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 quadrillion (ppq) range for aqueous 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.
Samples that have more than 1% solids are filtered prior to extraction and the aqueous and solid phases are extracted separately. One liter of sample is extracted with methylene chloride using a liquid-liquid extraction or solid phase extraction (SPE) by Method 3535. 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. |
| Required Preps: | 1L amber glass bottle |
| Collection Method: | Grab sampling following SW-846 Chapter 4 procedures. |
| 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.