高等学校化学学报 ›› 2020, Vol. 41 ›› Issue (9): 2003-2010.doi: 10.7503/cjcu20200165

• 分析化学 • 上一篇    下一篇

内部萃取电喷雾电离质谱对二氧化钛纳米线阵列光催化降解罗丹明B反应机理的研究

李肖乾1, 张华2, 路海健1, 刘畅1, 刘庆龙1, 马夏禹1, 方媛萍1, 梁大鹏1()   

  1. 1.吉林大学新能源与环境学院, 地下水资源与环境教育部重点实验室, 长春 130021
    2.吉林大学化学学院, 无机合成与制备化学国家重点实验室, 长春 130012
  • 收稿日期:2020-03-25 出版日期:2020-09-10 发布日期:2020-09-02
  • 通讯作者: 梁大鹏 E-mail:liangdp@jlu.edu.cn
  • 基金资助:
    国家级大学生创新创业训练计划(2018A2511)

Mechanism of Photocatalytic Degradation of Rhodamine B by TiO2 Nanowire Array with Internal Extraction Electrospray Ionization Mass Spectrometry

LI Xiaoqian1, ZHANG Hua2, LU Haijian1, LIU Chang1, LIU Qinglong1, MA Xiayu1, FANG Yuanping1, LIANG Dapeng1()   

  1. 1.Key Lab of Groundwater Resources and Environment of the Ministry of Education, College of New Energy and Enviroment, Jilin University, Changchun 130021, China
    2.State Key Laboratory of Inorganic Synthesis and Preparative Chemistry, College of Chemistry, Jilin University, Changchun 130012, China
  • Received:2020-03-25 Online:2020-09-10 Published:2020-09-02
  • Contact: LIANG Dapeng E-mail:liangdp@jlu.edu.cn
  • Supported by:
    Supported by the National College Student’s Innovative Entrepreneurship Training Program, China(2018A2511)

摘要:

利用水热合成法在掺杂F的SnO2导电玻璃(FTO)基底上制备TiO2纳米线阵列结构, 与内部萃取电喷雾电离质谱(iEESI-MS)联用, 实现了罗丹明B降解中间产物的检测, 并推测了反应机理. 考察了离子源电压、 离子传输管温度和洗脱剂组成对罗丹明B及其降解产物信号强度的影响. 结果表明, 在光催化反应时间为2 h, 反应溶液体积为15 μL, 离子源电压为3 kV, 离子传输管温度为300 ℃, 洗脱剂为0.5%乙酸-甲醇(体积比)混合溶液条件下, 可以获得最佳的罗丹明B及其中间产物信号. 在优化的条件下, 从罗丹明B反应溶液中共检测出8种中间产物, 基于此推测了罗丹明B的降解机理. 该方法对罗丹明B定量分析的检出限(S/N≥3)为0.1 μg/L, 相对标准偏差(RSD, n=6)为2.1%~7.3%, 具有检测限低、 灵敏度高、 样品耗量少、 分析速度快及操作简便等特点. 此外, 该方法还可用于其它光催化反应中间产物的检测, 拓宽了质谱分析法在环境领域中的应用范围, 为今后环境污染物降解机理的探究提供了新思路.

关键词: 二氧化钛纳米线阵列, 内部萃取电喷雾电离质谱, 罗丹明B, 光催化降解

Abstract:

By means of hydrothermal synthesis, the TiO2 nanowire array was prepared on the SnO2 conductive glass(FTO) substrate doped with F, and it was combined with the internal extraction electrospray ionization mass spectrometry(iEESI-MS) to realize the detection of Rhodamine B intermediate product and the conjecture of its reaction mechanism. The effects of ion source voltage, ion transmission tube temperature and eluting agent on the signal strength of rhodamine B and its degradation products were systematically investigated. The results showed that the optimum Rhodamine B intermediate product and its degradation product signal could be obtained under the condition that the photocatalytic reaction time was 2 h, the reaction solution volume was 15 μL, the ion source voltage was 3 kV, the ion transmission tube temperature was 300 ℃, and the eluting agent was 0.5% methanol-acetic acid(volume ratio). Under the optimized conditions, 8 kinds of intermediate products were detected from Rhodamine B reaction solution, and the degradation mechanism of rhodamine B was inferred. In this method, the detection limit(S/N≥3) of rhodamine B quantitative analysis is 0.1 μg/L, and the relative standard deviation(RSD, n=6) is 2.1%—7.3%, which shows that this method has the characteristics of low testing limit, high sensitivity, less sample consumption during detection, fast analysis speed and simple operation. In addition, this method can also be used to detect the intermediate products of other photocatalytic reactions, widen the application of mass spectrometry in the field of environment, and provide new ideas for the future exploration of the degradation mechanism of environmental pollutants.

Key words: TiO2 nanowire arrays, Internal extraction electrospray ionization mass spectrometry, Rhodamine B, Photocatalytic degradation

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