ASTM D8018 - 15

    Standard Test Method for Determination of (Tri-n-butyl)-n-tetradecylphosphonium chloride (TTPC) in Soil by Multiple Reaction Monitoring Liquid Chromatography/Mass Spectrometry (LC/MS/MS)

    Active Standard ASTM D8018 | Developed by Subcommittee: D34.01.06

    Book of Standards Volume: 11.04


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    Significance and Use

    5.1 This test method has been developed by the US EPA Region 5 Chicago Regional Laboratory (CRL).

    5.2 TTPC may be used in various industrial and commercial products for use as a biocide. Products containing TTPC have been approved for controlling algal, bacterial, and fungal slimes in industrial water systems.2 TTPC should not be persistent in water but may be deposited in sediments at concentrations of concern. Hence, there is a need for quick, easy, and robust method to determine TTPC concentration at trace levels in various soil matrices for understanding the sources and concentration levels in affected soils and sediments.

    5.3 This method has been used to determine TTPC in sand, a commercial top soil and four ASTM reference soils (Table 4).

    1. Scope

    1.1 This procedure covers the determination of (Tri-n-butyl)-n-tetradecylphosphonium chloride (TTPC) in a soil matrix by extraction with acetone, filtration, dilution with water, and analysis by liquid chromatography/tandem mass spectrometry. TTPC is a biocide that strongly adsorbs to soils.2 The sample extracts are prepared in a solution of 75 % acetone and 25 % water because TTPC has an affinity for surfaces and particles. The reporting range for this method is from 250 to 10 000 ng/kg. This analyte is qualitatively and quantitatively determine by this method. This method adheres to multiple reaction monitoring (MRM) mass spectrometry.

    1.2 The Method Detection Limit (Note 1) (MDL) and Reporting Range (Note 2) for the target analyte are listed in Table 1.

    (A) Acronyms are defined in 3.3.

    Note 1: The MDL is determined following the Code of Federal Regulations, 40 CFR Part 136, Appendix B, as a guide utilizing solvent extraction of soil. Two-gram sample of Ottawa Sand was utilized. A detailed process determining the MDL is explained in the reference and is beyond the scope of this standard to be explained here.

    Note 2: Reporting range concentration is calculated from Table 2 concentrations assuming a 50 μL injection of the Level 1 calibration standard for TTPC, and the highest level calibration standard with a 20 mL final extract volume of a 2 g soil sample. Volume variations will change the reporting limit and ranges.

    1.2.1 The reporting limit in this test method is the minimum value below which data are documented as non-detects. Analyte detections between the method detection limit and the reporting limit are estimated concentrations and are not reported following this test method. The reporting limit is calculated from the concentration of the Level 1 calibration standard as shown in Table 2 for TTPC after taking into account a 2 g sample weight and a final extract volume of 20 mL in 75 % acetone/25 % water. The final extract volume is 20 mL because a 15 mL volume of acetone is added to each soil sample and only the liquid layer after extraction is filtered leaving the solid behind followed by the addition of 5 mL of water to the acetone extract.

    1.3 Units—The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.

    1.4 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.


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

    Other Documents

    40 CFR Part 136, Appendix B Definition and Procedure for the Determination of the Method Detection Limit

    EPA Publication SW-846

    ASTM Standards

    D1193 Specification for Reagent Water

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

    D5681 Terminology for Waste and Waste Management

    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


    ICS Code

    ICS Number Code 13.080.10 (Chemical characteristics of soil)

    UNSPSC Code

    UNSPSC Code 11111501(Soil)


    Referencing This Standard
    Link Here
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    DOI: 10.1520/D8018-15

    Citation Format

    ASTM D8018-15, Standard Test Method for Determination of (Tri-n-butyl)-n-tetradecylphosphonium chloride (TTPC) in Soil by Multiple Reaction Monitoring Liquid Chromatography/Mass Spectrometry (LC/MS/MS), ASTM International, West Conshohocken, PA, 2015, www.astm.org

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