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ASTM D 7599 : 2016 : R2017

Superseded

Superseded

A superseded Standard is one, which is fully replaced by another Standard, which is a new edition of the same Standard.

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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)

Available format(s)

Hardcopy , PDF

Superseded date

20-05-2024

Language(s)

English

Published date

24-07-2017

€67.30
Excluding VAT

CONTAINED IN VOL. 11.02, 2017 Defines 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).

Committee
D 19
DocumentType
Test Method
Pages
10
ProductNote
Reconfirmed 2017
PublisherName
American Society for Testing and Materials
Status
Superseded
SupersededBy
Supersedes

1.1This 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.

1.2This test method has been developed by U.S. EPA Region 5 Chicago Regional Laboratory (CRL).

1.3The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.

1.4The 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

1.4.1The 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. 1Example SRM Chromatograms Signal/Noise Ratios

Example SRM Chromatograms Signal/Noise RatiosExample SRM Chromatograms Signal/Noise Ratios

1.4.2The 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

1.5This 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.

1.6This 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.

ASTM D 3694 : 1996 : R2011 Standard Practices for Preparation of Sample Containers and for Preservation of Organic Constituents
ASTM D 1129 : 2013 : REDLINE Standard Terminology Relating to Water
ASTM D 1129 : 2003 Standard Terminology Relating to Water
ASTM D 2777 : 2013 : REDLINE Standard Practice for Determination of Precision and Bias of Applicable Test Methods of Committee D19 on Water
ASTM D 1129 : 2013 Standard Terminology Relating to Water
ASTM D 1129 : 2013 : R2020 Standard Terminology Relating to Water
ASTM D 5847 : 1999 : REV A : EDT 1 Standard Practice for Writing Quality Control Specifications for Standard Test Methods for Water Analysis
ASTM D 3694 : 1996 Standard Practices for Preparation of Sample Containers and for Preservation of Organic Constituents
ASTM D 2777 : 2012 Standard Practice for Determination of Precision and Bias of Applicable Test Methods of Committee D19 on Water
ASTM D 1129 : 2013 : R2020 : EDT 2 Standard Terminology Relating to Water
ASTM D 1193 : 1977 : R1983 : EDT 1 Standard Specification for Reagent Water
ASTM D 5847 : 2002 : R2007 Standard Practice for Writing Quality Control Specifications for Standard Test Methods for Water Analysis
ASTM D 1129 : 2006 Standard Terminology Relating to Water
ASTM D 2777 : 2003 Standard Practice for Determination of Precision and Bias of Applicable Methods of Committee D-19 on Water
ASTM D 2777 : 2021 Standard Practice for Determination of Precision and Bias of Applicable Test Methods of Committee D19 on Water
ASTM D 2777 : 2013 Standard Practice for Determination of Precision and Bias of Applicable Test Methods of Committee D19 on Water
ASTM E 2554 : 2013 Standard Practice for Estimating and Monitoring the Uncertainty of Test Results of a Test Method Using Control Chart Techniques
ASTM D 5847 : 2002 : R2012 Standard Practice for Writing Quality Control Specifications for Standard Test Methods for Water Analysis
ASTM D 2777 : 1998 Standard Practice for Determination of Precision and Bias of Applicable Methods of Committee D-19 on Water
ASTM D 3694 : 1996 : R2017 Standard Practices for Preparation of Sample Containers and for Preservation of Organic Constituents
ASTM D 1129 : 2013 : R2020 : EDT 1 Standard Terminology Relating to Water
ASTM D 1129 : 1999 : REV A Standard Terminology Relating to Water
ASTM D 3856 : 2011 Standard Guide for Management Systems in Laboratories Engaged in Analysis of Water
ASTM D 1129 : 2006 : REV A Standard Terminology Relating to Water
ASTM D 1193 : 2006 : R2011 Standard Specification for Reagent Water
ASTM D 5847 : 2002 : R2020 Standard Practice for Writing Quality Control Specifications for Standard Test Methods for Water Analysis
ASTM D 1129 : 2003 : REV A Standard Terminology Relating to Water
ASTM D 3694 : 1996 : R2004 Standard Practices for Preparation of Sample Containers and for Preservation of Organic Constituents
ASTM D 1129 : 2002 Standard Terminology Relating to Water
ASTM E 2554 : 2018 : EDT 1 Standard Practice for Estimating and Monitoring the Uncertainty of Test Results of a Test Method Using Control Chart Techniques
ASTM D 1193 : 1991 Standard Specification for Reagent Water
ASTM D 3856 : 1995 : R2006 Standard Guide for Good Laboratory Practices in Laboratories Engaged in Sampling and Analysis of Water
ASTM D 1129 : 2004 Standard Terminology Relating to Water
ASTM D 5847 : 2022 Standard Practice for Writing Quality Control Specifications for Standard Test Methods for Water Analysis
ASTM D 2777 : 2008 Standard Practice for Determination of Precision and Bias of Applicable Test Methods of Committee D19 on Water
ASTM E 2554 : 2007 Standard Practice for Estimating and Monitoring the Uncertainty of Test Results of a Test Method in a Single Laboratory Using a Control Sample Program
ASTM D 3856 : 2011 : R2015 Standard Guide for Management Systems in Laboratories Engaged in Analysis of Water (Withdrawn 2024)
ASTM D 2777 : 2006 Standard Practice for Determination of Precision and Bias of Applicable Test Methods of Committee D19 on Water
ASTM D 3856 : 1995 : R2000 Standard Guide for Good Laboratory Practices in Laboratories Engaged in Sampling and Analysis of Water
ASTM D 1129 : 2002 : REV A Standard Terminology Relating to Water
ASTM E 2554 : 2018 Standard Practice for Estimating and Monitoring the Uncertainty of Test Results of a Test Method Using Control Chart Techniques
ASTM D 5847 : 2002 Standard Practice for Writing Quality Control Specifications for Standard Test Methods for Water Analysis
ASTM E 2554 : 2013-05 PRACTICE FOR ESTIMATING AND MONITORING THE UNCERTAINTY OF TEST RESULTS OF A TEST METHOD USING CONTROL CHART TECHNIQUES
ASTM D 1193 : 1970 Standard Specification For Reagent Water
ASTM D 1193 : 2006 Standard Specification for Reagent Water
ASTM D 1193 : 1999 Standard Specification for Reagent Water
ASTM D 1129 : 2010 Standard Terminology Relating to Water
ASTM D 1129 : 2006 : REV A : EDT 1 Standard Terminology Relating to Water
ASTM D 1129 : 2001 Standard Terminology Relating to Water
ASTM D 1129 : 2004 : EDT 1 Standard Terminology Relating to Water
ASTM D 3694 : 1996 : R2024 Standard Practices for Preparation of Sample Containers and for Preservation of Organic Constituents
ASTM D 1193 : 2006 : R2018 Standard Specification for Reagent Water
ASTM D 2777 : 2008 : EDT 1 Standard Practice for Determination of Precision and Bias of Applicable Test Methods of Committee D19 on Water

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