吹扫捕集-气相色谱-质谱联用测定水中的双环戊二烯
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摘要
建立了测定水中双环戊二烯(DCPD)的吹扫捕集-气相色谱-质谱联用方法。对吹扫捕集测定条件进行了考察和优化,确定的最佳实验条件如下,吹扫气流速为40 m L/min,吹扫时间为11 min,解吸温度为250℃,解吸时间为2. 0 min。选用选择离子模式(SIM)进行检测,在2. 0~200. 0 ng/L范围内,DCPD浓度与仪器响应值间的线性相关系数为0. 999 1,方法的测定下限为2. 0 ng/L;地下水、地表水和出厂水中三种不同浓度加标水平(2. 0、100. 0、180. 0 ng/L)的平均回收率为103. 30%~108. 77%,相对标准偏差<5%(n=6)。利用本方法测定的含有汽油味的水中的DCPD含量分别为地下水685. 921、5 380. 327 ng/L,地表水84. 589、151. 157 ng/L和饮用水12. 277、10. 924 ng/L。
The analysis method was established for the determination of dicyclopentadiene(DCPD) in water by gas chromatography-mass spectrometry with purge and trap(P & T-GC-MS). The optimum experimental conditions were as follows: purge gas flow rate was 40 m L/min,purge time was 11 min,the desorption temperature was 250 ℃,and desorption period was 2. 0 min. Under the selective ion monitoring( SIM) mode,a good linear relation was observed between the concentration of DCPD and the response of the signal within the range of 2. 0-200. 0 ng/L,the correlation coefficient was 0. 999 1. The lower limit of detection was 2. 0 ng/L. The relative standard deviation was less than 5%( n = 6). The average recovery of DCPD ranged from 103. 30%-108. 77% in the spiked concentration levels of 2. 0 ng/L,100. 0 ng/L and 180. 0 ng/L,respectively. Finally,the method established in the present study was examined by the gasoline-flavored water samples analysis. The content of DCPD detected was685. 921 ng/L and 5 380. 327 ng/L for ground water,84. 589 ng/L and 151. 157 ng/L for surface water,12. 277 ng/L and 10. 924 ng/L for drinking water,respectively.
The analysis method was established for the determination of dicyclopentadiene(DCPD) in water by gas chromatography-mass spectrometry with purge and trap(P & T-GC-MS). The optimum experimental conditions were as follows: purge gas flow rate was 40 m L/min,purge time was 11 min,the desorption temperature was 250 ℃,and desorption period was 2. 0 min. Under the selective ion monitoring( SIM) mode,a good linear relation was observed between the concentration of DCPD and the response of the signal within the range of 2. 0-200. 0 ng/L,the correlation coefficient was 0. 999 1. The lower limit of detection was 2. 0 ng/L. The relative standard deviation was less than 5%( n = 6). The average recovery of DCPD ranged from 103. 30%-108. 77% in the spiked concentration levels of 2. 0 ng/L,100. 0 ng/L and 180. 0 ng/L,respectively. Finally,the method established in the present study was examined by the gasoline-flavored water samples analysis. The content of DCPD detected was685. 921 ng/L and 5 380. 327 ng/L for ground water,84. 589 ng/L and 151. 157 ng/L for surface water,12. 277 ng/L and 10. 924 ng/L for drinking water,respectively.
引文
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[13]寇立娟,梁春实,魏树龙,等.固相微萃取-气相色谱-质谱联用测定水中痕量2-甲基异冰片和土臭素[J].分析化学,2011,39(12):1932-1933.Kou Lijuan,Liang Chunshi,Wei Shulong,et al.Determination of 2-methylisoborneol and geosmin in water by headspace solid phase microextraction-gas chromatography-mass spectrometry[J].Chinese Journal of Analytical Chemistry,2011,39(12):1932-1933(in Chinese).
[14]陈飒,李志梅,吴颖娟,等.顶空固相微萃取-气质法测定水中嗅味物质[J].中国给水排水,2016,32(12):137-142.Chen Sa,Li Zhimei,Wu Yingjuan,et al.Determination of odorous compounds in water by headspace solid-phase microextraction coupled with gas chromatography/mass spectrometry[J].China Water&Wastewater,2016,32(12):137-142(in Chinese).
[15]Pavlova A.Sensitive method for determination of dicyclopentadiene in gasoline by gas chromatography-mass spectrometry[J].Oxid Commun,2004,27(2):292-297.
[16]HJ 168-2010,环境监测分析方法标准制修订技术导则[S].北京:中国环境科学出版社,2010.HJ 168-2010,Environmental Monitoring-Technical Guideline on Drawing and Revising Analytical Method Standards[S].Beijing:China Environmental Science Press,2010(in Chinese).
[2]Rudelle E,Vollertsen J,Hvitved-Jacobsen T,et al.Kinetics of aerobic oxidation of volatile sulfur compounds in wastewater and biofilm from sewers[J].Water Sci Technol,2013,68(11):2330-2336.
[3]Sedighi M,Vahabzadeh F,Zamir S M,et al.Ethanethiol degradation by Ralstonia eutropha[J].Biotechnol Bioprocess Eng,2013,18(4):827-833.
[4]鹿文慧,马继平,肖荣辉,等.环境水体中致嗅有机物分析的样品前处理技术研究进展[J].分析测试学报,2009,28(5):621-626.Lu Wenhui,Ma Jiping,Xiao Ronghui,et al.Progress in pre-treatment techniques for analysis on odorous compounds in environmental water[J].Journal of Instrumental Analysis,2009,28(5):621-626(in Chinese).
[5]Suffet M,Khiari D,Bruchet A.The drinking water taste and odor wheel for the millennium:beyond geosmin and2-methylisoborneol[J].Water Sci Technol,1999,40(6):1-13.
[6]许冬梅,许俊鸽,苑宝玲,等.稳定性同位素稀释吹扫捕集-气质联用法测定水中典型臭味物质[J].分析化学,2011,39(2):248-252.Xu Dongmei,Xu Junge,Yuan Baoling,et al.Determination of typical odorous compounds in water using purgeand-trap gas chromatography-mass spectrometry combined with stable isotope dilution[J].Chinese Journal of Analytical Chemistry,2011,39(2):248-252(in Chinese).
[7]林麒,李俊荣,林坚,等.稳定性同位素内标-吹扫捕集-气相色谱-质谱联用分析水中硫化物[J].分析化学,2014,42(5):678-682.Lin Qi,Li Junrong,Lin Jian,et al.Determination of sulfide in water by purge and trap GC-MS coupled with stable isotope internal standard[J].Chinese Journal of Analytical Chemistry,2014,42(5):678-682(in Chinese).
[8]毛敏敏,张可佳,张土乔,等.大体积浓缩-固相微萃取-气相色谱-质谱联用测定水样中6种典型嗅味物质[J].分析化学,2013,41(5):760-765.Mao Minmin,Zhang Kejia,Zhang Tuqiao,et al.Determination of six typical taste and odor compounds using large volume concentration,solid phase micro-extraction and gas chromatography-mass spectrometry[J].Chinese Journal of Analytical Chemistry,2013,41(5):760-765(in Chinese).
[9]马康,张金娜,何雅娟,等.顶空固相微萃取-气质联用测定环境水样中7种痕量土霉味物质[J].分析化学,2011,39(12):1823-1829.Ma Kang,Zhang Jinna,He Yajuan,et al.Determination of seven musty odor compounds in water by gas chromatography mass spectrometry with headspace phase microextraction[J].Chinese Journal of Analytical Chemistry,2011,39(12):1823-1829(in Chinese).
[10]方菲菲,于建伟,杨敏,等.顶空固相微萃取法用于测定水中二甲基三硫醚[J].中国给水排水,2009,25(6):86-89.Fang Feifei,Yu Jianwei,Yang Min,et al.Determination of dimethyl trisulfide in water by headspace solid-phase micro-extraction coupled with gas chromatography/mass spectrometry[J].China Water&Wastewater,2009,25(6):86-89(in Chinese).
[11]辛晓东,王明泉,赵清华,等.饮用水嗅味物质检测与控制技术研究进展[J].中国给水排水,2013,29(14):13-15.Xin Xiaodong,Wang Mingquan,Zhao Qinghua,et al.State-of-the-art of detection and control technologies of odorous compounds in drinking water[J].China Water&Wastewater,2013,29(14):13-15(in Chinese).
[12]冯桂学,刘莉,顿咪娜,等.固相萃取-气相色谱-质谱法测定水中10种嗅味物质的含量[J].理化检验:化学分册,2017,53(5):502-506.Feng Guixue,Liu Li,Dun Mina,et al.SPE-GC-MEdetermination of 10 odorous materials in water[J].Physical Testing and Chemical Analysis(Part B:Chemical Analysis),2017,53(5):502-506(in Chinese).
[13]寇立娟,梁春实,魏树龙,等.固相微萃取-气相色谱-质谱联用测定水中痕量2-甲基异冰片和土臭素[J].分析化学,2011,39(12):1932-1933.Kou Lijuan,Liang Chunshi,Wei Shulong,et al.Determination of 2-methylisoborneol and geosmin in water by headspace solid phase microextraction-gas chromatography-mass spectrometry[J].Chinese Journal of Analytical Chemistry,2011,39(12):1932-1933(in Chinese).
[14]陈飒,李志梅,吴颖娟,等.顶空固相微萃取-气质法测定水中嗅味物质[J].中国给水排水,2016,32(12):137-142.Chen Sa,Li Zhimei,Wu Yingjuan,et al.Determination of odorous compounds in water by headspace solid-phase microextraction coupled with gas chromatography/mass spectrometry[J].China Water&Wastewater,2016,32(12):137-142(in Chinese).
[15]Pavlova A.Sensitive method for determination of dicyclopentadiene in gasoline by gas chromatography-mass spectrometry[J].Oxid Commun,2004,27(2):292-297.
[16]HJ 168-2010,环境监测分析方法标准制修订技术导则[S].北京:中国环境科学出版社,2010.HJ 168-2010,Environmental Monitoring-Technical Guideline on Drawing and Revising Analytical Method Standards[S].Beijing:China Environmental Science Press,2010(in Chinese).
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