DETERMINATION OF 60 VOLATILE ORGANIC COMPOUNDS IN GROUNDWATER OF ENTERPRISE LAND OF KEY INDUSTRIES
-
摘要:
建立了吹扫捕集-气相色谱质谱法测定重点行业企业用地地下水中60种挥发性有机物的分析方法.采用屈臣氏双蒸水作为空白水,选择离子与全扫描模式交替方式进行定性定量,确定了保护剂的种类和用量,优化了吹扫捕集条件.方法检出限范围在0.3~1.2 μg/L.该方法的线性范围为0~250 μg/L,相关系数R2在0.9907~0.9999之间,3种不同浓度的加标平均回收率为87.2%~117%,相对标准偏差在1.7%~9.7%之间,优于《重点行业企业用地调查质量保证与质量控制技术规定(试行)》对地下水挥发性有机物的质控要求.本方法增加了VOCs的测试种类,线性范围宽,灵敏度高,适合于各类重点行业企业用地地下水中60种挥发性有机物的快速批量分析.
Abstract:The purge and trap gas chromatography-mass spectrometry(GC-MS) is established for the determination of 60 volatile organic compounds (VOC) in groundwater of enterprise land of key industries. The purge and trap conditions are optimized by selecting Watsons double-distilled water as blank water, ion and full scanning alternating mode for qualitative-quantitative analysis and determination of types and dosages of protective agent. The detection limit of the method is 0.3-1.2 μg/L, with the linear range of 0-250 μg/L, and correlation coefficient(R2) of 0.9907-0.9999. The spiked average recovery of three different concentrations are 87.2%-117%, with the relative standard deviation of 1.7%-9.7%, which is better than the quality control requirements of "Technical Specifications on Quality Assurance and Control of Survey for Enterprise Land of Key Industries (Trial)" for VOCs in groundwater. The method adds test types of VOCs, with wide linear range and high sensitivity, suitable for rapid batch analysis of 60 VOCs in groundwater of enterprise land of various key industries.
-
表 1 空白试剂水的选择
Table 1. Selection of blank reagent water
试剂水 屈臣氏双蒸水 娃哈哈纯净水 实验室自制蒸馏水 处理过程 高纯氮气通气30 min 高纯氮气通气30 min 煮沸10 min后,高纯氮气通气30 min 二氯甲烷、三氯甲烷的检出情况 未检出 二氯甲烷检出 二氯甲烷、三氯甲烷均有检出 -
[1] 冯丽丽, 胡晓芳. 顶空固相微萃取/气相色谱-三重四极杆串联质谱法测定地表水与饮用水中的挥发性有机物[J]. 分析测试学报, 2019, 38(11): 1294-1300. doi: 10.3969/j.issn.1004-4957.2019.11.002
Feng L L, Hu X F. Determination of volatile organic compounds in surface water and drinking water by gas chromatography-triple Quadrupole tandem mass spectrometry with head space-solid phase microextraction[J]. Journal of Instrumental Analysis, 2019, 38(11): 1294-1300. doi: 10.3969/j.issn.1004-4957.2019.11.002
[2] 李秋萱, 刘玲花, 王学东, 等. 地下水中挥发性有机物的样品预处理与分析检测综述[J]. 首都师范大学学报(自然科学版), 2022, 43 (1): 91-96. https://www.cnki.com.cn/Article/CJFDTOTAL-SDSX202201015.htm
Li Q X, Liu L H, Wang X D, et al. Sample pretreatment and analysis detection of volatile organic compounds in groundwater[J]. Journal of Capital Normal University (Natural Science Edition), 2022, 43(1): 91-96. https://www.cnki.com.cn/Article/CJFDTOTAL-SDSX202201015.htm
[3] 梁小明, 孙西勃, 徐建铁, 等. 中国工业源挥发性有机物排放清单[J]. 环境科学, 2020, 41(11): 4767-4775. https://www.cnki.com.cn/Article/CJFDTOTAL-HJKZ202011002.htm
Liang X M, Sun X B, Xu J T, et al. Industrial Volatile Organic Compounds (VOCs) emission inventory in China[J]. Environmental Science, 2020, 41(11): 4767-4775. https://www.cnki.com.cn/Article/CJFDTOTAL-HJKZ202011002.htm
[4] 秦兴秀, 王来梁, 杨敏娜. 重点行业企业用地地下水中挥发性有机物分析方法探究[J]. 环境监控与预警, 2021, 13(1): 25-29. https://www.cnki.com.cn/Article/CJFDTOTAL-HTJK202101005.htm
Qin X X, Wang L L, Yang M N. Study on analytical methods of volatile organic compounds in groundwater of enterprise land pollution investigation[J]. Environmental Monitoring and Forewarning, 2021, 13 (1): 25-29. https://www.cnki.com.cn/Article/CJFDTOTAL-HTJK202101005.htm
[5] 封跃鹏, 杨刚, 房丽萍, 等. 地下水检测典型挥发性有机物标准样品研究[J]. 分析试验室, 2016, 35(12): 1419-1423.
Feng Y P, Yang G, Fang L P, et al. Development of certified reference materials for typical volatile organic compounds in groundwater[J]. Chinese Journal of Analysis Laboratory, 2016, 35(12): 1419-1423.
[6] Alquwaizany A S, Alfadul S M, Khan M A, et al. Occurrence of organic compounds in groundwater of Saudi Arabia[J]. Environmental Monitoring and Assessment, 2019, 191(10): 601. doi: 10.1007/s10661-019-7723-6
[7] Kang B, Wang D, Du S H. Source identification and degradation pathway of multiple persistent organic pollutants in groundwater at an abandoned chemical site in Hebei, China[J]. Exposure and Health, 2017, 9(2): 135-141. doi: 10.1007/s12403-016-0228-4
[8] Liu G, Niu J J, Zhang C, et al. Characterization and assessment of contaminated soil and groundwater at an organic chemical plant site in Chongqing, Southwest China[J]. Environmental Geochemistry and Health, 2016, 38(2): 607-618. doi: 10.1007/s10653-015-9746-4
[9] Liu Y, Hao S R, Zhao X R, et al. Distribution characteristics and health risk assessment of volatile organic compounds in the groundwater of Lanzhou City, China[J]. Environmental Geochemistry and Health, 2020, 42(11): 3609-3622. doi: 10.1007/s10653-020-00591-6
[10] 徐桂茹, 韦晨, 王帆, 等. 某金属冶炼企业场地环境污染现状调查与分析[J]. 上海船舶运输科学研究所学报, 2019, 42(4): 70-77. doi: 10.3969/j.issn.1674-5949.2019.04.013
Xu G R, Wei C, Wang F, et al. Investigation and analysis of site pollution in a metal smelter[J]. Journal of Shanghai Ship and Shipping Research Institute, 2019, 42(4): 70-77. doi: 10.3969/j.issn.1674-5949.2019.04.013
[11] 吕晓立, 邵景力, 刘景涛, 等. 某石油化工污染场地地下水中挥发性有机物污染特征及成因分析[J]. 水文地质工程地质, 2012, 39 (6): 97-102. https://www.cnki.com.cn/Article/CJFDTOTAL-SWDG201206021.htm
Lv X L, Shao J L, Liu J T, et al. Contamination characteristics and causes of volatile organic compounds in the groundwater at a petrochemical contaminated site[J]. Hydrogeology & Engineering Geology, 2012, 39(6): 97-102. https://www.cnki.com.cn/Article/CJFDTOTAL-SWDG201206021.htm
[12] 谭冰, 王铁宇, 李奇锋, 等. 农药企业场地土壤中苯系物污染风险及管理对策[J]. 环境科学, 2014, 35(6): 2272-2280. https://www.cnki.com.cn/Article/CJFDTOTAL-HJKZ201406036.htm
Tan B, Wang T Y, Li Q F, et al. Risk assessment and countermeasures of BTEX contamination in soils of typical pesticide factory[J]. Environmental Science, 2014, 35(6): 2272-2280. https://www.cnki.com.cn/Article/CJFDTOTAL-HJKZ201406036.htm
[13] 昌盛, 赵兴茹, 刘琰, 等. 滹沱河冲洪积扇地下水中挥发性有机物的分布特征与健康风险[J]. 环境科学研究, 2016, 29(6): 854- 862.
Chang S, Zho X R, Liu Y, et al. Distribution characteristics and health risk assessment of volatile organic compounds in Groundwater of Hutuo River Pluvial Fan[J]. Research of Environmental Sciences, 2016, 29(6): 854-862.
[14] 张茜, 刘炜伦, 路亚楠, 等. 顶空气相色谱-质谱联用技术的应用进展[J]. 色谱, 2018, 36(10): 962-971. https://www.cnki.com.cn/Article/CJFDTOTAL-SPZZ201810003.htm
Zhang X, Liu W L, Lu Y N, et al. Recent advances in the application of headspace gas chromatography-mass spectrometry[J]. Chinese Journal of Chromatography, 2018, 36(10): 962-971. https://www.cnki.com.cn/Article/CJFDTOTAL-SPZZ201810003.htm
[15] 姜洋, 房丽萍, 杨刚, 等. 水体中挥发性有机物分析方法研究进展[J]. 环境化学, 2015, 34(9): 1611-1618. https://www.cnki.com.cn/Article/CJFDTOTAL-HLKX202017004.htm
Jiang Y, Fang L P, Yang G, et al. Analytical methods of volatile organic compounds in water samples[J]. Environmental Chemistry, 2015, 34(9): 1611-1618. https://www.cnki.com.cn/Article/CJFDTOTAL-HLKX202017004.htm
[16] 葛璇, 战锡林, 陈燕朋, 等. 水中25种挥发性有机物的固相微萃取-气相色谱-质谱测定法[J]. 环境与健康杂志, 2020, 37(3): 251-254. https://www.cnki.com.cn/Article/CJFDTOTAL-HJYJ202003019.htm
Ge X, Zhan X L, Chen Y P, et al. Determination of 25 volatile organic compounds in water by solid phase microextraction-gas chromatography-mass spectrometry[J]. Journal of Environment and Health, 2020, 37(3): 251-254. https://www.cnki.com.cn/Article/CJFDTOTAL-HJYJ202003019.htm
[17] 张样盛, 肖霏, 吕萍. 自动顶空-气相色谱法测定水中二硫化碳的研究[J]. 环境科学导刊, 2017, 36(5): 80-83, 90. https://www.cnki.com.cn/Article/CJFDTOTAL-BFHJ201203038.htm
Zhang Y S, Xiao F, Lv P. Study on determination of carbon disulfide in water by automatic headspace gas chromatography[J]. Environmental Science Survey, 2017, 36(5): 80-83, 90. https://www.cnki.com.cn/Article/CJFDTOTAL-BFHJ201203038.htm
[18] 胡恩宇, 杨丽莉, 王美飞, 等. 顶空-气相色谱-质谱法测定地表水和废水中55种挥发性有机物含量[J]. 理化检验(化学分册), 2016, 52(10): 1131-1137.
Hu E Y, Yang L L, Wang M F, et al. Headspace GC-MS determination of 55 volatile organic compounds in surface water and waste water[J]. Physical Testing and Chemical Analysis (Part B: Chemical Analysis), 2016, 52(10): 1131-1137.
[19] 普学伟, 邵应春, 施艳峰, 等. 顶空-气相色谱-质谱法测定水中25种挥发性有机物的含量[J]. 理化检验(化学分册), 2015, 51 (8): 1194-1198. https://www.cnki.com.cn/Article/CJFDTOTAL-LHJH202001006.htm
Pu X W, Shao Y C, Shi Y F, et al. Headspace GC-MS determination of 25 volatile organic compounds in water[J]. Physical Testing and Chemical Analysis (Part B: Chemical Analysis), 2015, 51(8): 1194- 1198. https://www.cnki.com.cn/Article/CJFDTOTAL-LHJH202001006.htm
[20] 黄毅, 李国傲, 饶竹, 等. 城市环境地下水调查样品中挥发性有机物测定[J]. 质谱学报, 2012, 33(5): 301-307. https://www.cnki.com.cn/Article/CJFDTOTAL-ZPXB201205007.htm
Huang Y, Li G A, Rao Z, et al. Determination of volatile organic compounds in city groundwater by GC/MS with purge and trap sampling [J]. Journal of Chinese Mass Spectrometry Society, 2012, 33(5): 301-307. https://www.cnki.com.cn/Article/CJFDTOTAL-ZPXB201205007.htm
[21] 刘美美, 张小辉, 马娅妮, 等. 吹扫捕集-气相色谱-质谱联用法测定地下水中27种挥发性有机物[J]. 岩矿测试, 2012, 31(3): 495- 500. doi: 10.3969/j.issn.0254-5357.2012.03.021
Liu M M, Zhang X H, Ma Y N, et al. Determination of 27 volatile organic compounds in groundwater by gas chromatography-mass spectrometry with purge and trap sampling[J]. Rock and Mineral Analysis, 2012, 31(3): 495-500. doi: 10.3969/j.issn.0254-5357.2012.03.021
[22] 冯丽, 李诚, 张彦, 等. 吹扫捕集/气相色谱-质谱法测定地下水中30种挥发性有机物[J]. 岩矿测试, 2012, 31(6): 1037-1042. doi: 10.3969/j.issn.0254-5357.2012.06.023
Feng L, Li C, Zhang Y, et al. Determination of 30 volatile organic compounds in groundwater samples by purge and trap-gas chromatography-mass spectrometry[J]. Rock and Mineral Analysis, 2012, 31(6): 1037-1042. doi: 10.3969/j.issn.0254-5357.2012.06.023
[23] 贾静, 杨志鹏. 吹扫捕集-气相色谱/质谱法测定地下水中1, 4-二恶烷[J]. 岩矿测试, 2014, 33(4): 556-560. doi: 10.3969/j.issn.0254-5357.2014.04.017
Jia J, Yang Z P. Determination of 1, 4-dioxane in groundwater by purge and trap-gas chromatography/mass spectrometry[J]. Rock and Mineral Analysis, 2014, 33(4): 556-560. doi: 10.3969/j.issn.0254-5357.2014.04.017
[24] 刘倩, 谷东杰. 气相色谱-质谱法测定地下水中30种挥发性有机物[J]. 山东化工, 2020, 49(9): 102-103. https://www.cnki.com.cn/Article/CJFDTOTAL-SDHG202009042.htm
Liu Q, Gu D J. Determination of 30 volatile organic compounds in groundwater by gas chromatography-mass spectrometry[J]. Shandong Chemical Industry, 2020, 49(9): 102-103. https://www.cnki.com.cn/Article/CJFDTOTAL-SDHG202009042.htm
[25] 杜作灵, 邓昭祥, 邓云江. 吹扫捕集/气相色谱-质谱法测定地下水中56种挥发性有机物[J]. 广州化工, 2021, 49(12): 105-107. https://www.cnki.com.cn/Article/CJFDTOTAL-GZHA202112036.htm
Du Z L, Deng Z X, Deng Y J. Determination of 56 volatile organic compounds in groundwater by purge and trap/gas chromatography- mass spectrometry[J]. Guangzhou Chemical Industry, 2021, 49(12): 105-107. https://www.cnki.com.cn/Article/CJFDTOTAL-GZHA202112036.htm
[26] 林诗云, 杨梅, 李禹, 等. 吹扫捕集-气相色谱-质谱法测定水中丁基黄原酸及27种挥发性有机物[J]. 理化检验(化学分册), 2016, 52(4): 436-439.
Lin S Y, Yang M, Li Y, et al. GC-MS Determination of butylxanthic acid and 27 volatile organic compounds in water with purging and trapping[J]. Physical Testing and Chemical Analysis (Part B: Chemical Analysis), 2016, 52(4): 436-439.
[27] 肖刚, 李丽君, 杨柳, 等. 气相色谱-质谱法同时测定地下水中55种挥发性有机物[J]. 环境化学, 2012, 31(12): 2024-2025. https://www.cnki.com.cn/Article/CJFDTOTAL-HJHX201212036.htm
Xiao G, Li L J, Yang L, et al. Simultaneous determination of 55 volatile organic compounds in groundwater by gas chromatography- mass spectrometry[J]. Environmental Chemistry, 2012, 31(12): 2024-2025. (in Chinese) https://www.cnki.com.cn/Article/CJFDTOTAL-HJHX201212036.htm
[28] 王娜, 李丽君, 宋丽华, 等. 吹扫捕集-气相色谱-质谱法测定地下水中的挥发性有机物[J]. 理化检验(化学分册), 2016, 52(5): 607-611. https://www.cnki.com.cn/Article/CJFDTOTAL-LHJH200903012.htm
Wang N, Li L J, Song L H, et al. Determination of volatile organic compounds in groundwater by GC-MS with purge and trap sampling [J]. Physical Testing and Chemical Analysis (Part B: Chemical Analysis), 2016, 52(5): 607-611. https://www.cnki.com.cn/Article/CJFDTOTAL-LHJH200903012.htm
[29] 徐延勤, 石洪波, 雷建彬, 等. 吹扫捕集-气相色谱-质谱联用技术测定化工废水中挥发性有机物[J]. 石化技术与应用, 2021, 39 (3): 213-218. https://www.cnki.com.cn/Article/CJFDTOTAL-IZHM202103021.htm
Xu Y Q, Shi H B, Lei J B, et al. Determination of volatile organic compounds in chemical wastewater by combined technology of purge and trap-gas chromatography-mass spectrometry[J]. Petrochemical Technology & Application, 2021, 39(3): 213-218. https://www.cnki.com.cn/Article/CJFDTOTAL-IZHM202103021.htm