Conservation Science Department, Deutsches Museum, Museumsinsel 1, Munich, 80538, Germany.
J Sep Sci. 2021 May;44(9):1795-1804. doi: 10.1002/jssc.202001018. Epub 2021 Mar 1.
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.
本文介绍了一种适用于文化遗产中樟脑增塑硝酸纤维素（赛璐珞）的凝胶渗透色谱法的开发。目前的样品制备和溶解方法除了专注于天然、未衍生的纤维素外，还需要很长的准备时间，而且通常使用会引起降解的溶剂。本研究旨在开发一种系统的硝酸纤维素样品制备方法，该方法使用尽可能少的样品量、不具有降解性并且可以应用于不同老化程度的样品。这是通过确定合适的溶剂系统以及统计设计实验来测试影响分析的关键变量来实现的，即样品状态、样品和 N,N-二甲基乙酰胺中的盐浓度（氯化锂）。0.1%的样品用量不足以进行分析，因为它在任何盐浓度下都不能完全溶解，而 0.3%的样品则因其高分子量分布而对分析产生负面影响。0.2%的硝酸纤维素在 0.5%氯化锂的 N,N-二甲基乙酰胺溶液中提供了最一致和可重复的分子量数据。该方法尽可能地减小了样品的体积，适用于各种老化条件下的博物馆物品。
