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Practical aspects of the Boehm titration method are evaluated for obtaining reliable results in the quantification of oxygen-containing surface groups in a short time. Analytical criteria such as accuracy, repeatability, precision, and robustness are applied. Oxidized multi-walled carbon nanotubes (MWCNTs) are used as the model substance. Different reaction bases (NaHCO3(aq), Na2CO3(aq), NaOH(aq)) are applied and treatment times are studied. We also show that smaller amounts of carbon material can be reliably analyzed by using an autotitrator combined with a pH electrode. We find that indirect titration with Na2CO3 results in the highest titration precision and accuracy despite the lower base strength compared with NaOH. Therefore, CO2 impurities do not have to be removed and only 7 min is necessary for one titration. The titration error with respect to the proposed method is 0.15% of the aliquot volume. The mixing method during the carbon treatment with bases (stirring, shaking, ultrasound treatment) has no influence on the result as long as one allows a few hours for the reaction to complete. Finally, we provide a standard operating procedure for obtaining results with high precision during Boehm titration.

Boehm Titration Revisited (Part I): Practical Aspects for Achieving a High Precision in Quantifying Oxygen-Containing Surface Groups on Carbon Materials