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Selenium Speciation of Soil/ Sediment Determined with Sequential Extractions and Hydride Generation Atomic Absorption Spectrophotometry

机译:连续萃取 - 氢化物发生原子吸收分光光度法测定土壤/沉积物中硒的形态

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摘要

Understanding the speciation of the multioxidation states of selenium is vital to predicting the mineralization, mobilization, and toxicity of the trace element in natural systems. Asequential extraction scheme (SES) was developed for identification of Se oxidation states that first employed 0.1 M (pH 7.0) K2HPO4-KH2PO4 (P-buffer) to release soluble selenate (Se+VI) and selenide (Se-II) and ligand-exchangeable selenite (Se+IV). The second step involved oxidation of organic materials with 0.1 M K2S2O8 (90 °C) to release Se-II and Se+IV associated or occluded with organic matter. The final step used HNO3 (90 °C) to solubilize insoluble Se remaining in the sample. The solubilized Se compounds were speciated by a selective hydride generation atomic absorption spectrophotometry technique. Accuracy of the developed SES method (96-103% recovery) was verified by use of prepared Se compounds of known speciation, NIST standard reference materials, and existing seleniferous soils. The average precision (relative standard deviation) for the P-buffer extraction ranged from 5.5 to 7.7% (n = 12); the precision of the persulfate extraction ranged from 2.6 to 8.4% (n = 12); and the precision of the nitric acid extraction ranged from 2.8 to 7.4% (n = 12) for three soils extracted at four different time periods. The method was applied to analyze Se species in seleniferous plant, soil, and sediment samples.
机译:了解硒的多氧化态的形态对于预测自然系统中微量元素的矿化,迁移和毒性至关重要。开发了用于提取Se氧化态的顺序提取方案(SES),该方案首先使用0.1 M(pH 7.0)K2HPO4-KH2PO4(P-缓冲液)释放可溶性硒酸盐(Se + VI)和硒化物(Se-II),以及配体-可交换亚硒酸盐(Se + IV)。第二步涉及用0.1 M K2S2O8(90°C)氧化有机材料,以释放与有机物缔合或封闭的Se-II和Se + IV。最后一步使用HNO3(90°C)溶解残留在样品中的不溶硒。通过选择性氢化物发生原子吸收分光光度法技术确定了溶解的硒化合物。已开发的SES方法(回收率96-103%)的准确性已通过使用已知种的制备的Se化合物,NIST标准参考材料和现有的含硒土壤进行了验证。 P缓冲液提取的平均精度(相对标准偏差)为5.5至7.7%(n = 12);过硫酸盐萃取的精度为2.6%至8.4%(n = 12);在四个不同时间段内提取的三种土壤的硝酸提取精度为2.8%至7.4%(n = 12)。该方法用于分析硒类植物,土壤和沉积物样品中的硒物种。

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