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1.
本报导了以玻碳电极为基体的1∶12硅钼杂多阴离子薄膜化学修,铈电极的制备及其电化学特性。并应用于导数伏安法测定。在4.0×10^-3mol/L9NH4)6Mo7O24-66.8×10^-2mol/LNa3Cit-0.48mol/L NHO3体系中,硅浓度在8.3×10^-7~1.7×10^-3mol/L。对可溶性硅(以SiO2计)为245.05mg/L的黑液,稀释10倍后,取2.00mL平行测定 相似文献
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铜(Ⅱ)和锌(Ⅱ)分别在0.1mol/LKH_2PO_4-Na_2HPO_4缓冲溶液(pH6.5)和0.25mol/LNH_4Cl溶液中,与氟哌酸形成良好的络合吸附波,峰电位分别为-0.26V和-1.28V(vs;SCE);络合比分别为1:3和1:2;峰电流与铜(Ⅱ)和锌(Ⅱ)的浓度均在4.0×10 ̄(-7)~5.0×10 ̄(-6)mol/L范围内呈线性关系,检测限分别为7.0×10 ̄(-8)和5.0×10 ̄(-8)mol/L。用线性扫描和循环伏安法等手段研究体系的行为,表明均具吸附性,而铜(Ⅱ)-氟哌酸体系属络合物中铜(Ⅱ)的两电子还原的可逆过程。 相似文献
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氨基萘磺酸盐无保护流体室温磷光的取代基位置效应 总被引:1,自引:0,他引:1
以TINO3作重原子微扰剂,Na2SO3作化学除氧剂,在无需加入任何保护介质条件下,仅需仪器光源适当照射,1-氨基4-萘磺酸盐、1-氨基5-萘磺酸盐、2-氨基1-萘磺酸盐水溶液均能产生强而稳定的室温磷光信号(RTP)。3种氨基萘磺酸盐浓度分别在4.0×10^-8 ̄1.2×10^-5mol/L;1.2×10^-6 ̄1.6×10^-5mol/L;1.6×10^-7 ̄8.0×10^-6和8.0×10^- 相似文献
4.
一种基于形成杂多核络合物的荧光增敏效应的研究:Ⅲ.锰(Ⅱ),钴(… 总被引:3,自引:0,他引:3
本研究了Mn^2+和Co^2+对7-(8-羟基-3,6-二磺基萘偶氮)-8-羟基喹啉-5-磺酸-硼砂反应体系的混合荧光增敏作用。实验条件下,荧光增敏强度满足线性加和关系的范围是:Mn^2+浓度0 ̄2.9×10^-7mol/L;Co^2+浓度0 ̄8.8~10^-7mol/L;总浓度不超过1.0×10^-6mol/L。检出限量为Mn^2+4.5×10^-9mol/L和Co^2+1.4×10^-8mo 相似文献
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本报道一种测定哌仑西平的单扫描示波极谱法,在0.1mol/LNH4Cl-NH3.H2O(pH8.0±0.1)缓冲液中,哌仑西平有一极谱还原波,其峰电位为-1.51V(vs.SCE),其一阶导数峰高与哌仑西闰浓度在6.6×10^-7-4.6×10^-6mol/L(r=0.9981)和6.6×10^-6-1.6×10^-5mol/L(r=0.9991)范围内有线性关系,检测限为3.4×10-7mol 相似文献
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硅钼杂多阴离子薄膜修饰电极的研究和应用—线性扫描伏安法测定水中可溶性 总被引:1,自引:0,他引:1
本研究了以玻碳电极为基体的1:12硅钼杂多酸根修饰电极的制备及其电化学行为,将12-MSA电极应用于线性扫描伏安法测定天然水中可溶性硅酸盐,结果满意,硅浓度在8.0×10^-7-1.7×10^-3mol/L,相对标准偏差(n=7)为1.85%,加标回收率为98.2%-103.6%,SiMo12电极具有优良的选择性和稳定性。 相似文献
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铜(Ⅱ)锌(Ⅱ)—氟哌酸体系电化学行为及示波极谱法研究 总被引:1,自引:0,他引:1
铜(Ⅱ)和锌(Ⅱ)分别在0.1mol/LKH2PO4-Na2HPO4缓冲溶液(pH6.5)和0.25mol/LNH4Cl溶液中,与氟哌酸形成良好的络合吸附波,峰电位分别为-0.26V和-1.28V(vs.SCE),络合比分别为1:3和1:2,峰电流与铜(Ⅱ)和锌(Ⅱ)的浓度均在4.0×10^-7~5.0×10^-6nol/L范围内呈线性关系,检测限分别为7.0×10^-8和5.0×10^-8mol 相似文献
10.
单缺位Dawson型磷钨杂多酸掺杂聚吡咯的过氧化氢传感器研究 总被引:4,自引:1,他引:4
在金电极上,用电化学方法将单缺位Dawson型磷钨杂多酸盐a2-K10P2W17O6115H2O的阴离子(P2W17)掺杂到聚吡咯(PPy)薄膜中,制成PPy/P2W17/Au的H2O2传感器。研究了它对 H2O2电还原过程的催化机理.其 ipe与 CH2O2在 6.0× 10-5~8. 8×10-4 mol/L和8.8×10-4~6.0×10-3mol/L范围内呈良好的线性关系,检测下限为4.0×10-5mol/L。用于模拟水样中H2O2的测定,结果较满意. 相似文献
11.
Uroš Grošelj Mojca Žorž Amalija Golobič Branko Stanovnik Jurij Svete 《Tetrahedron》2013,69(52):11092-11108
A new and simple synthesis of novel N-protected methyl 5-substituted-4-hydroxypyrrole-3-carboxylates, which exist in equilibrium with their 4-oxo tautomers, has been developed in two steps starting from N-protected α-amino acids. The key intermediates are enaminones, which can also be isolated, characterized, and used for the construction of other functionalized heterocycles, before they spontaneously decompose to pyrrole products. 4-Hydroxypyrroles are prone to partial aerial oxidation but can be efficiently alkylated or reduced to stable polysubstituted pyrrolidine derivatives. 相似文献
12.
The chemoselectivity in the intramolecular CH insertion of various diazosulfonamides has been experimentally studied. The results reveal that the aliphatic 1,4-, 1,5-, or 1,6-C(sp3)?H insertions of diazosulfonamides are not accessible, while the aromatic 1,5-C(sp2)?H insertion can be realized specifically by adjusting the diazo-adjacent group. In addition, the general chemoselectivities in the intramolecular CH insertions of diazosulfonyl compounds are summarized. Generally, diazosulfones undergo both aromatic 1,5-C(sp2)?H and aliphatic 1,5- and 1,6-C(sp3)?H insertions, while diazosulfonates undergo aliphatic 1,5- and 1,6-C(sp3)?H insertions. However, diazosulfonamides only undergo aromatic 1,5-C(sp2)?H insertion. 相似文献
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N-Heterocyclic carbene-palladacyclic complexes 3 were successfully achieved in a one-pot procedure under mild conditions. The structure of 3a was unambiguously confirmed by X-ray single crystal diffraction and it was an active catalyst in the Buchwald-Hartwig amination and α-arylation of ketones even at very low catalyst loadings (0.01?mol%). 相似文献
14.
Shashikant U. Dighe Surya K. Samanta Shivalinga Kolle Sanjay Batra 《Tetrahedron》2017,73(17):2455-2467
An efficient iodine-mediated oxidative Pictet-Spengler reaction in dimethyl sulphoxide (DMSO) using terminal alkynes as the 2-oxoaldehyde surrogate for the synthesis of aryl (9H-pyrido[3,4-b]indol-1-yl)methanones is described. The scope of the protocol includes the total synthesis of Fascaplysin, Eudistomins Y1 and Y2. The methodology is extended for preparing pyrrolo[1,2-a]-quinoxaline and indolo[1,5-a]quinoxaline derivatives. The utility of 1-aroyl-β-carbolines was demonstrated by performing palladium-catalyzed β-carboline directed ortho-C(sp2)-H functionalization of the phenyl ring with thiomethyl (SMe) group using DMSO as source and for accessing 4-aryl-canthin-6-ones. 相似文献
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In this Letter, we described a facile method for constructing fused bicyclic 1-arylpyrazol-5-one ring system. We employed various methylene-containing carboxylic acids as the substrates and proved that the pyrazolone ring closure requires activated methylene group in intermediate II. Accordingly, a series of structurally diversified, fused bicyclic 1-arylpyrazol-5-ones was prepared in moderate to high yields using the requisite substrates. 相似文献
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Synthesis of substituted pyrrolo[1,2-a]pyrazines and pyrazino[1,2-a]indoles from the Morita-Baylis-Hillman derivatives of acrylates via saponification followed by Curtius reaction is described. 相似文献
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用正丁胺作为碳源,采用射频辉光放电制备碳膜,选用激光染料R6G和聚乙二醇混合液作为蒸气源,采用单源热蒸发,在蒸发室与染料同时沉积得到混合膜,用拉曼光谱和红外光谱分析了碳膜的结构和键合方式,分析表明:碳膜中存在胺基团和氢原子.混合膜的荧光谱测量结果表明,认为正丁胺对染料荧光谱的影响是因为胺基和氢原子的存在. 相似文献
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Jona Mirnik Eva Pušavec Kirar Sebastijan Ričko Uroš Grošelj Amalija Golobič Franc Požgan Bogdan Štefane Jurij Svete 《Tetrahedron》2017,73(24):3329-3337
A series of 20 CuAIAC reactions between eight 4-acylamino substituted pyrazolidine-3-one-1-azomethine imines and four terminal ynones were performed using Cu0 as catalyst. The corresponding fluorescent cycloadducts were obtained in very high yields upon simple workup. Thus, Cu-metal turned out to be a better catalyst than CuI in terms of yield and ease of isolation. Availability of azomethine imines, mild reaction conditions, and simple workup enable a “click” access to libraries of densely substituted 2,3-dihydro-1H,5H-pyrazolo[1,2-a]pyrazol-1-ones. Reactivity of differently substituted dipoles was evaluated experimentally and by quantum chemical methods (DFT). 相似文献
20.
George E. Magoulas Thomas Garnelis Constantinos M. Athanassopoulos Dionissios Papaioannou George Mattheolabakis Konstantinos Avgoustakis Dimitra Hadjipavlou-Litina 《Tetrahedron》2012,68(35):7041-7049
(E)-4-(Fullerenopyrrolidin-1-yl)-3-methylbut-2-enoic acid and its corresponding succinimidyl ester, readily obtained through Prato-type modification of C60, were used for the selective N-acylation of polyamines. The thus obtained conjugates were evaluated for their antioxidative and anti-inflammatory activity and their cytotoxicity was determined. Members of this family of compounds showed interesting anti-lipid peroxidation, anti-lipoxygenase and anti-inflammatory activity and comparable cytocompatibility to spermidine. 相似文献