Savannah River Nuclear Solutions, LLC, Aiken, SC 29808, USA.
Talanta. 2009 Nov 15;80(1):143-50. doi: 10.1016/j.talanta.2009.06.041. Epub 2009 Jun 24.
A new rapid separation method that allows separation and preconcentration of actinides in urine samples was developed for the measurement of longer lived actinides by inductively coupled plasma mass spectrometry (ICP-MS) and short-lived actinides by alpha spectrometry; a hybrid approach. This method uses stacked extraction chromatography cartridges and vacuum box technology to facilitate rapid separations. Preconcentration, if required, is performed using a streamlined calcium phosphate precipitation. Similar technology has been applied to separate actinides prior to measurement by alpha spectrometry, but this new method has been developed with elution reagents now compatible with ICP-MS as well. Purified solutions are split between ICP-MS and alpha spectrometry so that long- and short-lived actinide isotopes can be measured successfully. The method allows for simultaneous extraction of 24 samples (including QC samples) in less than 3h. Simultaneous sample preparation can offer significant time savings over sequential sample preparation. For example, sequential sample preparation of 24 samples taking just 15 min each requires 6h to complete. The simplicity and speed of this new method makes it attractive for radiological emergency response. If preconcentration is applied, the method is applicable to larger sample aliquots for occupational exposures as well. The chemical recoveries are typically greater than 90%, in contrast to other reported methods using flow injection separation techniques for urine samples where plutonium yields were 70-80%. This method allows measurement of both long-lived and short-lived actinide isotopes. (239)Pu, (242)Pu, (237)Np, (243)Am, (234)U, (235)U and (238)U were measured by ICP-MS, while (236)Pu, (238)Pu, (239)Pu, (241)Am, (243)Am and (244)Cm were measured by alpha spectrometry. The method can also be adapted so that the separation of uranium isotopes for assay is not required, if uranium assay by direct dilution of the urine sample is preferred instead. Multiple vacuum box locations may be set-up to supply several ICP-MS units with purified sample fractions such that a high sample throughput may be achieved, while still allowing for rapid measurement of short-lived actinides by alpha spectrometry.
开发了一种新的快速分离方法，用于通过电感耦合等离子体质谱法 (ICP-MS) 测量长寿命锕系元素和通过 α 谱法测量短寿命锕系元素；这是一种混合方法。该方法使用堆叠萃取色谱柱和真空箱技术来促进快速分离。如果需要预浓缩，则使用简化的磷酸钙沉淀进行。类似的技术已应用于通过 α 谱法测量之前分离锕系元素，但这种新方法已开发出与 ICP-MS 兼容的洗脱试剂。净化溶液在 ICP-MS 和 α 谱法之间进行分配，以便成功测量长寿命和短寿命锕系同位素。该方法允许在不到 3 小时内同时萃取 24 个样品（包括 QC 样品）。同时进行样品制备可以比顺序样品制备节省大量时间。例如，24 个样品的顺序样品制备每个只需 15 分钟，总共需要 6 小时才能完成。这种新方法的简单性和速度使其成为放射性应急响应的理想选择。如果进行预浓缩，则该方法也适用于职业暴露的较大样本等分试样。化学回收率通常大于 90%，而其他使用尿液样品流动注射分离技术的报告方法中，钚的产率为 70-80%。该方法允许测量长寿命和短寿命锕系同位素。(239)Pu、(242)Pu、(237)Np、(243)Am、(234)U、(235)U 和 (238)U 通过 ICP-MS 进行测量，而 (236)Pu、(238)Pu、(239)Pu、(241)Am、(243)Am 和 (244)Cm 通过 α 谱法进行测量。该方法也可以进行调整，以便如果首选直接稀释尿液样品进行铀测定，则不需要进行铀测定的分离。可以设置多个真空箱位置，为多个 ICP-MS 单元提供净化后的样品馏分，从而可以实现高通量样品，同时仍然允许通过 α 谱法快速测量短寿命锕系元素。
