基于超声-微纳米气泡辅助技术的可变光程水质多参数检测方法研究

doi:10.3964/j.issn.1000-0593(2024)07-2037-08

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摘要：针对目前国家标准分析检测水质多参数方法存在的科学与技术问题，提出了一种基于超声-微纳米气泡（US-MNB）辅助技术、连续光谱法和顺序注射分析法（SIA）的可变光程水质多参数检测新方法。设计水质多参数检测系统，通过检测总磷（TP）、化学需氧量（COD）、氨氮（NH₃-N）和六价铬（Cr⁶⁺）四种水质参数，验证了新方法的可行性。系统设计的核心是基于超声与微纳米气泡相结合的消解室以及具有可变光程功能的光谱扫描检测室，可达到快速消解和稳定检测的目的。同时系统基于国家水质检测标准，优化了水质多参数联合检测流程，并利用分光光度法和顺序注射分析技术对四种水质参数的含量进行连续光谱检测。首先，在常温常压下采用US-MNB辅助技术结合强氧化剂对TP进行消解，同时对检测室中NH₃-N参数显色反应后的化合物直接进行光谱扫描测定，消解后，再进行TP的测定。同理，消解COD的同时，对检测室中的Cr⁶⁺参数显色反应后的化合物直接进行光谱扫描测定，消解后，再进行COD的测定。整个检测过程所用时间大幅降低，可在短时间内自动完成水质多参数的测定，显著地提高了检测的效率。以上述四种水质参数为测定对象，利用最小二乘法构建回归模型，拟合回归方程并计算相关系数，并绘制各参数的浓度-吸光度标准工作曲线。结果表明：TP标准工作曲线拟合系数≥0.984 5，且浓度与吸光度成正相关，重复性（RSD）为3.05%~3.62%，加标回收率为97.8%~103.6%；COD标准工作曲线拟合系数≥0.998 7，且浓度与吸光度成负相关，重复性（RSD）为2.12%~2.74%，加标回收率为98.7%~104.7%；NH₃-N标准工作曲线拟合系数≥0.995 3，且浓度与吸光度成正相关，重复性（RSD）为3.41%~3.59%，加标回收率为99.2%~102.4%；Cr⁶⁺标准工作曲线拟合系数≥0.993 8，且浓度与吸光度成正相关，重复性（RSD）为3.51%~3.92%，加标回收率为98.9%~109.3%。系统可准确测定水样中TP、COD、NH₃-N和Cr⁶⁺的含量，且具有良好的稳定性与可靠性。基于超声-微纳米气泡辅助技术的可变光程水质多参数检测方法研究，对于拓宽光谱法在水质多参数快速检测领域的应用以及提升检测效率等方面的研究具有重要作用。

关键词：连续光谱；超声-微纳米气泡；顺序注射分析法；可变光程；多参数水质检测；联合检测

Abstract：A new method for multi-parameter water quality detection with variable optical range has been proposed, addressing scientific and technical challenges in the current national standard analytical methods. This method utilized ultrasound and micro-nano bubble (US-MNB), continuous spectrum analysis, and sequential injection analysis (SIA). A water quality multi-parameter detection system was designed and validated for the analysis of total phosphorus (TP), chemical oxygen demand (COD), ammonia nitrogen (NH₃-N), and hexavalent chromium (Cr⁶⁺). The feasibility of the new method was verified. The system's core consists of a digestion chamber integrating ultrasound and micro-nano bubbles and a detection chamber with an adjustable optical range. This structural design enabled rapid digestion and stable detection. The multi-parameter detection process was optimized based on national water quality testing standards. Spectrophotometry and sequential injection analysis techniques were employed for continuous spectral detection of the four water quality parameters. Firstly, the TP was digested by a US-MNB with strong oxidants at normal temperature and pressure. At the same time, the complexes were directly determined by spectral scanning after the color reaction of NH₃-N in the detection chamber, and thenthe TP was determined after digesting. Similarly, the compounds in the detection chamber after the chromogenic reaction of the Cr⁶⁺ were directly determined by spectral scanning. At the same time, the COD was digested, and then the COD was measured after digestion. The time used for the whole detection process was greatly reduced, and the determination of multi-parameter of water quality can be completed automatically in a short time, significantly improving the efficiency of detection. In this system, four water quality parameters(TP, COD, NH₃-N, and Cr⁶⁺)were measured, combined with the least squares method to establish a regression model, fit the regression equation and calculate the correlation coefficient, and plot the concentration-absorbance standard working curve of each parameter. The results showed that the TP standard working curve had a fitting coefficient ≥0.984 5, with a positive correlation between concentration and absorbance. The repeatability (RSD) ranged from 3.05% to 3.62%, and the spike recovery rate was 97.8% to 103.6%. The COD standard working curve had a fitting coefficient ≥0.998 7, with a negative correlation between concentration and absorbance. The repeatability (RSD) ranged from 2.12% to 2.74%, and the spike recovery rate was 98.7% to 104.7%. The NH₃-N standard working curve had a fitting coefficient ≥0.995 3, with a positive correlation between concentration and absorbance. The repeatability (RSD) ranged from 3.41% to 3.59%, and the spike recovery rate was 99.2% to 102.4%. The Cr⁶⁺ standard working curve had a fitting coefficient ≥0.993 8, with a positive correlation between concentration and absorbance. The repeatability (RSD) ranged from 3.51% to 3.92%, and the spike recovery rate was 98.9% to 109.3%. The system accurately determined the content of TP, COD, NH₃-N, and Cr⁶⁺ in water samples and demonstrated excellent stability and reliability. The studyon the multi-parameter detection method with variable optical range in water quality based on US-MNB is of great significance in broadening the application of spectroscopy in the field of rapid detection of water quality multi-parameters and improving detection efficiency.

Key words：Continuous spectrum; Ultrasound and micro-nano bubble; Sequential injection analysis; Variable optical path length; Multi-parameter water quality monitoring; Joint testing

收稿日期: 2023-04-03 修订日期: 2023-11-24

中图分类号:

TP216

基金资助: 国家自然科学基金项目(51205005)，北京市科技创新服务能力建设项目(PXM2017-014212-000013)资助

通讯作者: 李德健 E-mail: ldj5022729@126.com

作者简介: 李文，1975年生, 北方工业大学机电工程研究所副教授 e-mail: lw@ncut.edu.cn

引用本文:

李文，李德健，马永跃，田旺，陈银银，王利民，吕赫，李杰，骆紫云. 基于超声-微纳米气泡辅助技术的可变光程水质多参数检测方法研究[J]. 光谱学与光谱分析, 2024, 44(07): 2037-2044.
LI Wen, LI De-jian, MA Yong-yue, TIAN Wang, CHEN Yin-yin, WANG Li-min, LÜ He, LI Jie, LUO Zi-yun. Study on the Multi-Parameter Detection Method With Variable Optical Path Length for Water Quality Based on Ultrasound and Micro-Nano Bubble. SPECTROSCOPY AND SPECTRAL ANALYSIS, 2024, 44(07): 2037-2044.

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