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Comparison of electrodeposition and precipitation for the preparation of samples for iodine analysis by AMS

机译:AMS制备碘分析样品的电沉积和沉淀的比较

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Sample preparation for Accelerator Mass Spectrometry (AMS) analysis of I-129 from environmental samples typically involves isolation and purification of the iodine followed by precipitation as silver iodide. The silver iodide is mixed with silver or niobium powder as a binder and medium for electrical conductivity and approximately 3 mg of the mixture pressed into a cathode for AMS analysis. Electrodeposited silver iodide on a silver clad niobium 50 mu m diameter wire provides an attractive alternative to precipitation. Six inches of wire and electrodeposited silver iodide are easier to handle when pressing cathodes and minimizes possible cross contamination between samples. Although electrodeposition onto pure silver wires has been recently reported, the usage of silver clad niobium wires could offer an additional advantage. The use of niobium in the silver iodide matrix has been reported to result in higher intensity and long term stability of the iodide ion current. This paper presents a comparison of electrodeposition methods using silver and silver clad niobium wires to the traditional precipitated silver iodide mixed with silver and niobium powders. The comparison was done using materials with I-129/127 ratios having nominal values of 5 x 10(-)(10) and 5 x 10(-11).For each I-129/127 ratio material, eight samples were analyzed for each preparation method on three days, with seven replicate AMS measurements per sample. For each ratio, the measurements of the separate days were combined for each method, yielding 168 measurements per method. An analysis of variance indicated minor statistical differences between the precipitated and electro-deposited materials, with the pooled standard error of the means being 0.2% for both similar to 5 x 10(-10) and similar to 5 x 10(-11) ratios.
机译:从环境样品中进行I-129的加速器质谱分析(AMS)的样品前处理通常涉及碘的分离和纯化,然后沉淀为碘化银。将碘化银与作为粘合剂和导电性介质的银或铌粉混合,并将约3 mg的混合物压入阴极进行AMS分析。在直径为50μm的镀银铌金属丝上电镀碘化银提供了一种有吸引力的沉淀方法。压阴极时,六英寸长的导线和电沉积的碘化银更易于处理,并最大程度地减少了样品之间的交叉污染。尽管最近已经报道了在纯银导线上进行电沉积的方法,但是使用包银的铌导线可以提供额外的优势。据报道,在碘化银基体中使用铌会导致碘离子电流更高的强度和长期稳定性。本文介绍了使用银和包银的铌丝的电沉积方法与传统的沉淀碘化银和银和铌粉混合的电沉积方法的比较。使用标称值为5 x 10(-)(10)和5 x 10(-11)的I-129 / 127比率的材料进行比较。对于每种I-129 / 127比率的材料,分析了八个样品每种制备方法需三天,每个样品进行七次重复AMS测量。对于每种比率,每种方法的单独天数的测量值合并在一起,每种方法得出168次测量值。方差分析表明,沉淀和电沉积材料之间的统计差异较小,对于类似于5 x 10(-10)和类似于5 x 10(-11)的比率,均值的合并标准误差为0.2% 。

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