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Determination of Selenium(IV) by Electrothermal Atomic Absorption Spectrometry using Single Drop Extraction in Real Samples

机译:样品中单滴萃取-电热原子吸收光谱法测定硒(IV)

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摘要

In this investigation,two new chemical modifiers for determination of Se(IV) are reported.The first,is coating of Pd in graphite tube and injection of Pd solution on top of sample solution in tube ([Pd_((c))+Pd_((i))]).Second modifier is concurrent coating with each of W,Rh and Pd in graphite tube ([W.Rh.Pd]_((c))).These modifiers showed very low detection limits,higher sensitivity and longer lived than other modifiers previously adapted for selenium.Second modifier is useful for determination of Se(IV) in inorganic compounds.For obtaining higher sensitivity method of single drop extraction for determination of trace amounts of selenium is reported.In this method Se (IV) is reacted with o-phenylenedi-amine,the piasoselenol complex formed was then extracted into micro drop of 1,2 dichloroethane.After extraction,the micro drop was retracted and directly transferred into a graphite tube modified by [Pd_((c))+Pd_((i))].The detection limit was calculated to be 0.8 ng/mL (absolute value of 0.3 ng) based on 3S_b.The relative standard deviation for five replicate analysis of 10 ng/mL Se was 4.8 %.The calibration curve was linear in the range of 0.8 to 40 ng/mL with a sensitivity of 0.25 ng/mL.Recovery of the method was 96 % for tap water spiked with selenium.In order to evaluate the applicability of the method,the amount of Se(IV) in plants,sea water and milk was determined.
机译:在这项研究中,报道了两种用于测定Se(IV)的新化学改性剂。首先,是在石墨管中涂覆Pd并将Pd溶液注入管中的样品溶液顶部([Pd _((c))+ Pd_ (((i))])。第二种修饰剂是在石墨管中同时涂覆W,Rh和Pd([W.Rh.Pd] _((c)))。这些修饰剂的检出限非常低,灵敏度更高。第二种改性剂可用于测定无机化合物中的Se(IV)。报道了为了获得更高灵敏度的单滴萃取法测定痕量硒的方法。 IV)与邻苯二胺反应,然后将形成的吡咯烯醇复合物萃取到1,2氯乙烷的微滴中。萃取后,将微滴缩回并直接转移到[Pd _((c) )+ Pd _(((i))]。计算出的检出限为0.8 ng / mL(绝对值为0以3S_b为基准的.3 ng)。五次重复分析的10 ng / mL Se的相对标准偏差为4.8%。校准曲线在0.8至40 ng / mL范围内呈线性,灵敏度为0.25 ng / mL。用硒加标的自来水的方法回收率为96%。为评估该方法的适用性,测定了植物,海水和牛奶中Se(IV)的含量。

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