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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

Analyte DVL (μg/L) Reporting Range (μg/L)
Diethanolamine 5 25-500
Triethanolamine 5 25-500
N-Ethyldiethanolamine 5 25-500
N-Methyldiethanolamine 10 50-500

TABLE 2 Concentrations of Calibration Standards (PPB)

Analyte/Surrogate LV 1 LV 2 LV 3 LV 4 LV 5 LV 6 LV 7
Diethanolamine 25 50 75 150 250 350 500
Triethanolamine 25 50 75 150 250 350 500
N-Ethyldiethanolamine 25 50 75 150 250 350 500
N-Methyldiethanolamine 25 50 75 150 250 350 500
Diethanolamine-D8 (Surrogate) 25 50 75 150 250 350 500

TABLE 3 Multi-Laboratory Recovery Data in Reagent Water

Analyte Spike Conc.
(ppb)
# Results # Labs Bias Precision
Mean
Recovery
(%)
Min
Recovery
(%)
Max
Recovery
(%)
Overall SD
(%)
Pooled
within-lab
SD (%)
Overall
RSD (%)
Pooled
within-lab
RSD (%)
Diethanolamine 25 24 6 96.34 51.00 156.96 31.31 10.96 32.50 9.49
Diethanolamine 50 24 6 101.41 54.00 154.80 29.54 7.97 29.13 7.91
Diethanolamine 200 24 6 101.57 61.00 138.00 20.98 10.50 20.66 10.85
Diethanolamine 425 24 6 102.06 70.00 138.82 17.98 5.90 17.61 5.70
Triethanolamine 25 24 6 87.70 35.96 157.20 27.00 25.18 30.79 27.48
Triethanolamine 50 24 6 94.95 67.00 121.66 16.39 9.57 17.26 9.66
Triethanolamine 200 22 6 105.00 79.50 132.00 14.06 11.81 13.39 11.52
Triethanolamine 425 24 6 96.94 40.00 144.94 27.56 4.41 28.43 5.76
N-Ethyldiethanolamine 25 24 6 90.61 31.00 132.00 39.42 7.47 43.51 10.42
N-Ethyldiethanolamine 50 23 6 111.88 49.00 146.00 28.71 7.19 25.66 7.56
N-Ethyldiethanolamine 200 24 6 106.20 60.00 134.00 23.09 11.96 21.74 12.23
N-Ethyldiethanolamine 425 24 6 99.67 51.00 130.00 23.07 4.68 23.15 6.01
N-Methyldiethanolamine 25 24 6 88.43 41.72 133.60 25.24 13.29 28.55 16.70
N-Methyldiethanolamine 50 24 6 102.28 56.00 153.80 25.85 8.73 25.27 8.22
N-Methyldiethanolamine 200 24 6 101.02 59.00 136.50 20.07 9.51 19.87 9.54
N-Methyldiethanolamine 425 24 6 94.75 63.00 115.76 15.02 3.34 15.85 3.72
Diethanolamine-D8 (Surrogate) 200 96 6 103.02 60.00 151.95 21.13 9.40 20.51 9.25


FIG. 1 Example SRM Chromatograms Signal/Noise Ratios

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Published:
12/01/2009
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