全自动固相萃取-联合离子色谱-质谱法测定化工产业园区周边地表径流中微量氟乙酸、 碘乙酸、羟基乙酸、溴酸盐和高氯酸盐  

Determination of Trace Fluoroacetic Acid,Iodoacetic Acid,Hydroxy Acetic Acid,Bromate and Perchlorate in Surface Runoff around Chemical Industrial Park by IC-MS with Automatic SPE

作　　者：赵海军 赵光骞 李海景 ZHAO Haijun;ZHAO Guangqian;LI Haijing(Henan Province South to North Water Diversion Canal Head Ecological Environment Monitoring Emergency Center,Nanyang,Henan 474475,China;Nanyang Ecological Environment Monitoring Center of Province,Nanyang,Henan 473000,China;Tongbai Branch of Nanyang Ecological Environment Bureau,Nanyang,Henan 474750,China)

机构地区：[1]河南省南水北调渠首生态环境监测应急中心,河南南阳474475 [2]河南省南阳生态环境监测中心,河南南阳473000 [3]南阳市生态环境局桐柏分局,河南南阳474750

出　　处：《中国无机分析化学》2024年第5期560-566,共7页Chinese Journal of Inorganic Analytical Chemistry

摘　　要：为保护人们赖以生存的水资源环境,研究化工产业常用到的氟乙酸等6种原料在化工园区周边地表径流中的残留,为环保部门提供基础数据。通过对样品前处理方法和固相萃取柱等条件的研究,结果表明:将采集到的化工产业园区周边地表径流水样1000 mL置于干净的试剂瓶中,去除肉眼可见杂质,滤纸过滤;采用HLB固相萃取柱,上全自动固相萃取仪对处理后的水样进行富集、净化处理,处理后的水样氮吹至近干,1.0 mL甲醇溶解后过滤,上离子色谱-质谱仪定性、定量检测。氟乙酸、碘乙酸、羟基乙酸、溴酸盐和高氯酸盐在浓度0.005~2.0μg/mL时,线性相关系数分别为0.9992、0.9985、0.9988、0.9990、0.9991;检出限分别为0.021、0.023、0.0014、0.025和0.015μg/L;三水平加标回收率在83.8%~105%;相对标准偏差(RSD)分别为3.4%、4.0%、3.2%、2.9%、3.6%。方法检出限低、准确度和精密度好,适用于化工产业园区周边地表径流水样的检测分析。In order to protect the water resource environment that people rely on for survival,the residue of 6 raw materials such as fluoroacetic acid commonly used in the chemical industry in the surface runoff around the chemical park was studied to provide basic data for the environmental protection department.Sample pretreatment method,solid phase extraction column and other conditions were studied.The 1000 mL of collected surface runoff water sample around the chemical industry park was put into a clean reagent bottle,visible impurities was removed,and then the water was filtered with filter paper.The treated water samples were enriched and purified by using HLB solid phase extraction column and automatic solid phase extraction instrument.The treated water samples was blown to near-dry by nitrogen,dissolved and filtered by 1.0 mL methanol,and qualitative and quantitative detected by ion chromate-mass spectrometer.The linear correlation coefficients of fluoroacetic acid,iodoacetic acid,glycolic acid,bromic acid and perchlorate were 0.9992,0.9985,0.9988,0.9990 and 0.9991 at the concentration of 0.005—2.0μg/mL,respectively.The corresponding detection limits were 0.021,0.023,0.0014,0.025 and 0.015μg/L,respectively.The recovery of three-level spiked were 83.8%—105%.The relative standard deviations(RSD)were 3.4%,4.0%,3.2%,2.9%and 3.6%,respectively.The method has low detection limit,good accuracy and precision,and is suitable for the detection and analysis of surface runoff water samples around the chemical industry park.

关 键 词：全自动固相萃取 离子色谱-质谱法 化工产业园区 氟乙酸 溴酸盐 高氯酸盐 

分 类 号：O657.75[理学—分析化学] O657.63[理学—化学]