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PCB analyses, and this method (8081) for the organochlorine pesticides. If there is no informationof the likely presence of PCBs, either employ a PCB-specific screening procedure such as animmunoassay (e.g., Method 4020), or split the sample extract prior to any cleanup steps, andprocess part of the extract for organochlorine pesticide analysis and the other portion for PCBanalysis using Method 8082.1.3 The analyst must select columns, detectors and calibration procedures most appropriatefor the specific analytes of interest in a study. Matrix-specific performance data must be establishedand the stability of the analytical system and instrument calibration must be established for eachanalytical matrix (e.g., hexane solutions from sample extractions, diluted oil samples, etc.).1.4 Although performance data are presented for many of the target analytes, it is unlikelythat all of them could be determined in a single analysis. The chemical and chromatographicbehaviors of many of these chemicals can result in co-elution of some target analytes. Severalcleanup/fractionation schemes are provided in this method and in Method 3600.1.5 Several multi-component mixtures (i.e., Chlordane and Toxaphene) are listed as targetanalytes. When samples contain more than one multi-component analyte, a higher level of analystexpertise is required to attain acceptable levels of qualitative and quantitative analysis. The sameis true of multi-component analytes that have been subjected to environmental degradation ordegradation by treatment technologies. These result in "weathered" multi-component mixtures thatmay have significant differences in peak patterns than those of standards.1.6 Compound identification based on single-column analysis should be confirmed on asecond column, or should be supported by at least one other qualitative technique. This methoddescribes analytical conditions for a second gas chromatographic column that can be used toconfirm the measurements made with the primary column. GC/MS Method 8270 is alsorecommended as a confirmation technique, if sensitivity permits (Sec. 8.0).1.7 This method includes a dual-column option. The option allows a hardware configurationof two analytical columns joined to a single injection port. The option allows one injection to be usedfor dual-column analysis. Analysts are cautioned that the dual-column option may not be appropriatewhen the instrument is subject to mechanical stress, many samples are to be run in a short period,or when contaminated samples are analyzed.1.8 This method is restricted to use by, or under the supervision of, analysts experienced inthe use of gas chromatographs (GC) and skilled in the interpretation of gas chromatograms. Eachanalyst must demonstrate the ability to generate acceptable results with this method.1.9 Extracts suitable for analysis by this method may also be analyzed for organophosphoruspesticides (Method 8141). Some extracts may also be suitable for triazine herbicide analysis, if lowrecoveries (normally samples taken for triazine analysis must be preserved) are not a problem.1.10 The following compounds may also be determined using this method:CompoundCAS Registry No.Alachlor 15972-60-8Captafol 2425-06-1Chloroneb 2675-77-6CD-ROM 8081A - 2 Revision 1December 1996
CompoundCAS Registry No.Chloropropylate 99516-95-7Chlorothalonil 1897-45-6DCPA 1861-32-1Dichlone 117-80-6Dicofol 115-32-2Etridiazole 2593-15-9Halowax-1000 58718-66-4Halowax-1001 58718-67-5Halowax-1013 12616-35-2Halowax-1014 12616-36-3Halowax-1051 2234-13-1Halowax-1099 39450-05-0Mirex 2385-85-5Nitrofen 1836-75-5PCNB 82-68-8Permethrin 51877-74-8Perthane 72-56-0Propachlor 1918-16-7Strobane 8001-50-1trans-Nonachlor 39765-80-5Trifluralin 1582-09-81.11 Kepone extracted from samples or standards exposed to water or methanol may producepeaks with broad tails that elute later than the standard by up to 1 minute. This shift is presumablythe result of the formation of a hemi-acetal from the ketone functionality. As a result, Method 8081is not recommended for determining Kepone. Method 8270 may be more appropriate for theanalysis of Kepone.2.0 SUMMARY OF METHOD2.1 A measured volume or weight of sample (approximately 1 L for liquids, 2 g to 30 g forsolids) is extracted using the appropriate matrix-specific sample extraction technique.2.2 Liquid samples are extracted at neutral pH with methylene chloride using either Method3510 (separatory funnel), Method 3520 (continuous liquid-liquid extractor), or other appropriatetechnique.2.3 Solid samples are extracted with hexane-acetone (1:1) or methylene chloride-acetone(1:1) using Method 3540 (Soxhlet), Method 3541 (automated Soxhlet), Method 3545 (pressurizedfluid extraction), Method 3550 (ultrasonic extraction), or other appropriate technique.2.4 A variety of cleanup steps may be applied to the extract, depending on the nature of thematrix interferences and the target analytes. Suggested cleanups include alumina (Method 3610),Florisil (Method 3620), silica gel (Method 3630), gel permeation chromatography (Method 3640), andsulfur (Method 3660).CD-ROM 8081A - 3 Revision 1December 1996
Page 1: METHOD 8081AORGANOCHLORINE PESTICID
Page 6 and 7: confirmation techniques may be empl
Page 9 and 10: 5.7.2 1-bromo-2-nitrobenzene is sug
Page 11 and 12: columns. Table 2 lists average rete
Page 13 and 14: mean CF ' CF 'nj CF ii'1nwhere n is
Page 15 and 16: 7.5.6.1 For aqueous samplesConcentr
Page 17 and 18: 7.5.11 Identification of mixtures (
Page 19 and 20: Construct a similar baseline in the
Page 21 and 22: 8.0 QUALITY CONTROL8.1 Refer to Cha
Page 23 and 24: 8000, Sec. 8.0 for information on e
Page 25 and 26: TABLE 1GAS CHROMATOGRAPHIC RETENTIO
Page 27 and 28: TABLE 3aFACTORS FOR DETERMINATION O
Page 29 and 30: TABLE 5GC OPERATING CONDITIONS FOR
Page 31 and 32: TABLE 6 (continued)RETENTION TIMES
Page 33 and 34: TABLE 8GC OPERATING CONDITIONS FOR
Page 35 and 36: TABLE 10ANALYTE RECOVERY FROM DICHL
Page 37 and 38: TABLE 12SINGLE LABORATORY ACCURACY
Page 39 and 40: FIGURE 2GAS CHROMATOGRAM OF INDIVID
Page 41 and 42: FIGURE 4GAS CHROMATOGRAM OF TOXAPHE
Page 43 and 44: FIGURE 6GAS CHROMATOGRAM OF ORGANOC

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