Evaluation of the quality of colour changes of complexometric indicators in the titration of copper (II) with EDTA by tristimulus colorimetry

The quality of colour changes of the indicators hematoxylin, 4(2-pyridylazo)resorcinol (PAR), xylenol orange, pyrocatechol violet, chromazurolS and eriochrome cyanineR in the complexometric titration of copper(II) with ethylenediaminetetraacetic acid (EDTA) were studied with the help of tristimulus colorimetry, utilising a comparative study of the parameters SCD (specific colour discrimination), CIE La^*b^* 1976 and LABHNU 1977. Hematoxylin was found to be the best indicator among those studied. A screened indicator, viz. PAR + malachite green (52), was developed to enhance the quality of colour transition at the end-point and the accuracy of the titrimetric determination.     

High throughput continuous titration based on a flow ratiometry controlled with feedback-based variable triangular waves and subsequent fixed triangular waves

We propose a new approach for high-throughput continuous titration based on a flow ratiometry. The method was applied to potentiometric titrations of acids and bases. A base solution, the flow rate F_B of which was varied in response to controller output voltage V_c, was merged with an acid solution under constant total (acid + base) flow rate. Downstream, the pH of the mixed solution was measured with a flow-through glass electrode. Initially, V_c, and thus F_B was increased linearly. At the instant the equivalence point (EP) was sensed, the ramp direction of V_c was reversed from upward to downward. The direction was reversed to upward when EP was sensed again. Such the feedback-based operation gives a triangular waveform of V_c, because there is a delay corresponding mainly to the transit time of merged solutions to reach the sensor. The value of V_c that gives EP composition, V_E, was estimated by averaging the most recent maximum and minimum values of V_c. Next, fixed triangular waves of V_c was used to control F_B. The amplitude and the scan rate of the waves were fixed narrower and faster, respectively, than those in the feedback-based operation in order to improve the throughput rate. The EP can be located as long as the scan range covers V_E. These automated processes limited the titration to just the narrow range around EP, and thus realized extremely high throughput rate of maximally 17.6 titrations per minute (=3.4 s per titration) at R.S.D. = 0.35%.     

无机纳米管材料合成进展

无机材料的微观结构决定了材料的许多特性,如传输行为、催化活性、分离效率、粘附、储存和释放动力学。具有管状结构纳米尺度的材料由于其特殊的结构及由此带来的特殊性能正成为一个令人兴奋的化学研究领域。文章综述了近年来无机纳米管材料的合成途径和进展。     

Simultaneous deposition of Ni nanoparticles and wires on a tubular halloysite template: A novel metallized ceramic microstructure

Tubular halloysite can be used as a template to fabricate a novel metallized ceramic microstructure through electroless plating. Reduction of Pd ions by methanol is conducted to initiate Ni plating. There is a simultaneous deposition of Ni nanoparticles on the outer surface and discontinuous wires in the lumen site of the halloysite template obtained. The different deposition could be caused by the different composition distribution of ferric oxide impurity in the wall due to the isomorphic substitution during the formation of halloysite template. Its magnetic property is mainly attributed to the Ni nanoparticles, not the wires. The metallized ceramic microstructure has the potential to be utilized as a novel magnetic material.     

Ba-K-Bi-O和Ba-K-Pb-O氧化物的碘量滴定

本文提出了碘量法滴定Ba－K－Bi-O和Ba－K－Pb－O氧化物中Ba和Pb的名义价态，然后据此计算这些氧化物中K和Ba含量的方法。该法适用于正常条件下合成的具有ABO3型钙钛矿结构的Ba－K－Bi-O和Ba－K－Pb－O晶体。用本法的滴定结果表明，Tc为31K的Ba－K－Bi-O超导体的K含量为0．4，当K含量减少时，Tc随之下降。     

两相滴定法研究2-乙基己基膦酸单2-乙基己基酯从盐酸介质中萃取钕(Ⅲ)的动力学

本文利用两相滴定法作为分析手段,用恒界面池搅拌法考察了多种因素对2-乙基己基膦酸单2-乙基己基酯(HEHEHP,HA)从盐酸介质中萃取Nd(Ⅲ)动力学的影响,从实验结果推论出萃取过程为界面化学反应控制型机理。     

含吡啶环系西佛碱大环配合物和氮杂大环自由配体的合成

2,6-二羟甲基吡啶(1)经活性MnO_2氧化得到2,6-二甲酰基吡啶(2)。邻硝基苯酚与N-取代的二(氯乙基)胺在DMF溶液中反应,得到N-取代的1,5-二(邻硝基苯氧基)-3-氮杂戊烷(3a～3c),再经水合肼/Raney Ni还原,获得N-取代的1,5-二(邻氨基苯氧基)-3-氮杂戊烷(4a～4c)。利用Ba~(2 )作为模板离子,(2)分别与(4a～4c)反应,合成了一类新的含吡啶环系西佛碱大环配合物Ⅰ～Ⅲ,配合物Ⅰ、Ⅲ经与NaBH_4的乙醇溶液还原解络,得到氮杂大环自由配体Ⅳ和Ⅴ。所有西佛碱大环配合物和氮杂大环自由配体均经元素分析、IR、~1H NMR、MS等证实了它们的结构和组成。     

平行双铂丝微电极用于铁氰化钾电流滴定法测定抗坏血酸的研究

平行双柱微电极是一种基于可逆氧化还原物质在电极间反馈扩散使得信噪比进一步增大的新型微电极,作者首次将这种电极应用于电流滴定分析中。结果显示,电极间距很小时,终点突跃变敏锐,使灵敏度进一步提高。该方法不需搅拌溶液,单次测量样品量只需约3μ1,是一种有实用价值的新方法。