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5.1 N-Ethyldiethanolamine, N-methyldiethanolamine and triethanolamine are Schedule 3 compounds under the Chemical Weapons Convention (CWC). Schedule 3 chemicals include those that have been produced, stockpiled or used as a chemical weapon, poses otherwise a risk to the object and purpose of the CWC because they possess such lethal or incapacitating toxicity as well as other properties that might enable it to be used as a chemical weapon, poses otherwise a risk to the object and purpose of the CWC by virtue of it’s importance in the production of one or more chemicals listed in Schedules 1 or 2, or it may be produced in large commercial quantities for purposes not prohibited under the CWC.4 Ethanolamines have a broad spectrum of applications. They are used to produce adhesives, agricultural products, cement grinding aids, concrete additives, detergents, specialty cleaners, personal care products, gas treatments, metalwork, oil well chemicals, packaging and printing inks, photographic chemicals, rubber, textile finishing, urethane coatings, textile lubricants, polishes, pesticides, and pharmaceuticals. Ethanolamines are readily dissolved in water, biodegradable and the bio-concentration potential is low.55.2 This test method has been investigated for use with reagent and surface water.1.1 This procedure covers the determination of diethanolamine, triethanolamine, N-methyldiethanolamine and N-ethyldiethanolamine (referred to collectively as ethanolamines in this test method) in surface 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 single reaction monitoring (SRM) mass spectrometry.1.2 This test method has been developed by U.S. EPA Region 5 Chicago Regional Laboratory (CRL).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 The Detection Verification Level (DVL) and Reporting Range for the ethanolamines are listed in Table 1.TABLE 1 Detection Verification Level and Reporting RangeAnalyte DVL (μg/L) Reporting Range (μg/L)Diethanolamine 5 25–500Triethanolamine 5 25–500N-Ethyldiethanolamine 5 25–500N-Methyldiethanolamine 10 50–5001.4.1 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 at the DVLs and at higher concentrations for N-methyldiethanolamine.FIG. 1 Example SRM Chromatograms Signal/Noise Ratios1.4.2 The reporting limit is the concentration of the Level 1 calibration standard as shown in Table 2 for diethanolamine, triethanolamine, and N-ethyldiethanolamine and Level 2 for N-methyldiethanolamine. The reporting limit for N-methyldiethanolamine is set at 50 μg/L due to poor sensitivity at a 5 μg/L concentration which did not meet the DVL criteria. The DVL for N-methyldiethanolamine is at 10 μg/L, which forces a raised reporting limit (chromatograms are shown in Fig. 1). However, the multi-laboratory validation required a spike of all target analytes at 25 μg/L. The mean recovery for N-methyldiethanolamine at this level was 88 % as shown in Table 3. If your instrument’s sensitivity can meet the requirements in this test method, N-methyldiethanolamine may have a 25 μg/L reporting limit.TABLE 2 Concentrations of Calibration Standards (PPB)Analyte/Surrogate LV 1 LV 2 LV 3 LV 4 LV 5 LV 6 LV 7Diethanolamine 25 50 75 150 250 350 500Triethanolamine 25 50 75 150 250 350 500N-Ethyldiethanolamine 25 50 75 150 250 350 500N-Methyldiethanolamine 25 50 75 150 250 350 500Diethanolamine-D8 (Surrogate) 25 50 75 150 250 350 500TABLE 3 Multi-Laboratory Recovery Data in Reagent WaterAnalyte Spike Conc.(ppb) # Results # Labs Bias PrecisionMeanRecovery(%) MinRecovery(%) MaxRecovery(%) Overall SD(%) Pooledwithin-labSD (%) OverallRSD (%) Pooledwithin-labRSD (%)Diethanolamine 25 24 6 96.34 51.00 156.96 31.31 10.96 32.50 9.49Diethanolamine 50 24 6 101.41 54.00 154.80 29.54 7.97 29.13 7.91Diethanolamine 200 24 6 101.57 61.00 138.00 20.98 10.50 20.66 10.85Diethanolamine 425 24 6 102.06 70.00 138.82 17.98 5.90 17.61 5.70Triethanolamine 25 24 6 87.70 35.96 157.20 27.00 25.18 30.79 27.48Triethanolamine 50 24 6 94.95 67.00 121.66 16.39 9.57 17.26 9.66Triethanolamine 200 22 6 105.00 79.50 132.00 14.06 11.81 13.39 11.52Triethanolamine 425 24 6 96.94 40.00 144.94 27.56 4.41 28.43 5.76N-Ethyldiethanolamine 25 24 6 90.61 31.00 132.00 39.42 7.47 43.51 10.42N-Ethyldiethanolamine 50 23 6 111.88 49.00 146.00 28.71 7.19 25.66 7.56N-Ethyldiethanolamine 200 24 6 106.20 60.00 134.00 23.09 11.96 21.74 12.23N-Ethyldiethanolamine 425 24 6 99.67 51.00 130.00 23.07 4.68 23.15 6.01N-Methyldiethanolamine 25 24 6 88.43 41.72 133.60 25.24 13.29 28.55 16.70N-Methyldiethanolamine 50 24 6 102.28 56.00 153.80 25.85 8.73 25.27 8.22N-Methyldiethanolamine 200 24 6 101.02 59.00 136.50 20.07 9.51 19.87 9.54N-Methyldiethanolamine 425 24 6 94.75 63.00 115.76 15.02 3.34 15.85 3.72Diethanolamine-D8 (Surrogate) 200 96 6 103.02 60.00 151.95 21.13 9.40 20.51 9.251.5 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 and health 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 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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