Annual Book of ASTM Standards, Section 11, Water and Environmental Technology, Volume 11.02, Water (I)
Citation Information:
Annual Book of ASTM Standards, Section 11, Water and Environmental Technology, Volume 11.02, Water (I): The Annual Book of ASTM Standards consists of 73 volumes, divided among 16 sections, of which this volume is one. It contains approved ASTM standards, provisional standards, and related materials. The methods in this volume are applicable for sampling and analysis of water, waterborne materials and wastes, water-formed deposits and fluvial sediments, surface water hydraulics and hydrologic measurements. For further information, contact ASTM at the following: ASTM, 100 Barr Harbor Drive, West Conshohocken, PA, 19428, Telephone: (610) 832-9500, Fax: (610) 832-9555 Email: service@astm.org, Website: http://www.astm.org
Brief Method Summary
Pesticides in a water sample are extracted with methylene chloride (CH2Cl2) using a separatory funnel. The extract is dried, concentrated, exchanged to methyl tert-butyl ether (MTBE), and concentrated to 5 mL. Analysis is performed on a gas chromatograph equipped with an electron capture detector (ECD).
Scope and Application
This test method covers the capillary gas chromatographic determination of various organochlorine pesticides, including some of their degradation products and related compounds in finished drinking water. This test method is not limited to this particular aqueous matrix; however, its applicability to other aqueous matrices must be determined.
Applicable Concentration Range
Varies by analyte (ug/L).
Interferences
Glassware must be cleaned scrupulously as soon as possible after use. The use of high-purity reagents and solvents helps minimize interference problems. Purification of solvents by distillation in all-glass systems may be required. Phthalate esters, found frequently in plastics, paints, and other common laboratory items, produce a positive response on an electron capture detector. Interfering contamination may occur when a sample containing low concentrations of analytes is analyzed immediately following a sample containing relatively high concentrations of analytes. Matrix interferences may be caused by contaminants that are coextracted from the sample. Also, note that all of the analytes listed in the Scope are not resolved from each other on any one column; that is, one analyte of interest may be an interferant for another analyte of interest. Caution must be taken in the determination of endrin since it has been reported that the splitless injector may cause endrin degradation Variable amounts of pesticides and PCBs from aqueous solutions may adhere to glass surfaces. It is recommended that sample transfers and glass surface contacts be minimized to the extent possible. Aldrin and methoxychlor are oxidized by chlorine rapidly.
Quality Control Requirements
Minimum of IDLC, IPC, LRBs, LFM; if available - QCSs
Sample Handling
Collect the sample in accordance with either Specification D 1192 or Practices D 3370, whichever is applicable. Glass bottles (1-L recommended) equipped with TFE-fluorocarbon or aluminum foil-lined screw caps, prepared in accordance with Practices D 3694, are used for sample collection. Fill a sufficient number of sample bottles with sample to permit the running of duplicates, spikes, and reanalyses.
Maximum Holding Time
Extract within 7 days of sample collection. Analyze within 14 days of sample extraction.
This method has been tested by eleven laboratories using reagent water and finished drinking water. The waters were spiked with 29 pesticides at six concentration levels, as three Youden pairs.
Detection Level Note:
Revision
PDF/Link
1996
The Water Quality Portal contains
sample results from
sites that use this method.
