4－（6－甲基－2－苯并噻唑偶氮）间苯三酚反相高效液相色谱分离测定钒钴镍铬  

Separation and Determination of V(Ⅴ),Co(Ⅱ),Ni(Ⅱ)and Cr(Ⅵ)with 4-( 6-Methyl-2-Benzothiazolylazo)Phloroglucinol by Reversed-Phase HPLC

作　　者：缪予霞 王红[1] 张华山[1] 程介克[1] 

机构地区：[1]武汉大学化学系

出　　处：《分析试验室》1994年第6期1-4,共4页Chinese Journal of Analysis Laboratory

基　　金：国家自然科学基金

摘　　要：作者以新研制的４－（６－甲基－２－苯并噻唑偶氨）间苯三酚为柱前衍生试剂，用含１０ｍｍｏｌ／Ｌ的ｐＨ６．８０的ＨＡｃ－ＮａＡｃ缓冲溶液，１０ｍｍｏｌ／ＬＴＢＡ·Ｂｒ和１×１０￣（－４）ｍｏｌ／ＬＥＤＴＡ的甲醇－水溶液（７８：２２，Ｖ／Ｖ）作流动相，在Ｃ＿（１８）柱上，１１ｍｉｎ内反相ＨＰＬＣ分离测定了Ｃｒ（Ⅵ），Ｖ（Ⅴ）Ｃｏ（Ⅱ），Ｎｉ（Ⅲ）。当Ｓ／Ｎ＝３时，其检出限分别是Ｖ（Ⅴ）５．４５ｎｇ，Ｃｏ（Ⅱ）１．０９ｎｇ，Ｎｉ（Ⅱ）１．５０ｎｇ，Ｃｒ（Ⅵ）１．７０ｎｇ。A method for the separation and determination ofV(Ⅴ),Co(Ⅱ),Ni(Ⅱ)and Cr(Ⅵ)by using a newreagent 4-(6-methyl-2-benzothiazolylazo)phloroglucinol(6-MeBTAP)as the pre-columnderivative reagent by RP-HPLC was investigated inthis work.V(Ⅴ),Co(Ⅱ), Ni(Ⅱ)and Cr (Ⅵ)ionsreact with 6-MeBTAP in weak acidic medium to formstable red color chelates by heating in a boiling water-bath for about 20 minutes. The maximum absorptionsof the chelates were between 548 and 556nm, and thedetection wavelengthwas set at 550nm.It was foundthat the four chelates could be separated on a C_(18)column using a mobile phase consisted of methanol-water(78/22,V/V)containing 10 mmol/L pH6.80acetate buffer,10 mmol/L TBA·Br and 10￣(-4) mol/LEDTA,The detection limits were 1.7ng for Cr,0.9ngfor Co,1.5ng for Ni and 5.45ng for V when RSN=3。

关 键 词：间苯三酚 高效液相色谱 钒 钴 镍 铬 

分 类 号：O657.72[理学—分析化学]