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1.
催化动力学光计法测定微量碘的研究 总被引:9,自引:3,他引:9
基于微量碘离子对高碘酸钠氧化甲基紫反应的催化作用,建立了测定微量碘的动力学光度法。方法检出限0.22μg/mL线性范围0.30-1.40μg/mL,包括其它卤素在内的大多数阴离子、阳离子不干扰测定,用于食盐中微量碘的测定,有满意的结果。 相似文献
2.
吐温80—AuCl4^—化学发光新体系测定痕量碘离子的研究 总被引:6,自引:0,他引:6
基于碘离子对吐温80-AuCl4^-体系化学发光的强烈抑制作用,提出了一种测定痕量碘离子的新的化学发光分析法。方法的线性范围和检测分别为1.2×10^-8 ̄1.0×10^-6g/mL和5.1×10^-9g/mL碘离子。拟定的方法体系简单,选择性好,加碘酱油和实际水样中碘离子的测定,结果满意。 相似文献
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催化褪色光度法测定痕量铁的研究 总被引:7,自引:4,他引:7
研究了在pH4.5的弱酸性介质中,利用邻菲罗啉活化过氧化氢氧化紫脲酸铵褪色的指示反应,建立了催化动力学光度法测定痕量铁的新方法,方法的检出限为6.5×10^-7g/L线性范围为0~1.0μg/25mL,用于水,粮食中痕量铁的测定,结果满意。 相似文献
4.
催化动力学光度法测定微量碘的研究 总被引:11,自引:0,他引:11
基于微量碘离子对高碘酸钠氧化甲基紫反应的催化作用,建立了测定微量碘的动力学光度法。方法检出限0.22μg/mL,线性范围0.30~1.40μgmL,包括其它卤素在内的大多数阴离子、阳离子不干扰测定,用于食盐中微量碘的测定,有满意的结果。 相似文献
5.
催化动力学光度法测定痕量硫离子 总被引:2,自引:0,他引:2
基于氢氧化钠溶液中,S~(2-)对H_2O_2氧化I-的反应有催化作用,固定反应时间,将此催化体系与二苯胺碘酸钠氧化显色反应相偶合,建立了催化动力学光度法测定痕量硫离子的新方法,并讨论了其动力学条件。方法灵敏度1.4×10~(-11)g/mL,测定范围1.0~12.0ng/mL。操作简便快速,用于测定天然水及含硫工业废水中的痕量硫离子,结果满意。 相似文献
6.
在硫酸介质中,在过量碘化钾及阿拉伯胶存在下,IO-3氧化I-生成I-3,I-3再与结晶紫形成离子缔合物,缔合物的最大吸收波长为552nm,表观摩尔吸光系数ε552=5.38×105L·mol-1·cm-1,IO-3量在0~12μg/25mL范围内服从比耳定律.用于生物样品中碘的测定,结果满意 相似文献
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催化褪色光度法测定痕量钴的研究 总被引:15,自引:2,他引:15
研究了在PH10.5的Na2B4O7-NaOH介质中,痕量钴(Ⅱ)对过氧化氢氧化桑色素初色反应的催化作用,建立了催化动力学光度法测定痕量钴的新方法。方法的线性范围为0-1.2μ/mL检出限为4.4*10^-18g/L。用于水和维生素B12中钴的测定,结果满意。 相似文献
10.
高碘酸盐氧化罗丹明B催化光度法测定钌 总被引:4,自引:0,他引:4
在0.72mol/L磷酸和90℃水浴条件下,钌催化高碘酸盐氧化罗丹明B(RB),据此建立了高灵敏催化光度测定钌的方法。方法的检出限为8.0×10^-12g/mL,测定范围为0.2~15ng/25mL,对5、10、15ng/25mLRu(Ⅲ)测定的相对标准偏差分别为8.67%,5.94%和1.85%。本反应对Ru(Ⅲ)、RB、KIO4和H3PO4均为一级反应,表观活化能为36.05kJ/mol。13 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
17.
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