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Evaluation of a TEM based Approach for Size Measurement of Particulate (Nano)materials.

  • Verleysen E Trace elements and nanomaterials, Sciensano, Groeselenbergstraat 99, 1180 Uccle, Belgium. eveline.verleysen@sciensano.be.
  • Wagner T Biomedical Imaging Group, University of Applied Sciences and Arts Dortmund, Emil-Figge-Straβe 42, 44227 Dortmund, Germany.
  • Lipinski HG Biomedical Imaging Group, University of Applied Sciences and Arts Dortmund, Emil-Figge-Straβe 42, 44227 Dortmund, Germany.
  • Kägi R Eawag, Swiss Federal Institute of Aquatic Science and Technology, Überlandstrasse 133, CH-8600 Dübendorf, Switzerland.
  • Koeber R European Commission, Joint Research Centre, Retieseweg 111, 2440 Geel, Belgium.
  • Boix-Sanfeliu A European Commission, Joint Research Centre, Retieseweg 111, 2440 Geel, Belgium.
  • De Temmerman PJ Trace elements and nanomaterials, Sciensano, Groeselenbergstraat 99, 1180 Uccle, Belgium.
  • Mast J Trace elements and nanomaterials, Sciensano, Groeselenbergstraat 99, 1180 Uccle, Belgium.
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  • 2019-07-18
Published in:
  • Materials (Basel, Switzerland). - 2019
European Commission’s Recommendation for a definition of a nanomaterial
electron microscopy
image analysis
method validation
nanomaterial
particulate material
English An approach for the size measurement of particulate (nano)materials by transmission electron microscopy was evaluated. The approach combines standard operating procedures for specimen preparation, imaging, and image analysis, and it was evaluated on a series of certified reference materials and representative test materials with varying physical properties, including particle size, shape, and agglomeration state. The measurement of the median value of the minimal external particle diameter distribution was intra-laboratory validated. The validation study included an assessment of the limit of detection, working range, selectivity, precision, trueness, robustness, and ruggedness. An uncertainty that was associated to intermediate precision in the range of 1-7% and an expanded measurement uncertainty in the range of 7-20% were obtained, depending on the material and image analysis mode. No bias was observed when assessing the trueness of the approach on the certified reference materials ERM-FD100 and ERM-FD304. The image analysis method was validated in an inter-laboratory study by 19 laboratories, which resulted in a within-laboratory precision in the range of 2-8% and a between-laboratory precision of between 2% and 14%. The automation and standardization of the proposed approach significantly improves labour and cost efficiency for the accurate and precise size measurement of the particulate materials. The approach is shown to be implementable in many other electron microscopy laboratories.
Language
  • English
Open access status
gold
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https://sonar.ch/global/documents/99620
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