This article describes the development of a suitable Gel Permeation Chromatography method for cellulose nitrate plasticised with camphor (celluloid) found in cultural heritage. Current sample preparation and dissolution methods, apart from focusing on native, nonderivatised cellulose, require long preparation times, and often employ solvents that induce degradation. This study aims to develop a systematic method for sample preparation of cellulose nitrate that uses the least sample amount possible, is nondegrading, and can be applied on differently aged samples. This is investigated through identification of a suitable solvent system and a statistically designed experiment testing the critical variables affecting the analysis, namely sample condition, sample, and salt concentration (lithium chloride) in N,N-dimethylacetamide. The use of 0.1% sample was inadequate for analysis because it did not fully dissolve in any salt concentration, while the 0.3% negatively impacted the analysis with its high molecular weight distributions. The 0.2% cellulose nitrate in a solution of 0.5% lithium chloride in N,N-dimethylacetamide offered the most consistent and repeatable molecular weight data. This method miniaturised the sample as much as possible and is suitable for museum objects in various ageing conditions.
Keywords: N-dimethylacetamide; cellulose nitrate; gel permeation chromatography; lithium chloride/N; method development; sample preparation.
© 2021 The Authors. Journal of Separation Science published by Wiley-VCH GmbH.