EPA Method 8081B

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EPA Method 8081B:
Organochlorine Pesticides by GC-ECD. Official Name: Organochlorine Pesticides by Gas Chromatography

A measured volume or weight of sample (approximately 1 L for liquids, 2 to 30 g for solids) is extracted using the appropriate matrix-specific sample extraction technique. A variety of cleanup steps may be applied to the extract, depending on the nature of the matrix interferences and the target analytes. Suggested cleanups include alumina (Method 3610), Florisil (Method 3620), silica gel (Method 3630), gel permeation chromatography (Method 3640), and sulfur (Method 3660). After cleanup, the extract is analyzed by injecting a measured aliquot into a gas chromatograph with either a narrow-bore or wide-bore fused-silica capillary column, and either an electron capture detector (GC/ECD) or an electrolytic conductivity detector (GC/ELCD).

Method 8081 may be used to determine the concentrations of various organochlorine pesticides in extracts from solid and liquid matrices, using fused-silica, open-tubular, capillary columns with electron capture detectors (ECD) or electrolytic conductivity detectors (ELCD).

SW-846 Update IVB

(1) Contamination of samples, solvent, and carrier gases with target analytes (especially compounds common to environmental laboratories, like methylene chloride).(2) Contamination of samples with sulfur (primarily present in base-neutral fractions).(3) Septum bleed (compounds from the injection septum are analyzed with the sample).(4) Column bleed (compounds from column coating break down, decreasing column efficiency).(5) Ghost peaks (compounds adsorb strongly to the column and carry over to later runs).(6) Coelution of species.(7) Coextracted contaminants.(8) Phthalate esters interfere with detection of pesticides via electron capture detector.

QC Requirements:
(see ch.1, SW-846 Methods 3500, 8000), CV, calibration standard, initial demonstration of proficiency, MB, MS, MSD, LD, LCS, and the addition of surrogates to each field sample and QC sample, CS (after 20 samples)

Maximum Holding Time:
Aqueous samples - 7 days (sample), 40 days (extract). Solid samples - 14 days (sample), 40 (extract). Also, see SW-846 Chapter Four for information.



None given.

NOTE: SPIKING CONCENTRATION FOR PRECISION AND ACCURACY IS IN UNITS OF NANOGRAMS per GRAM (ng/g). Precision and accuracy data was obtained using three replicate analyses of a sewage sludge spiked with 500 to 1000 ng/g of analyte. Sample clean-up was performed using ultrasonic extraction (see SW-846 Method 3550). The method contains additional performance information obtained with Soxhlet Extraction and Solid Phase Extraction.

MDLs were determined using a solid phase extraction preparation (SW-846 Method 3535) through the analysis of 7 spiked wastewater replicates.

Revision Number:
Revision 2, November 2000