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中国物理学会期刊

基于预富集-CRDS原理的痕量H2S浓度测量

CSTR: 32037.14.aps.75.20251676

Measurement of trace H2S based on the preconcentration-CRDS principle

CSTR: 32037.14.aps.75.20251676
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  • 随着半导体、新能源、生命科学领域的发展, 气体中极低浓度的硫化氢(H2S)检测得到了越来越多的关注. 针对痕量H2S的检测难点, 本文将固体吸附剂预富集技术与腔衰荡吸收光谱技术(CRDS)相结合, 建立了一套针对痕量H2S杂质精确测量的预富集-CRDS系统. 系统介绍了固体吸附剂选择、系统结构设计与实验方案, 并基于可探测浓度工况(0.5 μmol/mol H2S)展示了预富集实验中H2S浓度演化过程, 建立H2S脱附峰值与初始浓度的定量关系. 在此基础上, 对预富集-CRDS检测系统的关键性能参数重复性与检测限进行定量评价. 最后, 利用本文搭建测量系统对常见的6种燃料气体CH4, C2H6, C2H4, C3H8, C4H10与CO中nmol/mol量级的H2S进行定量检测, 并结合工艺流程, 对H2S的可能来源与浓度分布进行详细分析. 结果表明, 本文构建的预富集-CRDS系统对于H2S气体具有出众的检测能力, 为实际应用中极低浓度H2S的气体提供了新的检测途径.

     

    With the advancement of semiconductor and new-energy engineering, detecting hydrogen sulfide (H2S) at extremely low concentrations has attracted increasing attention. To address challenges in trace H2S measurement, this study integrates preconcentration with cavity ring-down spectroscopy (CRDS) and develops a preconcentration-CRDS system for detecting trace H2S impurities. This paper systematically describes the selection of solid adsorbents, the system design, and the experimental protocols. First, based on the CRDS detection capability (0.5 μmol/mol H2S), the evolution of H2S concentration during the preconcentration process is investigated. Calibration experiments established a quantitative relationship between the maximum H2S concentration during the desorption stage and the initial H2S concentration in the sample gas. The results indicate that the preconcentration approach enhances the H2S concentration by more than sixfold. The system performance, including reproducibility, detection limit, and long-term measurement stability, is analyzed in detail. The relative error of the maximum H2S concentration across three experiments is 5.5%. The detection limit, defined as twice the zero-point noise, is approximately 36.8 nmol/mol. The stability, derived from Allan-variance analysis, is 0.4 nmol/mol. Finally, quantitative measurements of trace H2S in CH4, C2H6, C2H4, C3H8, C4H10, and CO are performed using the developed system. The H2S content in C4H10 is the highest, at approximately 83 nmol/mol. In contrast, for CH4 and C2H6, no H2S desorption is observed during the desorption stage. Based on the production processes and experimental findings, potential sources of H2S in different fuels are analyzed. Overall, the preconcentration-CRDS system demonstrated excellent performance for trace H2S detection, offering a promising and innovative approach for monitoring ultra-low H2S concentrations.

     

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