直接进样气相色谱-质谱法分析大气中的氪和氙

摘要

Volume concentration determination for atmospheric krypton and xenon is very important for krypton-85 and radioactive xenon isotopes monitoring. An injection setup integrated adjustable quantity sample injection and quantitative dilution function was designed. The effects of EI source parameters on the sensitivity of MS detector were studied. The optimized values were as following: ionization energy of 70 eV, emission current of 40 mA, cathode voltage of 27 mV, focus voltage of 85 mV and lens compensation of 20 V, respectively. A GC-MS method for the determination of krypton and xenon in atmosphere without of sample pretreatment was developed. The minimal detected concentrations for krypton and xenon were 3. 3×10-8(V/V) and 2. 6×10-9(V/V). Moreover, the krypton and xenon concentrations in the ground level air around our laboratory were measured with the results of 1 . 1 × 10-6 ( V/V ) and 9 . 3 × 10-8 ( V/V ) . The related combined standard uncertainties for krypton and xenon results were 2. 38% and 3. 15%, respectively.%大气中氪和氙体积比浓度的测量对于氪-85和放射性氙同位素监测具有重要意义。本实验设计了一套集成定量稀释功能的可调样量进样装置，对质谱检测器的工作参数进行了实验优化，确定了灯丝电离能量70 eV、灯丝发射电流40 mA、推斥极电压27 mV、离子聚焦电压85 mV和透镜补偿电压20 V等最佳工作条件。建立了空气样品直接进样条件下氪和氙的气质联用分析方法，氪和氙的最低可检测浓度分别为3.3×10-8(V/V)和2.6×10-9(V/V)。同时应用本方法测量了实验室所处开放空间大气中氪和氙的体积比浓度，分别为1.1×10-6(V/V)和9.3×10-8(V/V)，相对合成标准不确定度分别为2.38%和3.15%。