an official journal of: published by:
an official journal of: published by:
Editor in Chief: RAFFAELLO COSSU

THE INHERENT VARIABILITY OF SOME ENVIRONMENTAL ANALYTICAL METHODS HAMPERS THE CIRCULAR ECONOMY OF MATERIALS

  • Pierre Hennebert - RISK/COSM, INERIS, France
  • Anne-Françoise Stoffel - Direction Technique et Développement, Eurofins Analyses pour l’Environnement France, France
  • Mathieu Hubner - Direction Technique et Développement, Eurofins Analyses pour l’Environnement France, France
  • Daniel Fortmann - Direction Technique et Développement, Eurofins Analyses pour l’Environnement France, France
  • Patricia Merdy - IM2NP Institute of Materials Microelectronics Nanosciences of Provence, France
  • Giovanni Beggio - Department of Civil, Environmental and Architectural Engineering, University of Padova, Italy

Released under CC BY-NC-ND

Copyright: © 2022 CISA Publisher


Abstract

This paper is the third part of three papers on sampling by the number of particles, focusing on analytical variability. The objective is to propose a target variability of waste and contaminated soil analyses (extraction and quantification), that can be used for calculation of the size of a representative sample. Data of intra- and inter-laboratory variability are presented. As the variability of the quantification step (after extraction) is limited in waste and soil analyses to about 0.01, the analytical variability stems from three main sources: (i) non-homogeneous test portions; (ii) for partial extraction methods, variable extraction rate, due to presence of options in the method or insufficient time for equilibrium (leaching or percolation test, biotests); and (iii) ill-defined solid/liquid separation (leaching or percolation tests), critical since there are colloids and nanoparticles in the leachates, representing from 0 to 100% of the element fraction in the leachate. Counter-intuitively, the centrifugation (annex E of EN 12457) series before the 450 nm-filtration delivers leachates more concentrated in particles (median size 150 nm, 1 sample) and statistically more concentrated in elements (+13%, 27 samples, 287 paired data). Without centrifugation, the filter cake that builds up on the membrane is an additional filter. A target intra-laboratory variability of CVr = 0.10 (10%) and inter-laboratory variability of CVR = 0.20 (20%) is proposed for all analytical methods. The methods with higher CVr and CVR should be revisited to not jeopardise the sampling and characterisation efforts of waste and soil, particularly for valorisation in the circular economy.

Keywords


Editorial History

  • Received: 02 Aug 2022
  • Revised: 08 Oct 2022
  • Accepted: 03 Nov 2022
  • Available online: 30 Nov 2022

References

Beggio G, Hennebert P. 2022. A novel method to calculate the size of representative waste samples based on particles size. Detritus, 18, 3–11.
DOI 10.31025/2611-4135/2022.15187

CEN 2022. CEN/TC 351 FprCEN/TR 00351055:2022 “Construction products — Assessment of release of dangerous substances — Specific quality assurance measures”,

CEN 2007. CEN/TR 15310-1, 2007. Characterization of waste - Sampling of waste materials Part 1: Guidance on selection and application of criteria for sampling under various conditions. CEN, Brussels, Belgium

EC 2003. Council Decision of 19 December 2002 establishing criteria and procedures for the acceptance of waste at landfills pursuant to Article 16 of and Annex II to Directive 1999/31/EC (2003/33/EC). 16.1.2003. Official Journal of the European Communities L 11/27

EN 15002, 2015. Characterization of waste — Preparation of test portions from the laboratory sample. CEN, Brussels, Belgium

EN 15413, 2011. Solid recovered fuels - Methods for the preparation of the test sample from the laboratory sample. CEN, Brussels, Belgium

Environment Agency, NIEA, SEPA, Natural Resources Wales, 2021. WM3 v 1.2.GB 2021. Waste Classification: Guidance on the classification and assessment of waste (1st Edition v1.2 GB): Technical Guidance WM3. http://www.gov.uk/government/publications/waste-classification-technical-guidance

Esbensen K H and Ramsay C A, 2015. QC of sampling process – A first overview: from field to test portion. Journal of AOAC International, 98, 2, 282-287.
DOI 10.5740/jaoacint.14-288

European Commission (Directorate general for Environment), Bio Innovation, INERIS, RPA 2021. Study to support the assessment of impacts associated with the review of limit values in waste for POPs listed in Annexes IV and V of Regulation (EU) 2019/1021. April 2021. KH-06-21-119-EN-N. 596 p. https://op.europa.eu/en/publication-detail/-/publication/c7c70b73-3798-11ec-8daf-01aa75ed71a1/language-en
DOI 10.2779/63162

FprCEN/TR 00351055:2022.CEN/TC 351. Construction products — Assessment of release of dangerous substances — Specific quality assurance measures. 25 p

García-Ruiz, S., Linsinger, T., Cordeiro, F., Conneely, P., Emteborg, H. and Held, A.,2020. Interlaboratory comparison to evaluate the precision of measurement methods for the assessment of the release of inorganic substances from construction products, EUR 30071 EN, Publications Office of the European Union, Luxembourg, 2020, ISBN 978-92-76-10226-7, 86 p,
DOI 10.2760/288988, JRC119719

Gerassimidou S, C. A. Velis, R. A. Bourne, D. Komilis, E. Garcia-Taengua, P. T. Williams (2020). Statistical quantification of sub-sampling representativeness and uncertainty for waste-derived solid recovered fuel (SRF): Comparison with theory of sampling (ToS). Journal of Hazardous Materials 388 (2020) 122013.
DOI 10.1016/j.jhazmat.2019.122013

Gerlach, R. W., & Nocerino, J. M. (2004). Guidance for obtaining representative laboratory analytical subsamples from particulate laboratory samples. Washington, DC: US Environmental Protection Agency, Office of Research and Development, National Exposure Research Laboratory, Environmental Sciences Division

Gy, Pierre. 1996. Sampling batches of material for analysis (in French). Sciences de l’ingénieur. Masson ed., 148 p

Henderson Rayetta G., Violaine Verougstraete, Kim Anderson, José J. Arbildua, Thomas O. Brock, Tony Brouwers, Danielle Cappellini, Katrien Delbeke, Gunilla Herting, Greg Hixon, Inger Odnevall Wallinder, Patricio H. Rodriguez, Frank Van Assche, Peter Wilrich, Adriana R. Oller. 2014. Inter-laboratory validation of bioaccessibility testing for metals. Regulatory Toxicology and Pharmacology, Volume 70, Issue 1, 2014, Pages 170-181, ISSN 0273-2300,
DOI 10.1016/j.yrtph.2014.06.021

Hennebert P, Anderson A, Merdy P. 2017. Mineral nanoparticles in waste: potential sources, occurrence in some engineered nanomaterials leachates, municipal sewage sludges and municipal landfill sludges. J Biotechnol Biomater 2017, 7:2. 12 p

Hennebert P. 2018. Proposal of concentration limits for determining the hazard property HP 14 for waste using ecotoxicological tests. Waste Management 74, April 2018, 74-85

Hennebert P, Avellan A, Yan J, Aguerre-Chariol O. 2013. Experimental evidence of colloids and nanoparticles presence from 25 waste leachates. Waste Management 33 (2013) 1870–1881

Hennebert P, Beggio G. 2021. Sampling and sub-sampling of granular waste: size of a representative sample in terms of number of particles. Detritus 17 – 2021, 1-12.
DOI 10.31025/2611-4135/2021.15139

ISO 2016. Document ISO/TC 147/SC 2 N 1567. Date: 2016-02-08. Guidance document on designing an interlaboratory trial for validation of analytical methods within ISO/TC 147/SC 2

prEN 16637-3:2021 CEN/TC 351. Construction products: Assessment of release of dangerous substances — Part 3: Horizontal up-flow percolation test. Similar to pr-EN 17516:2021. CEN/TC 444. Waste — Characterization of granular solids with potential for use as construction material — Compliance leaching test — Up-flow percolation test. CEN, Brussels, Belgium. 72 p

SVDU 2020. Syndicat national du traitement et de la valorisation des déchets urbains et assimilés, France. « Classification déchets dangereux/non dangereux en France : MIDND » (MIDND = MSWI bottom ashes). Internal document. 31 p

UPDS 2021. Union des Professionnels de la Dépollution des Sites, France. Personnal communication

USEPA 2010. USEPA quality control acceptance criteria of BDE. USEPA Method 1614A p 68 Method 1614A Brominated Diphenyl Ethers in Water, Soil, Sediment, and Tissue by HRGC/HRMS, May 2010, 93 p

Viczek S A, K. Khodier, L. Kandlbauer, A. Aldrian, G. Redhammer, G. Tippelt, R. Sarc. 2021. The particle size-dependent distribution of chemical elements in mixed commercial waste and implications for enhancing SRF quality. Science of the Total Environment 776 (2021) 145343

Viczek, S.A., Kandlbauer, L., Khodier, K., Aldrian, A., Sarc, R., 2021. Sampling and analysis of coarsely shredded mixed commercial waste. Part II: particle size-dependent element determination. Int. J. Environ. Sci. Technol.
DOI 10.1007/s13762-021-03567-w