Degree of Sulfonation (DS) - Determination by Different Analytical Techniques in Ionomers Derived from Polystyrene

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Abstract Polymers with ion charges anchored to their structure, known as ionomers, are slightly modified materials with notable applications for electrochemical processes. However, the characterization and quantification of those sulfonic groups grafted to the polymer is uncommon, which can lead to inaccurate data regarding their performance. A styrene-co-butyl acrylate copolymer (80:20) was synthesized and further sulfonated with concentrated sulfuric acid. Analytical techniques such as proton nuclear magnetic resonance (¹H NMR) and thermogravimetric analysis (TGA) were employed to characterize ionomers and used to calculate the degree of sulfonation (DS). Membranes were prepared by casting from the sulfonated copolymer, using two different solvent systems; then, the ion exchange capacity (IEC) was evaluated to be able to calculate DS values. For the ionomer, a DS of 35.2% was obtained by ¹H NMR and 38.4% by TGA, while from membranes IEC results the DS ranged from 4.9% to 28%, depending on the solvent system used for membrane preparation. The DS evaluation in the ionomer is similar for both analytical techniques used, since measuring the presence of sulfonic groups; however, the most popular IEC technique to measure DS value must be taken with care, since the method is more related to the structural condition, where the ionic groups are available to exchange, highly affected by the membrane preparation method.
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Degree of Sulfonation (DS) - Determination by Different Analytical Techniques in Ionomers Derived from Polystyrene | Research Square window.SnipcartSettings = { analytics: { enabled: false } }; (function() { var accessVector = localStorage.getItem('access_vector') || ''; window.dataLayer = window.dataLayer || []; if (accessVector) { window.dataLayer.push({ user: { profile: { profileInfo: { snid: accessVector } } } }); } })(); (function(w,d,s,l,i){w[l]=w[l]||[];w[l].push({'gtm.start':new Date().getTime(),event:'gtm.js'});var f=d.getElementsByTagName(s)[0],j=d.createElement(s),dl=l!='dataLayer'?'&l='+l:'';j.async=true;j.src='https://www.googletagmanager.com/gtm.js?id='+i+dl;f.parentNode.insertBefore(j,f);})(window,document,'script','dataLayer','GTM-K279D39R'); Browse Preprints In Review Journals COVID-19 Preprints AJE Video Bytes Research Tools Research Promotion AJE Professional Editing AJE Rubriq About Preprint Platform In Review Editorial Policies Our Team Advisory Board Help Center Sign In Submit a Preprint Cite Share Download PDF Research Article Degree of Sulfonation (DS) - Determination by Different Analytical Techniques in Ionomers Derived from Polystyrene LUCIANO DA SILVA, J.C. Sánchez Hiza, R. Benavides, D. Morales Acosta This is a preprint; it has not been peer reviewed by a journal. https://doi.org/ 10.21203/rs.3.rs-7292633/v1 This work is licensed under a CC BY 4.0 License Status: Published Journal Publication published 13 Oct, 2025 Read the published version in Journal of Polymer Research → Version 1 posted 5 You are reading this latest preprint version Abstract Polymers with ion charges anchored to their structure, known as ionomers, are slightly modified materials with notable applications for electrochemical processes. However, the characterization and quantification of those sulfonic groups grafted to the polymer is uncommon, which can lead to inaccurate data regarding their performance. A styrene-co-butyl acrylate copolymer (80:20) was synthesized and further sulfonated with concentrated sulfuric acid. Analytical techniques such as proton nuclear magnetic resonance (¹H NMR) and thermogravimetric analysis (TGA) were employed to characterize ionomers and used to calculate the degree of sulfonation (DS). Membranes were prepared by casting from the sulfonated copolymer, using two different solvent systems; then, the ion exchange capacity (IEC) was evaluated to be able to calculate DS values. For the ionomer, a DS of 35.2% was obtained by ¹H NMR and 38.4% by TGA, while from membranes IEC results the DS ranged from 4.9% to 28%, depending on the solvent system used for membrane preparation. The DS evaluation in the ionomer is similar for both analytical techniques used, since measuring the presence of sulfonic groups; however, the most popular IEC technique to measure DS value must be taken with care, since the method is more related to the structural condition, where the ionic groups are available to exchange, highly affected by the membrane preparation method. Degree of sulfonation (DS) Ionomer Ion exchange capacity (IEC) analytical techniques. Full Text Cite Share Download PDF Status: Published Journal Publication published 13 Oct, 2025 Read the published version in Journal of Polymer Research → Version 1 posted Reviewers agreed at journal 03 Sep, 2025 Reviewers invited by journal 03 Sep, 2025 Editor invited by journal 20 Aug, 2025 Editor assigned by journal 05 Aug, 2025 First submitted to journal 04 Aug, 2025 You are reading this latest preprint version Research Square lets you share your work early, gain feedback from the community, and start making changes to your manuscript prior to peer review in a journal. As a division of Research Square Company, we’re committed to making research communication faster, fairer, and more useful. We do this by developing innovative software and high quality services for the global research community. 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