ASTM D7598-09e2

Standard Test Method for Determination of Thiodiglycol in Water by Single Reaction Monitoring Liquid Chromatography/Tandem Mass Spectrometry

SIGNIFICANCE AND USE
5.1 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.4  
5.2 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.
1.4.2 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.

General Information

• Status: Historical
• Publication Date: 30-Nov-2009
• ICS: 13.060.50 - Examination of water for chemical substances
• Technical Committee: D19 - Water
• Drafting Committee: D19.06 - Methods for Analysis for Organic Substances in Water

Relations

• Replaces: ASTM D7598-09e1 - Standard Test Method for Determination of Thiodiglycol in Water by Single Reaction Monitoring Liquid Chromatography/Tandem Mass Spectrometry
• Effective Date: 01-Dec-2009
• Replaced By: ASTM D7598-16 - Standard Test Method for Determination of Thiodiglycol in Water by Single Reaction Monitoring Liquid Chromatography/Tandem Mass Spectrometry
• Effective Date: 01-Feb-2016

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
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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
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 2. Referenced Documents
2
1.1 This procedure covers the determination of thiodiglycol 2.1 ASTM Standards:
(TDG) in surface water by direct injection using liquid D1129Terminology Relating to Water
chromatography (LC) and detected with tandem mass spec- D1193Specification for Reagent Water
trometry (MS/MS). TDG is qualitatively and quantitatively D2777Practice for Determination of Precision and Bias of
determined by this method. This method adheres to single Applicable Test Methods of Committee D19 on Water
reaction monitoring (SRM) mass spectrometry. D3856Guide for Management Systems in Laboratories
Engaged in Analysis of Water
1.2 ThistestmethodhasbeendevelopedbyUSEPARegion
D3694Practices for Preparation of Sample Containers and
5 Chicago Regional Laboratory (CRL).
for Preservation of Organic Constituents
1.3 The values stated in SI units are to be regarded as
D5847Practice for Writing Quality Control Specifications
standard. No other units of measurement are included in this
for Standard Test Methods for Water Analysis
standard.
E2554Practice for Estimating and Monitoring the Uncer-
tainty of Test Results of a Test Method Using Control
1.4 The Detection Verification Level (DVL) and Reporting
Range for TDG are listed in Table 1. Chart Techniques
1.4.1 The DVL is required to be at a concentration at least 2.2 Other Documents:
EPApublication SW-846Test Methods for Evaluating Solid
3 times below the reporting limit (RL) and have a signal/noise
3
ratio greater than 3:1. Fig. 1 displays the signal/noise ratio at Waste, Physical/Chemical Methods
the DVL.
3. Terminology
1.4.2 The RL is the concentration of the level 1 calibration
3.1 Definitions:
standard as shown in Table 2. The reporting limit for this
3.1.1 detection verification level (DVL), n—a concentration
method is 100 µg/L.
that has a signal/noise ratio greater than 3:1 and is at least 3
1.5 This standard does not purport to address all of the
times below the reporting limit (RL).
safety concerns, if any, associated with its use. It is the
3.1.2 reporting limit (RL), n—the concentration of the
responsibility of the user of this standard to establish appro-
lowest-level calibration standard used for quantification.
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
1
This test method is under the jurisdiction ofASTM Committee D19 on Water Standards volume information, refer to the standard’s Document Summary page on
andisthedirectresponsibilityofSubcommitteeD19.06onMethodsforAnalysisfor the ASTM website.
3
Organic Substances in Water. Available from National Technical Information Service (NTIS), U.S. Depart-
Current edition approved Dec. 1, 2009. Published January 2010. DOI: 10.1520/ ment of Commerce, 5285 Port Royal Road, Springfield, VA, 22161 or at http://
D7598-09E02. 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
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D7598−09
TABLE 1 Detection Verification Level and Reporting Range
6.4 Matrix interferences may be caused by contaminants
Analyte DVL (µg/L) Reporting Range (µg/L) that are co-extracted from the sample. The extent of matrix
Thiodiglycol 20 100–10 000
interferences can vary considerably from sample source de-
pending on variations of the sample matrix.
7. Apparatus
7.1 LC/MS/MS System
3.2 Abbreviations:
7.1.1 LiquidChromatography(LC)System—AcompleteLC
3.2.1 ND—non-detect
5
systemisneededinordertoanalyzesamples. Asystemthatis
capable of performing at the flows, pressures, controlled
4. Summary of Test Methods
temperatures, sample volumes and requirements of the stan-
4.1 This is a performance based method and modifications
dard may be used.
are allowed to improve performance.
7.1.2 Analytical Column-SIELC—PrimesepSB5µm,100Å
4.2 Forthiodiglycolanalysis,samplesareshippedtothelab
particle, 150 mm × 2.1 mm or equivalent.
between0°Cand6°Candanalyze
...