Значение и использование

5.1 N-Ethyldiethanolamine, N-methyldiethanolamine and triethanolamine are Schedule 3 compounds under the Chemical Weapons Convention (CWC). Schedule 3 chemicals include those that have been produced, stockpiled or used as a chemical weapon, poses otherwise a risk to the object and purpose of the CWC because they possess such lethal or incapacitating toxicity as well as other properties that might enable it to be used as a chemical weapon, poses otherwise a risk to the object and purpose of the CWC by virtue of it’s importance in the production of one or more chemicals listed in Schedules 1 or 2, or it may be produced in large commercial quantities for purposes not prohibited under the CWC.4 Ethanolamines have a broad spectrum of applications. They are used to produce adhesives, agricultural products, cement grinding aids, concrete additives, detergents, specialty cleaners, personal care products, gas treatments, metalwork, oil well chemicals, packaging and printing inks, photographic chemicals, rubber, textile finishing, urethane coatings, textile lubricants, polishes, pesticides, and pharmaceuticals. Ethanolamines are readily dissolved in water, biodegradable and the bio-concentration potential is low.5

5.2 This test method has been investigated for use with reagent and surface water.

Область применения

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

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.