Liquid Chromatograph-Catalytic Analysis as a Automatic and Fractional Determination Method with Extremely High Sensitivity

1、液相色谱催化分析钒（IV和V）和铁（II和III）的自动分级测定钒（II和III）采用空气分段连续流分析（ASCFA），基于与溴酸钾和Bindschedler绿白碱的催化反应。以Tosoh模型TSK凝胶ic -阳离子为分离柱，0.2 mM乙二胺和1.0 mM酒石酸的混合物（pH 3.0）为洗脱液，将钒（IV）和钒(V)相互分离。将这两种方法连接起来，实现了钒（IV）和钒(V)的自动分式测定。本方法对每种钒的测定范围为5 ~ 300 nM。铁也通过上述催化反应测定。然而，液相色谱法分离钒和铁还没有成功。我们一直在调查他们的分离采用岛津（Shimadzu） sim -pack IC-C1型凝胶为分离柱，0.3 M乳酸为洗脱液，将钴、锰、铁相互分离。这些元素是通过与过氧化氢和铁的催化反应用ASCFA测定的。现在，我们一直在尝试把这两种方法联系起来沿酸性河流苏卡瓦河收集的水体和沉积物元素组成表明，VO_2^+/VO^<2+>的还原电位表明，钒（IV）在酸性溶液中溶解更稳定。为了将液相色谱-催化法分析钒（IV和V）应用于天然酸性水样，我们对山形县Sukawa酸性河沿岸水域和沉积物的元素组成进行了初步研究。钒（IV和V）的总浓度很高，在2 ~ 5ma之间。

1 Automatic and fractional determination of vanadium (IV and V) and iron (II and III) by liquid chromatograph-catalytic analysisVanadium was determined sensitively by air-segmented continuous flow analysis (ASCFA) based on a catalytic reaction with potassium bromate and Bindschedler's green leuco base. Vanadium (IV and V) were separated each other by using the Tosoh model TSK gel IC-Cation as a separation column, and the mixture (pH 3.0) of 0.2 mM ethylenediamine and 1.0 mM tartaric acid as a eluate. By connecting these two methods, vanadium (IV and V) were determined automatically and fractionally. Determination range by the present method was 5 - 300 nM for each vanadium speciese.Iron was also determined by the above catalytic reaction. However, we have not succeed to separate vanadium and iron by liquid chromatography. We have been investigating their separation.2 Automatic and fractional determination of cobalt, manganese and iron by liquid chromatograph - catalytic analysisCobalt, manganese and iron were separated one another by using Shimadzu model Shim-pack IC-C1 gel as a separation column, and 0.3 M lactic acid as a eluate. These elements were determined by ASCFA based on a catalytic reaction with hydrogen peroxide and tiron. Now, we have been trying to connect these two methods.3 Elemental composition of waters and deposits collected along the acid river SukawaRedox potential of VO_2^+/VO^<2+> suggests that vanadium (IV) dissolves more stably in acid solution. We investigated preliminarily the elemental composition of waters and deposits collected along the acid river Sukawa, Yamagata Pref., in order to apply our liquid chromatograph-catalytic analysis for vanadium (IV and V) to natural acid water samples. Total concentration of vanadium (IV and V) was very high and ranged from 2 to 5 muM.