EPA Method 1658

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EPA Method 1658:
The Determination of Phenoxy-Acid Herbicides in Municipal and Industrial Wastewater

Samples containing low solids: If the solids content is less than or equal to 1%, the sample is extracted directly using continuous extraction techniques. The pH of a 1-L sample is raised to 12 to 13 to hydrolyze acid esters, and the sample is extracted with methylene chloride to remove interferences. The pH is lowered to less than 2 and the free acids are extracted with methylene chloride. Solids content 1 to 30%: The sample is diluted to 1% solids with reagent water, homogenized ultrasonically, and extracted as a low-solids sample. Solids content greater than 30%: The sample is placed in an extraction bottle and approximately 1 L of basic (pH 12 to 13) water is added. The bottle is tumbled for 18 hours. The water is removed and extracted as a low-solids sample.

This method is designed to meet the survey requirements of the Environmental Protection Agency (EPA). It is used to determine (1) the phenoxy-acid herbicides and herbicide esters associated with the Clean Water Act, the Resource Conservation and Recovery Act, and the Comprehensive Environmental Response, Compensation and Liability Act; and (2) other compounds amenable to extraction and analysis by automated, wide-bore capillary column gas chromatography (GC) with electron capture or halogen-selective detectors.

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