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5.1 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. PFAS have been detected in soils, sludges, surface, and drinking waters. This is a quick, easy, and robust method to quantitatively determine these compounds at trace levels in soil/biosolid matrices.5.2 This test method has been validated using four ASTM reference soils (CH-1, ML-1, CL-1, and SP-1). ASTM reference soil CH-1 is Fat Clay (CH)—Vicksburg Buckshot Clay; ASTM reference soil ML-1 is silt (ML)—Vicksburg silt; ASTM reference soil CL-1 is lean clay (CL)—Annapolis clay; and ASTM reference soil SP-1 is sand (SP)—Frederick sand and four biosolids (Missouri, California, Idaho, and Georgia). Refer to the Precision and Bias (Section 17).1.1 This test method covers the determination of per- and polyfluoroalkyl substances (PFAS) in soil/biosolid matrices by solvent extraction, filtering, separation using liquid chromatography (LC), and detection with tandem mass spectrometry (MS/MS). These analytes are extracted from soil/biosolids with basic water and methanol then qualitatively and quantitatively determined by this test method. Quantitation is by selected reaction monitoring (SRM), sometimes referred to as multiple reaction monitoring (MRM).1.2 The reporting limit (RL) and reporting range (see Note 2) for the target analytes are listed in Table 1. The reporting limit is calculated from the concentration of the Level 1 calibration standard as shown in Table 5 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. Sporadic PFAS hits due to PFAS contamination in consumables/collection tools used during sample collection and preparation is possible while executing this standard and must be monitored. All samples should be taken at a minimum as duplicates in order to compare the precision between the two prepared samples to help ensure the concentration/positive result is reliable.NOTE 1: This standard only includes the determination of the analytes listed in Table 1 and is only applicable to soil and biosolid matrices; any added compost or soil additives may contain PFAS that may be bound and not able to be determined by this method. Analysis of packaging materials and polymeric PFAS moieties are not amenable to this standard.NOTE 2: Injection volume variations and sensitivity of the instrument used will change the reporting limit and ranges.1.2.1 Recognizing continual advancements in the sensitivity of instrumentation, advancements in column chromatography, and other processes not recognized here, the reporting limit may be lowered assuming the minimum performance requirements of this test method at the lower concentrations are met.1.2.2 Depending on data usage, you may modify this test method but limit to modifications that improve performance while still meeting or exceeding the method quality acceptance criteria. Modifications to the solvents, ratio of solvent to sample, or shortening the chromatographic run simply to save time are 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 revalidate the modified test.1.2.3 Analyte detections under the reporting limit are estimated concentrations. If results are to be reported below the RL using this standard and following the method detection limit procedure in 40 CFR Part 136 Appendix B, data shall be qualified estimated and extra caution must be taken to evaluate and identify false positives.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 Separation and identification of stabilizers used in the manufacture of polypropylene is necessary in order to correlate performance properties with polymer composition. This test method provides a means to determine erucamide slip, Vitamin E, Irgafos 168, Irganox 3114, Irganox 1010, and Irganox 1076 levels in polypropylene samples. This test method is also applicable for the determination of other antioxidants, such as Ultranox 626, Ethanox 330, Santanox R, and BHT, but the applicability of this test method has not been investigated for these antioxidants.5.2 The additive-extraction procedure is made effective by the insolubility of the polymer sample in solvents generally used for liquid chromatographic analysis.5.3 Under optimum conditions, the lowest level of detection for a phenolic antioxidant is approximately 2 ppm.NOTE 2: Other methods that have been used successfully to remove additives from the plastics matrix include thin film, microwave, ultrasonic, and supercritical fluid extractions. Other methods have been used successfully to separate additives including SFC and capillary GC.5.4 Irgafos 168 is a phosphite antioxidant. Phosphites are known to undergo both oxidation and hydrolysis reactions. Less Irgafos 168 will be determined in the polymer when oxidation occurs during processing. The HPLC separation is capable of separating the phosphite, phosphate (oxidation product), and hydrolysis product and quantify them if standards are obtained. No significant breakdown of the phosphite antioxidant has been seen due to either extraction technique or the separation presented in this standard.1.1 This test method covers a liquid-chromatographic procedure for the separation of some additives currently used in polypropylene. These additives are extracted with a cyclohexane:methylene chloride mixture using either reflux or ultrasonic bath prior to liquid-chromatographic separation. The ultraviolet absorbance (200 nm) of the compound(s) is measured, and quantitation is performed using the internal standard method.1.2 The values stated in SI units are to be regarded as 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. Specific precautionary statements are given in Section 9.NOTE 1: There is no known ISO equivalent to this test method.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 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 has been developed by U.S. EPA Region 5 Chicago Regional Laboratory (CRL).5.2 The N-methyl carbamate (NMC) pesticides: aldicarb, carbofuran, methomyl, oxamyl, and thiofanox have been identified by EPA as working through a common mechanism. These affect the nervous system by reducing the ability of enzymes. Enzyme inhibition was the primary toxicological effect of regulatory concern to EPA in assessing the NMC’s food, drinking water, and residential risks. In most of the country, NMC residues in drinking water sources are at levels that are not likely to contribute substantially to the multi-pathway cumulative exposure. Shallow private wells extending through highly permeable soils into shallow, acidic ground water represent what the EPA believes to be the most vulnerable drinking water. Aldicarb sulfone and aldicarb sulfoxide are breakdown products of aldicarb and should also be monitored due to their toxicological effects.45.3 This test method has been investigated for use with reagent, surface, and drinking water for the selected carbamates: aldicarb, aldicarb sulfone, aldicarb sulfoxide, carbofuran, methomyl, oxamyl, and thiofanox.1.1 This test method covers the determination of aldicarb, aldicarb sulfone, aldicarb sulfoxide, carbofuran, methomyl, oxamyl, and thiofanox (referred to collectively as carbamates 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 carbamates 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 carbamates.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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Separation and identification of stabilizers used in the manufacture of linear low-density polyethylene are necessary in order to correlate performance properties with polymer composition. This test method provides a means to determine BHT, BHEB, Isonox 129, erucamide slip, Irganox 1010, and Irganox 1076 levels in linear low-density polyethylene samples. This test method should be applicable for the determination of other antioxidants such as Ultranox 626, Ethanox 330, Santanox R, and Topanol CA, but the applicability of this test method has not been investigated for these antioxidants.The additive extraction procedure is made effective by the insolubility of the polymer sample in solvents generally used for liquid chromatographic analysis.Under optimum conditions, the lowest level of detection for a phenolic antioxidant is approximately 2 ppm.Other methods that have been successfully used to remove additives from the plastics matrix include thin film, microwave, ultrasonic, and supercritical fluid extractions. Other methods have been successfully used to separate additive including SFC and GC.1.1 This test method covers a liquid-chromatographic procedure for the separation of some additives currently used in linear low-density polyethylene. These additives are extracted with either isobutanol or isopropanol prior to liquid-chromatographic separation. The ultraviolet absorbance (200 nm) of the compound(s) is measured; quantitation is performed using the internal standard method.1.2 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. Specific precautionary statements are given in Section 9.Note 1—There is no equivalent ISO standard.

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5.1 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. PFAS have been detected in soils, sludges, surface, and drinking waters. This is a quick, easy, and robust method to quantitatively determine these compounds at trace levels in water matrices.5.2 This test method has been validated using reagent water and waters from sites that include landfill leachate, metal finisher, POTW Effluent, Hospital, POTW Influent, Bus washing station, Power Plant and Pulp and paper mill effluent for selected PFAS, refer to the Precision and Bias (Section 17).1.1 This test method covers the determination of per- and polyfluoroalkyl substances (PFASs) in aqueous matrices using liquid chromatography (LC) and detection with tandem mass spectrometry (MS/MS). These analytes are co-solvated by a 1+1 ratio of sample and methanol then qualitatively and quantitatively determined by this test method. Quantitation is by selected reaction monitoring (SRM) or sometimes referred to as multiple reaction monitoring (MRM).1.2 The method detection limit (MDL) (see Note 1) and reporting range (see Note 2) for the target analytes are listed in Table 1. The target concentration for the reporting limit for this test method is an integer value that is calculated from the concentration from the lowest standard from the final volume of the prepared sample. This value may be lower than the calculated MDL due to sporadic PFAS hits due to PFAS contamination in consumables/collection tools used during sample collection and preparation. All samples should be taken at a minimal as duplicates in order to compare the precision between the two prepared samples to help ensure the concentration/positive result is reliable.NOTE 1: The MDL is determined following the Code of Federal Regulations (CFR), 40 CFR Part 136, Appendix B utilizing dilution and filtration. A detailed process determining the MDL is explained in the reference and is beyond the scope of this test method.NOTE 2: Injection volume variations, and sensitivity of the instrument used will change the reporting limit and ranges.1.2.1 Recognizing continual advancements in the sensitivity of instrumentation, advancements in column chromatography and other processes not recognized here, the reporting limit may be lowered assuming the minimum performance requirements of this test method at the lower concentrations are met.1.2.2 Depending on data usage, you may modify this test method but limit to modifications that improve performance while still meeting or exceeding the method quality acceptance criteria. Modifications to the solvents, ratio of solvent to sample, or shortening the chromatographic run simply to save time are 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.1.2.3 Analyte detections between the method detection limit and the reporting limit are estimated concentrations. The reporting limit is based upon the concentration of the Level 1 calibration standard as shown in Table 5.1.3 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 The crystallinity of petroleum coke, as reflected by the Lc value, is a general measure of quality affecting suitability for end use and is a function of the heat treatment.5.2 The crystallite thickness is used to determine the extent of such heat treatment, for example, during calcination. The value of the Lc determined is not affected by coke microporosity or the presence of foreign, non-crystalline materials such as dedust oil.1.1 This test method covers the determination of the mean crystallite thickness of a representative, pulverized sample of calcined petroleum coke by interpretation of a X-ray diffraction pattern produced through conventional X-ray scanning techniques.1.2 Calcined petroleum coke contains crystallites of different thicknesses. This test method covers the determination of the average thickness of all crystallites in the sample by empirical interpretation of the X-ray diffraction pattern. The crystallite diameter (La) is not determined by this test method.1.3 The values stated in SI (metric) units are to be regarded as the standard. The inch-pound units given in parentheses are provided for information purposes only.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 DPGBE and EGBE have a variety of residential and industrial applications such as cleaning formulations, surface coatings, inks, and cosmetics. These analytes may be released into the environment at levels that may be harmful to aquatic life.5.2 This test method has been investigated for use with reagent and sea water.1.1 This test method covers the determination of dipropylene glycol monobutyl ether (DPGBE) and ethylene glycol monobutyl ether (EGBE) in sea water by direct injection 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 selected reaction monitoring (SRM) mass spectrometry.1.2 The detection verification level (DVL) and reporting range for DPGBE and EGBE 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 single reaction monitoring (SRM) transition.FIG. 1 Detection Verification Level Signal/Noise RatioFIG. 2 Reporting Level (Calibration Standard) Signal/Noise Ratio1.2.2 The reporting limit is the concentration of the Level 1 calibration standard as shown in Table 4 for DPGBE and EGBE, taking into account the 20 % 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 test method has been developed by the U.S. EPA Region 5 Chicago Regional Laboratory (CRL).5.2 TTPC may be used in various industrial and commercial products for use as a biocide. Products containing TTPC have been approved for controlling algal, bacterial, and fungal slimes in industrial water systems.2 TTPC should not be persistent in water but may be deposited in sediments at concentrations of concern. Hence, there is a need for quick, easy, and robust method to determine TTPC concentration at trace levels in various soil matrices for understanding the sources and concentration levels in affected soils and sediments.5.3 This method has been used to determine TTPC in sand, a commercial top soil, and four ASTM reference soils (Table 4).1.1 This procedure covers the determination of (Tri-n-butyl)-n-tetradecylphosphonium chloride (TTPC) in a soil matrix by extraction with acetone, filtration, dilution with water, and analysis by liquid chromatography/tandem mass spectrometry. TTPC is a biocide that strongly adsorbs to soils.2 The sample extracts are prepared in a solution of 75 % acetone and 25 % water because TTPC has an affinity for surfaces and particles. The reporting range for this method is from 250 to 10 000 ng/kg. This analyte is qualitatively and quantitatively determined by this method. This method adheres to multiple reaction monitoring (MRM) mass spectrometry.1.2 The method detection limit (Note 1) (MDL) and reporting range (Note 2) for the target analyte are listed in Table 1.NOTE 1: The MDL is determined following the Code of Federal Regulations, 40 CFR Part 136, Appendix B, as a guide utilizing solvent extraction of soil. Two-gram sample of Ottawa sand was utilized. A detailed process determining the MDL is explained in the reference and is beyond the scope of this standard to be explained here.NOTE 2: Reporting range concentration is calculated from Table 2 concentrations assuming a 50-μL injection of the Level 1 calibration standard for TTPC, and the highest level calibration standard with a 20-mL final extract volume of a 2-g soil sample. Volume variations will change the reporting limit and ranges.1.2.1 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. The reporting limit is calculated from the concentration of the Level 1 calibration standard as shown in Table 2 for TTPC after taking into account a 2-g sample weight and a final extract volume of 20 mL in 75 % acetone/25 % water. The final extract volume is 20 mL because a 15-mL volume of acetone is added to each soil sample and only the liquid layer after extraction is filtered leaving the solid behind followed by the addition of 5 mL of water to the acetone extract.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.

定价: 646元 / 折扣价: 550 加购物车

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5.1 This practice has been developed in support of the U.S. EPA Office of Water, Office of Science and Technology by the Chicago Regional Laboratory (CRL).5.2 Nonylphenol (NP) and Octylphenol (OP) have been shown to have toxic effects in aquatic organisms. The prominent source of NP and OP is from common commercial surfactants which are longer chain APEOs. The most widely used surfactant is nonylphenol polyethoxylate (NPnEO) which has an average ethoxylate chain length of nine. The APEOs are readily biodegraded to form NP1EO, NP2EO, nonylphenol carboxylate (NPEC) and NP. NP will also biodegrade, but may be released into environmental waters directly at trace levels. This practice screens for the longer chain APEOs which may enter the STP at elevated levels and may cause a STP to violate its permitted discharge concentration of nonylphenol.1.1 This practice covers the determination of nonylphenol polyethoxylates (NPnEO, 3 ≤ n ≤ 18) and octylphenol polyethoxylates (OPnEO, 2 ≤ n ≤ 12) in water by Single Reaction Monitoring (SRM) Liquid Chromatography/ Tandem Mass Spectrometry (LC/MS/MS) using direct injection liquid chromatography (LC) and detected with tandem mass spectrometry (MS/MS) detection. This is a screening practice with qualified quantitative data to check for the presence of longer chain ethoxylates in a water sample.1.1.1 All data are qualified because neat standards of each alkylphenol ethoxylate (APEO) are not available and the synthesis and characterization of these neat standards would be very expensive. The Igepal2 brand standards, which contain a mixture of various chain lengths of the alkylphenol ethoxylates (APEOs), were used. The mixture was characterized in-house assuming the instrument response at an optimum electrospray ionization cone and collision voltage for each APEO was the same. This assumption, which may not be accurate, is used to determine qualified amounts of each ethoxylate in the standards. The n-Nonylphenol diethoxylate (n-NP2EO) surrogate was available as a neat characterized standard, therefore, this concentration and recovery data was not estimated. APEOs are not regulated by the EPA, but nonylphenol, a breakdown product of NPnEOs, is regulated for fresh and saltwater dischargers. A request by a sewage treatment plant (STP) was made to make this practice available through ASTM in order to screen for the influent or effluent from sources of APEOs coming into the STP. The interest lies in stopping the source of the longer chain APEOs from entering the STP in order to meet effluent guidelines. Based upon the above, this is a practice rather than a test method. A comparison between samples is possible using this practice to determine which has a higher concentration of APEOs.1.2 Units—The values stated in SI units are to be regarded as standard. No other units of measurement are included in this practice.1.3 The estimated screening range shown in Table 1 was calculated from the concentration of the Level 1 and 7 calibration standards shown in Table 4. These numbers are qualified, as explained in Section 1, and must be reported as such. Figs. 1-5 show the SRM chromatograms of each analyte at the Level 1 concentration with the signal to noise (S/N) ratio. This is a screening practice and method detection limits are not given. The S/N ratio for each analyte at the Level 1 concentration must be at least 5:1 for adequate sensitivity. If the instrument can not meet the criteria, the screening limit must be raised to an acceptable level.FIG. 1 SRM Chromatograms NP3EO-NP8EOFIG. 2 SRM Chromatograms NP9EO-NP14EOFIG. 3 SRM Chromatograms NP15EO-NP18EO and n-NP2EOFIG. 4 SRM Chromatograms OP2EO-OP7EOFIG. 5 SRM Chromatograms OP8EO-OP12EO1.4 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.

定价: 646元 / 折扣价: 550 加购物车

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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.

定价: 843元 / 折扣价: 717 加购物车

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