High-pressure ion chromatography (HPIC) was coupled with sector field inductively coupled plasma-mass spectrometry (SF-ICP-MS) to separate plutonium (Pu), uranium (U), neodymium (Nd) and gadolinium (Gd) nuclides from isobaric nuclides and to quantify them with high sensitivity. In this study, mixed bed ion exchange columns CG5A and CS5A were used, from which Pu and U were eluted first using 1 M nitric acid. The lanthanides were then separated using a gradient of 0.1-0.15 M oxalic acid with the pH adjusted to 4.5. The HPIC-SF-ICP-MS method was validated using different sample matrices, i.e. spent nuclear fuel and soil. The method was found to be repeatable and gave rise to transient signals suitable for quantification of nuclide-specific concentrations using external calibration. In terms of accuracy, the HPIC-SF-ICP-MS measurement results were in good agreement with those obtained using thermal ionization mass spectrometry (TIMS). Finally, the method provides an improvement in sample throughput (≤60 minutes per sample) and reduces exposure of the operator to radiation compared to off-line gravitational chromatography followed by TIMS.

中文翻译：

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通过在线高压离子色谱结合扇形场电感耦合等离子体质谱法测定核样品来测定镧系元素，铀和p。

高压离子色谱（HPIC）与扇形场电感耦合等离子体质谱（SF-ICP-MS）耦合，从同量异重酸中分离出（（Pu），铀（U），钕（Nd）和g（Gd）核素核素并以高灵敏度对其进行量化。在这项研究中，使用了混合床离子交换柱CG5A和CS5A，首先使用1 M硝酸从中洗脱Pu和U。然后使用0.1-0.15 M草酸的梯度将pH值调节至4.5来分离镧系元素。HPIC-SF-ICP-MS方法已使用不同的样品基质（即乏核燃料和土壤）进行了验证。发现该方法是可重复的，并产生了适用于使用外部校准对核素特异性浓度进行定量的瞬态信号。在准确性方面，HPIC-SF-ICP-MS的测量结果与使用热电离质谱（TIMS）获得的结果非常吻合。最后，与离线重力色谱法接着TIMS相比，该方法提高了样品通量（每个样品≤60分钟），并减少了操作员暴露在辐射下的风险。