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5.1 Silver may be used to treat consumer textile products to provide enhanced antimicrobial (fungi, bacteria, viruses) properties (3, 4). At any point in a textile product’s lifecycle, there may be a need to measure the amount of silver present. This standard prescribes a test method based on ICP-OES or ICP-MS analysis that manufacturers, producers, analysts, policymakers, regulators, and others may use for measurement of total silver in textiles. As described in Guide E3025, determination of total silver in a consumer textile product is one component of a tiered approach to determine if silver is present, possibly as nanomaterial(s) (one or more external dimensions in the nanoscale), prior to measuring the form and dimension of the Ag that is found. ICP-OES or ICP-MS analysis alone is not sufficient to determine whether a textile contains silver nanomaterial(s).NOTE 4: There are many different chemical and physical forms of silver that are used to treat textiles and an overview of this topic is provided in Guide E3025.5.2 As described in Guide E3025, the amount of silver in a textile can decrease over time as silver metal and silver compounds can react with oxygen and other oxidation-reduction (redox) active agents present in the environment to form soluble ionic species which are released by contact with moisture (for example, from ambient humidity, washing, body sweat, rain, or other sources). Hence, if silver is measured in a textile, the result may only be indicative of that moment in the article’s life cycle and great care is necessary in drawing temporal inferences from the results.5.3 If silver is measured by ICP-OES or ICP-MS analysis, additional analyses are needed to elucidate the form of silver in the textile specimen. This step is necessary because ICP-OES or ICP-MS results are for total silver independent of chemical and physical form and textiles may be treated with silver in sizes that range from the nanoscale (for example, salt nanoparticles) to the micrometer scale (for example, particulates or fibers).5.4 If no silver is detected by ICP-OES, the more sensitive ICP-MS should be used to determine if silver is present in a test specimen. If no silver is detected in a textile sample using appropriate (fit for purpose) analytical techniques, then testing can be terminated.NOTE 5: Typical method detection limits are 0.6 µg Ag/L by ICP-OES and 0.002 µg Ag/L by ICP-MS which are comparable to limits successfully used to detect silver in a range of products, including sports textiles and wound dressings (2).5.5 Results of ICP-OES or ICP-MS analysis may be qualitative or quantitative, depending upon the efficacy of the digestion procedure for the textile matrix. Regardless, ICP-OES or ICP-MS analysis is recommended as a first step to screen for the presence of silver in a textile and results can be used to inform subsequent more detailed analyses as part of a tiered approach to determine if a textile contains silver nanomaterial(s).1.1 This test method covers the use of inductively coupled plasma–optical emission spectrometry (ICP-OES) and inductively coupled plasma–mass spectrometry (ICP-MS) analyses for determination of the mass fraction of total silver in consumer textile products made of any combination of natural or manufactured fibers. Either ICP-OES or ICP-MS analysis is recommended as a first step to test for and quantify silver in a textile and results can be used to inform subsequent, more detailed analyses as part of the tiered approach described in Guide E3025 to determine if a textile contains silver nanomaterial(s).1.2 This test method prescribes acid digestion to prepare test sample solutions from samples of textiles utilizing an appropriate internal standard followed by external calibration and analysis with either ICP-OES or ICP-MS to quantify total silver.1.3 This test method is believed to provide quantitative results for textiles made of fibers of rayon, cotton, polyester, and lycra that contain metallic silver (see Section 17). It is the analyst’s responsibility to establish the efficacy (ability to achieve the planned and desired analytical result) of this test method for other textile matrices and forms of silver.1.4 Units—The values stated in SI units are to be regarded as standard. No other units of measurements 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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5.1 Ambient marine waters generally contain very low concentrations of toxic metals that require sensitive analytical methods, such as ICP-MS, to detect and measure the metal's concentrations.5.2 Due to the high dissolved salt concentrations present in seawater, sample pretreatment is required to remove signal suppression and significant polyatomic interferences due to the matrix both of which compromise detection limits.1.1 Toxic elements may be present in ambient waters and may enter the food chain via uptake by plants and animals; the actual concentrations of toxic metals are usually sub-ng/mL. The U.S. EPA has published its Water Quality Standards in the U.S. Federal Register 40 CFR 131.36, Minimum requirements for water quality standards submission, Ch. I (7-1-00 Edition), see Annex, Table A1.1. The U.S. EPA has also developed Method 1640 to meet these requirements, see Annex, Table A1.2.1.2 Inductively Coupled Plasma Mass Spectroscopy (ICP-MS) is a technique with sufficient sensitivity to routinely measure toxic elements in ambient waters, both fresh and saline (Test Method D5673). However saline and hard water matrices pose analytical challenges for direct multielement analysis by ICP-MS at the required sub-ng/mL levels.1.3 This practice describes a method used to prepare water samples for subsequent multielement analysis using ICP-MS. The practice is applicable to seawater and fresh water matrices, which may be filtered or digested. Samples prepared by this method have been analyzed by ICP-MS for the elements listed in Annex, Table A1.3).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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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 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 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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4.1 This technique is destructive, in that the glass fragments may need to be crushed, and digested in acid.4.2 Although the concentration ranges of the calibration curves shown in Appendix X1 are applicable to soda lime and borosilicate glass, this method is useful for the accurate measurement of element concentrations from a wide variety of glass samples.4.3 The determination of the element concentrations in glass yields data that can be used to compare fragments.4.4 It should be recognized that the method measures the bulk concentration of the target elements. Any extraneous material present on the glass that is not removed before digestion can result in inaccurate concentrations of the measured elements.4.5 The precision and accuracy of the method should be established in each laboratory that employs the method.1.1 One objective of a forensic glass examination is to compare glass samples to determine if they can be discriminated using their physical, optical or chemical properties (for example, color, refractive index (RI), density, elemental composition). If the samples are distinguishable in any of these observed and measured properties, it may be concluded that they did not originate from the same source of broken glass. If the samples are indistinguishable in all of these observed and measured properties, the possibility that they originated from the same source of glass cannot be eliminated. The use of an elemental analysis method such as inductively coupled plasma mass spectrometry yields high discrimination among sources of glass. (1-16)21.2 This test method covers a procedure for quantitative determination of the concentrations of magnesium (Mg), aluminum (Al), iron (Fe), titanium (Ti), manganese (Mn), rubidium (Rb), strontium (Sr), zirconium (Zr), barium (Ba), lanthanum (La), cerium (Ce), neodymium (Nd), samarium (Sm), and lead (Pb) in glass samples.1.3 This procedure is applicable to irregularly shaped samples as small as 200 micrograms, for the comparison of fragments of a known source to the recovered fragments from a questioned source. These elements are present in soda lime and borosilicate glass in μg/L to % levels.1.4 This procedure is applicable to other elements, other types of glass, and other concentration ranges with appropriate modifications of the digestion procedure (if needed for full recovery of the additional elements), calibration standards and the mass spectrometer conditions. Calcium and potassium, for example, could be added to the list of analytes in a modified analysis scheme. Alternative methods for the determination of concentrations of elements in glass are listed in the references.1.5 For any given glass, approximately 40 elements are likely to be present at detectable concentrations using this procedure with minor modifications. The element set stated here is an example of some of these elements that can be detected in glass and used for forensic comparisons.1.6 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.1.7 This standard cannot replace knowledge, skills, or abilities acquired through education, training, and experience and is to be used in conjunction with professional judgment by individuals with such discipline-specific knowledge, skills, and abilities.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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