Study on Enrichment of Semi-Volatile Organic Pollutants from Ground Water Samples Collected at Non-Fixed Experimental Sites by Adsorption on SPE Membranes, and Its Time of Preservation and Mode of Transportation under Stable State
摘 要
选择以硅胶为吸附剂的C18膜片为载体,在流量为100 mL·min-1的条件下使1 L水样流经膜片富集地下水中半挥发有机物(包括有机氯、多环芳烃、多氯联苯及酞酸酯等19种化合物),将膜片移入10 mL棕色小瓶中,加盖密封,在低于6℃条件下保存并运输。在所述条件下30 d内富集于膜片上的有机物有较好的稳定性。膜片上的富集物可用正己烷2.0 mL,在25℃左右超声洗脱10 min。从洗脱液中分取0.50 mL试液,按所设定工作条件用气相色谱-质谱法测定各富集物的含量。应用此方法对不同地域的多组地下水样品进行分析,并取其中3个样品作为基体在3个浓度水平上进行回收试验,测得回收率在75%~112%之间。对7个加标浓度为0.020 μg·L-1的水样按方法进行富集、洗脱和测定,测定值的相对标准偏差在4.9%~13%之间。此方法延长了在野外采得的样品的稳定保存时间,对在野外科研团队的持续工作带来方便。
Abstract
C18 membranes with silica gel as adsortent were selected to be carriers for enrichment of semi-volatile organic pollutants from sample of ground-water (1.0 L) at a flow-rate of 100 mL·min-1. 19 Compounds, including organochlorine pesticides, polycyclic aromatic hydrocarbons, poly-chlorinated biphenyls and phthalates were tested. The C18 membrane with the adsorbates was transferred to and sealed in a 10 mL brown glass bottle, and the adsorbates on the membrane could be kept stable for 30 days at temperatures below 6℃, and transported under this condition. The adsorbates were eluted ultrasonically from the C18 membrane with 2.0 mL of n-hexane at ca. 25℃ for 10 min, and 0.50 mL of the eluate was taken and used for GC-MS analysis. Several groups of ground water samples taken from various areas in our country were analyzed by the proposed method and 3 samples were selected to be used as matrixes in tests for recovery by standard addition at 3 concentration levels, the results of recovery found were in the range of 75% to 112%. Seven samples with addition of 0.020 μg·L-1 of the substitute standard in each sample were analyzed by the proposed method, giving values of RSDs (n=7) in the range of 4.9% to 13%. By using the conditions given in this method, the time of presevation of the adsorbates on the C18 membrane in their stable states were extended to 30 days, which was not only advantageous for storage and transportation of the analytes, but also facilitative for long-term field scientific works.
中图分类号 O652.6 DOI 10.11973/lhjy-hx201906002
所属栏目 试验与研究
基金项目
收稿日期 2018/8/27
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备注张莉,高级工程师,学士,研究方向为水中有机物分析
引用该论文: ZHANG Li,LI Xiaoya,LIU Jia,ZHANG Lin,LI Ke,ZHANG Chenling. Study on Enrichment of Semi-Volatile Organic Pollutants from Ground Water Samples Collected at Non-Fixed Experimental Sites by Adsorption on SPE Membranes, and Its Time of Preservation and Mode of Transportation under Stable State[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2019, 55(6): 627~633
张莉,李晓亚,刘佳,张琳,李科,张辰凌. 在非固定实验场所用固相萃取膜富集地下水中半挥发有机污染物及其稳定保存时间和运输条件的研究[J]. 理化检验-化学分册, 2019, 55(6): 627~633
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参考文献
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【2】赵国栋.地下水中有机污染物现场富集的方法[J].环境科学丛刊, 1986,7(6):53-58.
【3】SMITH P A, SNG M T, ECKENRODE B A, et al. Towards smaller and faster gas chromatography-mass spectrometry systems for field chemical detection[J]. Journal of Chromatography A, 2005,1067(1/2):285-294.
【4】MEUZELAAR H L C, DWORZANSKI J P, ARNOLD N S, et al. Advances in field-portable mobile GC/MS instrumentation[J]. Field Analytical Chemistry & Technology, 2000,4(1):3-13.
【5】刘岩,高杨,任国兴,等.海水持久性有机污染物(POPs)现场富集分析技术[J].环境科学与技术, 2010,33(增刊1):201-205.
【6】苏宇亮,胡克武.水中酚类化合物的固相萃取-气质联用法测定[J].分析测试学报, 2008,27(增刊1):127-129.
【7】俞是聃.圆盘膜萃取-色质联用仪及选择离子法(SIM)定量分析水中有机氯农药[J].质谱学报, 2006,27(4):209-214.
【8】那广水,刘春阳,张琳,等.固相膜萃取-超高效液相色谱-荧光法测定极地水体中多环芳烃[J].分析试验室, 2011,30(1):29-31.
【9】潘海祥,麦碧娴,庄汉平,等.使用C18固相萃取膜-色质联用定量分析饮用水中痕量多环芳烃的初步研究[J].分析化学, 1999,27(2):140-144.
【10】张莉,张永涛,李桂香,等.基质标准校正-气相色谱-质谱法同时检测地下水中有机氯农药和多环芳烃[J]分析试验室, 2010,29(2):18-22.
【11】US EPA Method 550.1 Determination of polycyclic aromatic hydrocarbons in drinking water by liquid-solid extraction and HPLC with coupled ultraviolet and fluorescence detection[S].
【12】张莉,张永涛,张辰凌,等.固相膜萃取-超声洗脱衍生法分析水中酚类化合物[J].质谱学报, 2018,39(5):623-629.
【13】US EPA Method 3550C Ultrasonic extraction[S].
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