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The Research on Detection Method of Methomyl-oxime in Water

Author: LiuLiLi
Tutor: TanPeiGong
School: Qingdao Technological University
Course: Environmental Engineering
Keywords: Methomyl-oxime Water quality HPLC Detection methods
CLC: X832
Type: Master's thesis
Year: 2013
Downloads: 9
Quote: 0
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Abstract


Methomyl-oxime is the synthetic intermediate of methomyl which is a kind of carbamateinsecticide. Methomyl-oxime is toxic and mainly presents in the methomyl andmethomyl-oxime industrial wastewater. It is significant to monitor the emission ofmethomyl-oxime in order to protect environment. This paper studied the detection of themethomyl-oxime in water environment,and systematically researched on the pretreatment andanalysis methods.The contents include the following three parts:Firstly, we searched the reviews of methomyl-oxime characteristics and its analysismethods, including methomyl-oxime environmental characteristics, synthesis crafts, removaltechnologies, and the domestic and foreign currently methomyl-oxime detection methodsreported in the literature.Secondly, we established two kinds of methomyl-oxime analytical methods usinghigh-performance liquid chromatography with methanol/water or acetonitrile/water as mobilephase, respectively. We also compared the different separation effects of C18and C8in thedetection of methomyl-oxime and its interfering substances, optimized the detectionwavelength and elution mode, and then completed the chromatographic conditions. Theresults showed that the two kinds of HPLC had the same method detection limit of0.010mg/L,and they also had a good linear relationship at0.05~100mg/L with a correlation coefficient of0.99998and0.99985, respectively. When the direct injection volume is1mg/L,50mg/L and80mg/L, the relative standard deviation of the two methods were0.22%~1.1%and0.29%~1.1%and recovery of standard addition were98.3%~99.9%and90.9%~103%,respectively.In the study of sample stability, we detected the methomyl-oxime water samples forcontinued30days in4kinds of different conditions by direct injection method. The resultsshowed that the methomyl-oxime water samples which were saved in dark at roomtemperature or refrigeration could remain stable for30days at least.Finally, we researched the enrichment methods of methomyl-oxime in water usingliquid-liquid extraction, solid phase extraction and acetonitrile extraction method, respectively.And we also compared the different extraction efficiencies of these three methods.We used four kinds of extractant(dichloromethane,ethyl acetate, methyl tert-butyl etherand n-hexane) to reach the highest recovery through adjusting pH and adding NaCl, and theoptimal result was30.3%. And then we used solid phase extraction with SDB-RPS, SDB-XC, HLB SPE disk and C18、Pesticarb solid phase extraction to extract methomyl-oxime in water,but an extremely low efficiency was obtained. While using HLB solid phase extractioncolumn at a flow rate of1mL/min to enriched methomyl-oxime in water, it achieved morethan85%efficiency.In study of extraction of methomyl-oxime using acetonitrile, through optimizingextraction conditions, we founded a method which used25mL acetonitrile to extract10mLsample. When this method combined with the HPLC using acetonitrile/water as mobile phasecan make MDL is1.1μg/L and Limit of Quantitation is4.4μg/L,achieved an actual samplerecovery as84%, which relative standard deviation of precision is2.6%~4.1%.

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CLC: > Environmental science, safety science > Environmental Quality Assessment and Environmental Monitoring > Environmental monitoring > Water quality monitoring
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