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1.
邓凡政  石影  张宝娟  王莉莉 《分析化学》1998,26(9):1115-1117
在 pH 4.0~6.0的 HAc-NaAc缓冲溶液中,Co(Ⅱ)、Fe(Ⅲ)、Ni(Ⅱ)、Cu(Ⅱ)等金属离子与亚硝基R盐可形成稳定络合物。加入HCI适当提高溶液酸度(HCI浓度在0.3~0.6mol/L),用聚乙二醇2000(PEG)-硫酸铵-亚硝基R盐体系萃取,Co(Ⅱ)可被PEG相几乎完全萃取,而Fe(Ⅲ)、Ni(Ⅱ)、Cu(Ⅱ)基本上不被萃取。实现了Co(Ⅱ)、Fe(Ⅲ)、Ni(Ⅱ)、Cu(Ⅱ)混合离子合成样品和硅酸盐岩矿实际样品中Co(Ⅱ)的分离与测定。同时吸收光谱、摩尔比、连续浓度变换、加入表面活性剂等实验表明,在萃取相Co(Ⅱ)与亚硝基R盐是1:3络阴离子形式存在的。  相似文献   

2.
邓凡政  石影 《分析化学》1998,26(9):1115-1117
在pH4.0~6.0的HAc-NaAc缓冲溶液中,Co(Ⅱ),Fe(Ⅲ),Ni(Ⅱ),Cu(Ⅱ)等金属离子与亚硝基R盐可形成稳定络合物,加入HCl适当提高溶液酸度(HCl浓度在0.3~0.6mol/L)用聚乙二醇2000(PEG)-硫酸铵-亚硝基R盐体系萃取,Co(Ⅱ)可被PEG相几乎完全萃取,而Fe(Ⅲ),Ni(Ⅱ),Cu(Ⅱ)基本上不被萃取,实现了Co(Ⅱ),Fe(Ⅲ),Ni(Ⅱ),Cu(Ⅱ)  相似文献   

3.
在pH3.8的H2SO4-NH4Ac介质中,Co(Ⅱ)-β-巯基丙酸(MPA)-NaNO2体系产生-灵敏的极谱催化波,峰电位在-0.84V(vs.SCE),钴浓度在0.02~100ng/mL范围内与峰电流呈线性关系。检出限为0.01ng/mL。本文对极谱波的性质和机理进行了初步探讨。本法用于土壤中总钴和有效钴的测定,结果满意。  相似文献   

4.
邻联甲苯胺-过氧化氢催化光度法测定钴   总被引:2,自引:0,他引:2  
李竹云  崔孟忠  郑莹 《分析化学》2000,28(8):1049-1049
1引言 在碱性介质中,痕量Co(Ⅱ)见对H2Q2氧化邻联甲苯胺(o-Tolidine)的显色反应具有强烈的催化作用,探讨了利用该反应进行痕量Co(Ⅱ)测定的影响因素,建立了测定痕量Co(Ⅱ)的催化动力学光度法,该方法的灵敏度为1.78 × 10-6g/L,测定的线性范围为0.8~3.6 μg/L Co2+,应用于维生素B12中痕量Co(Ⅱ)的测定,结果满意。2实验部分2.1仪器与试剂 721-100型分光光度计;电热恒温水浴槽;Nicolet FT-IR 5DX红外光谱仪。钴(Ⅱ)标准溶液:1mg/L;…  相似文献   

5.
林秋月  陈建荣 《分析化学》1999,27(8):920-923
研究了Tween80水溶液在(NH4)2SO4存在下,水溶性螯合剂1-(2-吡啶偶氮)-2-萘酚-磺酸与金属离子螯合物在该体系中两相间的分配行为。结果表明,Pd(Ⅱ),Co(Ⅱ),在pH2.0-3.5缓冲溶液中可被Tween相完全萃取,而Zn(Ⅱ),Cd(Ⅱ),Mn(Ⅱ),Al(Ⅲ)基本上不被萃取。  相似文献   

6.
新体系Co—H2O2—OCPF催化褪色光度法测定痕量钴的研究   总被引:12,自引:1,他引:11  
本文研究了在碱性介质中,钴(Ⅱ)对过氧化氢氧化邻氯苯基荧光酮(OCPF)褪色反应,建立了催化光度法测定痕量钴的新方法。其检出限为8.2pg/mL,在0-3.5ng/mL范围内,钴(Ⅱ)与log(Ao/A)有良好好线性关系。该指示反应灵敏度选择性好,应用于维生素B12和污水中钴的测定获得满意结果。  相似文献   

7.
道了聚乙烯基吡咯烷酮(PVP)-(NH4)2SO4-水的固-液萃取体系中Au(Ⅲ)、Pt(Ⅳ)、Pd(Ⅱ)溴络阴离子的萃取行为,在HBr介质中,可萃取贵金属Au(Ⅲ)、Pt(Ⅳ)、Pd(Ⅱ)而与贱金属Fe(Ⅲ)、Co(Ⅱ)、Ni(Ⅱ)、Al(Ⅲ)、Ca(Ⅱ)、Mg(Ⅱ)、Cu(Ⅱ)等分离,对合成样及实际样品进行了定量萃取分离测定,结果与其它方法相符,并对机理进行了初步探讨。  相似文献   

8.
钴(Ⅱ)—β—巯基丙酸—NaNO2体系的极谱化波研究   总被引:1,自引:0,他引:1  
在pH3.8的H2SO4-NH4Ac介质中,Co(Ⅱ)-β-巯基丙酸(MPA)-NaNO2体系产生-灵敏的极谱催化波,峰电位在-0.84V(vs.SCE)钴浓度在0.02~100ng/mL范围内与峰电流呈线性关系,检出限为0.01ng/mL。本文对极谱波的性质和机理进行了初步探讨,本法用于土壤中总钴和有效钴的测定,结果满意。  相似文献   

9.
邓凡政  石影 《分析化学》1997,25(2):215-218
研究了在聚乙二醇-硫酸铵-铝试剂体系中Fe(Ⅲ),Al(Ⅲ)、Cu(Ⅱ)、CoⅡ)Cd(Ⅱ)Mn(Ⅱ)、Ni(Ⅱ)的萃取分离行为。结果表明,在PH5.0-6.5HAc-NaAc缓冲溶液中,Fe(Ⅲ)、Al(Ⅲ)可被PEG相几乎完全萃取,而Cu(Ⅱ)、Co(Ⅱ)Cd(Ⅱ)Mn(Ⅱ)基本上不被萃取,从而实现了Fe(Ⅱ)与Cu(Ⅱ)Co(Ⅱ)Cd(Ⅱ)Mn(Ⅱ)及Al(Ⅲ)与Fe(Ⅲ)Co(Ⅱ)、Cu(  相似文献   

10.
在pH10.0的NH_3·H_2O-NH_4Cl缓冲溶液中,当有0.0030%CTMAB存在时,Cu(Ⅱ)与5-Br-PADN配合物在-0.45V产生一灵敏配合物吸附波,用于测定铜(Ⅱ)时,线性范围为0.0050~0.60μg/mL,检测下限为5.0×10 ̄(-8)mol/L。所提出的方法可用于矿石中微量铜的测定,回收率在92%~104%之间。  相似文献   

11.
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   

12.
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   

13.
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   

14.
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   

15.
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   

16.
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   

17.
An efficient approach to the synthesis of highly congested di, penta and hexacyclic pyrazoles as well as imidazole fragment containing novel heterocyclic molecule has been developed through a carbanion induced transformation of suitably functionalized 2H-pyran-2-ones, benzo[h]chromene and thiochromeno[4,3-b]pyrans. Due to the presence of fluorescence, we report their prime application metal sensor as off/on switching in ferric ions.  相似文献   

18.
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   

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.
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