An international round-robin study for the analysis of particulate semi-volatile organics by thermal desorption gas chromatography mass spectrometry

Abstract

Thermal desorption gas chromatography mass spectrometry (TD-GC/MS) is becoming more commonly used for the quantification and identification of organic compounds in particulate matter (PM), including ambient and source PM such as diesel particulate matter (DPM). It has been proven as an alternative to the traditional solvent extraction (SE) method and liquid injection gas chromatograph mass spectrometry (LI-GC/MS). However, little information is available on how different types of TD-GC/MS systems compare to each other for analysis of real-world PM samples or to direct LI-GC/MS for analysis of PM components in a test solution. To address this, CanmetENERGY Characterization Laboratory initiated a round robin with the participation of 10 laboratories worldwide. Three sample types were analysed: (i) a test solution with a suite of pure compounds commonly found in PM, analysed by TD-GC/MS and LI-GC/MS; (ii) a DPM sample, analysed by TD-GC/MS and SE; and (iii) an ambient PM sample, analysed by TD-GC/MS. The first part of the study showed good overall performance and comparability between the different TD-GC/MS systems and LI-GC/MS method for the analysis of PM components in a test solution, with some variability of results due to system types and parameters used, concentration of calibration standards, and whether or not an internal standards was used. The analysis of the DPM sample showed greater variability between laboratories and methods as many PM components were present near the detection limit and matrix effects particularly affected the TD-GC/MS analysis of heavier n-alkanes. In the last part of the study, for the analysis of an ambient PM sample by TD-GC/MS, the analysis of variance showed good comparison between labs for polycyclic aromatic hydrocarbons (94% non-significant), but slightly lower for n-alkanes (68%) and biomarkers (57%).

Keywords:

• thermal desorption
• round robin
• gas chromatography mass spectrometry
• TD-GC/MS
• ambient particulate matter
• solvent extraction

Acknowledgements

We would like to generously thank all the participants who devoted their time and effort to this study. We would also like to thank all the reviewers for their time and input.

ORCID

Gianni Caravaggio http://orcid.org/0000-0002-1696-1290

Chris Hebbern http://orcid.org/0000-0003-0378-9038

Sabit Cakmak http://orcid.org/0000-0001-9921-2107

Additional information

Funding

We would like to thank the Government of Canada Program on Energy Research and Development (PERD) for financial support.