ASTM-D7599 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)

ASTM-D7599 - 2016 R17 EDITION - CURRENT
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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)
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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 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

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

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.

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.

Keywords

ethanolamines; liquid chromatography; mass spectrometry; water;; ICS Number Code 13.060.50 (Examination of water for chemical substances)

To find similar documents by ASTM Volume:

11.02 (Water (II))

To find similar documents by classification:

13.060.50 (Examination of water for chemical substances)

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Document Number

ASTM-D7599-16(2017)

Revision Level

2016 R17 EDITION

Status

Current

Modification Type

Reapproval

Publication Date

July 15, 2017

Document Type

Test Method

Page Count

10 pages

Committee Number

D19.06