引用本文:沈晓瑜,石宇帆,高品,陈晓倩,贾丽娟,杨品川,邓芸芸.生活污水中典型cVMSs检测方法的建立及应用研究[J].环境监控与预警,2024,16(4):81-86
SHEN Xiaoyu,SHI Yufan,GAO Pin,CHEN Xiaoqian,JIA Lijuan,YANG Pinchuan,DENG Yunyun.Establishment and Application of a Typical Cyclic Volatile Methylsiloxane(cVMSs) Detection Method in Domestic Wastewater[J].Environmental Monitoring and Forewarning,2024,16(4):81-86
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生活污水中典型cVMSs检测方法的建立及应用研究
沈晓瑜1,石宇帆1,高品2,陈晓倩1,贾丽娟1,杨品川1,邓芸芸1*
1.上海市检测中心,上海 201203;2.东华大学,环境科学与工程学院,上海 201620
摘要:
环状挥发性甲基硅氧烷(cVMSs)具有高挥发性的特点,对其进行监测会受到高背景干扰,影响数据的准确性。通过综合优化进样隔垫、进样瓶内衬管、样品保存方法等干扰因素,确定了最佳预处理条件,建立了水中微量八甲基环四硅氧烷(D4)、十甲基环五硅氧烷(D5)和十二甲基环六硅氧烷(D6)的气相色谱-质谱(GC-MS)检测分析方法,并应用于实际生活污水中D4、D5和D6的检测。结果表明,所建立的方法检出限为1.43~3.14ng/L,在加标量分别为5和0.5μg/L条件下的平均回收率为92.2%~110.6%和75.1%~91.2%。针对实际生活污水的检测结果显示,污水处理厂进水中D5和D6平均质量浓度分别为1.071和524ng/L,D4未检出,而在所有出水中D4、D5和D6均未被检出。该方法的预处理和GC-MS检测分析方法过程简单,可以显著降低背景因素的干扰,可为污水中cVMSs的检测分析提供方法参考,并为环境监管部门决策提供依据。
关键词:  环状挥发性甲基硅氧烷  气相色谱-质谱  方法优化  同位素稀释法  生活污水  背景干扰
DOI:DOI:10.3969/j.issn.1674-6732.2024.04.009
分类号:X832
基金项目:浦东新区科技发展基金资助项目(PKJ2021-C05)
Establishment and Application of a Typical Cyclic Volatile Methylsiloxane(cVMSs) Detection Method in Domestic Wastewater
SHEN Xiaoyu1, SHI Yufan1, GAO Pin2, CHEN Xiaoqian1, JIA Lijuan1, YANG Pinchuan1, DENG Yunyun1*
1.Shanghai Academy of Public Measurement,Shanghai 201203, China; 2.College of Environmental Science and Engineering, Donghua University, Shanghai 201620, China
Abstract:
Cyclic volatile methylsiloxanes(cVMSs) are highly volatile, making their monitoring subject to high background interference, which affects data accuracy. By comprehensively optimizing factors such as injection septum, injection bottle insert, and sample preservation methods, the optimal pretreatment conditions were determined. An analytical method for detecting trace amounts of octamethylcyclotetrasiloxane(D4), decamethylcyclopentasiloxane(D5), and dodecamethylcyclohexasiloxane(D6) in water using gas chromatography–mass spectrometry(GC–MS) was established and applied to the detection of D4, D5, and D6 concentrations in actual domestic wastewater. The results showed that the method detection limits ranged from 1.43 to 3.14 ng/L, with average recoveries of 92.2% to 110.6% and 75.1% to 91.2% at spiked concentrations of 5 and 0.5 μg/L, respectively. The detection results for actual domestic wastewater indicated that the average concentrations of D5 and D6 in influent were 1 071 and 524 ng/L, respectively, with D4 not detected; D4, D5, and D6 were not detected in any effluent samples. The sample pretreatment and GC-MS detection method is simple and can significantly reduce background interference, providing a reference method for the detection and analysis of cVMSs in wastewater and supporting decision making for environmental regulatory agencies.
Key words:  cVMSs  GC-MS  Method optimization  Isotope dilution method  Domestic wastewater  Background interference