共振光猝灭法测定环境水样中痕量硒
Determination of Trace Selenium in Environmental Water Samples by Using Resonance Light Quenching Method
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摘要: 在阿拉伯树胶(AG)存在下,0.14 mol/L硫酸介质中,硒(Ⅳ)与过量的I-反应生成I-3,加入乙酸钠后I-3与亚甲基蓝反应成离子缔合物,在波长288 nm处共振光猝灭,建立了共振光散射法测定痕量硒的方法。确定了碘化钾、亚甲基蓝、乙酸钠和增溶剂阿拉伯树胶溶液的浓度,在室温(20~30℃)下反应15 min,提高了体系的灵敏度和稳定性。共振光散射猝灭值与硒(Ⅳ)浓度在0~0.24 μg/mL范围内线性关系良好,方法检出限为 1.01 μg/L。Fe3+、Pb2+、Cu2+和Zn2+的干扰用EDTA消除。方法用于测定环境水样中痕量硒,相对标准偏差(RSD)为1.3%~3.6%(n=5),回收率为97.4%~100.8%。Abstract: A new resonance light quenching method for the quantification of trace selenium has been developed. The method is based on the reaction of Se (Ⅳ) with excess I- in 0.14 mol/L H2SO4 solution to produce I-3 with arabic gum (AG). After adding NaAc, I-3 reacts with methylene blue (MB) to form an ion-association complex, resulting in resonance light quenching at a wavelength of 288 nm. The optimum concentrations of KI, MB, NaAc and solubilizer AG were decided. In addition, reaction for 15 min at room temperature (20-30℃) was found out. As a result, the sensitivity and stability of the system was improved. Good linear relationship between resonance light quenching intensity and Se(Ⅳ) concentration occurs in the content range of 0-0.24 μg/mL. The detection limit is 1.01 μg/L. The interferences of Fe3+, Pb2+, Cu2+ and Zn2+ are eliminated by EDTA. This method was applied to the quantification of trace selenium in environmental water samples with RSD of 1.3%-3.6% (n=5) and recoveries from 97.4% to 100.8%.
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