Single-laboratory validation of EPA Method 8150 for determination of chlorinated herbicides in hazardous waste

Method 8150, published in the second edition of Test Methods for Evaluating Solid Waste, Manual SW-846, required optimization, ruggedness testing, linearity determinations, precision tests, bias testing, gas chromatographic/mass spectrometric confirmation, and quality control guidelines for validation of the protocol. This single-laboratory validation, which is applicable to the determination of the herbicides dicamba, silvex, 2,4-D, 2,4-DB, 2,4,5-T, dinoseb, MCPP, MCPA, and dichlorprop in hazardous waste extracts, was completed and is described in this report. Final ruggedness testing of the optimized procedure gave a mean recovery of 89.3% with a standard deviation of 4.3%. Percent relative standard deviations are less than 10 (n = 20, each analyte) over a 10(2) linear range of concentration for MCPP and MCPA and over a 10(3) linear range of concentration for the other target herbicide esters. Instrumental detection limits for electron capture detection and mass spectrometric identity confirmation were determined and found to be matrix-dependent.