5.1 This test method has been developed by the U.S. EPA Region 5 Chicago Regional Laboratory (CRL). 5.2 PFAS are widely used in various industrial and commercial products; they are persistent, bio-accumulative, and ubiquitous in the environment. PFAS have been reported to exhibit developmental toxicity, hepatotoxicity, immunotoxicity, and hormone disturbance. A draft Toxicological Profile for Perfluoroalkyls from the U.S. Department of Health and Human Services is available.7 PFAS have been detected in soils, sludges, and surface and drinking waters. Hence, there is a need for a quick, easy, and robust method to determine these compounds at trace levels in various soil matrices for understanding of the sources and pathways of exposure. 5.3 This method has been used to determine selected PFAS in sand (Table 4) and four ASTM reference soils (Table 5). 1.1 This procedure covers the determination of selected polyfluorinated alkyl substances (PFAS) in a soil matrix using solvent extraction, filtration, followed by liquid chromatography (LC) and detection with tandem mass spectrometry (MS/MS). These analytes are qualitatively and quantitatively determined by this method. This method adheres to multiple reaction monitoring (MRM) mass spectrometry. This procedure utilizes a quick extraction and is not intended to generate an exhaustive accounting of the content of PFAS in difficult soil matrices. An exhaustive extraction procedure for PFAS, such as published by Washington et al.,2 for difficult matrices should be considered when analyzing PFAS. The approach from this standard was utilized to screen laboratory coats (textiles) to identify if PFAS would be leached from the materials. 1.2 Units—The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard. 1.3 The method of detection limit3 and reporting range4 for the target analytes are listed in Table 1. 1.3.1 The reporting limit in this test method is the minimum value below which data are documented as non-detects. Analyte detections between the method detection limit and the reporting limit are estimated concentrations and are not reported following this test method. In most cases, the reporting limit is calculated from the concentration of the Level 1 calibration standard as shown in Table 2 for the PFAS after taking into account a 2 g sample weight and a final extract volume of 10 mL, 50 % water/50 % MeOH with 0.1 % acetic acid. The final extract volume is assumed to be 10 mL because 10 mL of 50 % water/50 % MeOH with 0.1 % acetic acid was added to each soil sample and only the liquid layer after extraction is filtered, leaving the solid and any residual solvent behind. It is raised above the Level 1 calibration concentration for PFOS, PFHxA, FHEA, and FOEA; these compounds can be identified at the Level 1 concentration but the standard deviation among replicates at this lower spike level resulted in a higher reporting limit. 1.4 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. 1.5 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 Nitrosamines are a class of nitrogen-containing compounds with a known occurrence in wastewater. They may also be created in deionization and are a potential contaminant in water for reuse. The World Health Organization has issued a guideline for NDMA in drinking water at 0.1 µg/L. NDMA may occur in chlorinated effluents and other wastewaters. Other methods for nitrosamines employ solid phase extraction, which may not be applicable to wastewaters that contain particulate matter or a high organic load. This method analyses nitrosamines directly using LC-MS/MS.1.1 This test method covers the liquid chromatography tandem mass spectrometry (LC-MS/MS) detection and quantitation of N-nitrosamines after direct injection. It has been validated for groundwater, surface water, wastewater influents, and wastewater effluents. This test method is not limited to these aqueous matrices; however, the applicability of this test method to other aqueous matrices must be demonstrated.1.2 This test method is applicable to nitrosamines that can be chromatographed and detected using a mass spectrometry procedure. Table 1 lists the compounds that have been validated for this test method. This test method is not limited to the compounds listed in Table 1; however, the applicability of the test method to other compounds must be demonstrated.1.3 Analyte concentrations from 0.05 µg/L up to approximately 5 µg/L may be determined without dilution of the sample. Analytes with insufficient sensitivity will not be detected, but they can be measured with acceptable accuracy and precision when present in sufficient amounts. In addition, newer instruments, or instruments of improved sensitivity may be used to lower detection limits.1.4 Analytes that are not separated chromatographically, but that have different mass spectra and noninterfering quantitation ions, can be identified and measured in the same calibration mixture or water sample. Analytes that have very similar product ions cannot be individually identified and measured in the same calibration mixture or water sample unless they have different retention times.1.5 It is the responsibility of the user to ensure the validity of this test method for untested matrices.1.6 This test method is restricted to use by or under the supervision of analysts experienced in the use of a liquid chromatograph with tandem mass spectrometry (LC-MS/MS).1.7 Depending on data usage, you may modify this test method but limit to modifications that improve performance while still meeting method quality acceptance criteria. Shortening the chromatographic run simply to save time is not allowed. Use Practice E2935 or similar statistical tests to confirm that modifications produce equivalent results on non-interfering samples. In addition, use Guide E2857 or equivalent statistics to re-validate the modified test.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 DOSS is an anionic detergent that is approved by the United States Food and Drug Administration (U.S. FDA) and is used widely as a laxative, emulsifying, solubilizing, and dispersing agent, and is used in the cosmetic industry.4 DOSS may also be used as a dispersing agent to treat oil. DOSS may be released into the environment at levels that may be harmful to aquatic life. The U.S. EPA aquatic life benchmark for DOSS is 40 ppb.55.2 This test method has been investigated for use with reagent and sea water.1.1 This test method covers the determination of dioctyl sulfosuccinate (DOSS) in sea water by direct injection using liquid chromatography (LC) and detection with tandem mass spectrometry (MS/MS). This analyte is qualitatively and quantitatively determined by this test method. This test method adheres to selected reaction monitoring (SRM) mass spectrometry.1.2 The detection verification level (DVL) and reporting range for DOSS are listed in Table 1.1.2.1 The DVL is required to be at a concentration at least 3 times below the reporting limit (RL) and have a signal/noise ratio greater than 3:1. Fig. 1 and Fig. 2 display the signal/noise ratio of the selected reaction monitoring (SRM) transition.FIG. 1 Detection Verification Level Signal/Noise RatioFIG. 2 Reporting Level Signal/Noise Ratio1.2.2 The reporting limit is the concentration of the Level 1 calibration standard as shown in Table 5 for DOSS, taking into account the 50 % sample preparation dilution factor.1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.1.4 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.1.5 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 is a performance-based method, and modifications are allowed to improve performance.5.1.1 Due to the rapid development of newer instrumentation and column chemistries, changes to the analysis described in this standard are allowed as long as better or equivalent performance data result. Any modifications shall be documented and performance data generated. The user of the data generated by this standard shall be made aware of these changes and given the performance data demonstrating better or equivalent performance.5.2 TDG is a Schedule 2 compound under the Chemical Weapons Convention (CWC).6 Schedule 2 chemicals include those that are precursors to chemical weapons, chemical weapons agents, or have a number of other non-military commercial uses. Schedule 2 chemicals can also be found in applications unrelated to chemical weapons. These chemicals are used as ingredients to produce insecticides, herbicides, lubricants, and some pharmaceutical products. TDG is a mustard gas precursor and a degradant as well as an ingredient in water-based inks, ballpoint pen inks, dyes, and some pesticides.5.3 This method has been investigated for use on surface wipes. TDG is also a human metabolite resulting from sulfur mustard exposure but this method has not been investigated for such determinations.1.1 This procedure details the determination of thiodiglycol (TDG), also known as 2,2’-thiobis-ethanol, on wipes with 3,3’-thiodipropanol (TDP) as the surrogate. This method is based upon solvent extraction of wipes by either sonication or a pressurized fluid extraction (PFE) technique as an alternative option. The extract is filtered, concentrated, and analyzed by liquid chromatography/tandem mass spectrometry (LC/MS/MS). TDG is qualitatively and quantitatively determined.1.2 Units—The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.1.3 The method detection limit (MDL)2 and reporting range3 for TDG are listed in Table 1.1.4 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.1.5 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 has been developed by U.S. EPA Region 5 Chicago Regional Laboratory (CRL).5.2 Bromadiolone, brodifacoum, diphacinone and warfarin are rodenticides for controlling mice, rats, and other rodents that pose a threat to public health, critical habitats, native plants and animals, crops, food and water supplies. These rodenticides also present human and environmental safety concerns. Warfarin and diphacinone are first-generation anticoagulants, while bromadiolone and brodifacoum are second-generation. The anticoagulants interfere with blood clotting, and death can result from excessive bleeding. The second-generation anticoagulants are especially hazardous for several reasons. They are highly toxic and persist a long time in body tissues. The second-generation anticoagulants are designed to be toxic in a single feeding, but time-to-death occurs in several days. This allows rodents to feed multiple times before death, leading to carcasses containing residues that may be many times the lethal dose.45.3 This test method has been investigated for use with reagent, surface, and drinking water for the selected rodenticides.1.1 This test method covers the determination of bromadiolone, brodifacoum, diphacinone and warfarin (referred to collectively as rodenticides in this test method) in water by direct injection using liquid chromatography (LC) and detected with tandem mass spectrometry (MS/MS). These analytes are qualitatively and quantitatively determined by this test method. This test method adheres to multiple reaction monitoring (MRM) mass spectrometry.1.2 The Detection Verification Level (DVL) and Reporting Range for the rodenticides are listed in Table 1.1.2.1 The DVL is required to be at a concentration at least 3 times below the Reporting Limit (RL) and have a signal/noise ratio greater than 3:1. Fig. 1 displays the signal/noise ratios of the primary single reaction monitoring (SRM) transitions, and Fig. 2 displays the confirmatory SRM transitions at the DVLs for the rodenticides.1.2.2 The reporting limit was calculated from the concentration of the Level 1 calibration standard, as shown in Table 4, accounting for the dilution of a 40 mL water sample up to a final volume of 50 mL with methanol to ensure analyte solubility.1.3 Units—The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.1.4 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.1.5 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 developed for the analysis of TPs in soil and sediment samples is based upon an LC/MS/MS analysis. Any type of coupled liquid chromatography/mass spectrometry system may be used that meets the study objectives of the individual project. These may include, but are not limited to: trap, single quadrupoles, time-of-flight, high resolution, and others not mentioned here. 5.2 The MDL and reporting range for TPs are listed in Table 1. This SOP has been tested on Ottawa sand, four ASTM soil types, biosolid sample, and one commercial soil. The P&A QC acceptance criteria are listed in Table 3. Tables 4-17 display the TC and surrogate recoveries in the various soil types. 40 CFR Part 136, Appendix B was used as a guide to determine the MDLs. The 40 CFR Part 136 MDL criteria were not met for NP2EO; this does not affect the method because the SOP only reports to the RL and is not a regulatory method. All site sample results are not reported below the RL using this method. RLCS concentrations may be reported below the RL because they are spiked at or near the RL. (A) Uncertainty calculation based upon 95 % confidence interval and a two-tailed Student t distribution. Uncertainty = Student t Value [(standard deviation) / (number of LCS)1/2]. (A) P&A values are after subtraction of average of MB if ≥RL. (A) P&A values are after subtraction of average of MB if ≥RL. (A) 5.3 The RL for a specific soil sample may differ from that listed depending on the nature of the interferences in the sample matrix. Variability in historical LCS spike recovery may be used to estimate uncertainty. The estimate of minimum laboratory contribution to measurement uncertainty of this test method for each analyte is listed in Table 3. These values are derived from P&A samples from the initial IDOC study for this test method. The uncertainty will be greater near the RL and much greater near the DL. Also, uncertainty estimated based on variability in LCS recovery is conservative because some sources of variability are not included, such as subsample variability and matrix analyte recovery. This SOP covers multiple soil matrices and the uncertainty among the various matrices is variable. 1.1 This test method covers analysis of nonylphenol (NP), nonylphenol monoethoxylate (NP1EO), nonylphenol diethoxylate (NP2EO), octylphenol (OP), and bisphenol A (BPA), referred to collectively as target phenols (TPs), in soil, sediments, and biosolids by extraction with acetone, filtration, dilution with water, and analysis by liquid chromatography/tandem mass spectrometry. The sample extracts are prepared in a solution of 75 % acetone and 25 % water because TPs have an affinity for surfaces and particles that is more pronounced at lower concentrations. The range of applicability of the test method is shown in Table 1. The method may be extended outside of these ranges depending on additional performance studies not undertaken here. 1.2 Units—The values stated in SI units are to be regarded as the standard. No other units of measurement are included in this standard. 1.3 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. 1.4 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 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 PFASs are widely used in various industrial and commercial products; they are persistent, bio-accumulative, and ubiquitous in the environment. PFASs have been reported to exhibit developmental toxicity, hepatotoxicity, immunotoxicity, and hormone disturbance. A draft Toxicological Profile for Perfluoroalkyls from the U.S. Department of Health and Human Services is available.6 PFASs have been detected in soils, sludges, surface, and drinking waters. Hence, there is a need for quick, easy, and robust method to determine these compounds at trace levels in water matrices for understanding of the sources and pathways of exposure.5.2 This test method has been investigated for use with reagent, surface, sludge and wastewaters for selected PFASs. This test method has not been evaluated on drinking water matrices.1.1 This procedure covers the determination of selected per- and polyfluoroalkyl substances (PFASs) in a water matrix using liquid chromatography (LC) and detection with tandem mass spectrometry (MS/MS). These analytes are qualitatively and quantitatively determined by this test method. This test method adheres to a technique known as selected reaction monitoring (SRM) or sometimes referred to as multiple reaction monitoring (MRM). This is not a drinking water method; performance of this test method has not been evaluated on drinking water matrices.1.2 The method detection limit (MDL)2 and reporting range3 for the target analytes are listed in Table 1. The target concentration for the reporting limit for this test method was 10 ng/L for most of the target analytes at the time of development.1.2.1 The reporting limit in this test method is the minimum value below which data are documented as non-detects. The reporting limit may be lowered providing your lab meets the minimum performance requirements of this test method at the lower concentrations, this test method is performance based and modifications are allowed to improve performance. Analyte detections between the method detection limit and the reporting limit are estimated concentrations and are not reported following this test method. In most cases, the reporting limit is the concentration of the Level 1 calibration standard as shown in Table 4 for the PFASs after taking into account the 50 % dilution with methanol. It is above the Level 1 calibration concentration for FHEA and FOEA, these compounds can be identified at the Level 1 concentration but the standard deviation among replicates at this lower spike level resulted in a higher reporting limit.1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.1.4 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.1.5 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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