苯类有机污染物。通过实验选择正辛醇为萃取剂,考察了萃取剂的体积、萃取温度、萃取时间、搅拌速度、样品顶空体积以及盐效应等对萃取的影响。在最佳萃取和测定条件下,方法的线性范围为0.1~800μg/L,检出限(S/N=3)为0.05~0.1μg/L。用本方法测定了实际样品及回收率,结果满意。 相似文献
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研究了盐析剂浓度和水相PH值对分配比D的影响。研究了烷基膦酸萃取剂P507和喹吉林 类萃取剂N601协萃锗的机理,并对萃取平衡常数和热效应进行了估算。 相似文献
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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%. 相似文献
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Toward new camptothecins. Part 6: Synthesis of crucial ketones and their use in Friedländer reaction
Laurent Gavara Thomas Boisse Jean-Pierre Hénichart Adam Daïch Philippe Gautret 《Tetrahedron》2010,66(38):7544-5571
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. 相似文献
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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. 相似文献
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Rebecca J. Burton Mandy L. CrowtherNeal J. Fazakerley Shaun M. FilleryBarry M. Hayter Jason G. KettleCaroline A. McMillan Paula PerkinsPeter Robins Peter M. SmithEmma J. Williams Gail L. Wrigley 《Tetrahedron letters》2013
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. 相似文献
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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. 相似文献
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N. A. Nedolya 《Chemistry of Heterocyclic Compounds》2008,44(10):1165-1219
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. 相似文献
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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. 相似文献
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《Tetrahedron》2014,70(21):3377-3384
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. 相似文献
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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. 相似文献