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    ASTM D7598 - 16(2017)

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

    Active Standard ASTM D7598 | Developed by Subcommittee: D19.06

    Book of Standards Volume: 11.02

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    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 test method has been investigated for use with reagent and surface water.

    1. 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 test method. This test method adheres to single reaction monitoring (SRM) mass spectrometry.

    1.2 This test method has been developed by U.S. 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.

    TABLE 1 Detection Verification Level and Reporting Range


    DVL (μg/L)

    Reporting Range (μg/L)



    100–10 000

    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.

    FIG. 1 Example SRM Chromatograms Signal/Noise at Detection Verification Level

    Example SRM Chromatograms Signal/Noise at Detection
 Verification LevelExample SRM Chromatograms Signal/Noise at Detection
 Verification Level

    1.4.2 The RL is the concentration of the Level 1 calibration standard as shown in Table 2. The reporting limit for this test method is 100 μg/L.

    TABLE 2 Concentrations of Calibration Standards (PPB)


    LV 1

    LV 2

    LV 3

    LV 4

    LV 5

    LV 6

    LV 7





    1 000

    2 500

    5 000

    10 000





    1 000

    2 500

    5 000

    10 000

    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.

    1.6 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

    2. Referenced Documents (purchase separately) The documents listed below are referenced within the subject standard but are not provided as part of the standard.

    ASTM Standards

    D1129 Terminology Relating to Water

    D1193 Specification for Reagent Water

    D2777 Practice for Determination of Precision and Bias of Applicable Test Methods of Committee D19 on Water

    D3694 Practices for Preparation of Sample Containers and for Preservation of Organic Constituents

    D3856 Guide for Management Systems in Laboratories Engaged in Analysis of Water

    D5847 Practice for Writing Quality Control Specifications for Standard Test Methods for Water Analysis

    E2554 Practice for Estimating and Monitoring the Uncertainty of Test Results of a Test Method Using Control Chart Techniques

    Other Documents

    U.S. EPA publication SW-846 Test Methods for Evaluating Solid Waste, Physical/Chemical Methods Available from National Technical Information Service (NTIS), U.S. Department of Commerce, 5285 Port Royal Road, Springfield, VA, 22161 or at http://www.epa.gov/epawaste/hazard/testmethods/index.htm.

    ICS Code

    ICS Number Code 13.060.50 (Examination of water for chemical substances)

    UNSPSC Code

    UNSPSC Code

    Referencing This Standard
    Link Here
    Link to Active (This link will always route to the current Active version of the standard.)

    DOI: 10.1520/D7598-16R17

    Citation Format

    ASTM D7598-16(2017), Standard Test Method for Determination of Thiodiglycol in Water by Single Reaction Monitoring Liquid Chromatography/Tandem Mass Spectrometry, ASTM International, West Conshohocken, PA, 2017, www.astm.org

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