ASTM D7597-09e2
(Test Method)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
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
SIGNIFICANCE AND USE
5.1 Organophosphate pesticides affect the nervous system by disrupting the enzyme that regulates acetylcholine, a neurotransmitter. They were developed during the early 19th century, but their effects on insects, which are similar to their effects on humans, were discovered in 1932. Some are poisonous and were used as chemical weapon agents. Organophosphate pesticides are usually not persistent in the environment.4, 5
5.2 This test method is for the analysis of selected organophosphorous-based chemical weapon agent degradation products from Sarin (GB), Soman (GD), Tabun (GA) and VX. This method has been investigated for use with reagent and surface water.
SCOPE
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. 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 instrument’s 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.
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Designation:D7597 −09
StandardTest 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
1
Spectrometry
This standard is issued under the fixed designation D7597; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1
ε NOTE—This test method was changed editorially in February 2012.
2
ε NOTE—Added research report footnote to Section 16 editorially in June 2013.
1. Scope phonates except for MPAin the ESI negative mode which is at
Level 2 due to not meeting the DVL criteria at the lower
1.1 This procedure covers the determination of diisopropyl
concentration level. The DVL for MPA in the ESI negative
methylphosphonate (DIMP), ethyl hydrogen dimethylami-
mode is at 20 µg/L, which forces a raised reporting limit.
dophosphate (EHDMAP), ethyl methylphosphonic acid
However,themulti-laboratoryvalidationrequiredaspikeofall
(EMPA), isopropyl methylphosphonic acid (IMPA), methyl-
target analytes at Level 1 concentrations. The mean recovery
phosphonic acid (MPA) and pinacolyl methylphosphonic acid
for MPAin the ESI negative mode at this level was 98.7% as
(PMPA)(referredtocollectivelyasorganophosphonatesinthis
shown in Table 3. If your instrument’s sensitivity can meet the
test method) in surface water by direct injection using liquid
requirements in this test method, MPA may have a 50 µg/L
chromatography (LC) and detected with tandem mass spec-
reporting limit.
trometry (MS/MS) using electrospray ionization (ESI). These
analytesarequalitativelyandquantitativelydeterminedbythis
1.5 This standard does not purport to address all of the
method. This method adheres to single reaction monitoring
safety concerns, if any, associated with its use. It is the
(SRM) mass spectrometry.
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica-
1.2 ThistestmethodhasbeendevelopedbyUSEPARegion
bility of regulatory limitations prior to use.
5 Chicago Regional Laboratory (CRL).
1.3 The values stated in SI units are to be regarded as
2. Referenced Documents
standard. No other units of measurement are included in this
2
standard.
2.1 ASTM Standards:
D1129Terminology Relating to Water
1.4 The detection verification level (DVL) and reporting
D1193Specification for Reagent Water
range for the organophosphonates are listed in Table 1.
D2777Practice for Determination of Precision and Bias of
1.4.1 The DVL is required to be at a concentration at least
Applicable Test Methods of Committee D19 on Water
three times below the reporting limit (RL) and have a signal/
D3856Guide for Management Systems in Laboratories
noise ratio greater than 3:1. Fig. 1 displays the signal/noise
Engaged in Analysis of Water
ratios at the DVLs for the organophosphonates in the ESI
D3694Practices for Preparation of Sample Containers and
positive mode and Fig. 2 in the ESI negative mode.
for Preservation of Organic Constituents
1.4.2 The reporting limit is the concentration of the Level 1
D5847Practice for Writing Quality Control Specifications
calibration standard as shown in Table 2 for the organophos-
for Standard Test Methods for Water Analysis
1
This test method is under the jurisdiction ofASTM Committee D19 on Water
2
andisthedirectresponsibilityofSubcommitteeD19.06onMethodsforAnalysisfor For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Organic Substances in Water. contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Current edition approved Dec. 1, 2009. Published January 2010. DOI: 10.1520/ Standards volume information, refer to the standard’s Document Summary page on
D7597-09E02. the ASTM website.
Copyright ©ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA19428-2959. United States
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D7597−09
TABLE 1 Detection Verification Level and Reporting Range
Analyte ESI Mode DVL (µg/L) Reporting Range (µg/L)
Diisopropyl methylphosphonate Positive 1 5–150
Ethyl hydrogen dimethylamidophosphate Negative 0.25 5–150
Ethyl hydrogen dimethylamidophosphate Positive 0.25 5–150
Ethyl methylphosphonic acid Negative 5 50–1500
Ethyl methylphosphonic acid Positive 5 50–1500
Isopropyl methylphosphonic acid Negative 10 50–1500
Isopropyl Methylphosphonic acid Positive 5 50–1500
Methylphosphonic acid Negative 20 100–1500
Methylphosphonic acid Positive 10 50–1500
Pinacolyl methylphospho
...
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