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A pilot interlaboratory comparison of protocols that simulate aging of nanocomposites and detect released fragments

Wendel Wohlleben A E , Gemma Vilar B , Elisabet Fernández-Rosas B , David González-Gálvez B , Claus Gabriel C , Sabine Hirth A , Thomas Frechen A , Deborah Stanley D , Justin Gorham D , Li-Piin Sung D , Hsiang-Chun Hsueh D , Yu-Fan Chuang D , Tinh Nguyen D E and Socorro Vazquez-Campos B E
+ Author Affiliations
- Author Affiliations

A BASF SE, Advanced Materials and Systems Research, Department of Material Physics, D-67056 Ludwigshafen, Germany.

B LEITAT Technological Center, c/de la Innovació 2, E-08225 Terrassa (Barcelona), Spain.

C BASF SE, Advanced Materials and Systems Research, Department of Structural Materials, D-67056 Ludwigshafen, Germany.

D National Institute of Standards and Technology, 100 Bureau Drive, Gaithersburg, MD 20899, USA.

E Corresponding authors. Email: wendel.wohlleben@basf.com; tinh.nguyen@nist.gov; svazquez@leitat.org

Environmental Chemistry 11(4) 402-418 https://doi.org/10.1071/EN14072
Submitted: 5 April 2014  Accepted: 28 June 2014   Published: 8 August 2014

Environmental context. Nanoparticles are contained in many commercialised products, but the lack of validated methods to assess their potential release into the environment hampers our ability to perform a reliable risk assessment. Equipment to simulate aging is available, but the challenge is to sample released entities, and to analyse those fragments with suitable nano-analytics. We describe methods to characterise the degradation and surface accumulation of nanoparticles, and to quantify fragments released during UV irradiation of polymer nanocomposites.

Abstract. The safe use of nanoparticles as fillers in nanocomposite materials depends, in part, on a good understanding of what is released from aging nanocomposites, and at which rate. Here we investigated the critical parameters of the nanoparticle release phenomenon by a pilot inter-laboratory study of a polyamide containing 4 mass % of silica nanoparticles (nanosilica). The main focus is on the validity range of the aging and release protocols. Both induced release by mechanical shear after dry weathering at different UV intensities and spontaneous release during wet weathering were investigated. We propose a combined protocol based on the finding that the characteristics of released fragments – which are the essential input for fate, transport and (eco-)toxicological testing – were reproducible between laboratories and between different aging, sampling and analysis protocols: the released fragments were a polydisperse mixture of predominantly composite fragments from the nanometre up to several micrometre diameter, and of clustered or individual nanosilica unbound to polymer. The unbound fraction was microscopically observed but could not be quantified. We found that aging conditions are very critical for the release rates, not for release characteristics. The sampling protocol tolerates some differences. Simplified aging + immersion protocols can at least partially replace, complement and extend dedicated weathering apparatus with run-off collection.

Additional keywords: dry aging, lifecycle, nanosilica, polyamide, release, wet aging.


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