Key Comparison Study-Organic Solvent Calibration Solution Gravimetric preparation and value assignment of deoxynivalenol (DON) in acetonitrile (ACN)

The CCQM-K154.c comparison was coordinated by the BIPM and NIM on behalf of the CCQM Organic Analysis Working Group (OAWG) for National Measurement Institutes (NMIs) and Designated Institutes (DIs) which provide measurement services in organic analysis under the 'Comité International des Poids et Mesures' Mutual Recognition Arrangement (CIPM MRA) and/or have participated in the BIPM's Mycotoxin Metrology Capacity Building and Knowledge Transfer (MMCBKT) project as part of its "Metrology for Safe Food and Feed in Developing Economies" Capacity Building Programme. Gravimetrically prepared solutions having an assigned mass fraction of specified organic analytes are routinely used to calibrate measurement processes for the quantification of the same analytes in matrix samples. Appropriate assignments of the property value and associated uncertainty of calibration solutions thus underpin the traceability of routine analysis and are critical for accurate measurements. Evidence of successful participation in relevant international comparisons is needed to document calibration and measurement capability claims (CMCs) made by national metrology institutes and designated institutes. In total, ten NMIs/DIs participated in the Track C, Model II, Key Comparison CCQMK154.c [Gravimetric preparation and value assignment of deoxynivalenol (DON) in acetonitrile (ACN)] for emerging areas of global interest and innovation. Participants were requested to gravimetrically prepare calibration solutions and value assign the mass fractions, expressed in mg/kg, of deoxynivalenol (DON) in the acetonitrile (ACN) solution. Study samples, with assigned values and associated uncertainties were prepared by the comparison participants and sent to the coordinating laboratory for comparison. The Key Comparison Reference Values (KCRVs) were assigned of all participant values that agreed within their expanded uncertainty with the values measured by the coordinating laboratory based on calibrations obtained from independent gravimetrically prepared calibrant solutions. Successful participation in CCQM-K154.c for MMCBKT participants was intended to demonstrate measurement capabilities for preparation and value assignment of deoxynivalenol (DON) calibration solutions in the mass fraction range of 10 mg/kg to 100 mg/kg, prepared from a mycotoxin stock solution of pre-assigned content or solid of known purity. Successful participation for other participants, having value assigned their pure Primary Reference Materials, was intended to demonstrate measurement capabilities for the purity value assignment capabilities of organic materials with molar mass in the range 100 g/mol to 500 g/mol and polarity (pKow) > -2, with relative uncertainties at or above the relative uncertainty achieved in the comparison for calibration solutions as well as for the preparation and value assignment of single component organic calibration solutions with polar analytes in the mass fraction range of 10 mg/kg to 100 mg/kg, polarity (pKow) > ‐2, with molar mass in the range of 100 g/mol to 500 g/mol.