RESUMEN
To survey the conformity and quality of results among laboratories for microplastics determination worldwide, an international laboratory intercomparison and development exercise was organized. The 34 participants were requested to determine the polymer type and number or mass of polymer particles in 12 samples, i.e. six samples containing of pre-production pellets, five dissolvable soda tablets containing different (smaller) polymer particles and one blank soda tablet. A novel method for providing the test materials in aluminium strips was used. Thirty laboratories (88%) submitted data using their own method of choice, resulting in a variety of identification and quantification methods (n = 7). The majority of the labs (53-100%) correctly identified the type of polymer in all samples but one. The performance of the laboratories in quantifying and weighing the pellets was very good. The analysis of the number of the particles in the soda tablets varied considerably between laboratories (29-91%). The results of this study highlight the complexity of microplastics analysis and the need for harmonization of both reporting format and methods. Continued development and assessment of the comparability among analytical methods and laboratories are urgently needed to support monitoring programmes, research and decision-making.
RESUMEN
As short-chain chlorinated paraffins (SCCPs) are listed on several monitoring programs, validated methods are essential. However, their complexity and the lack of commercially available certified reference materials (RMs) hinder a proper validation of methods. Instead, one method is usually 'validated' by evaluating performances and results of spiked materials with that of one other method, which could easily lead to unreliable results. This study evaluated four analytical methods with different principles (i.e. comprehensive two dimensional GC coupled to a micro electron capture detector, developed for this study, chloride enhanced atmospheric pressure chemical ionization triple quadrupole time of flight MS (APCI-QToF-HRMS), GC coupled to an electron capture negative ion low resolution MS (GC-ECNI-LRMS) and carbon skeleton GC-MS), investigated the comparability in SCCP determination in spiked and naturally contaminated samples and determined SCCP amounts in candidate RMs for possible certification. The results cast doubt on the use of the most commonly applied method (i.e. GC-ECNI-LRMS), as well as using spiked materials for method validation. The APCI-QToF-HRMS method was found most promising as it achieves the required MS resolution (>21,000), is relatively fast and can detect also other CPs. The suitable identified SCCP levels in the candidate RMs and the agreement in results between the methods bring the first certification of a RM for SCCPs within reach.