首页> 外文期刊>Radiochimica Acta: International Journal for Chemical Aspects of Nuclear Science and Technology >Differential pulse cathodic stripping voltammetric determination of uranium with arsenazo-III at the hanging mercury dropping electrode
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Differential pulse cathodic stripping voltammetric determination of uranium with arsenazo-III at the hanging mercury dropping electrode

机译:悬挂式滴汞电极上的偶氮azoⅢ-差示脉冲阴极溶出伏安法测定铀

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摘要

An accurate, inexpensive and less laborious controlled adsorptive accumulation of uranium(VI)-arsenazo-III on a hanging mercury drop electrode (HMDE) has been developed for uranium(VI) determination. The method is based upon the collection of uranium(VI)-arsenazo-III complex at pH 5-6 at the HMDE and subsequent direct stripping measurement of the element in the nanomolar concentration level. The cathodic peak current (i(p,c)) of the adsorbed complex ions of uranium(VI) was measured at -0.35 V vs. Ag/AgCl reference electrode by differential pulse cathodic stripping voltammetry (DP-CSV), proceeded by an accumulation period of 150s2.5 in Britton-Robinson buffer of pH 5. The plot of the resulting ip,, vs. uranium(VI) concentration was linear in the range 2.1 x 10(-9) to 9.60 x 10(-7) mol L-1 uranium(VI) and tended to level off at above 9.6 x 10(-7) mol L-1. The limits of detection and quantification of uranium(VI) were found to be 4.7 x 10(-10) and 1.5 x 10(-9) mol L-1, respectively. A relative standard deviation of 2.39% (n = 5) at 8.5 x 10(-7) mol L-1 uranium(VI) was obtained. The method was validated by comparing the results with that obtained by ICP-MS method with RSD less than 3.3%. The method was applied successfully for the analysis of uranium in certified reference material (IAEA soil-7), and in phosphate fertilizers.
机译:已经开发了一种准确,廉价且省力的可控的铀(VI)-砷偶氮-III在悬挂式汞滴电极(HMDE)上的吸附累积法,用于铀(VI)的测定。该方法基于在HMDE上于pH 5-6收集铀(VI)-)-III配合物,并随后以纳摩尔浓度水平对元素进行直接汽提测量。通过差分脉冲阴极溶出伏安法(DP-CSV)在相对于Ag / AgCl参比电极的-0.35 V下测量了铀(VI)吸附的复合离子的阴极峰值电流(i(p,c))。在pH 5的Britton-Robinson缓冲液中累积150s2.5的时间。所得的ip,铀(VI)浓度曲线在2.1 x 10(-9)至9.60 x 10(-7)范围内呈线性关系摩尔L-1铀(VI)并趋于稳定在9.6 x 10(-7)摩尔L-1以上。铀(VI)的检出限和定量限分别为4.7 x 10(-10)和1.5 x 10(-9)mol L-1。在8.5 x 10(-7)mol L-1铀(VI)下获得的相对标准偏差为2.39%(n = 5)。通过与RSD小于3.3%的ICP-MS方法进行比较,验证了该方法的有效性。该方法已成功用于分析标准物质(IAEA土壤7)和磷酸盐肥料中的铀。

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