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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.

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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.

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5.1 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 water matrices for understanding the sources and concentration levels in affected areas. 5.2 This method has been used to determine TTPC in reagent water and a river water (Table 8). (A) Solution A: Level 8 stock solution prepared according to Section 12 and at Table 4 concentrations.(B) Solution B: 75 % Acetone, 25 % Water. Note 1: This test method has been used to characterize TTPC in real world water samples with success and similar recoveries as shown in Table 8. 1.1 This test method covers the determination of (Tri-n-butyl)-n-tetradecylphosphonium chloride (TTPC) in water by dilution with acetone, filtration and analysis by liquid chromatography/tandem mass spectrometry. This test method is not amenable for the analysis of isomeric mixtures of Tributyl-tetradecylphosphonium chloride. TTPC is a biocide that strongly adsorbs to soils.2 The water samples 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 100 ng/L to 4000 ng/L. This analyte is qualitatively and quantitatively determined by this method. This test method adheres to multiple reaction monitoring (MRM) mass spectrometry. 1.2 A full collaborative study to meet the requirements of Practice D2777 has not been completed. This test method contains single-operator precision and bias based on single-operator data. Publication of standards that have not been fully validated is done to make the current technology accessible to users of standards, and to solicit additional input from the user community. 1.3 The Method Detection Limit3 (MDL) and Reporting Range4 for the target analyte 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. The reporting limit is calculated from the concentration of the Level 1 calibration standard as shown in Table 4 for TTPC after taking into account a 2.5 mL water sample volume and a final diluted sample volume of 10 mL (75 % acetone/25 % water). The final solution volume is 10 mL because a 7.5 mL volume of acetone is added to each 2.5 mL water sample which is shaken and filtered. 1.4 Units—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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Separation and identification of stabilizers used in the manufacture of low density polyethylene are necessary in order to correlate performance properties with polymer composition. This test method provides a means to determine the BHT, BHEB, Isonox-129, erucamide slip, Irganox-1010 and Irganox-1076 levels in low density polyethylene samples.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.1.1 This test method describes a liquid chromatograph procedure for the separation of some additives currently used in low density polyethylene. These additives are extracted with 2-propanol 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. For a specific hazards statement, see Section 9.Note 1—There is no similar or equivalent ISO standard.

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5.1 TDG is a Schedule 2 compound under the Chemical Weapons Convention (CWC). Schedule 2 chemicals include those that are precursors to chemical weapons, chemical weapons agents, or have a number of other commercial uses. They are used as ingredients to produce insecticides, herbicides, lubricants, and some pharmaceutical products. Schedule 2 chemicals can be found in applications unrelated to chemical weapons. TDG is both a mustard gas precursor and a degradant as well as an ingredient in water-based inks, ballpoint pen inks, dyes, and some pesticides.55.2 This method has been investigated for use with soil.1.1 This procedure covers the determination of thiodiglycol (TDG) in soil using pressurized fluid extraction (PFE). A commercially available PFE system2 is used, followed by analysis using liquid chromatography (LC), and detected with tandem mass spectrometry (MS/MS). TDG is qualitatively and quantitatively determined by this method. This method adheres to single reaction monitoring (SRM) mass spectrometry.1.2 The method detection limit (MDL) and reporting range for TDG are listed in Table 1.1.2.1 The MDL is determined following the Code of Federal Regulations, 40 CFR Part 136, Appendix B.1.2.2 The reporting limit (RL) is calculated from the concentration of the Level 1 calibration standard as shown in Table 4. The RL for this method is 200 ppb. Reporting range concentrations are calculated from Table 4 concentrations assuming a 5 μL injection of the lowest level calibration standard, 5 g sample, and a 2 mL final extract volume.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 Separation and identification of stabilizers used in the manufacture of polyethylene resins are necessary in order to correlate performance properties with polymer composition. This test method provides a means to determine the polymer additives listed in Table 1 in polyethylene samples. This test method is capable of the determination of other antioxidants, but the stability of these during extraction has not been investigated.5.2 The additive extraction procedure is made effective by the relatively low solubility of the polymer sample in solvents generally used for liquid chromatographic analysis. In this method, isopropanol and cyclohexane were chosen because of their excellent extraction efficiencies as well as for safety reasons. Other solvents including ethylacetate, isobutanol, chloroform and methylene chloride can also be used.5.3 Methods other than refluxing that have been used to remove additives from the polymer matrix including pressurized liquid, microwave, ultrasonic, and supercritical fluid extractions. For the separation of the extracted additives, SFC and GC have been used successfully for several of the additives.5.4 Under optimum conditions, the lowest level of detection for an antioxidant is approximately 2 ppm.1.1 This test method covers a liquid-chromatographic procedure for the separation of primary and secondary antioxidant and slip additives currently used in polyethylene plastics. These additives are extracted with either isopropanol (resin densities < 0.94 g/cm3) or cyclohexane (resin densities > 0.94 g/cm3) prior to liquid-chromatographic separation. The ultraviolet absorbance of the eluting compound(s) is measured and quantitation is performed using external calibration.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 standard.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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YD/T 1272.1-2018 光纤活动连接器第1部分:LC 现行 发布日期 :  2018-12-21 实施日期 :  2019-04-01

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本标准规定了动物源食品中α-玉米赤霉醇、β-玉米赤霉醇、α-玉米赤霉烯醇、β-玉米赤霉烯醇、玉米赤霉酮和玉米赤霉烯酮残留量的高效液相色谱检测方法以及高效液相色谱-质谱/质谱检测确证方法。
本标准适用于猪肉、鸡肉、鱼肉、牛肝、牛奶、鸡蛋及肉罐头等动物源食品中α-玉米赤霉醇、β-玉米赤霉醇、α-玉米赤霉烯醇、β-玉米赤霉烯醇、玉米赤霉酮和玉米赤霉烯酮残留量的定性确证和定量测定。液相色谱法不适用于猪肉样品。

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YD/T 2554.1-2013 塑料光纤活动连接器第1部分:LC 现行 发布日期 :  2013-04-25 实施日期 :  2013-06-01

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