EPA Method 1618 Organo-Halide, -Phosphorus Pesticides, and Phenoxy-acid Herbicides by Wide Bore Capillary Column GC
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BED43FEB06C041B8B4DADBC0D1F2A088 |
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1.54 |
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38 |
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2024-8-11 |
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0IA0006086,United States Environmental Protection Agency,Office of Water Regulations and Standards,Industrial Technology Division,Office of Water July 1989,品;落淬エon ] : ■---,战点”丒巩沁ー,.(,，励 02203-22n,Method 1618: Organo-halide Pesticides,Organo-phosphorus Pesticides, and,Phenoxy-acid Herbicides by Wide Bore,Capillary Column Gas Chromatography,with Selective Detectors,Method 1618 Revision A July 1989,Organo-halide Pesticides, Organo-phosphorus Pesticides, and,Phenoxy-acid Herbicides by Wide Bore Capillary Column,Gas Chromatography with Selective Detectors,1 SCOPE AND APPLICATION,1.1 This method is designed to meet the survey,requi rements of the USEPA ITD, The method,is used to determine the organo-halide,pesticides and polychlorinated biphenyls,(PCB^), the organo-phosphorus pesticides,and the phenoxy-acid herbicides and,herbicide esters, associated with the,Clean Water Act (as amended 1987); the," Resource Conservation and Recovery Act (as,amended 1986); the Comprehensive,Environmental Response, Compensation and,Liability Act (as amended 1986); and other,compounds amenable to extraction and,analysis by automated, wide bore capillary,column gas chromatography (GC) with,halogen specific and organo-phosphorus,detectors.,1.2 The chemical compounds listed in Tables 1,-3 may be determined in waters, soiIs,sediments, and sludges by this method.,The method is a consolidation of EPA,Methods 608, 608.1, 614, 615, 617, 622,and 701. For waters, the sample,extraction and concentration steps are,essentially the same as in these methods.,However, the extraction and concentration,steps have been extended to other sample,matrices. The method should be applicable,to other pesticides and herbicides- The,quaIity assurance/quaIity control requirements,in Section 8.6 of this method give,the steps necessary to determine its,applicabiIity.,1.3 When this method is applied to analysis of,unfamiliar samples, compound identity,shal I be supported by at least one,additional qualitative technique. This,method describes analytical conditions for,a second gas chromatographic column that,can be used to confirm measurements made,with the primary column. Gas,chromatography-rnass spectrometry (GCMS),can be used to conf i rm compounds in,extracts produced by this method when,analyte levels are sufficient.,1.4 The detection limits of this method are,usually dependent on the level of,interferences rather than instrumental,limitations. The limits in Tables 4 - 6,typify the mi ninon quant i t i es that can be,detected with no interferences present.,1.5 This method is for use by or under the,supervision of analysts experienced in the,use of a gas chromatograph and in the,interpretation of gas chromatographic,data. Each laboratory that uses this,method must demonstrate the ability to,generate acceptable results using the,procedure in Section 8.2.,2 SUMMARY OF METHOD,2.1 Extraction,2.1.1 The percent sol ids content of a sample is,determined.,2.1.2 Aqueous samples containing 1 - 30 percent,solids "- The sample is di luted to one,percent solids, if necessary. The,pesticides and PCB!s are extracted from a,one liter sample with methylene chloride,using cont i nuous extraction techniques.,For the herbicides, the pH of the sample,is raised to 12 - 13 to hydrolyze esters,the san^le is back-extracted to remove,basic and neutral species, the pH is then,reduced to less than 2, and the sample is,extracted with diethyl ether using,separatory funnel techniques-,2.1.3 Samples containing greater than 30 percent,solids -- The sample is extracted with,acetonitrile and then methylene chloride,using ultrasonic techniques- The extract,is back extracted with two percent (w/v),sodium sulfate in reagent water to remove,water soluble interferences and residual,acetonitrile. Samples in which phenoxyacid,herbicides are to be determined are,acidified prior to extraction.,2.2 Concentration and cleanup -- For samples,in which pesticides are to be determined,each extract is dried over sodium sulfate,concentrated using a Kuderna-Danish,evaporator, cleaned1' up (if necessary),using gel permeation chromatography (GPC),4 SAFETY 5 APPARATUS AND MATERIALS,4.1 The toxicity or carcinogenicity of each,compound or reagent used in this method,has not been precisely determined;,however, each chemical compound should be,treated as a potential health hazard.,Exposure to these compounds,reduced to the Lowest possible,laboratory is responsible for,a current awareness file,should be,level. The,maintaining,of OSHA,regulations regarding the safe handling of,the chemicals specified in this method. A,reference file of material handling sheets,should also be made availab……
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