Electrospray Ionization InterFace and Its Application in Electrophoresis/Mass Spectrometry

论述了ESI的工作原理、结构和CE-ESI-MS的应用The principle,conFiguration and application of CE EI MS are discussed.国家自然科学基

A Novel Hydride Generation Technique—— Movable Reduction Bed Hydride Generator Ⅰ. The Configuration and Characteristic of the Movable Reduction Bed Hydride Generator

发展了一种新型的氢化物发生技术———可移动还原床氢化物发生器，可以实现微升级样品的分析而不需要对样品进行酸化和使用气-液分离器。给出了装置的结构、操作，试验并优化了固体还原剂与有机酸的质量配比、反应腔体体积、进样量等反应条件。该技术易于实现自动化，可作为液相色谱、毛细管电泳和其他色谱分离技术与光谱检测技术之间的接口。A novel hydride generation system termed “movable reduction bed hydride generator” has been developed in this work.It will accomplish the hydride generation at micro liter sample volume without the need for an external addition of acid, and the use of a gas liquid separator.The technique may offer a possibility of automatic operation, as well be used as an interface for liquid chromatography(LC), capillary electrophoresis(CE) and other chromatograph.国家自然科学基

A Novel Hydride Generation Technique\=Movable Reduction Bed Hydride Generator\=. As an Interface between Capillary Zone\=Electrophoresis and ICPAES for\= Arsenic Speciation Analysis

发展了一种新型的氢化物发生装置———可移动还原床氢化物发生器（MrbHg）。应用该技术可将经毛细管区带电泳（CzE）分离之后的各种砷的化合物转换为相应的氢化物，然后再被引入到电感耦合等离子体发射光谱（ICP-AES）进行检测。对不同形态砷的不同化合物的CzE分离条件进行了优化，包括缓冲溶液的PH值及浓度、进样量等。CzE-MrbHg-ICP-AES应用于4种砷化合物的定量测定，峰面积的rSd（n＝5）在1.9%~11.7%。4种砷的浓度检出限分别为：AS（Ⅲ）、甲胂酸和AS（V）0.32Mg/l，二甲胂酸钠0.35Mg/lHydride generation technique may significantly improve the detection limits for a number of hydride forming elements with atomic spectrometric determination. In order to harmonize the microliter level eluent from capillary zone electrophoresis (CZE) and the milliliter sample volume commonly needed in ICPAES, a specially designed technique movable reduction bed hydride generation (MRBHG) has been developed. One of the advantages of the MRBHG is that it could be simply operated and might carry out the hydride generation for micro sample volume without the use of a gasliquid separator and the addition of an acid dehydrator. Thus the technique could be used to convert arsenic compounds from CZE separation to corresponding volatile hydrides followed by ICPAES analysis. The separation characteristics of arsenic species by capillary zone electrophoresis are presented in this paper including the optimization of experimental parameters such as pH and concentration of buffer solution, as well as sample国家自然科学基

A Novel Hydride Generation Technique\=Movable Reduction Bed Hydride Generator\= . Study of Interferences and Applications

新型的氢化物发生技术———可移动还原床氢化物发生器（MrbHg）可以实现微升级样品的测定而不需要对样品进行酸化和使用气-液分离器。应用MrbHg-电感耦合等离子体发射光谱取得了同等质量而不同形态的AS、SE的相同信号强度，证明了在MrbHg体系中氢化物元素之间的干扰得到消除，方法用于合金钢、富硒茶叶等实际样品的测定，标准加入的回收率在93%~114%。Some characteristics of the novel hydride generation systemmovable reduction bed hydride generator (MRBHG) is reported in this paper.Besides accomplishing the hydride generation at microliter sample volume without the need for an external addition of acid and use of a gasliquid separator, interferences among hydride forming elements are also greatly reduced in this system.The similar hydride generation efficiency for different valency and species of As and Se is obtained.The hydride forming elements in alloy steel and tea samples were determined by ICPAES with MRBHG system.The recoveries of standard addition for As and Se in alloy steels and a Chinese tea sample are 93%107% and 98%114% respectively.\=\=国家自然科学基

Studies on Speciation of Arsenious Compounds by Capillary Zone Electrophoresis

采用毛细管区带电泳，以磷酸盐为缓冲溶液分离了5种砷的化合物：AS（Ⅲ）、dMA、AnA、MMA和AS（V）.用紫外吸收法在191nM波长下，对实验条件进行了优化；使用扩展光程毛细管研究了实验方法的重现性；测定了各种砷化合物的峰面积与浓度的关系，在最大进样量时测定了检出限，并将该方法用于合成样品的分析.Using phosphate as buffer solution, five arsenic species: arsenite (As (Ⅲ)),monomethylarsonic acid (MMA), arsanilic acid (ANA), sodium dimethylarsinate (DMA) and arsenate (As (Ⅴ) ) have been separated by capillary zone electrophoresis.Experiment conditions were optimized when the on-line UV detection was operated at 191 nm.The reproducibility of this method has been studied using extended light length capillary.Relation between signal peak area and sample concentration has been measured, and using the largest injection volume, the detection limit has been determined.Some kind of spiked sample has also been detected.国家自然科学基

Studies on speciation of arsenious compounds by capillary zone electrophoresis

Using phosphate as buffer solution, five arsenic species: arsenite(As(II)), monomethylarsonic acid(MMA), arsanilic acid(ANA), sodium dimethylarsinate(DMA) and arsenate (As(V)) have been separated by capillary zone electrophoresis, Experiment conditions were optimized when the on-line UV detection was operated at 191 nm. The reproducibility of this method has been studied using extended light length capillary. Relation between signal peak area and sample concentration has been measured, and using the largest injection volume, the detection limit has been determined. Some kind of spiked sample has also been detected