Key comparison CCQM-K78.b - non-polar analytes in organic solvent: methoxychlor and trifluralin in acetonitrile
Authors: Westwood S , Josephs R D , Choteau T , Martos G , Wielgosz R , Sarzuri Y Acho , Mendoza E , Rego E C Pires do , Violante F G Marques , Souza W da Silva , Carvalho L Junqueira de , Fernandes J L Nogueira , Bates J , Rajotte I , Melanson J E , Li H , Guo Z , Su F , Wang S , Huang T , Lalerle B , Gantois F , Piechotta C , Philipp R , Kaminski K , Klyk-Seitz U-A , Giannikopoulou P , Skotidaki E , Kakoulides E , Pui-Kwan C , Kuroe M , Itoh N , Calderón M A Avila , Contreras L Regalado , Osuna M Arce , Alrashed M , Ting L , Mei G E , Juan W , Sze C Pui , Lin T Tang , Quinn L , Swiegelaar C , Fernandes-Whaley M , Ahn S , Chaiphet T , Sudsiri N , Bellazreg W , Bilsel M , Binici B , Hambidge T , Almirón F , Colombo G 
Published: February 2025

Main text

The CCQM-K78.b key comparison was coordinated by the Bureau International des Poids et Mesures (BIPM) on behalf of the CCQM Organic Analysis Working Group (OAWG) of the 'Comité Consultatif pour la Quantité de Matière' (CCQM), for National Measurement Institutes (NMIs) and Designated Institutes (DIs) providing measurement services in organic analysis under the 'Comité International des Poids et Mesures' (CIPM) Mutual Recognition Arrangement (MRA).

This key comparison was conducted as a 'Track A' comparison within the OAWG's 10-year strategic plan. The goal of CCQM-K78.b was to underpin capabilities for the value assignment of calibration solutions containing low polarity/non-polar organic analytes in organic solvents. The selected model system consisted of a two-component pesticide solution in acetonitrile, comprising methoxychlor and trifluralin.

Participants were tasked with assigning the mass fractions, in units of μg/g, of methoxychlor and trifluralin in acetonitrile solution. The mass fraction levels and analytical challenges of the selected analytes were representative of those encountered for calibration solutions of non-polar organic analytes. Participation in CCQM-K78.b allowed for the benchmarking of capabilities for assigning the mass fraction of non-polar organic compounds (pKow < -2) in solution, at mass fractions above 5 μg/g, in an organic solvent. Additionally, the comparison assessed the capabilities for the quantitative assignment of thermally labile compounds.

Participants were provided by the BIPM with ampoules containing methoxychlor and trifluralin in acetonitrile. Each participant reported the mass fraction content of each analyte in μg/g. All participants ensured the metrological traceability of their results through the use of a Primary Reference Material (PRM), which was used to prepare a primary calibrator solution for each analyte using a gravimetric procedure. The twenty participating institutes primarily used analysis procedures based on GC-MS, -IDMS, -MS/MS, -ECD, and -FID, with some participants also using LC-UV for the value assignment.

The analysis of methoxychlor and trifluralin in acetonitrile solution presented several challenges, including the thermal stability of the analytes under selected analytical techniques, control of solvent volatility, and considerable variation in some results using MS-based quantification methods. The mass fraction assignments for methoxychlor and trifluralin, consistent with the key comparison reference values (KCRVs), were achieved with associated relative standard uncertainties of (0.38 - 2.9) % for methoxychlor and (0.35 - 2.5) % for trifluralin.

To reach the main text of this paper, click on Final Report. Note that this text is that which appears in Appendix B of the BIPM key comparison database https://www.bipm.org/kcdb/.

The final report has been peer-reviewed and approved for publication by the CCQM, according to the provisions of the CIPM Mutual Recognition Arrangement (CIPM MRA).