ASTM International - ASTM D7599-09e1

Standard Test Method for Determination of Diethanolamine, Triethanolamine, N-Methyldiethanolamine and N-Ethyldiethanolamine in Water by Single Reaction Monitoring Liquid Chromatography/Tandem Mass Sp

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Organization: ASTM International
Publication Date: 1 December 2009
Status: historical
Page Count: 9
ICS Code (Examination of water for chemical substances): 13.060.50
significance And Use:

N-Ethyldiethanolamine, N-methyldiethanolamine and triethanolamine are Schedule 3 compounds under the Chemical Weapons Convention (CWC). Schedule 3 chemicals include those that have... View More

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 by US 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.

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 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.

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.

TABLE 1 Detection Verification Level and Reporting Range

AnalyteDVL (μg/L)Reporting Range (μg/L)
Diethanolamine525-500
Triethanolamine525-500
N-Ethyldiethanolamine525-500
N-Methyldiethanolamine1050-500

TABLE 2 Concentrations of Calibration Standards (PPB)

Analyte/SurrogateLV 1LV 2LV 3LV 4LV 5LV 6LV 7
Diethanolamine255075150250350500
Triethanolamine255075150250350500
N-Ethyldiethanolamine255075150250350500
N-Methyldiethanolamine255075150250350500
Diethanolamine-D

8 (Surrogate)

255075150250350500

TABLE 3 Multi-Laboratory Recovery Data in Reagent Water

AnalyteSpike Conc.
(ppb)
# Results# LabsBiasPrecision
Mean
Recovery
(%)
Min
Recovery
(%)
Max
Recovery
(%)
Overall SD
(%)
Pooled
within-lab
SD (%)
Overall
RSD (%)
Pooled
within-lab
RSD (%)
Diethanolamine2524696.3451.00156.9631.3110.9632.509.49
Diethanolamine50246101.4154.00154.8029.547.9729.137.91
Diethanolamine200246101.5761.00138.0020.9810.5020.6610.85
Diethanolamine425246102.0670.00138.8217.985.9017.615.70
Triethanolamine2524687.7035.96157.2027.0025.1830.7927.48
Triethanolamine5024694.9567.00121.6616.399.5717.269.66
Triethanolamine200226105.0079.50132.0014.0611.8113.3911.52
Triethanolamine42524696.9440.00144.9427.564.4128.435.76
N-Ethyldiethanolamine2524690.6131.00132.0039.427.4743.5110.42
N-Ethyldiethanolamine50236111.8849.00146.0028.717.1925.667.56
N-Ethyldiethanolamine200246106.2060.00134.0023.0911.9621.7412.23
N-Ethyldiethanolamine42524699.6751.00130.0023.074.6823.156.01
N-Methyldiethanolamine2524688.4341.72133.6025.2413.2928.5516.70
N-Methyldiethanolamine50246102.2856.00153.8025.858.7325.278.22
N-Methyldiethanolamine200246101.0259.00136.5020.079.5119.879.54
N-Methyldiethanolamine42524694.7563.00115.7615.023.3415.853.72
Diethanolamine-D

8 (Surrogate)

200966103.0260.00151.9521.139.4020.519.25


FIG. 1 Example SRM Chromatograms Signal/Noise Ratios

Document History

June 15, 2017
Standard Test Method for Determination of Diethanolamine, Triethanolamine, N-Methyldiethanolamine and N-Ethyldiethanolamine in Water by Single Reaction Monitoring Liquid Chromatography/Tandem Mass Spectrometry (LC/MS/MS)
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...
February 1, 2016
Standard Test Method for Determination of Diethanolamine, Triethanolamine, N-Methyldiethanolamine and N-Ethyldiethanolamine in Water by Single Reaction Monitoring Liquid Chromatography/Tandem Mass Spectrometry (LC/MS/MS)
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...
December 1, 2009
Standard Test Method for Determination of Diethanolamine, Triethanolamine, N-Methyldiethanolamine and N-Ethyldiethanolamine in Water by Single Reaction Monitoring Liquid Chromatography/Tandem Mass Sp
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...
ASTM D7599-09e1
December 1, 2009
Standard Test Method for Determination of Diethanolamine, Triethanolamine, N-Methyldiethanolamine and N-Ethyldiethanolamine in Water by Single Reaction Monitoring Liquid Chromatography/Tandem Mass Sp
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...
December 1, 2009
Standard Test Method for Determination of Diethanolamine, Triethanolamine, N-Methyldiethanolamine and N-Ethyldiethanolamine in Water by Single Reaction Monitoring Liquid Chromatography/Tandem Mass Sp
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...
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