2903184

ASTM D7599-16(2017)

Standard Test Method for Determination of Diethanolamine, Triethanolamine, <emph type="ital">N</emph>-Methyldiethanolamine and <emph type="ital">N</emph >-Ethyldiethanolamine in Water by Single Reaction Monitoring Liquid Chromatography/Tandem Mass Spectrometry (LC/MS/MS)

standard by ASTM International , 06/15/2017

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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 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 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
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.
FIG. 1 Example SRM Chromatograms Signal/Noise Ratios
Example SRM Chromatograms Signal/Noise RatiosExample SRM Chromatograms Signal/Noise Ratios
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.
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  

Product Details

Published:
06/15/2017
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10
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1 file , 260 KB
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Document History

  1. ASTM D7599-16(2024)


    Standard Test Method for Determination of Diethanolamine, Triethanolamine, <emph type="ital">N</emph>-Methyldiethanolamine and <emph type="ital">N</emph >-Ethyldiethanolamine in Water by Single Reaction Monitoring Liquid Chromatography/Tandem Mass Spectrometry (LC/MS/MS)

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  2. ASTM D7599-16(2017)

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    Standard Test Method for Determination of Diethanolamine, Triethanolamine, <emph type="ital">N</emph>-Methyldiethanolamine and <emph type="ital">N</emph >-Ethyldiethanolamine in Water by Single Reaction Monitoring Liquid Chromatography/Tandem Mass Spectrometry (LC/MS/MS)

    • Historical Version

  3. ASTM D7599-16


    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)

    • Historical Version

  4. ASTM D7599-09e2


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

    • Historical Version

  5. 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

    • Historical Version

  6. ASTM D7599-09


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

    • Historical Version

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