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动力学荧光法测定对苯二酚的研究 总被引:2,自引:0,他引:2
基于在稀H2SO4介质中,对苯二酚对H2O2氧化罗丹明B产生的荧光猝灭有显著的催化作用,建立了测定对苯二酚的动力学荧光分析法。反应在80℃的水浴中进行12 min,方法的线性范围为4.0~600.0μg/L,检出限为3.7μg/L。该方法用于水样中对苯二酚的测定,加标回收率在96.4%~101.3%之间,相对标准偏差为2.2%。 相似文献
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阻抑动力学荧光光度法测定苯胺 总被引:11,自引:0,他引:11
在醋酸介质中,痕量苯胺对溴酸钾和过氧化氢氧化罗丹明6G使其荧光猝灭的反应有抑制作用,据此建立了阻抑动力学荧光法灵敏测定痕量苯胺的新方法。方法检出限为0.50μg/L,测定范围为8.40-58.7μg/L。方法用于环境废水中苯胺的测定,结果令人满意。 相似文献
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动力学荧光分析法测定间苯三酚的研究 总被引:1,自引:0,他引:1
基于在稀H2SO4介质中,痕量间苯三酚对高碘酸钾氧化罗丹明B具有显著的催化作用,使溶液的荧光猝灭,建立了动力学荧光法测定间苯三酚的新方法。方法的线性范围为0.80~800.0μg/L,检出限为0.40μg/L。本法用于针剂中的间苯三酚含量的测定,结果满意。 相似文献
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在pH3.8的醋酸-醋酸钠缓冲介质中,壳聚糖对核固红的荧光强度有明显的猝灭作用,且在一定浓度范围内,壳聚糖的质量浓度与荧光猝灭程度呈线性关系,据此建立了荧光猝灭法测定壳聚糖含量的新方法。方法的线性范围为0.008~2.5mg/L,检出限为5.4μg/L。对猝灭机理进行了初步探讨,并将方法用于保健食品中壳聚糖含量的测定,回收率高,结果满意。 相似文献
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在pH 8.0的缓冲体系中,肝素使得罗丹明6G的荧光发生明显猝灭,罗丹明6G的荧光猝灭程度在一定范围内与肝素的浓度成正比,据此建立了荧光猝灭法测定痕量肝素的方法,并对体系的荧光猝灭机理进行了讨论。体系的激发波长为482 nm,发射波长为560 nm,线性范围为0.05~3.0 mg/L,检出限为6.1μg/L。方法已应用于肝素钠注射液中肝素含量的测定。 相似文献
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动力学荧光猝灭法测定柠檬酸的研究 总被引:5,自引:0,他引:5
在稀H2SO4介质中,柠檬酸活化钒(Ⅴ)催化溴酸钾氧化吡口罗红Y的褪色反应,使其荧光猝灭,建立了动力学荧光猝灭法测定柠檬酸的新方法。反应在沸水浴中进行10min,测定柠檬酸的线性范围为0.1~4.0μg/mL,检出限为6.0×10-8g/L。本法用于饮料中柠檬酸的测定,并进行了加标回收试验,回收率在96%~103%之间。 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