Department of Chemistry, Jagiellonian University, 30-060 Kraków, Ingardena 3, Poland.
J Chromatogr A. 2010 Oct 15;1217(42):6462-8. doi: 10.1016/j.chroma.2010.07.071. Epub 2010 Aug 11.
The paper deals with the application of size exclusion chromatography (SEC) for the studies of paper degradation phenomena. The goal is to solve some of the technical problems connected with the calibration of multi-detector SEC system and to find the correlation between SEC and viscometric results of degree of polymerization of cellulose. The results gathered for the paper samples degraded by acidic air pollutant (NO(2)) are used as an example of SEC-MALLS application. From the correlation between intrinsic viscosities and absolute value of molecular masses obtained with SEC/MALLS (Multi Angle Laser Light Scattering) technique, Mark-Houwink coefficients for cellulose in cupri-ethylenediamine solution were determined. Thus obtained coefficients were used for the determination of viscometric degree of polymerization (molecular mass) of the aged samples. An excellent correlation was found between the chromatographic values of molecular masses obtained with SEC-UV/VIS detection and the viscometric ones utilizing the improved values of Mark-Houwink coefficients.
本文探讨了尺寸排阻色谱(SEC)在纸降解现象研究中的应用。目的是解决与多检测器 SEC 系统校准相关的一些技术问题,并找到 SEC 与纤维素聚合度的比浓黏度结果之间的相关性。以受酸性空气污染物(NO2)降解的纸样的结果为例,展示 SEC-MALLS 的应用。从 SEC/MALLS(多角度激光光散射)技术获得的特性黏度与绝对分子量之间的相关性,确定了铜乙二胺溶液中纤维素的马克-霍温克系数。利用该方法获得的系数用于确定老化样品的比浓黏度聚合度(分子量)。利用改进的马克-霍温克系数,发现 SEC-UV/VIS 检测获得的分子量色谱值与比浓黏度值之间存在极好的相关性。