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As the commercial use of synthetic amorphous silica nanomaterials (SiO 2 -NPs) increases, their effects on the environment and human health have still not been explored in detail. An often-insurmountable obstacle for SiO 2 -NP fate and hazard research is the challenging analytics of solid particulate silica species, which involves toxic and corrosive hydrofluoric acid (HF). We therefore developed and validated a set of simple hydrofluoric acid-free sample preparation methods for the quantification of amorphous SiO 2 micro- and nanoparticles. To circumvent HF, we dissolved the SiO 2 -NPs by base-catalyzed hydrolysis at room temperature or under microwave irradiation using potassium hydroxide, replacing the stabilizing fluoride ions with OH − , and exploiting the stability of the orthosilicic acid monomer under a strongly basic pH. Inductively coupled plasma – optical emission spectroscopy (ICP-OES) or a colorimetric assay served to quantify silicon. The lowest KOH: SiO 2 molar ratio to effectively dissolve and quantify SiO 2 -NPs was 1.2 for colloidal Stöber SiO 2 -NPs at a pH >12. Fumed SiO 2 -NPs (Aerosil ® ) or food grade SiO 2 (E551) containing SiO 2 -NPs were degradable at higher KOH: SiO 2 ratios >8000. Thus, hydrofluoric acid-free SiO 2 -NP digestion protocols based on KOH present an effective (recoveries of >84%), less hazardous, and easy to implement alternative to current methods.

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