5.1 The extensive and widespread use of organochlorine pesticides and PCBs has resulted in their presence in all parts of the environment. These compounds are persistent and may have adverse effects on the environment. Thus, there is a need to identify and quantitate these compounds in water samples.1.1 This test method (1-3)2 is applicable to the determination of the following analytes in finished drinking water, drinking water during intermediate stages of treatment, and the raw source water: Analyte Chemical Abstract ServiceRegistry Number AAlachlor 5972-60-8  Aldrin 309-00-2  Chlordane 57-74-9  Dieldrin 60-57-1  Endrin 72-20-8  Heptachlor 76-44-8  Heptachlor Epoxide 1024-57-3  Hexachlorobenzene 118-74-1  Lindane 58-89-9  Methoxychlor 72-43-5  Toxaphene 8001-35-2  Aroclor B 1016 12674-11-2  Aroclor B 1221 11104-28-2  Aroclor B 1232 11141-16-5  Aroclor B 1242 53469-21-9  Aroclor B 1248 12672-29-6  Aroclor B 1254 11097-69-1  Aroclor B 1260 11096-82-5  (A) Numbering system of CAS Registry Services, P.O. Box 3343, Columbus, OH 43210-0334.(B) Aroclor is a registered trademark of Monsanto Co.1.2 Detection limits for most test method analytes are less than 1 μg/L. Actual detection limits are highly dependent on the characteristics of the sample matrix and the gas chromatography system. Table 1 contains the applicable concentration range for the precision and bias statements. Only Aroclor 1016 and 1254 were included in the interlaboratory test used to derive the precision and bias statements. Data for other PCB products are likely to be similar.(A) Bias = C − X.(B) X  = Mean recovery.(C) C = True concentration value.(D) St = Overall standard deviation.(E) So = Single analyst standard deviation.1.3 Chlordane, toxaphene, and Aroclor products (polychlorinated biphenyls) are multicomponent materials. Precision and bias statements reflect recovery of these materials dosed into water samples. The precision and bias statements may not apply to environmentally altered materials or to samples containing complex mixtures of polychlorinated biphenyls (PCBs) and organochlorine pesticides.1.4 For compounds other than those listed in 1.1 or for other sample sources, the analyst must demonstrate the applicability of this test method by collecting precision and bias data on spiked samples (groundwater, tap water) (4) and provide qualitative confirmation of results by gas chromatography/mass spectrometry (GC/MS) (5) or by GC analysis using dissimilar columns.1.5 This test method is restricted to use by or under the supervision of analysts experienced in the use of GC and in the interpretation of gas chromatograms. Each analyst must demonstrate the ability to generate acceptable results using the procedure described in Section 13.1.6 Analytes that are not separated chromatographically, (analytes that have very similar retention times) cannot be individually identified and measured in the same calibration mixture or water sample unless an alternative technique for identification and quantitation exists (see 13.4).1.7 When this test method is used to analyze unfamiliar samples for any or all of the analytes listed in 1.1, analyte identifications and concentrations should be confirmed by at least one additional technique.1.8 The values stated in SI units are to be regarded as standard. The values given in parentheses are mathematical conversions to inch-pound units that are provided for information only and are not considered standard.1.9 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use. For specific hazard statements, see Section 9.1.10 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

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1.1 This test method covers the determination of certain polychlorinated biphenyls (PCBs) including: Aroclors 1221, 1232, 1242, 1248, 1254, 1260, and 1016. 1.2 The detection limit is in the range from 0.1 to 0.5 [mu]g/L for Aroclor 1254 and 1260 when analyzing 1 L of water using an electron capture detector. The detection limit is compound dependent and is also determined by instrumental sensitivity and interferences present. When using a microcoulometric or conductivity detector, the detection limit is approximately 1.0 [mu]g/L. 1.3 Precision and bias statements reflect recovery of PCB products dosed into water samples. These statements may not apply to environmentally altered PCBs. 1.4 As the precision and bias statements given may apply only to waters used, it is the user's responsibility to ensure the validity of the test method for waters of untested matrices. 1.5 The values stated in SI units are to be regarded as the standard. The values given in parentheses are provided for information only. 1.6 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. For a specific hazard statement, see Note 2.

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5.1 Pesticides and PCBs are Environmental Protection Agency (EPA)-regulated contaminants in treated drinking water, wastewater, and ground water. Liquid-liquid and solid-phase extraction (SPE) are generally applicable procedures for extracting these target analytes before GC/MS/MS analysis.5.2 This test method is applicable to pesticides that are extracted from aqueous solution using methylene chloride and can be chromatographed and detected using tandem mass spectrometry procedures. Table 1 lists pesticides and Table 2 lists PCBs validated by this test method. This test method is not limited to the compounds listed in Table 1 or Table 2; however, the applicability of the test method to other compounds shall be demonstrated. Refer to Guide E2857 for guidance in validating the method for additional parameters.5.3 Analyte concentrations up to approximately 250 ng/L may be determined. Analytes that are inefficiently extracted from water will not be detected when present at low concentrations, but they can be measured with acceptable accuracy and precision when present in sufficient amounts.5.4 Analytes that are not separated chromatographically but that have different transitions can be identified and quantitatively measured.5.5 This test method may be used to determine the concentrations of Aroclor6 mixtures or PCB congeners, or both, present in the sample. See Appendix X1 and Appendix X2 for suggested transitions and collisional energies for all 209 congeners. Separation of all 209 congeners may not be possible and may require additional GC columns and operating conditions. Analysis of all congeners is not expected to be achieved by this test method.5.6 Method detection limits (MDL) and minimum reporting level (MRL) for analytes in Tables 1 and 2 are given in Table 3. These limits must be met if the method is used for National Pollutant Discharge Elimination System (NPDES) reporting.(A) Priority Pollutant listed in Table 1 of EPA Method 608.3.(B) Priority Pollutant listed in Table 2 of EPA Method 608.3.1.1 This test method covers the identification and simultaneous measurement of extractable chlorinated pesticides and polychlorinated biphenyls (PCBs) by gas chromatography/mass spectrometry/mass spectrometry (GC/MS/MS).1.2 This test method has been validated for wastewater influents, effluents, industrial discharges, surface water, and ground water.1.3 This test method is not limited to these particular aqueous matrices; however, the applicability of this test method to other aqueous matrices shall be demonstrated.1.4 This test method is restricted to use by or under the supervision of analysts experienced in the use of a gas chromatograph with tandem mass spectrometry. Each laboratory that uses this test method shall demonstrate the ability to generate results that meet or exceed the performance criteria of this test method.1.5 If sensitivity permits, compound tentative identification of unknowns may be made by analyzing the extract in full-scan mode or, if the system allows simultaneous timed single-reaction monitoring (SRM)/full-scan acquisition. Identify unknown peaks according to Guide D4128.1.6 This test method is performance-based. Minor modifications, as allowed by CFR 40 Part 136.6, may be made to improve the method performance, but changes may not be made to the extraction, the extraction solvent, sample-to-solvent ratio, or the MS/MS detection technique.1.7 Units—The values stated in SI units are to be regarded as the standard. No other units of measurement are included in this standard.1.8 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.1.9 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

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5.1 This test method provides sufficient PCB data for many regulatory requirements. While the most common regulatory level is 50 ppm (dry weight corrected), lower limits are used in some locations. Since sensitivities will vary for different types of samples, one shall demonstrate a sufficient method detection limit for the matrix of interest.5.2 This test method differs from Test Method D4059 in that it provides for more sample clean-up options, utilizes a capillary column for better pattern recognition and interference discrimination, and includes both a qualitative screening and a quantitative results option.1.1 This test method2 covers a two-tiered analytical approach to PCB screening and quantitation of liquid and solid wastes, such as oils, sludges, aqueous solutions, and other waste matrices.1.2 Tier I is designed to screen samples rapidly for the presence of PCBs.1.3 Tier II is used to determine the concentration of PCBs, typically in the range of from 2 mg/kg to 50 mg/kg. PCB concentrations greater than 50 mg/kg are determined through analysis of sample dilutions.1.4 This is a pattern recognition approach, which does not take into account individual congeners that might occur, such as in reaction by-products. This test method describes the use of Aroclors3 1016, 1221, 1232, 1242, 1248, 1254, 1260, 1262, and 1268, as reference standards, but others could also be included. Aroclors 1016 and 1242 have similar capillary gas chromatography (GC) patterns. Interferences or weathering are especially problematic with Aroclors 1016, 1232, and 1242 and may make distinction between the three difficult.1.5 This test method provides sample clean up and instrumental conditions necessary for the determination of Aroclors. Gas chromatography (GC) using capillary column separation technique and electron capture detector (ECD) are described. Other detectors, such as atomic emission detector (AED) and mass spectrometry (MS), may be used if sufficient performance (for example, sensitivity) is demonstrated. Further details about the use of GC and ECD are provided in Practices E355, E697, and E1510.1.6 Quantitative results are reported on the dry weights of waste samples.1.7 Quantification limits will vary depending on the type of waste stream being analyzed.1.8 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.1.9 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.1.10 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

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5.1 This practice is recommended for use primarily for non-occupational exposure monitoring in domiciles, public access buildings, and offices.5.2 The methods described in this practice have been successfully applied to measurement of pesticides and PCBs in outdoor air and for personal respiratory exposure monitoring.5.3 A broad spectrum of pesticides are commonly used in and around the house and for insect control in public and commercial buildings. Other semivolatile organic chemicals, such as PCBs, are also often present in indoor air, particularly in large office buildings. This practice promotes needed precision and bias in the determination of many of these airborne chemicals.1.1 This practice covers the sampling of air for a variety of common pesticides and polychlorinated biphenyls (PCBs) and provides guidance on the selection of appropriate analytical measurement methods. Other compounds such as polychlorinated dibenzodioxins/furans, polybrominated biphenyls, polybrominated diphenyl ethers, polycyclic aromatic hydrocarbons, and polychlorinated naphthalenes may be efficiently collected from air by this practice, but guidance on their analytical determination is not covered by this practice.1.2 The sampling and analysis of PCBs in air can be more complicated than sampling PCBs in solid media (for example, soils, building materials) or liquids (for example, transformer fluids). PCBs in solid or liquid material are typically analyzed using Aroclor2 distillation groups in chromatograms. In contrast, recent research has shown that analysis of PCBs in air samples by GC-ECD has also been found to exhibit potential uncertainties due to changes in the PCB patterns, differences in responses in distillation groups, peak co-elutions and differences in response factors within a homolog group (1, 2).3 As such it is recommended that PCBs in air not be quantified using AroclorTM distillation groups. In addition, it is recommended that analysis of PCBs in air be done using GC-MS rather than GC-ECD. Any mention, to outdated practices for “Aroclor” and GC-ECD analysis of PCBs herein are retained solely for historical perspective.1.3 A complete listing of pesticides and other semivolatile organic chemicals for which this practice has been tested is shown in Table 1.1.4 This practice is based on the collection of chemicals from air onto polyurethane foam (PUF) or a combination of PUF and granular sorbent (for example, diphenyl oxide, styrene-divinylbenzene), or a granular sorbent alone.1.5 This practice is applicable to multicomponent atmospheres, 0.001 μg/m3 to 50 μg/m3 concentrations, and 4 h to 24 h sampling periods. The limit of detection will depend on the nature of the analyte and the length of the sampling period.1.6 The analytical method(s) recommended will depend on the specific chemical(s) sought, the concentration level, and the degree of specificity required.1.7 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.1.8 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use. For specific hazards statements, see 10.24 and A1.1.1.9 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

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5.1 United States governmental regulations mandate that electrical apparatus and electrical insulating fluids containing PCB be handled and disposed of through specific procedures. The procedure to be used for a particular apparatus or quantity of insulating fluid is determined by the PCB content of the fluid. The results of this analytical technique can be useful in selecting the appropriate handling and disposal procedure.5.2 Quantification in this technique requires a peak-by-peak comparison of the chromatogram of an unknown specimen with that of standard Aroclor test specimens obtained under identical conditions. The amount of PCB producing each peak in the standard chromatogram shall be known independently.5.3 The technique described is based on data for standard chromatograms of Aroclors 1242, 1254, and 1260 obtained using specific chromatographic column packing materials and operating conditions.4 Relevant chromatograms are reproduced in Fig. 1, Fig. 2, and Fig. 35, for isothermal packed columns and in Figs. X4.1 through X4.3) for temperature programmed mega-bore capillary columns. Each peak is identified by its retention time relative to that of a standard. The types and amounts of PCB associated with each peak have been determined by mass spectroscopy and are given in Table 1, Table 2, and Table 3.4 Other chromatographic operating conditions, and in particular, other column packing materials, may give different separations. The data given in the tables should not be used if chromatograms of the standards differ significantly from those shown in the figures. The peaks in such standard chromatograms shall be independently identified and quantified.5.4 Different isomers of PCB with the same number of chlorine substituents can cause substantially different responses from EC detectors. Mixtures of PCB containing the same amount of PCB, but with a different ratio of isomers, can give quite different chromatograms. This technique is effective only when the standard PCB mixtures and those found in the unknown test specimen are closely related. Aroclors 1242, 1254, and 1260 are adequate standards because they have been found to be the most common PCB contaminant in electrical insulating oils.1.1 This test method describes a quantitative determination of the concentration of polychlorinated biphenyls (PCBs) in electrical insulating liquids by gas chromatography. It also applies to the determination of PCB present in mixtures known as askarels, used as electrical insulating liquids.1.2 The PCB mixtures known as Aroclors2 were used in the formulation of the PCB-containing askarels manufactured in the United States. This test method may be applied to the determination of PCBs in insulating liquids contaminated by either individual Aroclors or mixtures of Aroclors. This technique may not be applicable to the determination of PCBs from other sources of contamination.1.3 The precision and bias of this test method have been established only for PCB concentrations in electrical insulating mineral oils and silicones. The use of this test method has not been demonstrated for all insulating fluids. Some insulating liquids, such as halogenated hydrocarbons, interfere with the detection of PCBs and cannot be tested without pretreatment.1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.1.5 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.1.6 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

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