Development and Validation of an Alternate Procedure for PCDD/PCDF analysis by EPA Method 1613B. Adaptation of HRMS Protocols and Criteria to MS/MS.

Vendor Lunch Speaker
Oral Presentation

Prepared by C. Hamilton
SGS AXYS, 2045 Mills Road West, Sidney, BC, V8L 5X2, Canada

Contact Information:; 250 655 5802


Historically, standard methods for the analysis of chlorinated dioxins and furans, PCBs and other halogenated compounds have relied on GC/HRMS to achieve high sensitivity and specificity and reliable quantification. HRMS is being replaced by newer technologies such as MS/MS which offers many of the specificity and sensitivity advantages of HRMS with lower instrument costs and more versatility in operation.

SGS Axys has adapted EPA Method 1613B to PCDD/PCDF analysis by MS/MS. All HR-specific protocols and specifications have been replaced with MS/MS based protocols and specifications and an “Alternate Test Method” has been written for submission to the EPA. Tier 3 Validation of this Alternate Test Method has been completed using a Waters Corporation APGC-Xevo TQ-XS system.

In this presentation I will describe the proposed changes to 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. The impact of potential interferences, such as PCBs and chlorinated diphenyl ethers, will be described and recommendations for routine monitoring will be made.

The results of the method validation will be described. MDL and 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.