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Interlaboratory comparison exercise for the determination of As, Cd, Ni and Pb in PM10 in Europe.

Gerboles, M*; Buzica, D*; Brown, R J C; Yardley, R E; Hanus-Illnar, A*; Salfinger, M*; Vallant, B*; Adriaenssens, E*; Claeys, N*; Roekens, E*; Sega, K*; Jurasovic, J*; Rychlik, S*; Rabinak, E*; Tanet, G*; Passarella, R*; Pedroni, V*; Karlsson, V*; Alleman, L*; Pfeffer, U*; Gladtke, D*; Olschewski, A*; O'Leary, B*; O'Dwyer, M*; Pockeviciute, D*; Biel-Cwikowska, J*; Tursic, J* (2011) Interlaboratory comparison exercise for the determination of As, Cd, Ni and Pb in PM10 in Europe. Atmos. Environ., 45 (20). pp. 3488-3499.

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This paper presents the results of an intercomparison exercise for the determination of lead (Pb), arsenic (As), nickel (Ni) and cadmium (Cd) in PM10 which are the heavy metals regulated by European Directives. Thirteen laboratories participated, generally using the European reference methods of measurements which consist in of microwave digestion followed by analysis with by ICP-MS or GF-AAS. Each participant had was asked to analyse five test samples: a liquid Certified Reference Material (CRM), two sub-samples of a NIST dust CRM (one already digested and one digested by participants) and two loaded filters (one already digested and one digested by participants).
Participants were able to reach the Data Quality Objectives (DQOs) of the European Directives (uncertainty of 25 % for Pb and 40 % for As, Cd and Ni) for 93 % of all test samples except for the loaded filter that they had to digest by themselves. In fact, only 76 % of DQOs were met for this test sample, the closest to a routine sample analysis every day work in the laboratory. The difficulties in analysing this test sample mainly came from digestion, preparation or and contamination processes. Satisfactory results were obtained using other digestion techniques (Soxhlet extraction and high pressure methods) and analytical methods (ICP-OES for Cd, Ni and Pb, EDXRF for Pb and Ni or Voltammetry for As, Ni, and Pb).
Participants claimed uncertainties that were about 10 % for Pb and between 15 and 20 % for As, Cd and Ni. These uncertainties were confirmed for 77 % of results. The reproducibility of the methods of measurements was between 41 and 54 % while repeatability remained between 5 and 12 % except for the analysis of As on filter which was up to 20 %. A majority of participant results showed higher between-day variability (14 ± 11 %) than within-day variability (6.0 ± 5.3 %).

Item Type: Article
Keywords: Heavy metals, PM10, Particulate matter, air quality legislation, uncertainty of measurement
Subjects: Analytical Science
Analytical Science > Trace Analysis and Electrochemistry
Identification number/DOI: 10.1016/j.atmosenv.2010.12.020
Last Modified: 23 Jul 2018 14:08
URI: http://eprintspublications.npl.co.uk/id/eprint/4998

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