1. Scope

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 method. This method adheres to single reaction monitoring (SRM) mass spectrometry.

1.2 This test method has been developed in support of the National Homeland Security Research Center, US EPA by Region 5 Chicago Regional Laboratory.

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.

1.4.1 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.

1.4.2 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 ? g/L due to poor sensitivity at a 5 ? g/L concentration which did not meet the DVL criteria. The DVL for N -methyldiethanolamine is at 10 ? g/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 ? g/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 ? g/L reporting limit.

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 and health practices and determine the applicability of regulatory limitations prior to use.

2. Referenced Documents (purchase separately) The documents listed below are referenced within the subject standard but are not provided as part of the standard.

ASTM Standards

D1129 Terminology Relating to Water

D1193 Specification for Reagent Water

D2777 Practice for Determination of Precision and Bias of Applicable Test Methods of Committee D19 on Water

D3694 Practices for Preparation of Sample Containers and for Preservation of Organic Constituents

D3856 Guide for Management Systems in Laboratories Engaged in Analysis of Water

D5847 Practice for Writing Quality Control Specifications for Standard Test Methods for Water Analysis

E2554 Practice for Estimating and Monitoring the Uncertainty of Test Results of a Test Method in a Single Laboratory Using a Control Sample Program

Other Documents

Keywords

ethanolamines; liquid chromatography; mass spectrometry; water;

ICS Code

ICS Number Code 13.060.50 (Examination of water for chemical substances)

DOI: 10.1520/D7599-09

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