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土壤中痕量铅(Ⅱ)的偶合反应流动注射化学发光增敏法测定 被引量:3

Determination of Trace Pb(Ⅱ) in Soil by Increasing Sensitivity Method with Coupling Reaction of Flow Injection/Chemiluminescence
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摘要 [目的]建立了测定铅的新方法。[方法]基于Ph(Ⅱ)能置换出Fe(Ⅱ)-EDTA络合物中的Fe(Ⅱ)和鲁米诺-罗丹明B—Fe(Ⅱ)产生化学发光的反应,建立了简易、快速测定土壤中铅的置换偶合反应流动注射化学发光增敏法。[结果]实验建立的优化条件为:鲁米诺溶液和罗丹明B的流速为75r/min,Pb(Ⅱ)和Fe-EDTA的流速为30r/min,混合管L1的长度为150cm,L2的长度为5cm,在pH值为3、0的硝酸介质中Fe(Ⅱ)与EDTA的络合比为1:1,化学发光反应在pH值为10.6,鲁米诺和罗丹明B浓度分别为5.0×10^-5和1.0×10^-5mol/L,负高压为1190V。在优化的实验条件下,铅的线性范围为6.0×10^-9 ~2.8×10^-7mg/L,检出限为2.0×10^-9mg/L。[结论]该法适用于土壤中铅的测定。 [ Objective] The study was to establish a new method for the determination of Pb. [ Method] Based on the replacement of Fe ( Ⅱ ) by Pb ( Ⅱ ) from Fe ( Ⅱ ) -EDTA complex, and the chemiluminescence reaction of Fe( Ⅱ ) -luminol-RhB, the increasing sensitivity method with coupling replacement reaction of flow injection/chemiluminescence was established for simple and quick determination on Pb in soil. [ Result] The optimum conditions established in the experiment were that: the flow rate of lumino solution and RhB were 75 r/min, that of Pb ( Ⅱ ) and Fe-EDTA was 30 r/min, The length of mixing pipe L1 was 150 cm, and that of L2 was 5 cm. The complexation rate of Fe ( Ⅱ ) and EDTA was 1:1 in nitric acid medium with pH of 3.0. During chemiluminescence reaction, its pH value was 10.6, the concn, of luminal and RhB was 5.0 × 10^-5 and 1.0 × 10^-5 mol/L resp. , and the negative high-voltage was 1 190 V. Under the optimum experimental conditions, the linear range of Pb was 6.0 ×10^-9 - 2.8 × 10^-7 mg/L with a detection limit of 2.0 × 10^-9 mg/L. [ Conclusion] The method was suitable to determine Pb ( Ⅱ ) in soil.
出处 《安徽农业科学》 CAS 北大核心 2008年第23期10071-10073,共3页 Journal of Anhui Agricultural Sciences
基金 贵州省教育厅自然科学青年项目(黔教科2007072)
关键词 流动注射 化学发光 土壤 Flow injection Chemiluminescence Soil Pb
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