采用奎宁修饰树脂微柱分离/预富集水中钒的形态，并通过氟化辅助电热蒸发（FETV）-电感耦合等离子体发射光谱法（ICP-OES）进行测定。
Speciation of vanadium in water with quinine modified resin micro-column separation/preconcentration and their determination by fluorination assisted electrothermal vaporization (FETV)-inductively coupled plasma optical emission spectrometry (ICP-OES).
作者信息
Wu Yiwei, Jiang Zucheng, Hu Bin
机构信息
Department of Chemistry, Wuhan University, Wuhan, P.R. China.
出版信息
Talanta. 2005 Oct 15;67(4):854-61. doi: 10.1016/j.talanta.2005.04.014.
A simple and selective method of flow injection (FI) using a micro-column packed with quinine modified resin as solid phase extractant has been developed for preconcentration and separation of trace amount of vanadium(V) and vanadium(IV) in water samples, followed by determination with fluorination assisted electrothermal vaporization (FETV)-inductively coupled plasma optical emission spectrometry (ICP-OES). At pH 3 approximately 3.8, the modified resin is selective towards V(V) and almost not towards V(IV), while, V(IV) could be quantitatively adsorbed by the modified resin at pH 5 approximately 7. The two vanadium species adsorbed by modified resin could be readily desorbed quantitatively with 0.3 ml of 0.5 mol l(-1) HCl. Both vanadium species in elution were then determined by ETV-ICP-OES with the use of polytetrafluoroethylene (PTFE) as chemical modifier. Effects of acidity, sample flow rate, concentration of elution solution and interfering ions on the recovery of the analytes have been systematically investigated. Under the optimal conditions, the adsorption capacities of the quinine modified resin for V(V) and V(IV) are 7.6 and 8.0 mg g(-1), respectively. The detection limit (3sigma) of V is 0.072 ng ml(-1) for FETV-ICP-OES and 0.56 pg ml(-1) for FETV-ICP-MS with enrichment factor of 62.5, and the relative standard deviation (R.S.D.) is 4.9% (n=9, C=0.2 microg ml(-1)) and 3.8% (n=9, C=1.0 ng ml(-1)), respectively. The proposed method has been applied to the determination of trace V(V) and V(IV) in different water samples, and the recoveries of V(V) and V(IV) are 100+/-10%. In order to further verify the accuracy of the developed method, FETV-ICP-MS was employed to analyze the vanadium species in water samples after separation/preconcentration, and analytical results are in good agreement with that obtained by the proposed method. The developed method was also applied to the analysis of the total V in GBW07401 soil certified reference material and in GBW07605 tea leaves certified reference material, and the determined values coincided with the certified values very well.
建立了一种简单且选择性的流动注射（FI）方法，该方法使用填充有奎宁改性树脂的微柱作为固相萃取剂，用于预富集和分离水样中的痕量钒（V）和钒（IV），随后采用氟化辅助电热蒸发（FETV）-电感耦合等离子体发射光谱法（ICP-OES）进行测定。在pH约为3.8时，改性树脂对V（V）具有选择性，对V（IV）几乎无选择性，而在pH约为5至7时，V（IV）可被改性树脂定量吸附。被改性树脂吸附的两种钒物种可用0.3 ml 0.5 mol l⁻¹ HCl轻松定量解吸。然后使用聚四氟乙烯（PTFE）作为化学改性剂，通过ETV-ICP-OES测定洗脱液中的两种钒物种。系统研究了酸度、样品流速、洗脱液浓度和干扰离子对分析物回收率的影响。在最佳条件下，奎宁改性树脂对V（V）和V（IV）的吸附容量分别为7.6和8.0 mg g⁻¹。对于FETV-ICP-OES，V的检测限（3σ）为0.072 ng ml⁻¹，对于FETV-ICP-MS，富集因子为62.5时检测限为0.56 pg ml⁻¹，相对标准偏差（R.S.D.）分别为4.9%（n = 9，C = 0.2 μg ml⁻¹）和3.8%（n = 9，C = 1.0 ng ml⁻¹）。所提出的方法已应用于不同水样中痕量V（V）和V（IV）的测定，V（V）和V（IV）的回收率为100±10%。为了进一步验证所开发方法的准确性，采用FETV-ICP-MS分析分离/预富集后的水样中的钒物种，分析结果与所提出的方法获得的结果非常吻合。所开发的方法还应用于GBW07401土壤标准参考物质和GBW07605茶叶标准参考物质中总V的分析，测定值与认证值非常吻合。
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