| 尹亮亮,田青,黄微,邵宪章,吉艳琴.ICP-MS法分析尿中总铀和235U/238U比值及其不确定度评价[J].中华放射医学与防护杂志,2017,37(5):376-380 |
| ICP-MS法分析尿中总铀和235U/238U比值及其不确定度评价 |
| ICP-MS method for the determination of uranium concentration and 235U/238U ratio in urine and its uncertainty evaluation |
| 投稿时间：2017-01-15 |
| DOI：10.3760/cma.j.issn.0254-5098.2017.05.011 |
| 中文关键词: 铀 235U/238U比值 电感耦合等离子体质谱 尿 不确定度 |
| 英文关键词:Uranium 235U/238U ratio Inductively coupled plasma mass spectrometry (ICP-MS) Urine Uncertainty |
| 基金项目:国家科技基础性工作专项（2014YF211000）；卫生行业科研项目（201002009） |
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| 中文摘要: |
| 目的 建立电感耦合等离子体质谱（ICP-MS）快速测量尿中总铀含量和235U/238U比值的方法，并进行不确定度评价。方法 尿样经浓HNO3和H2O2处理后，一部分定容直接进入ICP-MS测定总铀含量；一部分经磷酸三丁酯（TBP）萃淋树脂分离富集铀，采用ICP-MS测定其中235U/238U比值。以人尿样为例，通过样品前处理、测量、标准曲线计算，建立数学模型分析总铀及235U/238U比值的不确定度来源，进行不确定度合成。结果 该方法分析尿中总铀加标回收率为98.4%~102.4%，方法检出限为0.002 μg/L。经过不确定度评价，尿样中总铀含量的相对扩展不确定度为 0.26（k=2）；235U/238U比值的相对扩展不确定度为0.001 1（k=2）。结论 该方法加标回收率高，检出限低，精密度较好，能够实现尿中总铀的定量和235U/238U比值的快速分析，适用于放射职业照射或核应急的公众照射中尿铀及235U/238U比值的分析；尿中总铀及235U/238U比值不确定度评定结果准确可靠。 |
| 英文摘要: |
| Objective To establish a method of analyzing total uranium and 235U/238U ratio in urine using inductively coupled plasma mass spectrometry (ICP-MS) and uncertainty assessment.Methods Urine sample was digested with HNO3 and H2O2, and total uranium was determined using ICP-MS method directly. The digested urine sample was separated to concentrate uranium with tributyl phosphate (TBP) column, and 235U/238U ratio was analyzed using ICP-MS. The uncertainty was evaluated through sample pre-treatment, measurement and standard curve calculation. Results The recovery of total uranium in urine was 98.4%-102.4%, detection limit was 0.002 μg/L. The relative expanded uncertainty of total uranium concentration in urine was 0.26 (k=2). 235U/238U ratio was 0.001 1 (k=2). Conclusions This study offers a low detection limit, good recovery and precision method for rapid determination of total uranium and 235U/238U ratio in urine samples. It is potential used for both in occupational exposure assessment and nuclear emergency situation. The uncertainty evaluation of total uranium and 235U/238U ratio in urine are reliable. |
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