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首页> 外文期刊>International Journal of Analytical Mass Spectrometry and Chromatography >Separation Behavior of U(VI) and Th(IV) on a Mixed Ion Exchange Column Using 2,6-Pyridine Dicarboxylic Acid as a Complexing Agent and Determination of Trace Level Thorium in Uranium Matrix Employing High Performance Ion Chromatography
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Separation Behavior of U(VI) and Th(IV) on a Mixed Ion Exchange Column Using 2,6-Pyridine Dicarboxylic Acid as a Complexing Agent and Determination of Trace Level Thorium in Uranium Matrix Employing High Performance Ion Chromatography

机译:2,6-吡啶二甲酸为络合剂在混合离子交换柱上的U(VI)和Th(IV)分离行为以及采用高效离子色谱法测定铀基质中痕量Level

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Retention behavior of U(VI) and Th(IV) as their 2, 6-pyridine dicarboxylic acid (PDCA) complexes on reversed phase and ion exchange (cation, anion and mixed ion exchange) columns was studied and based on the results, a simple ion chromatography method for the determination of trace level thorium in uranium oxide using 0.075mM 2, 6-pyridine dicarboxylic acid (PDCA) and 1M KNO3 in 1.2M HNO3 as eluent (flow rate 1 mL/min)was proposed. The advantage of the developed method is that the separation of uranium matrix is not required prior to the ion chromatographic determination of trace Th. Separation was carried out on a mixed ion exchange stationary phase and a 10?4 M arsenazo (III) solution was used as post column reagent for detecting the separated metal ions. The separation of Th from uranium using PDCA in the present investigation is attributed through cation exchange mechanism. A calibration plot was constructed by following the standard addition method over the concentration range of 0.25 to 10 ppm of Th in the presence of uranium matrix, which resulted in a linear regression coefficient of 0.9978. The precision of the method was better than 5% and the LOD for Th was found to be 0.1ppm (S/N=3). The method has been validated by comparing the results with the results obtained from ICP-MS analysis where the This separated from the uranium matrix. The proposed method is simple, rapid, accurate and cost effective compared to techniques like ICP-MS or ICP-AES and is suitable for the routine kind of analysis.
机译:研究了U(VI)和Th(IV)作为它们的2,6-吡啶二羧酸(PDCA)配合物在反相和离子交换(阳离子,阴离子和混合离子交换)色谱柱上的保留行为,并基于结果,提出了一种简单的离子色谱法,用于测定铀氧化物中的痕量level,采用0.075mM 2、6-吡啶二甲酸(PDCA)和1.2M HNO3中的1M KNO3作为洗脱液(流速1 mL / min)。所开发方法的优点是,在离子色谱法测定痕量Th之前不需要分离铀基质。在混合的离子交换固定相上进行分离,并使用10?4 M的砷偶氮(III)溶液作为柱后试剂,以检测分离出的金属离子。本研究中使用PDCA从铀中分离Th,归因于阳离子交换机制。在铀基质存在下,通过按照标准添加方法在0.25至10 ppm的Th浓度范围内构建校准图,其线性回归系数为0.9978。该方法的精密度优于5%,Th的LOD为0.1ppm(S / N = 3)。通过将结果与从ICP-MS分析获得的结果(与铀基质分离)进行比较,验证了该方法的有效性。与ICP-MS或ICP-AES等技术相比,该方法简单,快速,准确且具有成本效益,适合常规分析。

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