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Size characterization of airborne SiO2 nanoparticles with on-line and off-line measurement techniques: an interlaboratory comparison study

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Abstract

Results of an interlaboratory comparison on size characterization of SiO2 airborne nanoparticles using on-line and off-line measurement techniques are discussed. This study was performed in the framework of Technical Working Area (TWA) 34—“Properties of Nanoparticle Populations” of the Versailles Project on Advanced Materials and Standards (VAMAS) in the project no. 3 “Techniques for characterizing size distribution of airborne nanoparticles”. Two types of nano-aerosols, consisting of (1) one population of nanoparticles with a mean diameter between 30.3 and 39.0 nm and (2) two populations of non-agglomerated nanoparticles with mean diameters between, respectively, 36.2–46.6 nm and 80.2–89.8 nm, were generated for characterization measurements. Scanning mobility particle size spectrometers (SMPS) were used for on-line measurements of size distributions of the produced nano-aerosols. Transmission electron microscopy, scanning electron microscopy, and atomic force microscopy were used as off-line measurement techniques for nanoparticles characterization. Samples were deposited on appropriate supports such as grids, filters, and mica plates by electrostatic precipitation and a filtration technique using SMPS controlled generation upstream. The results of the main size distribution parameters (mean and mode diameters), obtained from several laboratories, were compared based on metrological approaches including metrological traceability, calibration, and evaluation of the measurement uncertainty. Internationally harmonized measurement procedures for airborne SiO2 nanoparticles characterization are proposed.

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Acknowledgments

We gratefully acknowledge financial support by C’Nano for LNE, LISA and IRSN laboratories. ILAQH and QUT laboratories acknowledge the support of the Australian Research Council through the Grants DP1112773 and LP1110056. Work at NMIA was supported by the Australian Government’s National Enabling Technologies Strategy. The authors warmly thank J.-M. Aublant (LNE) and J. Fagan (NIST) for supporting this study as project 3 “Techniques for characterizing size distribution of airborne nanoparticles” in the VAMAS framework. The authors acknowledge valuable contributions by H. J. Catchpoole (NMIA), V. A. Coleman (NMIA), J. Herrmann (NMIA), M. Roy (NMIA), P. Palmas (LNE), H. M. Park (KRISS), and F. Calcagnino (UNIGE). We also thank Sukhvir Singh, Prabhat Kumar Gupta, Shankar Aggarwal, Bibhash Chakraborty of the National Physical Laboratory of India (NPLI), and P. Quincey of the UK’s National Physical Laboratory (NPL) for their implication and technical advices for this project.

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Authors and Affiliations

  1. Laboratoire National de Métrologie et d’Essais (LNE), 1 rue Gaston Boissier, 75724, Paris Cedex 15, France

    C. Motzkus, T. Macé, F. Gaie-Levrel, S. Ducourtieux, A. Delvallee & S. Vaslin-Reimann

  2. Danish Fundamental Metrology (DFM), Matematiktorvet 307, 2800, Kgs. Lyngby, Denmark

    K. Dirscherl

  3. BAM Federal Institute for Materials Research and Testing, 12200, Berlin, Germany

    V.-D. Hodoroaba

  4. Unit for Nanocharacterization, The Hebrew University of Jerusalem, Supply Dept Building Ground Floor, Givat Ram, 91904, Jerusalem, Israel

    I. Popov

  5. National Physical Laboratory of Israel (INPL), Danciger “A” Bldg, Givat Ram, 91904, Jerusalem, Israel

    O. Popov & I. Kuselman

  6. National Metrology Institute of Japan (NMIJ), National Institute of Advanced Industrial Science and Technology (AIST), 1-1-1 Umezono, Tsukuba, Ibaraki, 305-8563, Japan

    K. Takahata & K. Ehara

  7. Laboratoire Interuniversitaire des Systèmes Atmosphériques (LISA), UMR CNRS 7583, Université Paris-Est Créteil et Université Paris-Diderot, 61 Avenue du Général de Gaulle, 94010, Créteil, France

    P. Ausset & M. Maillé

  8. PSN-RES, SCA, LPMA, Institut de Radioprotection et de Sûreté Nucléaire (IRSN), Saclay, 91192, Gif-sur-Yvette, France

    N. Michielsen, S. Bondiguel & F. Gensdarmes

  9. International Laboratory for Air Quality and Health (ILAQH), Queensland University of Technology (QUT), 2 George Street, Brisbane, QLD, 4001, Australia

    L. Morawska, G. R. Johnson & E. M. Faghihi

  10. Division of Industrial Metrology, Korea Research Institute of Standards and Science (KRISS), 1 Doryong-Dong, Yuseong-Gu, Taejon, 305-340, Korea

    C. S. Kim, Y. H. Kim & M. C. Chu

  11. Area de Metrología de Materiales, Centro Nacional de Metrología (CENAM), Carretera a los Cués km 4,5, 76246, El Marqués, QRO, Mexico

    J. A. Guardado & A. Salas

  12. Department of Chemistry and Industrial Chemistry, University of Genoa (UNIGE), via Dodecaneso 31, 16146, Genoa, Italy

    G. Capannelli & C. Costa

  13. Science and Engineering Faculty, Queensland University of Technology (QUT), GPO Box 2434, Brisbane, QLD, 4001, Australia

    T. Bostrom

  14. National Measurement Institute Australia (NMIA), PO Box 264, Lindfield, NSW, 2070, Australia

    Å. K. Jämting & M. A. Lawn

  15. National Metrology Institute of South Africa (NMISA), Private Bag X34, Lynnwood Ridge, 0040, South Africa

    L. Adlem

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  1. C. Motzkus
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  2. T. Macé
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  3. F. Gaie-Levrel
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  10. I. Kuselman
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  11. K. Takahata
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  12. K. Ehara
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  13. P. Ausset
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  14. M. Maillé
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  15. N. Michielsen
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  17. F. Gensdarmes
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  18. L. Morawska
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  19. G. R. Johnson
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  20. E. M. Faghihi
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  21. C. S. Kim
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  24. J. A. Guardado
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  25. A. Salas
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  26. G. Capannelli
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  27. C. Costa
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  28. T. Bostrom
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  29. Å. K. Jämting
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  30. M. A. Lawn
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  31. L. Adlem
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  32. S. Vaslin-Reimann
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Corresponding author

Correspondence to C. Motzkus.

Appendix

Appendix

See Tables 3, 4, 5, 6, 7, 8, 9, 10, 11, 12, 13, and 14.

Table 3 Operating parameters of on-line measurement systems used by each laboratory in the interlaboratory comparison
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Table 4 Summary of the involved atomic force microscopes
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Table 5 SEM operating parameters used by each laboratory at the interlaboratory comparison
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Table 6 TEM operating parameters used by each laboratory during the interlaboratory comparison
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Table 7 SMPS measurement results of mean and mode diameters of aerosol OP
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Table 8 SMPS measurement results of mean and mode diameters of aerosol DP
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Table 9 AFM measurement results for aerosol OP (the same sample on a mica substrate, indicated by “M*”, performed by laboratory SMPS4, was measured by laboratories AFM1, 2, and 4)
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Table 10 AFM measurement results of aerosol DP (the same sample on a mica substrate, indicated by “M*”, performed by laboratory SMPS4, was measured by laboratories AFM1 and 2)
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Table 11 SEM measurement results for aerosol OP
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Table 12 SEM measurement results of aerosol DP
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Table 13 Size measurements of silica Aerosol OP by TEM
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Table 14 Size measurements of silica Aerosol DP by TEM
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Motzkus, C., Macé, T., Gaie-Levrel, F. et al. Size characterization of airborne SiO2 nanoparticles with on-line and off-line measurement techniques: an interlaboratory comparison study. J Nanopart Res 15, 1919 (2013). https://doi.org/10.1007/s11051-013-1919-4

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