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Calixarene-based Extraction Chromatographic Separation of Cs-135 and Cs-137 in Environmental and Waste Samples Prior to Sector Field ICP-MS Analysis

机译:基于杯芳烃的萃取色谱分离环境和废物样品中的Cs-135和Cs-137,然后进行行业现场ICP-MS分析

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Advances in the sensitivities achievable by sector field inductively coupled plasma mass spectrometry (ICP-SFMS) offer the prospect of low-level measurement of shorter and longer lived radionuclides, thus expanding options for environmental and radioactively contaminated land assessment. In ICP-SFMS, the critical requirement for accurate detection is the effective chemical separation of isobaric and polyatomic interferences prior to sample introduction. As instrumental detection limit capability improves, accurate radionuclide determination requires highly effective separation materials that combine high analyte selectivity with subsequent quantitative analyte recovery compatible with ICP-SFMS detection. Two radioactive isotopes measurable by ICP-SFMS are the high yield fission products Cs-135 and Cs-137 that have entered the environment as a result of anthropogenic nuclear activities. ICP-SFMS enables reliable measurement of Cs-135/Cs-137 ratios, which can be used as a forensic tool in determining the source of nuclear contamination. The critical requirement for accurate detection is the effective removal of isobaric interferences from Ba-135 and Ba-137 prior to measurement. A number of exchange materials can effectively extract Cs; however, non-quantitative elution of Cs makes subsequent ICP-SFMS quantification challenging. A novel extraction chromatographic resin has been developed by dissolving calix[4]arene-bis(tert-octylbenzo-crown-6) (BOBCalixC6) in octan-1-ol and loading onto an Amberchrom CG-71 prefilter resin material. Preparation of the material takes less than 1 h and, at an optimal concentration of 3 M HNO3, shows high selectivity toward Cs, which is effectively eluted in 0.05 M HNO3. The procedure developed shows high Cs selectivity and Ba decontamination from digests of complex matrixes including a saltmarsh sediment contaminated by aqueous discharges from a nuclear fuel reprocessing facility. Repeated tests show the resin can be reused up to four times. For low-level ICP-SFMS quantification, more complex sample matrixes benefit from a cation resin cleanup stage prior to using BOBCalixC6 that serves to enhance Ba decontamination and Cs recovery.
机译:扇形场电感耦合等离子体质谱法(ICP-SFMS)可实现的灵敏度方面的进展为低水平测量寿命较短和更长的放射性核素提供了前景,从而为环境和放射性污染土地评估提供了更多选择。在ICP-SFMS中,准确检测的关键要求是在引入样品之前有效地化学分离等压和多原子干扰。随着仪器检测极限能力的提高,准确的放射性核素测定需要高效的分离材料,这些材料必须具有较高的分析物选择性以及与ICP-SFMS检测兼容的后续定量分析物回收率。 ICP-SFMS可测量的两种放射性同位素是高产裂变产物Cs-135和Cs-137,它们是由于人为核活动而进入环境的。 ICP-SFMS能够可靠地测量Cs-135 / Cs-137的比率,可用作确定核污染源的法医工具。准确检测的关键要求是在测量之前有效消除Ba-135和Ba-137中的等压干扰。许多交换材料可以有效地提取Cs。然而,Cs的非定量洗脱使得随后的ICP-SFMS定量分析具有挑战性。通过将杯[4]芳烃-双(叔辛基苯并-冠-6)(BOBCalixC6)溶解在辛烷-1-醇中并加载到Amberchrom CG-71预过滤树脂材料上,开发了一种新型的萃取色谱树脂。该材料的制备过程不到1小时,并且在3 M HNO3的最佳浓度下,显示出对Cs的高选择性,可在0.05 M HNO3中有效洗脱。所开发的程序显示出对复杂基质的消化物具有很高的Cs选择性和Ba净化能力,其中包括被核燃料后处理设施的水排放污染的盐沼沉积物。重复测试表明该树脂最多可重复使用四次。对于低级ICP-SFMS定量分析,在使用BOBCalixC6之前,更复杂的样品基质可从阳离子树脂净化阶段中受益,而BOBCalixC6可增强Ba的去污染和Cs的回收率。

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