Norm

ASTM D7597 - 09e1 en

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 Chro

  • Deze norm is ingetrokken sinds 01-12-2009

57,20 69,21 Incl BTW

Over deze norm

Status Ingetrokken
Aantal pagina's 12
Gepubliceerd op 01-12-2009
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.

1.4.2 The reporting limit is the concentration of the Level 1 calibration standard as shown in Table 2 for the organophosphonates except for MPA in the ESI negative mode which is at Level 2 due to not meeting the DVL criteria at the lower concentration level. The DVL for MPA in the ESI negative mode is at 20 μg/L, which forces a raised reporting limit. However, the multi-laboratory validation required a spike of all target analytes at Level 1 concentrations. The mean recovery for MPA in the ESI negative mode at this level was 98.7 % as shown in Table 3. If your instruments sensitivity can meet the requirements in this test method, MPA may have a 50 μg/L reporting limit.

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.

TABLE 1 Detection Verification Level and Reporting Range

AnalyteESI ModeDVL (μg/L)Reporting Range (μg/L)
Diisopropyl methylphosphonatePositive15150
Ethyl hydrogen dimethylamidophosphateNegative0.255150
Ethyl hydrogen dimethylamidophosphatePositive0.255150
Ethyl methylphosphonic acidNegative5501500
Ethyl methylphosphonic acidPositive5501500
Isopropyl methylphosphonic acidNegative10501500
Isopropyl Methylphosphonic acidPositive5501500
Methylphosphonic acidNegative201001500
Methylphosphonic acidPositive10501500
Pinacolyl methylphosphonic acidNegative5501500
Pinacolyl methylphosphonic acidPositive5501500

TABLE 2 Concentrations of Calibration Standards (PPB)

Analyte/Surrogate LV 1LV 2LV 3LV 4LV 5LV 6LV 7
Diisopropyl methylphosphonate510203550100150
Ethyl hydrogen dimethylamidophosphate510203550100150
Ethyl methylphosphonic acid5010020035050010001500
Isopropyl methylphosphonic acid5010020035050010001500
Methylphosphonic acid5010020035050010001500
Pinacolyl methylphosphonic acid5010020035050010001500
DIMP-D14 (Surrogate)510203550100150
PMPA-13C4 (Surrogate)2550100175250500750
MPA-D3 (Surrogate)2550100175250500750

TABLE 3 Multi-Laboratory Recovery Data in Reagent Water

AnalyteESI
Mode
Spike Conc.
(ppb)
# Results# LabsBiasPrecision
Mean
Recovery
(%)
Min
Recovery
(%)
Max
Recovery
(%)
Overall SD
(%)
Pooled
within-lab
SD (%)
Overall
RSD (%)
Pooled
within-lab
RSD (%)
DIMPPos516495.165.8136.017.619.421.322.4
DIMPPos1019598.280.0121.06.15.513.613.8
DIMPPos25266102.974.4128.05.65.714.514.1
DIMPPos12522596.680.4120.04.44.511.011.4
DIMP-D14Pos25866102.654.8127.69.89.511.210.9
EHDMAPNeg512357.50.0220.031.422.371.1123.6
EHDMAPNeg1016447.10.0178.013.310.866.8142.0
EHDMAPNeg2522584.154.0141.26.96.622.927.3
EHDMAPNeg12518487.464.2141.65.05.125.429.1
EHDMAPPos516477.00.0134.27.48.051.466.8
EHDMAPPos1020570.00.0143.07.710.053.676.5
EHDMAPPos2526689.660.0128.85.26.223.526.2
EHDMAPPos12522587.559.0123.25.26.023.927.3
EMPANeg50164110.174.8170.622.417.225.623.3
EMPANeg100205108.387.7175.011.18.724.822.9
EMPANeg250266104.882.0122.66.15.511.811.3
EMPANeg1250225101.587.2126.48.48.111.211.0
EMPAPos5016495.477.6122.812.913.313.113.7
EMPAPos10020596.061.4132.59.59.515.916.6
EMPAPos25026699.770.0133.25.95.418.218.2
EMPAPos125021593.984.0108.42.73.07.78.2
IMPANeg5016488.056.6140.423.726.023.526.7
IMPANeg10020588.068.5118.012.914.313.415.2
IMPANeg25026698.172.8144.013.111.919.219.6
IMPANeg125021590.773.1103.05.56.18.79.6
IMPAPos5016498.347.8139.619.220.527.227.7
IMPAPos10019595.472.3120.59.810.312.413.0
IMPAPos25026697.079.2188.47.47.610.911.2
IMPAPos125021591.370.4115.55.15.211.412.5
MPANeg5016498.73.3175.014.225.360.561.3
MPANeg100205100.041.9142.08.99.230.830.8
MPANeg25026699.566.0124.57.67.614.514.5
MPANeg1250225102.781.8130.510.59.912.412.1
MPAPos5016468.39.8139.613.420.336.653.6
MPAPos10020580.548.4149.714.012.626.833.3
MPAPos25026691.733.9153.78.07.831.834.7
MPAPos125022595.831.8208.212.68.343.445.3
MPA-D3Neg250846111.257.2190.816.212.530.026.9
MPA-D3Pos250685104.458.4151.814.314.018.017.3
PMPANeg5015487.877.6124.48.48.213.815.7
PMPANeg10019591.683.698.22.83.04.44.8
PMPANeg250266101.077.2123.85.04.812.112.0
PMPANeg125022599.284.8126.54.94.812.312.4
PMPAPos5016490.860.8148.815.816.125.628.2
PMPAPos10015495.286.8114.03.84.07.98.3
PMPAPos250205103.885.2136.14.53.815.314.7
PMPAPos125012399.888.8117.55.25.07.57.5
PMPA-13C6Neg25083699.574.8128.39.49.211.111.1


FIG. 1 Example ESI Positive Mode SRM Chromatograms Signal/Noise Ratios


FIG. 2 Example ESI Negative Mode SRM Chromatograms Signal/Noise Ratios

Details

ICS-code 13.060.50
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 Chro
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