SEC–MALLS analysis of cellulose using LiCl/1,3-dimethyl-2-imidazolidinone as an eluent

SEC–MALLS analysis of cellulose using LiCl/1,3-dimethyl-2-imidazolidinone as an eluent
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DOI:
10.1023/b:cell.0000025388.92043.ec
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发表时间:
2004-06
期刊:
影响因子:
5.7
通讯作者:
M. Yanagisawa;I. Shibata;A. Isogai
M. Yanagisawa;I. Shibata;A. Isogai
中科院分区:
材料科学2区
文献类型:
--
作者:
M. Yanagisawa;I. Shibata;A. Isogai

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采用氯化锂/1,3-二甲基-2-咪唑啉酮(LiCl/NH 4)溶剂体系作为体积排阻色谱(SEC)分析纤维素的移动的相,并采用多角度激光光散射和13 C-NMR分析方法考察了该体系的适用性。结果表明,8%(w/v)LiCl/LiCl ID是纤维素的真正溶剂,1%(w/v)LiCl/LiCl ID溶解的纤维素分子在SEC系统中根据其分子质量(MM)或均方根(RMS)半径而有序分离。实际上,在稀释的纤维素/LiCl/Na 2SO 4溶液中未检测到聚集体。此外,已证明纤维素/LiCl/LiCl溶液的高稳定性;即使在室温下储存6个月后,也仅观察到ID平均MM下降百分之几。阔叶木漂白硫酸盐浆ID 1%LiCl/H2O的RMS半径和MM之间的关系估计为以下方程:βgαβ0.59,对应于0.77的Mark-Houwink-Sakurada指数。
The lithium chloride/1,3-dimethyl-2-imidazolidinone (LiCl/DMI) solvent system for cellulose was adopted as a mobile phase of size-exclusion chromatographic (SEC) analysis of cellulose, and the applicability of this system was examined using multi-angle laser light scattering and13C-NMR analysis. The results indicate that 8% (w/v) LiCl/DMI ID a true solvent for cellulose, and that cellulose molecules dissolving ID 1% (w/v) LiCl/DMI are separated orderly depending on their molecular mass (MM) or root-mean-square (RMS) radius by the SEC system. Practically, no aggregates were detected ID the dilute cellulose/LiCl/DMI solutions. Furthermore, high stability of cellulose/LiCl/DMI solutions has been demonstrated; only a few percent of decline ID average MM was observed even after storage for 6 months at room temperature. Relationships between RMS radius and MM for hardwood bleached kraft pulp ID 1% LiCl/DMI was estimated as the following equation: βgαβ0.59, corresponding to a Mark–Houwink–Sakurada exponent of 0.77.