A New Alternative Test Procedure for the Determination of Dioxins & Furans by Method 1613b Replacing GC-HRMS with GC-MS/MS

Collaborative Efforts to Improve Environmental Monitoring
Oral Presentation

Prepared by J. Morgan1, W. Lipps2
1 - Pace Analytical Services, 7210 Franklin Road, Lebanon, TN, 37090, United States
2 - Shimadzu, 7102 Riverwood Drive, Columbia, Maryland, 21046, United States

Contact Information: [email protected]; 615-347-5418


EPA Method 1613 Revision B, for the analysis of polychlorinated dioxins and furans (PCDDs/PCDFs) was developed in response to reports of very low, but measurable concentrations of 2,3,7,8-TCDD and 2,3,7,8- TCDF in finished paper products and wastewater effluents. The method is a gas chromatography with high-resolution mass spectrometry (GC/HRMS) that identifies target analytes in the presence of other organic contaminants at very low picogram per liter (pg/L) concentrations. In past three decades, however, there has been a significant decrease in the number of vendors that manufacture and support GC/HRMS instruments making them expensive to keep operating and maintained. Tandem Gas Chromatography Mass Spectrometry (GC/MS/MS), also known as Triple Quadrupole GCMS combines two mass spectrometers are assembled in series with a third quadrupole (or octapole) inserted between them to act as a collision cell. These instruments distinguish analytes of interest with high confidence at low concentrations offering many of the advantages of GC/HRMS without the need of high mass resolution. A GC/MS/MS method for measurement of PCDDs/PCDFs takes advantage of this newer technology. This presentation describes development and optimization of a new Alternative Test Procedure (ATP) for dioxins and furans by GC-MS/MS. The study was done in two phases, first development of instrument parameters, verification of sensitivity, and conducting interference studies. Next, real world matrices including multiple wastewater, soils and biosolids, and fish and tissue samples were evaluated. Data are compared to Method 1613b acceptance limits and to GC-HRMS data collected by Method 1613b.