Several techniques were evaluated for the establishment of reliable water/moisture content of single-wall carbon nanotubes. Karl Fischer titration (KF) provides a direct measure of the water content and was used for benchmarking against results obtained by conventional oven drying, desiccation over anhydrous magnesium perchlorate as well as by thermogravimetry and prompt gamma-ray activation analysis. Agreement amongst results was satisfactory with the exception of thermogravimetry, although care must be taken with oven drying as it is possible to register mass gain after an initial moisture loss if prolonged drying time or elevated temperatures (120 °C) are used. Thermogravimetric data were precise but a bias was evident that could be accounted for by considering the non-selective loss of mass as volatile carbonaceous components. Simple drying over anhydrous magnesium perchlorate for a minimum period of 8–10 days is recommended if KF is not available for this measurement.
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The authors thank G. Robertson of NRCC’s Institute for Chemical Process and Environmental Technology (ICPET) for making available the TGA-FT-IR apparatus used in this study, F. Toll (ICPET) for performing the carbon content measurements and P. Rasmussen (Health Canada) for measurements of the SWCNT agglomerate particle size.
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Sturgeon, R.E., Lam, J.W., Windust, A. et al. Determination of moisture content of single-wall carbon nanotubes. Anal Bioanal Chem 402, 429–438 (2012). https://doi.org/10.1007/s00216-011-5509-y
- Single-wall carbon nanotubes
- Moisture determination
- Oven drying
- Desiccator drying
- Karl Fischer titration
- Prompt gamma-ray activation analysis