ASTM D8025-23

Standard Test Method for Determination of Select Pesticides in Water by Multiple Reaction Monitoring Liquid Chromatography Tandem Mass Spectrometry

SIGNIFICANCE AND USE
5.1 Pesticides may be used in various agricultural and household products. These products may enter waterways at low levels through run-off or misuse near water resources. Hence, there is a need for quick, easy and robust method to determine pesticide concentration in water matrices for understanding the sources and concentration levels in affected areas.  
5.2 This method has been single-laboratory validated in reagent water and surface waters (Tables 12-14).
SCOPE
1.1 This test method covers a method for analysis of selected pesticides in a water matrix by filtration followed with liquid chromatography/electrospray ionization tandem mass spectrometry analysis. The samples are prepared in 20 % methanol, filtered, and analyzed by liquid chromatography/tandem mass spectrometry. This method was developed for an agricultural run-off study, not for low level analysis of pesticides in drinking water. This method may be modified for lower level analysis. The analytes are qualitatively and quantitatively determined by this method. This 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 standard 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 A reporting limit check sample (RLCS) is analyzed during every batch to ensure that if an analyte was present in a sample at or near the reporting limit it would be positively identified and accurately quantitated within set quality control limits. A method detection limit (MDL) study was not done for this method, the method detection limits would be much lower than the reporting limits in this method and would be irrelevant. A RLCS was determined to be more applicable for this standard. If this method is adapted to report much lower or near the MDL then a MDL study would be warranted.  
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 The Reporting Range for the target analytes are listed in Table 1.  
1.5.1 The reporting limit in this test method is the minimum value below which data are documented as non-detects. The reporting limit is calculated from the concentration of the Level 1 calibration standard as shown in Table 6 after taking into account an 8 mL water sample volume and a final diluted sample volume of 10 mL (80 % water/20 % methanol).  
1.6 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.  
1.7 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: D8025 − 23
Standard Test Method for
Determination of Select Pesticides in Water by Multiple
Reaction Monitoring Liquid Chromatography Tandem Mass
1
Spectrometry
This standard is issued under the fixed designation D8025; 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 1.5 The Reporting Range for the target analytes are listed in
Table 1.
1.1 This test method covers a method for analysis of
1.5.1 The reporting limit in this test method is the minimum
selected pesticides in a water matrix by filtration followed with
value below which data are documented as non-detects. The
liquid chromatography/electrospray ionization tandem mass
reporting limit is calculated from the concentration of the Level
spectrometry analysis. The samples are prepared in 20 %
1 calibration standard as shown in Table 6 after taking into
methanol, filtered, and analyzed by liquid chromatography/
account an 8 mL water sample volume and a final diluted
tandem mass spectrometry. This method was developed for an
sample volume of 10 mL (80 % water/20 % methanol).
agricultural run-off study, not for low level analysis of pesti-
1.6 This standard does not purport to address all of the
cides in drinking water. This method may be modified for
safety concerns, if any, associated with its use. It is the
lower level analysis. The analytes are qualitatively and quan-
responsibility of the user of this standard to establish appro-
titatively determined by this method. This method adheres to
priate safety, health, and environmental practices and deter-
multiple reaction monitoring (MRM) mass spectrometry.
mine the applicability of regulatory limitations prior to use.
1.2 A full collaborative study to meet the requirements of
1.7 This international standard was developed in accor-
Practice D2777 has not been completed. This standard contains
dance with internationally recognized principles on standard-
single-operator precision and bias based on single-operator
ization established in the Decision on Principles for the
data. Publication of standards that have not been fully validated
Development of International Standards, Guides and Recom-
is done to make the current technology accessible to users of
mendations issued by the World Trade Organization Technical
standards, and to solicit additional input from the user com-
Barriers to Trade (TBT) Committee.
munity.
2. Referenced Documents
1.3 A reporting limit check sample (RLCS) is analyzed
2
during every batch to ensure that if an analyte was present in
2.1 ASTM Standards:
a sample at or near the reporting limit it would be positively
D1129 Terminology Relating to Water
identified and accurately quantitated within set quality control
D1193 Specification for Reagent Water
limits. A method detection limit (MDL) study was not done for
D2777 Practice for Determination of Precision and Bias of
this method, the method detection limits would be much lower
Applicable Test Methods of Committee D19 on Water
than the reporting limits in this method and would be irrel-
D3856 Guide for Management Systems in Laboratories
evant. A RLCS was determined to be more applicable for this
Engaged in Analysis of Water
standard. If this method is adapted to report much lower or near
D4841 Practice for Estimation of Holding Time for Water
the MDL then a MDL study would be warranted.
Samples Containing Organic and Inorganic Constituents
D5847 Practice for Writing Quality Control Specifications
1.4 Units—The values stated in SI units are to be regarded
for Standard Test Methods for Water Analysis
as standard. No other units of measurement are included in this
E2554 Practice for Estimating and Monitoring the Uncer-
standard.
tainty of Test Results of a Test Method Using Control
Chart Techniques
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
Organic Substances in Water. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved April 15, 2023. Published June 2023. Originally contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
approved in 2016. Last previous edition approved in 2016 as D8025 – 16. DOI: Standards volume information, refer to the standard’s Document Summary page on
10.1520/D8025-23. the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, Wes
...

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: D8025 − 16 D8025 − 23
Standard Test Method for
Determination of Select Pesticides in Water by Multiple
Reaction Monitoring Liquid Chromatography Tandem Mass
1
Spectrometry
This standard is issued under the fixed designation D8025; 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 procedure test method covers a method for analysis of selected pesticides in a water matrix by filtration followed with
liquid chromatography/electrospray ionization tandem mass spectrometry analysis. The samples are prepared in 20 % 20 %
methanol, filtered, and analyzed by liquid chromatography/tandem mass spectrometry. This method was developed for an
agricultural run-off study, not for low level analysis of pesticides in drinking water. This method may be modified for lower level
analysis. The analytes are qualitatively and quantitatively determined by this method. This 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 standard 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 A reporting limit check sample (RLCS) is analyzed during every batch to ensure that if an analyte was present in a sample
at or near the reporting limit it would be positively identified and accurately quantitated within set quality control limits. A method
detection limit (MDL) study was not done for this method, the method detection limits would be much lower than the reporting
limits in this method and would be irrelevant. A RLCS was determined to be more applicable for this standard. If this method is
adapted to report much lower or near the MDL then a MDL study would be warranted.
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 The Reporting Range for the target analytes are listed in Table 1.
1.5.1 The reporting limit in this test method is the minimum value below which data are documented as non-detects. The reporting
limit is calculated from the concentration of the Level 1 calibration standard as shown in Table 6 after taking into account an 8
mL water sample volume and a final diluted sample volume of 10 mL (80 % water/20 % methanol).
1.6 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 2016June 2023. Originally approved in 2016. Last previous edition approved in 2016 as
D8025 – 16. DOI: 10.1520/D8025-16.10.1520/D8025-23.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

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D8025 − 23
TABLE 1 Reporting Range
Analyte Reporting Ranges, (ng/L)
2,4-D 250–10 000
Acetochlor 250–10 000
Alachlor 250–10 000
Aldicarb 250–10 000
Atrazine 62.5–2 500
Desethylatrazine 62.5–2 500
Desisopropylatrazine 125–5 000
Azoxystrobin 31.2–1 250
Bentazon 250–10 000
Carbaryl 250–10 000
Chlorpyrifos 250–10 000
Clopyralid 25 000–1 000 000
Clothianidin 62.5–2 500
Diazinon 62.5–2 500
Dicamba 12 500–500 000
Fipronil 250–10 000
Imidacloprid 62.5–2 500
Malathion 125–5 000
Methomyl 250–10 000
Metolachlor 62.5–2 500
Metribuzin 125–5 000
Picloram 6 250–250 000
Propiconazole 62.5–2 500
Simazine 62.5–2 500
Tebuconazole 62.5–2 500
Thiamethoxam 62.5–2 500
Triclopyr 1 250–5 000
1.7 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 O
...