Preprint Article Version 1 Preserved in Portico This version is not peer-reviewed

Critical Evaluation of the Methods for the Characterisation of the Degree of Sulfonation for Electron Beam Irradiated and Non-Irradiated Sulfonated Poly(ether ether ketone) Membranes

Version 1 : Received: 8 August 2023 / Approved: 9 August 2023 / Online: 10 August 2023 (10:19:46 CEST)

A peer-reviewed article of this Preprint also exists.

Pakalniete, L.D.; Maskova, E.; Zabolockis, R.J.; Avotina, L.; Sprugis, E.; Reinholds, I.; Rzepna, M.; Vaivars, G.; Pajuste, E. Critical Evaluation of the Methods for the Characterization of the Degree of Sulfonation for Electron Beam Irradiated and Non-Irradiated Sulfonated Poly(ether ether ketone) Membranes. Materials 2023, 16, 6098. Pakalniete, L.D.; Maskova, E.; Zabolockis, R.J.; Avotina, L.; Sprugis, E.; Reinholds, I.; Rzepna, M.; Vaivars, G.; Pajuste, E. Critical Evaluation of the Methods for the Characterization of the Degree of Sulfonation for Electron Beam Irradiated and Non-Irradiated Sulfonated Poly(ether ether ketone) Membranes. Materials 2023, 16, 6098.

Abstract

The aim of this study is to compare different methods used for determination of the DS for sulfonated membranes before and after high dose irradiation. Commercial PEEK was homogenously sulfonated up to DS of 60-90% and the membranes were prepared using solvent casting method. Part of the samples were irradiated with 10 MeV electron beam up to 500 kGy dose to assess the ionising radiation induced effects. Both non-irradiated and irradiated membranes were characterized by Fourier Transformation infrared (FT-IR) spectrometry, thermogravimetric analysis (TGA), proton nuclear magnetic resonance (1H-NMR), electrochemical impedance analysis and for the first time for non-irradiated membranes by spectrophotometric analysis with Cr(III). Comparison of the above-mentioned methods for application for DS assessment was done. It was observed that irradiated membranes presented a higher value of DS. Appearance of different new signals in 1H-NMR and FT-IR spectra of irradiated membranes indicated the effects of radiation induced changes in the structure of SPEEK materials. It was determined that the novel method with Cr(III) is applicable for the determination of SPEEK DS under 80%.

Keywords

Sulfonated poly(ether ether ketone); degree of sulfonation; electron beam irradiation

Subject

Chemistry and Materials Science, Polymers and Plastics

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