碲氢化钠与胺烷基化苯并三氮唑的反应

碲氢化钠是一个用途广泛的磁试剂,自作为有用的去溴试剂以来,日益受到化学工作者的关注,不断有文献报道它的合成及应用.例如能有效地还原卤代烃、硝基化合物、叠氮化合物和亚胺等.近年来,Katritzky报道了胺烷基化苯并三氮唑衍生物的合成及应用,此衍生物中的苯并三氮唑基是很好的离去基团,易被各种亲核试剂所取代.我们在前文中对硒氢化钠与胺烷基化苯并三氮唑反应生成二苄基二硒醚的合成进行了报道.本文用碲氢化钠与胺烷基化苯并三氮唑反应,结果生成还原产物N-取代胺.     

流动注射比浊法测定人体体液中钾

基于四苯硼钠与钾作用产生浊度 ,探讨并优化了流动注射分析条件 ,从而建立了测定人体体液中钾的新方法。方法简便、快速 ,每小时进样 6 0次 ,线性范围为 1.0× 10 - 4～ 1.0× 10 - 3mmol·ml- 1,所测尿样和血样的相对标准偏差分别为 3.0 8%和 2 .6 3%。     

氨基酸与钠离子非共价键相互作用的电喷雾质谱研究

实验研究中常常观察到钠离子与一些多肽或蛋白质有较强的非共价键结合能力,这种非共价键相互作用可能与生物的一些功能和活性有关。为了进一步了解这一结合作用,我们应用电喷雾质谱研究了常见的20种氨基酸与钠离子在溶液中的非共价键相互作用。实验研究中发现脯氨酸和苯丙胺酸与钠离子有较强的非共价键结合能力。     

钠硼硅酸盐玻璃分相及浸析的NMR研究

用多种ＮＭＲ方法，包括＾２９Ｓｉ、＾２３Ｎａ，＾１１Ｂ ＭａＳ及＾２９Ｓｉ ＣＰ／ＭＡＳ ＮＭＲ，研究了一定组成的ａ２Ｏ－Ｂ２Ｏ３－ＳｉＯ２三元体系玻璃在不同温度下分相处理２４小时及用酸浸析处理后的结构变化。结果表明，在低于分相上界临界温度的范围内，存在着一个温度转折点，低于这一温度时，受动力学因素影响，分相未达平衡态，温度愈低，距平衡态愈过，分相愈下完全。超过这一温度，分相可达平衡态，受热力学控     

Hypervalent Iodine(III) Sulfonate Mediated Synthesis of Imidazo[1,2‐a]pyridines

A direct and efficient method for the conversion of alkyl aryl ketones to imidazo[1,2‐α]pyridines has been developed based on initial formation of α‐organosulfonyloxy ketones and their subsequent cyclocondensation by 2‐aminopyridines in one‐pot conditions.     

Phase Analysis of the Binary System of Cryolite (Na3AlF6) and Sodium Metasilicate (Na2SiO3)

The phase analysis of cryolite (Na₃AlF₆) and sodium metasilicate (Na₂SiO₃) was performed by thermal analysis. The eutectic system with a region of two immiscible substances at a concentration of Na₂SiO₃ between 42.8 and 46.3 mol‐% was identified and the eutectic temperature determined to (886±2) °C. Based on the results of mass‐loss measurements, it was assumed that the introduced Na₂SiO₃ reacts with Na₃AlF₆ due to the formation of some nonvolatile stable compounds. The stable reaction products were identified by X‐ray diffraction analysis and IR spectroscopy of the spontaneously cooled samples, which established the formation of NaF and stable amorphous aluminosilicate compounds.     

Vapor pressure,speciation, and chemical activities in highly concentrated sodium borate solutions at 277 and 317°C

The system H₂O-B₂O₃-Na₂O has been studied experimentally at 277 and 317°C. The activities of water and boric acid have been determined at mole ratios Na/B from 0 to 1.5, and total dissolved solids 3 to 80 weight percent. The activity of boric acid has been fitted to within experimental error using a speciation model with eight complex species. This model is consistent with the model previously published by Mesmer et al. The electrolyte properties of the liquid are modeled using the Pitzer-Simonson model of very concentrated electrolyte solutions. The calculated values of water activity agree with experiment, and the activity of NaOH and pOH have also been calculated. The potassium borate system also was briefly studied at 317°C, and is adequately described by a model with five complex species. The potassium borate liquid is more alkaline at K/B= 1 than a sodium borate liquid at the same mole ratio, but pOH in the two systems is the same at lower mole ratios.     

丙醇-氯化钠双水相体系萃取分离铂、钯、铑、金中的铱及其吸收光谱分析研究

提出了一种丙醇－氯化钠双水相体系萃取铱的分离－吸收光谱分析方法，在HCl介质中基于铱生成三氯亚锡酸络阴离子动力学速率与铂、钯、铑、金差异使铱与铂、钯、铑、金分离，其后在KI介质中萃取铱使其与贱金属基体分离，研究了在丙醇萃取相中铱的吸收光谱分析，并应用于实际样品中铱的测定。     

Solid-phase microextraction–capillary gas chromatography combined with microwave-induced plasma atomic-emission spectrometry for selenite determination

The use of solid-phase microextraction (SPME) with gas chromatography coupled to microwave-induced plasma atomic-emission detection (GC–MIP-AED) is described for selenite [Se(IV)] speciation. Aqueous standards were derivatised with sodium tetraethyl- or tetrapropylborate and extracted by SPME. Headspace extraction of the ethyl and propyl derivatives was studied. Relevant experimental conditions were optimised, including conditions for derivatisation and extraction and those of gas chromatographic analysis. The limits of detection achieved for headspace sampling of derivatised Se(IV) were in the low ng mL^–1 range for both ethylation and propylation. When the method was applied to analysis of selenite in selenised yeast reference material results were in good agreement with the indicated values.     

三硝基苯磺酸离子选择电极的制备和应用

三硝基苯磺酸是氨基酸分析常用试剂,在水溶液中它是稳定的一价阴离子。Sarantonis曾研制液膜型三硝基苯磺酸离子选择电极,间接测定氨基酸的浓度,其电极的线性响应范围为1.1×10~(-1)～5.1×10~(-5)mol·L~(-1)。