流动注射-电化学发光法测定煤灰中痕量钼(Ⅵ)
Determination of Trace Amount of Molybdenum(Ⅵ) in Coal Ash by Flow Injection-Electrochemiluminescence
摘 要
基于钼(Ⅵ)在-0.60 V(vs.Ag/AgCl)电位下在线还原为钼(Ⅲ),且在碱性条件下钼(Ⅲ)与鲁米诺发生化学发光反应,据此提出了流动注射-电化学发光法测定煤灰中痕量钼(Ⅵ)的方法。钼(Ⅵ)的质量浓度与化学发光强度的增加值在5.0×10-7~5.0×10-4g·L-1范围内呈线性关系,检出限(3s/k)为5×10-8g·L-1。对1.0×10-6g·L-1钼(Ⅵ)标准溶液进行11次测定,测定值的相对标准偏差为2.6%。方法可用于煤灰中痕量钼(Ⅵ)的测定,测定值与国标方法测定值相符。
电化学发光法
流动注射
煤灰
Molybdenum(Ⅵ)
Electrochemiluminescence
Flow injection
Coal ash
Abstract
Based on the on-line reduction of molybdenum(Ⅵ) to molybdenum(Ⅲ) at the potential of -0.60 V(vs.Ag/AgCl), and the chemiluminescence (CL) reaction of luminol with molybdenum(Ⅲ) in alkaline condition, a method of flow injection-electrochemiluminescence for the determination of trace amount of molybdenum in coal ash was proposed. Linear relationship between values of increase in CL intensity and mass concentration of molybdenum(Ⅵ) was obtained in the range of 5.0×10-7-5.0×10-4g·L-1, with detection limit (3s/k) of 5×10-8g·L-1. Values of RSD (n=11) obtained for molybdenum(Ⅵ) at a concentration of 1.0×10-6g·L-1 was 2.6%. The proposed method was applied to the determination of molybdenum in coal ash, giving results in consistency with those obtained by the GB standard method.
中图分类号 O657.32
所属栏目 试验与研究
基金项目 国家自然科学基金资助项目(20275023)
收稿日期 2011/6/2
修改稿日期
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联系人作者杨玲娟(gstsylj@126.com)
备注杨玲娟(1970-),女,陕西宝鸡人,副教授,硕士,主要研究方向为化学发光分析和色谱分析。
引用该论文: YANG Ling-juan,LI Xiao-dong,WANG Xiao-feng. Determination of Trace Amount of Molybdenum(Ⅵ) in Coal Ash by Flow Injection-Electrochemiluminescence[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2012, 48(7): 753～755
杨玲娟,李晓东,王晓峰. 流动注射-电化学发光法测定煤灰中痕量钼(Ⅵ)[J]. 理化检验－化学分册, 2012, 48(7): 753～755
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【3】杨瑞春,夏芳.电感耦合等离子体质谱法测定烟草中总钼［J］.理化检验-化学分册, 2010,46(10):1215-1217.
【4】FERREIRA S L C, SANTOS H C D, CANRPOS R C. The determination of molybdenum in water and biological samples by graphite furnace atomic spectrometry after polyurethane foam column separation and preconcentration ［J］. Talanta, 2003,61:789-795.
【5】陈文,王正猛,吴晓蓉,等.钢铁中微量钼的单扫描极谱测定［J］.四川有色金属, 2003(3):38-40.
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【10】杨玲娟,吕九如,王小芳.恒电位电生还原剂与鲁米诺化学发光分析研究［J］.天水师范学院学报, 2003,23(2):40-42.
【11】贺慧彤.探讨煤灰成分测定中的几个问题［J］.煤质技术, 2009(6):27-29.
【12】吴诚.金属材料分析方法的选择和施行［J］.理化检验-化学分册, 2003,38(5):261-264.
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