Speciation Analysis of Inorganic Tin (Sn(II)/Sn(IV)) by Graphite Furnace Atomic Absorption Spectrometry Following Ion-Exchange Separation

A new method based on anion exchange resin separation and graphite furnace atomic absorption spectrometry (GFAAS) detection is proposed for the determination of inorganic tin species. The result showed that Sn(IV) was quantitatively retained on the resin when [HCl] = 9.0 mol · L⁻¹, but Sn(II) could not be adsorbed on the resin under the same condition. Thus, a separation of Sn(II) and Sn(IV) has been realized. When the concentration of NaOH solution was between 2.0–7.0 mol · L⁻¹, Sn(IV) that adsorbed on the resin could be eluated from the resin completely. Meanwhile, under the atmosphere and the nitrogen states, the translation between Sn(II) and Sn(IV) was investigated. Under the optimal conditions, the detection limit of Sn(IV) is 0.40 μg · L⁻¹ with RSD of 2.3% (n = 5, c = 2.0 μg · L⁻¹). The proposed method was applied to the speciation analysis of tin in different water samples and the recovery of total Sn was in the range of 98.7–101.7%. In order to verify the accuracy of the method, a certified reference water sample was analyzed and the results obtained were in good agreement with the certified value.     

Organic synthesis based on cathodic deprotonation of acids

The results of studies on electrosynthesis involving carb- and heteroanions generated by cathodic deprotonation of acids (CDA), carried out in the laboratory headed by the author, are surveyed. These studies resulted in the elaboration of efficient electrochemical versions of the known Michaelis-Becker, Wittig-Horner, and Perkin reactions; electrochemical analogs of homolytic aromatic substitution, alkylation, heterocyclization,etc. were developed. Based on CDA, convenient and promising methods for preparing variousN-, O-, P-, S-, andC-alkylated and arylated substances have been developed.Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 8, pp. 1411–1422, August, 1995.The author is grateful to Professor V. A. Dorokhov, Professor V. P. Litvinov, and researchers from the laboratories of N. D. Zelinsky Institute of Organic Chemistry headed by them, who participated in joint studies.The work was carried out with financial support from the International Science Foundation (Grant No. MHYOO).     

The role of variable surface charge and surface complexation in the adsorption of humic acid on magnetite

The ionic strength dependence of humic acid (HA) adsorption on magnetite (Fe₃O₄) was investigated at pH 5, 8 and 9, where variable charged magnetite is positive, neutral and negative, respectively. The adsorption studies revealed that HA has high affinity to magnetite surface especially at lower pH, where interacting partners have opposite charges. However, in spite of electrostatic repulsion at pH 9 notable amounts of humate are adsorbed. Increasing ionic strength enhances HA adsorption at each pH due to charge screening. The dominant interaction is probably a ligand-exchange reaction, nevertheless the Coulombic contribution to the organic matter accumulation on oxide surface is also significant under acidic condition. The results from size exclusion chromatography demonstrate that the smaller size HA fractions enriched with functional groups are adsorbed preferentially on the surface of magnetite at pH 8 in dilute NaCl solution.     

Nitroxide‐mediated radical polymerization in miniemulsion: Bimolecular termination in monomer‐free model systems

Bimolecular termination in nitroxide‐mediated radical polymerization in miniemulsion has been investigated through the heating of a polystyrene–2,2,6,6‐tetramethylpiperidinyl‐1‐oxy macroinitiator and its 4‐hydroxy‐2,2,6,6‐tetramethylpiperidinyl‐1‐oxy analogue in an aqueous toluene dispersion with sodium dodecyl benzenesulfonate as a surfactant at 125 °C. The level of bimolecular termination by combination, evaluated from the high‐molecular‐weight shoulder, was higher in miniemulsion than in solution and increased with decreasing particle size. Quantitative analysis revealed that these results cannot be rationalized solely by nitroxide partitioning to the aqueous phase. The results are explained by an interface effect, by which nitroxide is adsorbed or located at the aqueous–organic interface. © 2007 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 45: 4995–5004, 2007     

An efficient palladium catalyzed synthesis of 2-arylbenzothiazoles

A novel and convergent palladium catalyzed synthesis of 2-arylbenzothiazoles has been investigated. The key step in the synthesis is a Suzuki biaryl coupling of 2-bromobenzothiazole with aryl boronic acids to provide a variety of 2-arylbenzothiazole derivatives in good yield. The synthetic utility of this methodology is demonstrated by the synthesis of 2-(4-aminophenyl)-6-methoxybenzothiazole, a PET probe precursor for the in vivo imaging of Alzheimer's disease.     

A note on strongly π-regular rings

Let R be an associative ring with unit and let N(R) denote the set of nilpotent elements of R. R is said to be stronglyπ-regular if for each x∈R, there exist a positive integer n and an element y∈R such that x ⁿ=x ^{n +1} y and xy=yx. R is said to be periodic if for each x∈R there are integers m,n≥ 1 such that m≠n and x ^m=x ⁿ. Assume that the idempotents in R are central. It is shown in this paper that R is a strongly π-regular ring if and only if N(R) coincides with the Jacobson radical of R and R/N(R) is regular. Some similar conditions for periodic rings are also obtained. This revised version was published online in June 2006 with corrections to the Cover Date.     

α，ω-二羧基-甲基丙烯酸丁酯低聚物的合成及MS分析

利用传统自由基聚合法，在四氢呋喃溶液中自由基引发聚合甲基丙烯酸丁酯单体而得到ω-羧基-甲基丙烯酸丁酯低聚物(CTBMA)(分子量在1500左右)；利用CTBMA末端酯基的反应特性，在二氧六环／水／KOH混合溶液中皂化CTBMA，使之转化为α，ω-羧基甲基丙烯酸丁酯低聚物(di-CTBMA)；研究了溶剂的类别、反应时间等反应条件对皂化产物结构的影响；利用MALDI-TOF-MS及LSIMS对皂化各阶段产物进行了分析监测．实验表明，在适当的皂化条件下，CTBMA皂化时主要为末端酯基转化为羧基，相应得到的产物di-CTMBA具有很好的结构特性，其官能团度(functionality)接近2．     

副品红共振光散射法测定脱氧核糖核酸

本文基于脱氧核糖核酸 (DNA)对有机染料副品红的共振光散射的增强效应 ,拟定了一种测定DNA的共振光散射法。在pH =0 5～ 1 5范围内 ,有机染料副品红于 35 5nm处的共振光散射强度被DNA强烈增强 ,且增强程度与DNA浓度呈线性关系 ,线性范围为 0 10～ 15 μg·mL- 1 ,检出限可达 36ng·mL- 1 。该方法简便、快速、具有较高的灵敏度和准确度 ,且线性范围较宽。将该方法用于混合样品中DNA的测定 ,结果令人满意。     

一种新颖的测定和分析羟自由基氧化损伤RNA及其分子机理的化学发光体系

近年来，羟自由基（^.OH)对DNA氧化损伤已受到广泛关注，但是很少研究^.OH对RNA的氧化损伤。其实，RNA与DNA一样，也是核酸的两大组分之一，也有许多重要功能。所以^.OH攻击RNA也会引起重后果，会造成细胞功能衰退甚至细胞死亡等。为此，我们建立了Vit.C-CuSO4-Phen-H2O2-PNA这一产生和测定^.OH氧化损伤RNA的化学发光体系，以便加强^.OH氧化损伤RNA的研究。通过对本体系测定条件的研究，得出了本体系最佳组方是：Vit.C,CuSO4,Phen,H2O2和RNA，浓度分别为350μmol/L,55μmol/L,350μmol/L,0.2mol/L和20μg/mL,体系pH为5．5，体系终体积为1mL。随后，利用本体系检测了槲皮素，咖啡酸，黄芩甙和芦丁抗^.OH氧化损伤RNA的作用，发现这四种抗氧化剂均能有效抑制^.OH氧化损伤RNA的分子机理，结果发现，^.OH清除剂硫脲几乎抑制全部发光，推测是因硫脲清除了引发剂^.OH所致；O^-.2清除剂SOD只能抑制小部分发光；^1O2清除剂叠氮化钠和苯甲酸都能抑制绝大部分发光。这些事实提示，^.OH是RNA氧化损伤的引发剂；O^-.2只是导致RNA氧化损伤的次要因素，^1O2才是导致RNA氧化损伤的最主要因素。