IC-MC-ICP-MS 测量环境水样品中钚同位素比值的方法研究
Determination of Pu Isotope Ratio in Environmental Water Samples by IC-MC-ICP-MS
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摘要: 为了实现快速分离钚与其他基体,准确测定钚同位素比值,建立了离子色谱(IC)与多接收电感耦合等离子体质谱(MC-ICP-MS)联用测定环境水样品中钚同位素比值的方法。实验选取7.5 mol/L 硝酸作为色谱柱的上柱液,以0.35 mol/L HNO3和0.01 mol/L HF 的混合溶液为淋洗液,用 Pu 计数最高点法(peak apex ratio)作为最终同位素比值的测定方法。实验对模拟环境水样进行测定,测量相对标准偏差为0.50%,与 Pu 标准同位素比值的相对偏差为5.7%。采用该方法对实际环境水样品进行测定,测量相对标准偏差为0.97%,与传统的 TBP-7402色谱柱离线分离法测量的钚同位素比值进行对比,相对偏差为1.3%。结果表明,该方法的样品预处理简单、分离速度快、结果可靠,具有广阔的应用前景。
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关键词:
- 环境水样品 /
- 钚 /
- 离子色谱(IC) /
- 多接收电感耦合等离子体质谱(MC-ICP-MS)
Abstract: The environmental sampling (ES)analysis is one of important nuclear safe-guards’technologies of International Atomic Energy Agency (IAEA),which has been used for detecting the undeclared nuclear activities.Plutonium is regarded as the signifi-cant element in nuclear safeguards.In the aspect of ES,bulk analysis is adept at the analysis of plutonium ratio in environmental samples.In this paper,the method of on-line analysis of plutonium ratio in water samples was established by combination of ion chromatography (IC)and multicollector inductively coupled plasma mass spectrometry (MC-ICP-MS ). The separation conditions of liquid chromatographic column, the column acidity,eluent composition were optimized.The AS4A-SC anion chromato-graphic column was made sure as separation medium.The separation conditions in which the acidity of column was 7.5 mol/L and the eluent composition was 0.35 mol/L HNO3 mixed with 0.01 mol/L HF were determined by optimization experiments.The concentrations of uranium in various types of environmental water samples were meas-ured.The interface was determined in order to combine IC and MC-ICP-MS.The effect was confirmed better when using PEEK two way valve to connect IC and MC-ICP-MS. The technique of peek apex ratio was adapted as the method for the measurement of dynamic plutonium ratio by MC-ICP-MS.The simulated water samples were measured. The RSD is 0.50%,and the relative bias compared with the plutonium certified refer-ence material is 5.7%.The actual water samples were also measured.The RSD is 0.97%,and the relative bias is 1.3% compared with the typical separation methods by TBP and 7402 chromatography column.This method has high efficiency and fast analyt-ical speed,which can be used for the measurement of plutonium ratio in other environ-mental samples with more complicated matrices. -
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