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Shimadzu Scientific Instruments, a Shimadzu Group company in the United States, and PACE Analytical Services have developed an alternate test procedure (ATP) to EPA method 1613B – PAM-16130-SSI: Determination of 2,3,7,8-Substituted Tetra- through Octa-Chlorinated Dibenzo-p-Dioxins and Dibenzofurans (CDDs/CDFs) Using Shimadzu Gas Chromatography Mass Spectrometry (GC-MS/MS).

This ATP allows the use of GC-MS/MS in place of high-resolution mass spectrometry (GC/HRMS) for the determination of 2,3,7,8 tetra through octa chlorinated dibenzo-p-dioxins and dibenzofurans in wastewater, fish tissue and soils. PAM-16130-SSI uses a Shimadzu GCMS-TQ8050NX triple quadrupole GC-MS/MS instrument with a Boosted Efficiency Ion Source (BEIS) and Multiple Reaction Monitoring (MRM) in place of the GC/HRMS used in EPA Method 1613B to identify the target analytes in the presence of other organic contaminants. This new procedure addresses the challenge of using GC/HRMS instruments, including the high cost to purchase and maintain and difficulty in obtaining parts from manufacturers.

All the sample preparation, extraction and cleanup steps in Method 1613B are included in the ATP, which means the matrix-specific extraction procedures in both methods are the same. In both methods, each sample is spiked with the same suite of carbon-labeled standards prior to extraction and those standards are used for isotope dilution quantitation, in the same way. All the relevant quality control acceptance criteria are the same in both methods as well.

PAM-16130-SSI is slated to be proposed for nationwide approval. In the interim, laboratories may obtain approval to use this method instead of EPA 1613B from their regulatory authority or regional ATP coordinator. Approval of this GC-MS/MS method for measurement of PCDDs/PCDFs has the potential to lower laboratory costs and expand the pool of available laboratories, while not compromising method performance.

Advantages of PAM-16130-SSI include:

• No verification of mass accuracy required every 12 hours. Instead, a passing continuing calibration verification (CCV) at the end of the run is acceptable.
• The triple quad GCMS-TQ8050NX enables a slow bleed of PFTBA into the system throughout the entire run without any additional hardware.
• During validation, no recalibration was needed, even after instrument maintenance was performed or running out of carrier gas.
• Use of Shimadzu’s Automatic Adjustment of Retention Time (AART) function for accelerating the retention time adjustments in acquisition and processing methods after significant column maintenance. This proprietary algorithm, which calculates linear retention indices based on constant linear velocity during the run, enables accurate, reproducible chromatographic separation with proper resolution of dioxins and furans, after every column maintenance and with your original method.

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