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Application of colloidal palladium modifier for the determination of As, Sb and Pb in a spiked sea water sample by electrothermal atomic absorption spectrometry

机译:胶态钯改性剂在电热原子吸收光谱法测定加标海水样品中砷,锑和铅中的应用

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Colloidal palladium was used as a chemical modifier for analysis of complex samples by electrothermal atomic absorption spectrometry. In order to demonstrate high potnetial of the modifier, optimization of the time-temperature program of the atomizer was limited with only pyrolysis and atomization temperatures, Fixed palladium modified masses were applied (6 #mu#g for pure analyte solutions and 15 #mu#g for matrix-containing solutions). It was shown that in the presence of colloidal palladium, interference-free determinations of As, Sb and Pb are possible up to at least 450 #mu#g of chloride ion, or 40 #mu#g of sulfate ion (as their sodium salts) in the atomizer. Colloidal palladium was used for the direct determination of As, Sb and Pb in a spiked sea water sample (from Bosphorus channel near istanbul) by means of the calibration graphs prepared with pure analyte solutions. The detection limits for As, Sb and Pb in a sea water matrix calculated according to 2#sigma# criteria are 5.4, 3.6 and 1.1 ng ml~(-1), respectively (for sample volume 10 #mu#l). In unspiked sea water, the contents of As, Sb and Pb were found to be below the detection limits. Recoveries of spiked analytes (25 and 50 ng ml~(-1)) were in the region of 98-112% depending on the nature of analyte and the concentration of spike.
机译:胶体钯用作化学修饰剂,用于通过电热原子吸收光谱法分析复杂的样品。为了证明改性剂的高电位性,仅通过热解和雾化温度限制了雾化器时间-温度程序的优化,使用了固定的钯改性物质(纯分析物溶液为6#mu#g,15#mu# g用于含基质的溶液)。结果表明,在胶体钯的存在下,砷,锑和铅的无干扰测定可能达到至少450#mu#g氯离子或40#mu#g硫酸根离子(作为其钠盐) )在雾化器中。通过使用纯分析物溶液制备的校准图,使用胶体钯直接测定加标海水样品(来自伊斯坦布尔附近的博斯普鲁斯海峡)中的砷,锑和铅。根据2#sigma#标准计算的海水基质中As,Sb和Pb的检出限分别为5.4、3.6和1.1 ng ml〜(-1)(样品量为10#mu#l)。在未加标海水中,As,Sb和Pb的含量低于检出限。加标分析物(25和50 ng ml〜(-1))的回收率在98-112%左右,这取决于分析物的性质和加标浓度。

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