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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).
1.1 This procedure 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 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 .
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 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.
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
D3856 Guide for Management Systems in Laboratories Engaged in Analysis of Water
D4841 Practice for Estimation of Holding Time for Water Samples Containing Organic and Inorganic Constituents
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 DocumentEPA 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 Number Code 13.060.50 (Examination of water for chemical substances)
UNSPSC Code 10191500(Pesticides or pest repellents)
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ASTM D8025-16, Standard Test Method for Determination of Select Pesticides in Water by Multiple Reaction Monitoring Liquid Chromatography Tandem Mass Spectrometry, ASTM International, West Conshohocken, PA, 2016, www.astm.orgBack to Top