铀元素的激光诱导击穿光谱测量分析

doi:10.3964/j.issn.1000-0593(2023)01-0057-05

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摘要：为促进LIBS技术在微量重金属元素检测以及核污染检测领域的应用，提高检测灵敏度和准确性，采用了激光双脉冲LIBS技术和光电双脉冲LIBS技术，分别对土壤和二氧化硅中的铀元素进行分析。首先，对激光脉冲能量、电压和采集延时等参数进行优化，提高铀元素特征谱线的强度和信噪比；然后在优化实验参数条件下，对含不同浓度铀元素的土壤样品和二氧化硅样品进行激发；选取UII 367.01 nm、UII 454.36 nm两条铀元素的特征谱线作为分析线，通过铀元素浓度与特征谱线强度的线性关系，建立定标曲线。双脉冲激光激发条件为：激光脉冲1作为预脉冲，主要参数为1 064 nm，90 mJ，9.2 ns，激光脉冲2作为再加热脉冲，主要参数为355 nm，50 mJ，8 ns，两个脉冲的时间间隔800 ns，光谱采集相对第二个脉冲延时1 μs，得到铀元素在土壤和二氧化硅两种样品中的浓度检测下限分别为572和110 mg·kg^-1，拟合优度值R²分别为0.958和0.999。在光电双脉冲激发条件下，激光脉冲作为预脉冲，主要参数为355 nm，50 mJ，8 ns，高压电脉冲作为再加热脉冲，主要参数为3 900 V、方波、脉宽50 μs，两个脉冲的时间间隔1 μs，得到铀元素在土壤和二氧化硅两种样品中的浓度检测限分别为108和64 mg·kg^-1，拟合优度值R²分别为0.991和0.997。研究结果表明：在相同激发条件下，铀元素的特征谱线存在明显的基体效应，在二氧化硅样品中具有更高的光谱强度、更低的检测限和更高的拟合优度值；相比于激光双脉冲，光电双脉冲能显著增强铀元素特征谱线的强度、稳定性和提高信噪比，且光电双脉冲系统的光路更简单，这对于LIBS技术的发展以及应用具有重要参考意义。该研究方法和研究结果可为土壤重金属污染检测、核泄漏时土壤和气溶胶的应急监测提供技术支持。

关键词：光谱学；激光诱导击穿光谱；激光双脉冲技术；光电双脉冲技术；铀元素

Abstract：To promote the application of LIBS technology in the detection of trace heavy metals and nuclear pollution detection, and improve the sensitivity and accuracy of detection, laser double-pulse LIBS technology and photoelectric double-pulse LIBS technology were used to analyze the uranium elements in soil and silica respectively. Firstly, optimizing the laser pulse energy, voltage and acquisition delay parameters to improve the intensity and signal-to-noise ratio of the characteristic spectrum of uranium; Then, under the conditions of optimized experimental parameters, the soil samples and silica samples containing different concentrations of uranium were analyzed. Two characteristic spectral lines of uranium element UII 367.01 nm and UII 454.36 nm were selected as the analysis line, and the calibration curve was established through the linear relationship between the uranium element concentration and the characteristic spectral line intensity. Under the condition of laser double pulse excitation, laser 1 was used as the pre-pulse, the main parameters were 1 064 nm, 90 mJ, 9.2 ns, and laser 2 was used as the reheating pulse, the main parameters are 355 nm, 50 mJ, 8 ns. The time interval between the two pulses is 800 ns, and the spectral acquisition is delayed by 1 μs, the lower detection limits of the concentration of uranium in the soil and silica samples were 572 and 110 mg·kg^-1, respectively, and the goodness of fit value R² were respectively 0.958 and 0.999. Under the condition of photoelectric double pulse excitation, the laser pulse was used as the pre-pulse, the main parameters were 355 nm, 50 mJ, 8 ns, the high-voltage electric pulse was used as the reheating pulse, the main parameters were 3 900 V, square wave, pulse width 50 μs, the time interval of the two pulses 1 μs. The lower detection limits of the concentration of uranium in soil and silica samples were 108 and 64 mg·kg^-1, and the goodness-of-fit values R² were 0.991 and 0.997, respectively. The research results show that under the same excitation conditions, the characteristic spectrum of uranium has an obvious matrix effect, which has higher spectral intensity, lower detection limit and higher goodness of fit value in silica samples. Compared with double laser pulse, the photoelectric double pulse can significantly enhance the intensity, stability and signal-to-noise ratio of the characteristic spectrum of uranium element, and the optical path of the photoelectric double pulse system is simpler has an important reference for the development and application of LIBS technology significance. The research method and results can provide technical support for detecting heavy metal pollution in soil and the emergency monitoring of soil and aerosol in the event of nuclear leakage.

Key words：Spectroscopy; Laser-induced breakdown spectroscopy; Laser double-pulse technology; Photoelectric double-pulse technology; Uranium

收稿日期: 2021-11-11 修订日期: 2022-04-22

中图分类号:

O433.4

基金资助: 国家自然科学基金项目(11972313)，国家自然科学基金委员会与中国工程物理研究院联合基金项目(U1530109)，中国科学院光谱成像技术重点实验室基金项目(LSIT202001W)资助

通讯作者: 邱荣 E-mail: 43951700@qq.com

作者简介: 张志威，1996年生，西南科技大学理学院硕士研究生 e-mail: 1131408402@qq.com

引用本文:

张志威，邱荣，姚胤旭，万情，潘高威，史晋芳. 铀元素的激光诱导击穿光谱测量分析[J]. 光谱学与光谱分析, 2023, 43(01): 57-61.
ZHANG Zhi-wei, QIU Rong, YAO Yin-xu, WAN Qing, PAN Gao-wei, SHI Jin-fang. Measurement and Analysis of Uranium Using Laser-Induced Breakdown Spectroscopy. SPECTROSCOPY AND SPECTRAL ANALYSIS, 2023, 43(01): 57-61.

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