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Characterising plasticised cellulose acetate-based historic artefacts by NMR spectroscopy: a new approach for quantifying the degree of substitution and diethyl phthalate contents

Da Ros, S; Aliev, AE; Del Gaudio, I; King, R; Pokorska, A; Kearney, M; Curran, K; (2021) Characterising plasticised cellulose acetate-based historic artefacts by NMR spectroscopy: a new approach for quantifying the degree of substitution and diethyl phthalate contents. Polymer Degradation and Stability , 183 , Article 109420. 10.1016/j.polymdegradstab.2020.109420. Green open access

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Abstract

As one of the first semi-synthetic plastics produced industrially, cellulose acetate (CA)-based artefacts represent valued items in museum collections and archives which, however, present stability issues. High temperature and relative humidity conditions have long been known to promote changes in CA properties, for instance, due to the deacetylation of CA polymer chains and the loss of plasticiser from the polymer matrix. However, there is a need for improved methods for the quantification of plasticiser loss and CA deacetylation. In this context, this contribution presents a new approach for enabling the investigation of plasticiser loss and deacetylation degradation processes in historic plasticised CA-based artefacts which is based on high-resolution proton nuclear magnetic resonance spectroscopy (1H NMR). The proposed methods allow for simple and fast quantification of diethyl phthalate contents and average degree of substitution (DS), while requiring no need for extractive separation between the plasticiser and the CA polymer matrix prior to analysis. Both methods are demonstrated by their application towards a series of reference samples, historic artefacts and artificially aged plasticised CA materials. Our analysis indicates that plasticiser content and DS can be accurately quantified by using high-resolution 1H NMR and both methods have been compared to analyses performed using infrared spectroscopy.

Type: Article
Title: Characterising plasticised cellulose acetate-based historic artefacts by NMR spectroscopy: a new approach for quantifying the degree of substitution and diethyl phthalate contents
Open access status: An open access version is available from UCL Discovery
DOI: 10.1016/j.polymdegradstab.2020.109420
Publisher version: https://doi.org/10.1016/j.polymdegradstab.2020.109...
Language: English
Additional information: This version is the author accepted manuscript. For information on re-use, please refer to the publisher’s terms and conditions.
Keywords: Cellulose acetate, stability, NMR spectroscopy, plasticiser loss, deacetylation, degree of substitution
UCL classification: UCL
UCL > Provost and Vice Provost Offices > UCL BEAMS
UCL > Provost and Vice Provost Offices > UCL BEAMS > Faculty of Maths and Physical Sciences
UCL > Provost and Vice Provost Offices > UCL BEAMS > Faculty of Maths and Physical Sciences > Dept of Chemistry
UCL > Provost and Vice Provost Offices > UCL BEAMS > Faculty of the Built Environment
UCL > Provost and Vice Provost Offices > UCL BEAMS > Faculty of the Built Environment > Bartlett School Env, Energy and Resources
URI: https://discovery.ucl.ac.uk/id/eprint/10114697
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