摘要
农田土壤中Hg^(2+)精准评估对于建设高标准农田和保护粮食安全具有重要意义。针对污染土壤中汞离子浓度低、共存干扰未知的问题,提出一种基于电化学联用激光诱导击穿光谱技术(EC-LIBS)的土壤中Hg^(2+)检测方法。试验首先采用循环伏安法进行Hg^(2+)电沉积,与沉积前金电极基底相比较,得出沉积后金电极基底在HgⅠ435.835 nm存在明显发射信号,并且沉积后纳米金颗粒表面亮度提升、黄度下降,结果表明电化学沉积可以通过在金电极表面形成金汞齐完成汞离子液固转换。其次探究了溶剂pH和沉积电压对沉积效果的影响,得出最优的沉积参数为pH 7.0,电压为-400 mV。最终获取样品LIBS谱线并进行惠特克基线校正和PLS模型构建,得出当Lambda=1.0,p=0.01时,基线校正效果明显,所构建PLS模型预测集RMSEP和MRAEP分别为5.24 mg·kg^(-1)和4.86%,表明EC-LIBS技术结合该标准模型可以用于土壤中Hg^(2+)精准检测。
Accurate assessment of Hg^(2+)in farmland soil is significant for constructing high-standard farmland and protecting food security.To solve the problem of low mercury ion concentration and unknown coexisting interference in polluted soil,a method of Hg^(2+)detection in soil based on electrochemical laser-induced breakdown spectrometry(EC-LIBS)was proposed in this study.First,cyclic voltammetry was used for Hg^(2+)electrodeposition.Compared with the gold electrode substrate before deposition,it was found that the gold electrode substrate after deposition had obvious emission signals at HgⅠ435.835 nm,and the surface brightness of the gold nanoparticles increased and the yellowness decreased after deposition.The results show that electrochemical deposition can complete the liquid-solid conversion of mercury ions by forming gold amalgam on the surface of the gold electrode.Secondly,the influence of solvent pH and deposition voltage on the deposition effect was investigated,and the optimal deposition parameters were pH 7.0 and voltage of-400 mV.Finally,the sample LIBS spectral line was obtained,and the Whittaker baseline correction and PLS model were carried out.It was concluded that when Lambda=1.0 and p=0.01,the baseline correction effect was obvious,and the prediction sets RMSEP and MRAEP of the developed PLS model were 5.24 mg·kg^(-1) and 4.86%,respectively.It shows that EC-LIBS technology combined with the standard model can accurately detect Hg^(2+)in soil.
作者
段宏伟
赵斯杰
郭梅
牛其建
黄晶
刘飞
DUAN Hong-wei;ZHAO Si-jie;GUO Mei;NIU Qi-jian;HUANG Jing;LIU Fei(Key Laboratory of Northwest Agricultural Equipment,Ministry of Agriculture and Rural Affairs,Shihezi 832000,China;College of Mechanical and Electrical Engineering,Shihezi University,Shihezi 832000,China;School of Agricultural Engineering,Jiangsu University,Zhenjiang 212013,China;College of Biosystems Engineering and Food Science,Zhejiang University,Hangzhou 310058,China;Key Laboratory of Spectroscopy Sensing,Ministry of Agriculture and Rural Affairs,Hangzhou 310058,China)
出处
《光谱学与光谱分析》
北大核心
2025年第4期980-985,共6页
Spectroscopy and Spectral Analysis
基金
农业农村部光谱检测重点实验室开放基金课题(2022ZJUGP001)
现代农业机械兵团重点实验室开放课题(XDNJ2022-001)
国家自然科学基金项目(62101216)
中国博士后科学基金面上项目(2024MD753958)
新疆维吾尔自治区“天池英才”项目(CZ002504)
石河子大学自主支持科研项目(XJ2023001601)资助。
