ASTM D8024-23

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

SIGNIFICANCE AND USE
5.1 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 water matrices for understanding the sources and concentration levels in affected areas.  
5.2 This method has been used to determine TTPC in reagent water and a river water (Table 8). (A) Solution A: Level 8 stock solution prepared according to Section 12 and at Table 4 concentrations.(B) Solution B: 75 % Acetone, 25 % Water.    
Note 1: This test method has been used to characterize TTPC in real world water samples with success and similar recoveries as shown in Table 8.
SCOPE
1.1 This test method covers the determination of (Tri-n-butyl)-n-tetradecylphosphonium chloride (TTPC) in water by dilution with acetone, filtration and analysis by liquid chromatography/tandem mass spectrometry. This test method is not amenable for the analysis of isomeric mixtures of Tributyl-tetradecylphosphonium chloride. TTPC is a biocide that strongly adsorbs to soils.2 The water samples 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 100 ng/L to 4000 ng/L. This analyte is qualitatively and quantitatively determined by this method. This test method adheres to multiple reaction monitoring (MRM) mass spectrometry.  
1.2 A full collaborative study to meet the requirements of Practice D2777 has not been completed. This test method contains single-operator precision and bias based on single-operator data. Publication of standards that have not been fully validated is done to make the current technology accessible to users of standards, and to solicit additional input from the user community.  
1.3 The Method Detection Limit3 (MDL) and Reporting Range4 for the target analyte are listed in Table 1.      
1.3.1 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 4 for TTPC after taking into account a 2.5 mL water sample volume and a final diluted sample volume of 10 mL (75 % acetone/25 % water). The final solution volume is 10 mL because a 7.5 mL volume of acetone is added to each 2.5 mL water sample which is shaken and filtered.  
1.4 Units—The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
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, health, and environmental 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.

General Information

• Status: Published
• Publication Date: 14-Apr-2023
• 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

Standards Content (Sample)

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.
Designation: D8024 − 23
Standard Test Method for
Determination of (Tri-n-butyl)-n-tetradecylphosphonium
chloride (TTPC) in Water by Multiple Reaction Monitoring
1
Liquid Chromatography/Mass Spectrometry (LC/MS/MS)
This standard is issued under the fixed designation D8024; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope 1.3.1 The reporting limit in this test method is the minimum
value below which data are documented as non-detects. Ana-
1.1 This test method covers the determination of (Tri-n-
lyte detections between the method detection limit and the
butyl)-n-tetradecylphosphonium chloride (TTPC) in water by
reporting limit are estimated concentrations and are not re-
dilution with acetone, filtration and analysis by liquid
ported following this test method. The reporting limit is
chromatography/tandem mass spectrometry. This test method
calculated from the concentration of the Level 1 calibration
is not amenable for the analysis of isomeric mixtures of
standard as shown in Table 4 for TTPC after taking into
Tributyl-tetradecylphosphonium chloride. TTPC is a biocide
2 account a 2.5 mL water sample volume and a final diluted
that strongly adsorbs to soils. The water samples are prepared
sample volume of 10 mL (75 % acetone/25 % water). The final
in a solution of 75 % acetone and 25 % water because TTPC
solution volume is 10 mL because a 7.5 mL volume of acetone
has an affinity for surfaces and particles. The reporting range
is added to each 2.5 mL water sample which is shaken and
for this method is from 100 ng ⁄L to 4000 ng ⁄L. This analyte is
filtered.
qualitatively and quantitatively determined by this method.
This test method adheres to multiple reaction monitoring 1.4 Units—The values stated in SI units are to be regarded
(MRM) mass spectrometry. as standard. No other units of measurement are included in this
standard.
1.2 A full collaborative study to meet the requirements of
1.5 This standard does not purport to address all of the
Practice D2777 has not been completed. This test method
safety concerns, if any, associated with its use. It is the
contains single-operator precision and bias based on single-
responsibility of the user of this standard to establish appro-
operator data. Publication of standards that have not been fully
priate safety, health, and environmental practices and deter-
validated is done to make the current technology accessible to
mine the applicability of regulatory limitations prior to use.
users of standards, and to solicit additional input from the user
1.6 This international standard was developed in accor-
community.
dance with internationally recognized principles on standard-
3
1.3 The Method Detection Limit (MDL) and Reporting
ization established in the Decision on Principles for the
4
Range for the target analyte are listed in Table 1.
Development of International Standards, Guides and Recom-
mendations issued by the World Trade Organization Technical
Barriers to Trade (TBT) Committee.
1
This test method is under the jurisdiction of ASTM Committee D19 on Water
and is the direct responsibility of Subcommittee D19.06 on Methods for Analysis for
2. Referenced Documents
Organic Substances in Water.
5
Current edition approved April 15, 2023. Published May 2023. Originally
2.1 ASTM Standards:
approved in 2016. Last previous edition approved in 2016 as D8024 – 16. DOI:
D1129 Terminology Relating to Water
10.1520/D8024-23.
2 D1193 Specification for Reagent Water
More information on TTPC can be found at http://www.buruenergy.com/wp-
content/uploads/BE-Environmental-Properties-of-Proposed-Biocide-BE-91.pdf
D2777 Practice for Determination of Precision and Bias of
(2014) and http://iaspub.epa.gov/sor_internet/registry/substreg/searchandretrieve/
Applicable Test Methods of Committee D19 on Water
advancedsearch/externalSearch.do?p_type=CASNO&p=81741-28-8 (2014).
D3856 Guide for Management Systems in Laboratories
3
The MDL is determined following the Code of Federal Regulations, 40 CFR
Engaged in Analysis of Water
Part 136, Appendix B, as a guide. A detailed process determining the MDL is
explained in the reference and is beyond the scope of this test method to be
explained here.
4
Reporting range concentration is calculated from Table 4 concentrations
5
assuming a 50 μL injection of the Level 1 calibration standard for TTPC, and the For referenced ASTM standards, visit the ASTM website, www.astm.org, or
highest leve
...

This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation: D8024 − 16 D8024 − 23
Standard Test Method for
Determination of (Tri-n-butyl)-n-tetradecylphosphonium
chloride (TTPC) in Water by Multiple Reaction Monitoring
1
Liquid Chromatography/Mass Spectrometry (LC/MS/MS)
This standard is issued under the fixed designation D8024; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope
1.1 This test method covers the determination of (Tri-n-butyl)-n-tetradecylphosphonium chloride (TTPC) in water by dilution with
acetone, filtration and analysis by liquid chromatography/tandem mass spectrometry. This test method is not amenable for the
2
analysis of isomeric mixtures of Tributyl-tetradecylphosphonium chloride. TTPC is a biocide that strongly adsorbs to soils. The
water samples 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 100–4000100 ng ng/L. ⁄L to 4000 ng ⁄L. This analyte is qualitatively and quantitatively
determined by this method. This test method adheres to multiple reaction monitoring (MRM) mass spectrometry.
1.2 A full collaborative study to meet the requirements of Practice D2777 has not been completed. This test method contains
single-operator precision and bias based on single-operator data. Publication of standards that have not been fully validated is done
to make the current technology accessible to users of standards, and to solicit additional input from the user community.
3 4
1.3 The Method Detection Limit (MDL) and Reporting Range for the target analyte are listed in Table 1.
1.3.1 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 4
for TTPC after taking into account a 2.5 mL water sample volume and a final diluted sample volume of 10 mL (75 % acetone/25
% water). The final solution volume is 10 mL because a 7.5 mL volume of acetone is added to each 2.5 mL water sample which
is shaken and filtered.
1.4 Units—The values stated in SI units are to be regarded as standard. No other units of measurement are included in this
standard.
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, health, and environmental practices and determine the applicability of
regulatory limitations prior to use.
1
This test method is under the jurisdiction of ASTM Committee D19 on Water and is the direct responsibility of Subcommittee D19.06 on Methods for Analysis for
Organic Substances in Water.
Current edition approved June 1, 2016April 15, 2023. Published August 2016May 2023. Originally approved in 2016. Last previous edition approved in 2016 as
D8024 – 16. DOI: 10.1520/D8024-16.10.1520/D8024-23.
2
More information on TTPC can be found at http://www.buruenergy.com/wp-content/uploads/BE-Environmental-Properties-of-Proposed-Biocide-BE-91.pdf (2014) and
http://iaspub.epa.gov/sor_internet/registry/substreg/searchandretrieve/advancedsearch/externalSearch.do?p_type=CASNO&p=81741-28-8 (2014).
3
The MDL is determined following the Code of Federal Regulations, 40 CFR Part 136, Appendix B, as a guide. A detailed process determining the MDL is explained
in the reference and is beyond the scope of this test method to be explained here.
4
Reporting range concentration is calculated from Table 4 concentrations assuming a 50 μL injection of the Level 1 calibration standard for TTPC, and the highest level
calibration standard with a 10 mL final diluted sample volume starting with a 2.5 mL water sample. Volume variations will change the reporting limit and ranges.
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1

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D8024 − 23
TABLE 1 Method Detection Limit and Reporting Range
MDL Reporting Range
Analyte
(ng/L) (ng/L)
TTPC 13 100–4000
1.6 This international standard was developed in accordance with internation
...