ASTM D7597-09e1
(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
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. ,
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. 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 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.
TABLE 1 Detection Verification Level and Reporting Range AnalyteESI ModeDVL (μg/L)Reporting Range (μg/L) Diisopropyl methylphosphonatePositive15–150 Ethyl hydrogen dimethylamidophosphateNegative0.255–150 Ethyl hydrogen dimethylamidophosphatePositive0.255–150 Ethyl methylphosphonic acidNegative550–1500 Ethyl methylphosphonic acidPositive550–1500 Isopropyl methylphosphonic acidNegative1050–1500 Isopropyl Methylphosphonic acidPositive550–1500 Methylphosphonic acidNegative20100–1500 Methylphosphonic acidPositive1050–1500 Pinacolyl methylphosphonic acidNegative550–1500 Pinacolyl methylphosphonic acidPositive550–1500
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 (...
General Information
Relations
Buy Standard
Standards Content (Sample)
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
´1
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
´ NOTE—This Test Method was changed editorially in 2012.
1. Scope Level 2 due to not meeting the DVL criteria at the lower
concentration level. The DVL for MPA in the ESI negative
1.1 This procedure covers the determination of diisopropyl
mode is at 20 µg/L, which forces a raised reporting limit.
methylphosphonate (DIMP), ethyl hydrogen dimethylami-
However,themulti-laboratoryvalidationrequiredaspikeofall
dophosphate (EHDMAP), ethyl methylphosphonic acid
target analytes at Level 1 concentrations. The mean recovery
(EMPA), isopropyl methylphosphonic acid (IMPA), methyl-
for MPAin the ESI negative mode at this level was 98.7% as
phosphonic acid (MPA) and pinacolyl methylphosphonic acid
shown in Table 3. If your instrument’s sensitivity can meet the
(PMPA)(referredtocollectivelyasorganophosphonatesinthis
requirements in this test method, MPA may have a 50 µg/L
test method) in surface water by direct injection using liquid
reporting limit.
chromatography (LC) and detected with tandem mass spec-
1.5 This standard does not purport to address all of the
trometry (MS/MS) using electrospray ionization (ESI). These
safety concerns, if any, associated with its use. It is the
analytesarequalitativelyandquantitativelydeterminedbythis
responsibility of the user of this standard to establish appro-
method. This method adheres to single reaction monitoring
priate safety and health practices and determine the applica-
(SRM) mass spectrometry.
bility of regulatory limitations prior to use.
1.2 ThistestmethodhasbeendevelopedbyUSEPARegion
5 Chicago Regional Laboratory (CRL).
2. Referenced Documents
1.3 The values stated in SI units are to be regarded as 2
2.1 ASTM Standards:
standard. No other units of measurement are included in this
D1129Terminology Relating to Water
standard.
D1193Specification for Reagent Water
1.4 The detection verification level (DVL) and reporting
D2777Practice for Determination of Precision and Bias of
range for the organophosphonates are listed in Table 1.
Applicable Test Methods of Committee D19 on Water
1.4.1 The DVL is required to be at a concentration at least
D3856Guide for Management Systems in Laboratories
three times below the reporting limit (RL) and have a signal/
Engaged in Analysis of Water
noise ratio greater than 3:1. Fig. 1 displays the signal/noise
D3694Practices for Preparation of Sample Containers and
ratios at the DVLs for the organophosphonates in the ESI for Preservation of Organic Constituents
positive mode and Fig. 2 in the ESI negative mode.
D5847Practice for Writing Quality Control Specifications
1.4.2 The reporting limit is the concentration of the Level 1 for Standard Test Methods for Water Analysis
calibration standard as shown in Table 2 for the organophos-
E2554Practice for Estimating and Monitoring the Uncer-
phonatesexceptforMPAintheESInegativemodewhichisat tainty of Test Results of a Test Method in a Single
Laboratory Using a Control Sample Program
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
CurrenteditionapprovedDec.1,2009.PublishedFebruary2012.DOI:10.1520/ Standards volume information, refer to the standard’s Document Summary page on
D7597-09E01. the ASTM website.
Copyright ©ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA19428-2959. United States
1
---------------------- Page: 1 ----------------------
´1
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 Po
...
Questions, Comments and Discussion
Ask us and Technical Secretary will try to provide an answer. You can facilitate discussion about the standard in here.