Development of an Alternate Test Procedure (ATP) for Analysis of Chlorinated Dibenzo-p-dioxins and Dibenzofurans by GC-MS/MS. SGS AXYS Method 16130

Collaborative Efforts to Improve Environmental Monitoring (Session 2)
Oral Presentation

Prepared by C. Hamilton1, J. Romano2, F. Dorman3, T. Anumol4, L. Walker, Jr5
1 - SGS AXYS Analytical Services Ltd., 2045 Mills Rd, Sidney, BC, V8L 5X2, Canada
2 - Joe Romano Consulting, , , United States
3 - Waters Corporation, , , United States
4 - Agilent Technologies, , , United States
5 - US Environmental Protection Agency, , , United States

Contact Information: [email protected]; 250-655-5802


In 2018 SGS AXYS, Waters, Agilent agreed to collaborate on development of protocols for GC-MS/MS analysis of Chlorinated Dibenzo-p-dioxins and Dibenzofurans with the goal of producing a fully validated method that has the same level of quality control as EPA Method 1613B and could result in an Alternate Test Procedure (ATP). Lem Walker guided us through the requirements for an ATP application.
SGS Method 16130 is the result of this process and an ATP application was submitted in June 2020. EPA determined that this method meets all requirements for measurement of 2,3,7,8-substituted tetra- through octa-chlorinated dibenzo-p-dioxins and dibenzofurans (PCDDs/PCDFs) in wastewater and plans to include the method in a future regulatory action after the normal notice-and-comment rulemaking process required for methods to be approved for nationwide use.
In this presentation I will describe the changes to EPA Method 1613B to incorporate the MS/MS operating protocols and to replace the method QC protocols that are specific to HRMS with analogous ones (achieving the same purpose) but appropriate for an MS/MS system. Validation of the method using an Agilent 7890 gas chromatograph with both the Waters Corporation APGC-Xevo TQ-XS system and the Agilent the 7010B Triple Quadrupole GC/MS will also be described, including analysis of environmental samples with complex matrices.
The results of the method validation will be described. Method detection limits (MDL) and Initial precision and recovery (IPR) data demonstrate the sensitivity and accuracy of the method. In addition, comparative data (HRMS versus MS/MS) has been acquired for nine different samples of each matrix type (aqueous/wastewater, solids, biosolids and tissues) demonstrating the applicability to this technique to samples with varied and complex matrix that provide data equivalent to existing EPA 1613B. Application of GC-MS/MS to other traditionally HRMS methods such as PCB congeners (EPA Method 1668), pesticides (EPA method 1699) and brominated diphenyl ethers (EPA Method 1614) will also be discussed.