ASTM D7598-09e1
(Test Method)Standard Test Method for Determination of Thiodiglycol in Water by Single Reaction Monitoring Liquid Chromatography/Tandem Mass Spectrometry
Standard Test Method for Determination of Thiodiglycol in Water by Single Reaction Monitoring Liquid Chromatography/Tandem Mass Spectrometry
SIGNIFICANCE AND USE
Thiodiglycol is a Schedule 2 compound under the Chemical Weapons Convention (CWC). Schedule 2 chemicals include those that are precursors to chemical weapons, chemical weapons agents or have a number of other commercial uses. They are used as ingredients to produce insecticides, herbicides, lubricants, and some pharmaceutical products. Schedule 2 chemicals can be found in applications unrelated to chemical weapons. Thiodiglycol is both a mustard gas precursor and degradant as well as an ingredient in water-based inks, ballpoint pen inks, dyes and some pesticides.
This method has been investigated for use with reagent and surface water.
SCOPE
1.1 This procedure covers the determination of thiodiglycol (TDG) in surface water by direct injection using liquid chromatography (LC) and detected with tandem mass spectrometry (MS/MS). TDG is 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 TDG are listed in Table 1.
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 ratio at the DVL.
1.4.2 The RL is the concentration of the level 1 calibration standard as shown in Table 2. The reporting limit for this method is 100 μg/L.
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 AnalyteDVL (μg/L)Reporting Range (μg/L) Thiodiglycol20100–10 000
TABLE 2 Concentrations of Calibration Standards (PPB) Analyte/Surrogate LV 1LV 2LV 3LV 4LV 5LV 6LV 7 Thiodiglycol10025050010002500500010 000 3,3’-Thiodipropanol10025050010002500500010 000
FIG. 1 Example SRM Chromatograms Signal/Noise at Detection Verification Level
General Information
Relations
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:D7598 −09
StandardTest Method for
Determination of Thiodiglycol in Water by Single Reaction
Monitoring Liquid Chromatography/Tandem Mass
1
Spectrometry
This standard is issued under the fixed designation D7598; 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 D1193Specification for Reagent Water
D2777Practice for Determination of Precision and Bias of
1.1 This procedure covers the determination of thiodiglycol
Applicable Test Methods of Committee D19 on Water
(TDG) in surface water by direct injection using liquid
D3856Guide for Management Systems in Laboratories
chromatography (LC) and detected with tandem mass spec-
Engaged in Analysis of Water
trometry (MS/MS). TDG is qualitatively and quantitatively
D3694Practices for Preparation of Sample Containers and
determined by this method. This method adheres to single
for Preservation of Organic Constituents
reaction monitoring (SRM) mass spectrometry.
D5847Practice for Writing Quality Control Specifications
1.2 ThistestmethodhasbeendevelopedbyUSEPARegion
for Standard Test Methods for Water Analysis
5 Chicago Regional Laboratory (CRL).
E2554Practice for Estimating and Monitoring the Uncer-
1.3 The values stated in SI units are to be regarded as tainty of Test Results of a Test Method in a Single
Laboratory Using a Control Sample Program
standard. No other units of measurement are included in this
standard.
2.2 Other Documents:
EPApublication SW-846Test Methods for Evaluating Solid
1.4 The Detection Verification Level (DVL) and Reporting
3
Waste, Physical/Chemical Methods
Range for TDG are listed in Table 1.
1.4.1 The DVL is required to be at a concentration at least
3. Terminology
3 times below the reporting limit (RL) and have a signal/noise
ratio greater than 3:1. Fig. 1 displays the signal/noise ratio at 3.1 Definitions:
3.1.1 detection verification level (DVL), n—a concentration
the DVL.
1.4.2 The RL is the concentration of the level 1 calibration that has a signal/noise ratio greater than 3:1 and is at least 3
times below the reporting limit (RL).
standard as shown in Table 2. The reporting limit for this
method is 100 µg/L.
3.1.2 reporting limit (RL), n—the concentration of the
lowest-level calibration standard used for quantification.
1.5 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
3.2 Abbreviations:
responsibility of the user of this standard to establish appro-
3.2.1 ND—non-detect
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use.
4. Summary of Test Methods
4.1 This is a performance based method and modifications
2. Referenced Documents
are allowed to improve performance.
2
2.1 ASTM Standards:
4.2 Forthiodiglycolanalysis,samplesareshippedtothelab
D1129Terminology Relating to Water
between0°Cand6°Candanalyzedwithin7daysofcollection.
1
Inthelab,thesamplesarespikedwithsurrogate,filteredusing
This test method is under the jurisdiction ofASTM Committee D19 on Water
andisthedirectresponsibilityofSubcommitteeD19.06onMethodsforAnalysisfor
a syringe driven Millex HV PVDF filter unit and analyzed
Organic Substances in Water.
directly by LC/MS/MS.
CurrenteditionapprovedDec.1,2009.PublishedFebruary2012.DOI:10.1520/
D7598-09E01.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
3
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Available from National Technical Information Service (NTIS), U.S. Depart-
Standards volume information, refer to the standard’s Document Summary page on ment of Commerce, 5285 Port Royal Road, Springfield, VA, 22161 or at http://
the ASTM website. www.epa.gov/epawaste/hazard/testmethods/index.htm.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
---------------------- Page: 1 ----------------------
´1
D7598−09
TABLE 1 Detection Verification Level and Reporting Range
7.1.2 Analytical Column-SIELC—PrimesepSB5µm,100Å
Analyte DVL (µg/L) Reporting Range (µg/L) particle, 150 mm × 2.1 mm or equivalent.
Thiodiglycol 20 100–10 000
7.1.3 Tandem Mass Spectrometer (MS/MS) System—A
6
MS/MS system capable of MRM analysis. A system that is
capableofperformingattherequirementsinthisstandardmay
4.3 Thiodiglycol and 3,3’-thiodipropanol (surrogate) are
be used.
identifiedbyretentiontimeandoneSRMtransition.Thetarget
7.2 Filtration Device
analyteandsurrogatearequantitatedusingtheSRMtransitions
7.2.1 Hypodermic syringe—Alocktipglasssyringecap
...
Questions, Comments and Discussion
Ask us and Technical Secretary will try to provide an answer. You can facilitate discussion about the standard in here.