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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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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 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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