Development of homogeneous liquid-liquid extraction method and its application to high performance separation-detection system

本研究将均相液-液萃取法作为预富集方法与一些仪器分析方法相结合，建立了一种新的高效分离检测系统。研究结果如下：1.新相分离现象的研究：研究了9种金属离子作为含氟表面活性剂（全氟辛烷磺酸）的反离子。其中，钙离子的使用导致液相沉淀相通过离子对发生相分离现象。2.荧光X射线分析（XRF）：建立了高价金属离子{Ti（IV），V（V），Zr（VI），Nb（V），Ta（V）}的选择性分离和富集、10 μ <-8>M级的XRF同时测定以及铝铜合金中杂质元素Ti，Zr，V的分析方法。 ...更多信息 采用基于全氟辛酸pH相关相分离现象的均相液-液萃取法作为TXRF的预富集方法，该方法可将目标元素富集到几μ l体积，而不受熔融试剂的影响。同时，采用TXRF法同时测定了陶瓷或石墨样品中的微量杂质元素Fe、Ni、Cu。4.高效液相色谱法：采用均相液-液萃取法对水/乙酸/氯仿三元体系进行了pH相关相分离，建立了高效液相色谱法（HPLC）分离富集体系，并用分光光度法测定了ppb级的铜（II）和钯（II）采用超高灵敏度的螯合试剂四（4-吡啶基）卟啉展开，按原计划进行，获得了满意的结果。在不久的将来，这一有用的方法将被应用到广泛的实际样品。少

This study has developed a new high-performance separation-detection system by combinating homogeneous liquid-liquid extraction method as preconcentration and some instrumental methods of analysis. The produced fruits during the term of two years are as follows.1.Research of new phase separation phenomenon : Nine kinds of metal ion were examined as a counter ion for fluorosurfactant (perfluorooctane sulfonic acid). Among them, the use of calcium ion led to liquid sedimented phase by ion-pair phase separation phenomenon. The extraction method developed is well suited for concentration of vital substance, because this sedimented phase contains much water.2.Fluorescent X-rays analysis (XRF) : The selective separation and concentration for high-valence metal ions {Ti (IV), V (V), Zr (VI), Nb (V), Ta (V)}, simultaneous determination of 10^<-8> M levels for these ions by XRF and analysis of Ti, Zr, V as impurity element in Al-Cu alloy were established.3.Total reflection X-ray fluorescence : … More Homogeneous liquid-liquid extraction method based on pH dependent phase separation phenomenon using perfluorooctanoic acid was applied as a preconcentration of TXRF.In this extraction method, the purpose element was concentrated to a few ul of volume without having influence of much molten agent. Moreover, small amounts of impurity element such as Fe, Ni and Cu in ceramics or graphite sample were simultaneously determined by TXRF.4.High-performance liquid chromatography : Homogeneouse liquid-liquid extraction method based on pH dependent phase separation of water/acetic acid/chloroform ternary components system was applied as preconcentration of HPLC.Spectrophotometric detection-HPLC of ppb levels of copper (II) and palladium (II) was developed with ultra-highly sensitive chelating reagent {i.e.tetrakis (4-pyridyl) porphine}.In conclusion, satisfactory results were, obtained in this study according to the original plan. In the near future, this useful method will be applied to wide range of practical sample. Less