1,2-二羟基蒽醌-3-磺酸钠固相萃取光度法测定微量钒(Ⅴ)  

Solid phase extraction and spectrophotometric determination of trace vanadium with 1,2-dihydroxyanthraquinone-3-sulfonic acid sodium

作　　者：李慧芝[1] 许崇绢[1] 解文秀[1] 

机构地区：[1]济南大学化学化工学院,山东济南250022

出　　处：《冶金分析》2008年第1期40-43,共4页Metallurgical Analysis

基　　金：山东省自然科学基金资助项目(Y2000B09)

摘　　要：研究了1，2-二羟基蒽醌-3-磺酸钠与钒（Ⅴ）的显色反应，建立了测定钒的光度分析新方法。在pH4．0的醋酸一醋酸钠缓冲溶液中，在溴化十六烷基三甲基铵（CTMAB）存在下，1，2-二羟基蒽醌-3-磺酸钠与钒（Ⅴ）反应生成摩尔比为2：1稳定络合物，该络合物可用阳离子交换树脂固相萃取柱富集，吸附柱上富集的络合物用乙醇洗脱后用分光光度法测定。分离后的测定液中，络合物最大吸收波长为420nm，表现摩尔吸光系数ε=1．16×10^5L·mol^-1·cm^-1，钒量在0～0．4μg／mL内符合比尔定律，相关系数r=0．9989，对30余种共存离子进行试验，大多数常见离子不干扰测定。方法用于合金、矿石、粉煤灰中钒的分析，相对标准偏差小于3％，加标回收率为96％～105％。A new spectrophotometric method was developed for the determination of trace vanadium based on the rapid reaction of vanadium（Ⅴ） with 1,2-dihydroxyanthraquinone-3-sulfonic acid sodium. In the presence of CTMAB, 1, 2-dihydroxyanthraquinone-3-sulfonic acid sodium reacts with vanadium（Ⅴ） to form a stable complex with molar ratio of 2 ： 1 in HAc-NaAc buffer solution （pH 4.0）. The complex was extracted by cation exchange resin cartridge and was eluted with ethanol, then be determined by spectrophotometry. The apparent molar absorptivity ε is 1.16× 10^5L·mol^-1·cm^-1 at 420 nm. Beer＇s law is obeyed in the range of 0-0.4 μg/mL for V（Ⅴ） and r=0. 998 9. More than 30 coexistent ions didn＇t disturb the determination. This method has been applied to the determination of vanadium（Ⅴ） in alloy, rock and fly ash samples with the RSD less than 3% and the recovery of 96%- 105%.

关 键 词：固相萃取 1 2-二羟基蒽醌-3-磺酸钠 钒 分光光度法 

分 类 号：O657.3[理学—分析化学]