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1.
单宁的电化学氧化及伏安测定法 总被引:8,自引:0,他引:8
以玻碳电极(GCE)为工作电极,KH2PO4-Na2HPO4为支持电解质,通过循环伏安法首次观测到了单宁的不可逆氧化峰。在单宁浓度为1.0×10~(-7)~1.2 × 10~(-5)mol/L范围内与其峰电流呈线性关系;检出限为 1.3×10~(-8)mol/L。在中药五倍子浸提液中用标准加入法进行回收实验,其平均回收率为100.6%。该法简便、快速,用1.0×10~(-6)mol/L的单宁溶液重复测定11次,RSD为2.l%。对其反应机理作了初步探讨。 相似文献
2.
在含有0.05mol/LHAc-NaAc(pH5.6)、0.1mol/LKCl和1.5×10 ̄(-5)mol/L茜素紫的溶液中,镓(Ⅲ)-茜素紫络合物在单扫示波极谱仪上产生一灵敏的导致极谱波,峰电位在-1.11V(vs.SCE),峰电流与镓(Ⅲ)浓度在2.0×10 ̄(-8)~2.0×10 ̄(-6)mol/L范围内呈线性关系,检测限达1×10 ̄(-8)moL/L机理研究表明,峰电流是由吸附在电极表面的络合物中的中心离子和配位体同时还原而产生的。方法已应用于铝合金中镓的测定,结果满意。 相似文献
3.
镓—茜素紫极谱络合吸附波的研究 总被引:3,自引:0,他引:3
在含有0.05mol/L HAc-NaAc(pH5.6)、0.1mol/L KCL和1.5×10^-5mol/L茜素紫的溶液中,镓(Ⅲ)-茜素紫络合物在单扫示波极谱仪上产生一灵敏的导数极谱波,峰电位在-1.11V(vs.SCE),峰电流与镓(Ⅲ)浓度在2.0×10^-8mol/L。机理研究表明,峰电流是由吸附在电极表面的络合物中的中心离子和配位体同时还原而产生的。方法已应用于铝合金中镓的测定,结果 相似文献
4.
在1.0mol/L甲酸-甲酸钠-0.03mol/L邻苯二甲酸氢钾混合底液(pH3.5)中,锑-茜素络合剂(ALC)络合物在单扫示波极谱上于一0.53V(vs.SCE)产生一极谱波,加入1.6×10^-3mol/LCu(Ⅱ)后,灵敏度有较大提高,峰电流与锑浓度在2.0×10^-8~3.0×10^-6mol/L范围内呈线性关系,检测限达1.0×10^-8mol/L,研究了电极反应机理,方法应用于铜合金 相似文献
5.
磷钼杂多酸-L-半胱氨酸自组装超分子膜电极对亚硝酸根电催化还原的研究 总被引:5,自引:0,他引:5
制备了磷钼杂多酸-L-半胱氨酸自组装超分子膜电极(P2Mo18-L-Cys/Au)。采用水平衰减全反射(ATR-FTIR)光谱表征了膜的组成。研究了该膜电极的电化学性质,发现它在1.0 mol/L H2SO4溶液中,于0.0~0.7V(vs.SCE)间CV扫描出现两对稳定、可逆的氧化还原峰,其中峰电位分别为Em1=0.334 V,Em2=0.188V,对应着P2Mo18O_(62)~(6-)的两步2电子-2质子反应;计时库仑法计算了薄膜内的电子传递系数D为5.01 × 10~(-8)cm2·s~(-1)。该膜电极对酸性溶液中的NO_2~-有明显的电催化还原作用,初步探讨了电催化机理。用差分脉冲伏安法(DPV)测定其还原峰电流与NO_2~-的浓度在2.0 ×10~(-6)~2.0 × 10~(-4)mol/L范围内呈良好的线性关系,相关系数为0.9953,检测限5.0×10~(-7)mol/L。该电极用于模拟水样中NO_2~-的测定,结果满意。 相似文献
6.
砷锑钨杂多酸络合吸附波的研究及其分析应用 总被引:2,自引:0,他引:2
研究并建立了砷锑钨三元杂多酸体系导数示波极谱测定微量砷的新方法。在硫酸(1.0mol/L)-丙酮(25%)溶液中,于50℃,As(V)和Sb(Ⅲ)及W(Ⅵ)形成具有电活性的砷锑钨三元杂多酸;在硫酸(0.4 mol/L)-丙酮(10%)介质中,于-0. 37 V(vs SCE)产生一灵敏的还原峰,灵敏度比同类方法提高 10倍。其二次导数电流峰高(ipn)与砷量在 5. 3 × 10-9~5. 3×10-7mol/L范围内呈线性关系。相关系数(r)和检出限分别为0.9998和2.8×10-9mol/LAs(V)。已用于高温合金(经蒸馏分离)和饮用水样(不须分离)中微、痕量砷的测定,结果满意。文中还详细研究了该杂多酸的电化学行为、络合性、电流特性和电极反应机理. 相似文献
7.
镧取代Dawson型磷钨杂多酸聚吡咯修饰电极的制备及其电化学性能 总被引:2,自引:0,他引:2
通过缺位填充法合成了分子式为α2-K7P2W17O61(La· OH2)的镧(Ⅲ)取代十八钨磷酸盐。在玻碳电极(GC)上,用电化学方法将单取代Dawson型杂多酸盐α2-K7P2W17O61(La·OH2)的阴离子(P2W17La)掺杂到聚吡咯(PPY)薄膜中制成P2W17La/PPY/GC化学修饰电极,既保持该杂多酸的电化学活性和电催化性能,又具有良好的稳定性和灵敏度。研究表明, 0. 50 mol/L HCI溶液中,聚吡咯薄膜中 P2W17La的第一对氧化还原峰对 NO2的电还原具有良好的催化活性,其催化电流与 NO2浓度在 6.0 × 10-5- 1.0 × 10-2mol/L范围内呈线性关系。 相似文献
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10.
本文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 ̄(-3)m0l/L(NH_4)_6MO_7O_(24)-6.8×10 ̄(-2)mol/LNa_3Cit-0.48mol/LNHO_3体系中,硅浓度在8.3×10 ̄(-7)~1.7×10 ̄(-3)mol/L范围内与峰电流呈良好线性关系,检测限为8.0×10 ̄(-7)mol/L。对可溶性硅(以SiO_2计)为245.05mg/L的黑液,稀释10倍后,取2.00mL平行测定9次,RSD为0.58%,加标回收率在97.3%~104.4%间。 相似文献
11.
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
12.
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
13.
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
14.
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
15.
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
16.
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
17.
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
18.
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
19.
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
20.
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