This method is for the determination of polychlorinated dibenzo-p-dioxins (tetra- through octachlorinated homologues; PCDDs), and polychlorinated dibenzofurans (tetra- through octachlorinated homologues; PCDFs) including the seventeen tetra- through octa-chlorinated 2,3,7,8-substituted CDDs/CDFs using high resolution gas chromatography coupled with high resolution mass spectrometry (HRGC/HRMS). Method 8290 extends minimum levels of quantitation of CDDs/CDFs into the low parts per trillion range for solid matrices. The use of HRGC/HRMS for detection and quantitation of CDDs/CDFs as well as the method's use of isotope dilution techniques result- in improved sensitivity, precision, and accuracy over previous methods.
Extraction methods vary dependent upon the matrix type. One to ten grams of sample are typical sample sizes for solids. Soil, sediment, fly ash, and pulp/paper sample are extracted with toluene using Soxhlet extractor. Fuel oil and aqueous sludge samples are extracted with toluene using Dean-Stark Soxhlet, pressurized fluid extraction (PFE) by Method 3545, or microwave extraction by Method 3546. The extracts are acid-base washed, dried, solvent exchanged and then cleaned up using column chromatography using alumina, silica gel, and activated carbon. The extract is concentrated and analyzed by HRGC/HRMS.
2,3,7,8-TCDF must be separated from its closest eluting isomers and a confirmation analysis on a second column is needed if separation can't be acheived on the column used for the initial analysis.
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| Hold Times, Preservatives, Preps, Collection, Analytical & Documentation | |
|---|---|
| Holding Time: | 30 days from collection to extraction and 45 days from extraction to analysis |
| Preservatives: | Cool to ≤ 6°C. Protect sample from light. Tissue samples should be frozen at -20°C in the dark |
| Required Preps: | 4oz amber glass bottle |
| Collection Method: | Grab sampling, SW-846 Chapter 4 |
| Analytical Methodology: | HRGC/HRMS |
| Documentation: | 
8290A
|
* The analytes and detection limits listed for each method represent the typical detection limits and analytes reported for that particular method. Keep in mind that analyte lists may vary from laboratory to laboratory. Detection limits may also vary from lab to lab and are dependent upon the sample size, matrix, and any interferences that may be present in the sample.