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Advances in low level uranium and plutonium isotope mass spectrometry using multiple ion counting and filament carburization

机译：多重离子计数和灯丝渗碳技术在低水平铀和p同位素质谱研究中的进展

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After upgrading IRMM's mass spectrometric capabilities for certification measurements for uranium and plutonium using large sample sizes during the previous years, now in 2006-2007 we focused on necessary improvements in the area of low-level isotopic analyses for uranium and plutonium. This project was driven firstly by the need for reliable verification measurements for the Nuclear Signatures Measurement Evaluation Programme (NUSIMEP) samples at IRMM, secondly by the need for verification measurements on single uranium oxide reference particles and thirdly by the request from the IAEA's Safeguards Analytical Laboratory (SAL) to provide assistance for this type of analyses through the EC support programme. Improving low-level isotope mass spectrometry for uranium and plutonium at IRMM consisted of three steps. First a new thermal ionization mass spectrometer was acquired in order to have an instrument which can be used for peak-jumping measurements in ion counting mode, and which can be subsequently upgraded with a “Multiple Ion Counting” (MIC) system. This detector system allows the simultaneous detection of up to seven small ion beams with currents of 10~-19 – 10~-14 Ampere in ion counting mode, corresponding to count rates of 1–60.000 counts per second. As a result of test measurements with the MIC system it turned out that static measurements using the MIC system with a sample-versus-standard type external calibration can be associated with uncertainties even higher than in peak-jumping mode. The second step of improvement to tackle this situation was to implement the principle of "multi-dynamic" measurements for both uranium and plutonium measurements. This "multi-dynamic" measurement procedure provides an internal calibration of the MIC system and therefore circumvents the need for complicated inter-calibration routines. As a third step, a filament carburization procedure was implemented by which the ionization efficiencies for uranium and plutonium were improved by a factor of 3 and 10, respectively. Results for measurements performed on samples of previous NUSIMEP campaigns will be shown in comparison to results from various techniques employed by participating laboratories.
机译：在过去几年中提高了IRMM使用大样本量进行铀和p认证测量的质谱能力之后，现在在2006-2007年，我们专注于铀和p低水平同位素分析领域的必要改进。该项目首先是由于需要对IRMM的核特征测量评估程序（NUSIMEP）样品进行可靠的验证测量，其次是由于需要对单个铀氧化物参考颗粒进行验证测量，其次是由IAEA保障分析实验室的要求（SAL）通过EC支持计划为此类分析提供帮助。 IRMM改进铀和p的低级同位素质谱分析包括三个步骤。首先，为了获得一种可以在离子计数模式下用于峰跃测量的仪器，并购置了新的热电离质谱仪，该仪器随后可以通过“多离子计数”（MIC）系统进行升级。该检测器系统允许在离子计数模式下以10〜-19 – 10〜-14安培的电流同时检测多达七个小离子束，对应于每秒1–60.000个计数的计数率。 作为使用MIC系统进行测试测量的结果，事实证明，使用MIC系统进行样品对标准类型的外部校准的静态测量所带来的不确定性甚至比峰值跳跃模式还要高。解决这种情况的第二步改进是对铀和p的测量实施“多动态”测量原理。这种“多动态”测量程序提供了MIC系统的内部校准，因此避免了对复杂的相互校准例程的需求。 第三步，实施了灯丝渗碳程序，通过该程序，铀和p的电离效率分别提高了3倍和10倍。与参与实验室采用的各种技术的结果相比，将显示对先前NUSIMEP活动样本进行测量的结果。

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