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尺寸排阻色谱法和粘度测定法用于纤维素表征的比较评估

Comparative evaluation of size-exclusion chromatography and viscometry for the characterisation of cellulose.

作者信息

Dupont Anne-Laurence, Mortha Gérard

机构信息

Centre de Recherches sur la Conservation, Centre national de la Recherche Scientifique, Ministère de la Culture et de la Communication, Muséum National d'Histoire Naturelle,75005 Paris, France.

出版信息

J Chromatogr A. 2004 Feb 13;1026(1-2):129-41. doi: 10.1016/j.chroma.2003.11.002.

Abstract

The analysis using size-exclusion chromatography (SEC) with multi-angle light scattering (MALS) and differential refractive index (DRI) detection of cellulose dissolved in lithium chloride/N,N-dimethylacetamide (LiCI/DMAc) is evaluated and compared to two other methods currently used for cellulose analysis. These are SEC with low-angle light scattering (LALS) and ultra-violet detection of cellulose derivatised to tricarbanilates (CTC), and viscometry in cadmium triethylene diamine dihydroxide (cadoxen). The cellulose source is Whatman No. 1 paper, unaged or artificially aged with a combination of heat and humidity. The values of the molar mass (Mr) averages of cellulose obtained with the different methods resulted quite different for both aged and unaged paper. SEC of cellulose in LiCl/DMAc provided the highest Mr averages values, followed by SEC of CTC, while viscometry yielded the lowest values. These differences were more or less pronounced depending on the initial degradation state of the paper. Several hypotheses are presented in order to explain these discrepancies and each method is discussed on the basis of its suitability to characterise the aging-induced degradation.

摘要

采用尺寸排阻色谱法(SEC)结合多角度光散射(MALS)和示差折光检测(DRI)对溶解于氯化锂/N,N-二甲基乙酰胺(LiCl/DMAc)中的纤维素进行分析,并与目前用于纤维素分析的其他两种方法进行比较。这两种方法分别是采用低角度光散射(LALS)和紫外检测的纤维素三苯氨基甲酸酯(CTC)的SEC法,以及在氢氧化镉三乙二胺(镉试剂)中的粘度测定法。纤维素来源为Whatman No. 1滤纸,未老化或经热和湿度组合人工老化。对于老化和未老化的纸张,用不同方法获得的纤维素摩尔质量(Mr)平均值差异很大。LiCl/DMAc中纤维素的SEC法得到的Mr平均值最高,其次是CTC的SEC法,而粘度测定法得到的值最低。这些差异根据纸张的初始降解状态或多或少地有所不同。为了解释这些差异,提出了几种假设,并根据每种方法对表征老化诱导降解的适用性进行了讨论。

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