Norm

ASTM D7597-16

Standard Test Method for Determination of Diisopropyl Methylphosphonate, Ethyl Hydrogen Dimethylamidophosphate, Ethyl Methylphosphonic Acid, Isopropyl Methylphosphonic Acid, Methylphosphonic Acid and Pinacolyl Methylphosphonic Acid in Water by Liquid Chromatography/Tandem Mass Spectrometry

61,51

Over deze norm

Status Definitief
Aantal pagina's 13
Commissie D19.06
Gepubliceerd op 01-02-2016
Taal Engels

1.1 This procedure covers the determination of diisopropyl methylphosphonate (DIMP), ethyl hydrogen dimethylamidophosphate (EHDMAP), ethyl methylphosphonic acid (EMPA), isopropyl methylphosphonic acid (IMPA), methylphosphonic acid (MPA) and pinacolyl methylphosphonic acid (PMPA) (referred to collectively as organophosphonates in this test method) in surface water by direct injection using liquid chromatography (LC) and detected with tandem mass spectrometry (MS/MS) using electrospray ionization (ESI). 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 organophosphonates are listed in Table 1.

1.4.1 The DVL is required to be at a concentration at least three 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 for the organophosphonates in the ESI positive mode and Fig. 2 in the ESI negative mode.

RSD (%)

DIMP

Pos

5

16

4

95.1

65.8

136.0

17.6

19.4

21.3

22.4

DIMP

Pos

10

19

5

98.2

80.0

121.0

6.1

5.5

13.6

13.8

DIMP

Pos

25

26

6

102.9

74.4

128.0

5.6

5.7

14.5

14.1

DIMP

Pos

125

22

5

96.6

80.4

120.0

4.4

4.5

11.0

11.4

DIMP-D14

Pos

25

86

6

102.6

54.8

127.6

9.8

9.5

11.2

10.9

EHDMAP

Neg

5

12

3

57.5

0.0

220.0

31.4

22.3

71.1

123.6

EHDMAP

Neg

10

16

4

47.1

0.0

178.0

13.3

10.8

66.8

142.0

EHDMAP

Neg

25

22

5

84.1

54.0

141.2

6.9

6.6

22.9

27.3

EHDMAP

Neg

125

18

4

87.4

64.2

141.6

5.0

5.1

25.4

29.1

EHDMAP

Pos

5

16

4

77.0

0.0

134.2

7.4

8.0

51.4

66.8

EHDMAP

Pos

10

20

5

70.0

0.0

143.0

7.7

10.0

53.6

76.5

EHDMAP

Pos

25

26

6

89.6

60.0

128.8

5.2

6.2

23.5

26.2

EHDMAP

Pos

125

22

5

87.5

59.0

123.2

5.2

6.0

23.9

27.3

EMPA

Neg

50

16

4

110.1

74.8

170.6

22.4

17.2

25.6

23.3

EMPA

Neg

100

20

5

108.3

87.7

175.0

11.1

8.7

24.8

22.9

EMPA

Neg

250

26

6

104.8

82.0

122.6

6.1

5.5

11.8

11.3

EMPA

Neg

1250

22

5

101.5

87.2

126.4

8.4

8.1

11.2

11.0

EMPA

Pos

50

16

4

95.4

77.6

122.8

12.9

13.3

13.1

13.7

EMPA

Pos

100

20

5

96.0

61.4

132.5

9.5

9.5

15.9

16.6

EMPA

Pos

250

26

6

99.7

70.0

133.2

5.9

5.4

18.2

18.2

EMPA

Pos

1250

21

5

93.9

84.0

108.4

2.7

3.0

7.7

8.2

IMPA

Neg

50

16

4

88.0

56.6

140.4

23.7

26.0

23.5

26.7

IMPA

Neg

100

20

5

88.0

68.5

118.0

12.9

14.3

13.4

15.2

IMPA

Neg

250

26

6

98.1

72.8

144.0

13.1

11.9

19.2

19.6

IMPA

Neg

1250

21

5

90.7

73.1

103.0

5.5

6.1

8.7

9.6

IMPA

Pos

50

16

4

98.3

47.8

139.6

19.2

20.5

27.2

27.7

IMPA

Pos

100

19

5

95.4

72.3

120.5

9.8

10.3

12.4

13.0

IMPA

Pos

250

26

6

97.0

79.2

188.4

7.4

7.6

10.9

11.2

IMPA

Pos

1250

21

5

91.3

70.4

115.5

5.1

5.2

11.4

12.5

MPA

Neg

50

16

4

98.7

3.3

175.0

14.2

25.3

60.5

61.3

MPA

Neg

100

20

5

100.0

41.9

142.0

8.9

9.2

30.8

30.8

MPA

Neg

250

26

6

99.5

66.0

124.5

7.6

7.6

14.5

14.5

MPA

Neg

1250

22

5

102.7

81.8

130.5

10.5

9.9

12.4

12.1

MPA

Pos

50

16

4

68.3

9.8

139.6

13.4

20.3

36.6

53.6

MPA

Pos

100

20

5

80.5

48.4

149.7

14.0

12.6

26.8

33.3

MPA

Pos

250

26

6

91.7

33.9

153.7

8.0

7.8

31.8

34.7

MPA

Pos

1250

22

5

95.8

31.8

208.2

12.6

8.3

43.4

45.3

MPA-D3

Neg

250

84

6

111.2

57.2

190.8

16.2

12.5

30.0

26.9

MPA-D3

Pos

250

68

5

104.4

58.4

151.8

14.3

14.0

18.0

17.3

PMPA

Neg

50

15

4

87.8

77.6

124.4

8.4

8.2

13.8

15.7

PMPA

Neg

100

19

5

91.6

83.6

98.2

2.8

3.0

4.4

4.8

PMPA

Neg

250

26

6

101.0

77.2

123.8

5.0

4.8

12.1

12.0

PMPA

Neg

1250

22

5

99.2

84.8

126.5

4.9

4.8

12.3

12.4

PMPA

Pos

50

16

4

90.8

60.8

148.8

15.8

16.1

25.6

28.2

PMPA

Pos

100

15

4

95.2

86.8

114.0

3.8

4.0

7.9

8.3

PMPA

Pos

250

20

5

103.8

85.2

136.1

4.5

3.8

15.3

14.7

PMPA

Pos

1250

12

3

99.8

88.8

117.5

5.2

5.0

7.5

7.5

PMPA-13C6

Neg

250

83

6

99.5

74.8

128.3

9.4

9.2

11.1

11.1

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.

Details

ICS-code 13.060.50
Nederlandse titel Standard Test Method for Determination of Diisopropyl Methylphosphonate, Ethyl Hydrogen Dimethylamidophosphate, Ethyl Methylphosphonic Acid, Isopropyl Methylphosphonic Acid, Methylphosphonic Acid and Pinacolyl Methylphosphonic Acid in Water by Liquid Chromatography/Tandem Mass Spectrometry
Engelse titel Standard Test Method for Determination of Diisopropyl Methylphosphonate, Ethyl Hydrogen Dimethylamidophosphate, Ethyl Methylphosphonic Acid, Isopropyl Methylphosphonic Acid, Methylphosphonic Acid and Pinacolyl Methylphosphonic Acid in Water by Liquid Chromatography/Tandem Mass Spectrometry

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