QUANTITATIVE P-31 NMR ANALYSIS OF LIGNINS, A NEW TOOL FOR THE LIGNIN CHEMIST
QUANTITATIVE P-31 NMR ANALYSIS OF LIGNINS, A NEW TOOL FOR THE LIGNIN CHEMIST
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DOI：
10.1080/02773819408003085
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发表时间：
1994-01-01
影响因子：
2
通讯作者：
ARGYROPOULOS, DS
中科院分区：
文献类型：
--
作者：
ARGYROPOULOS, DS
已经开发出一种新的定量方法来测定木质素中存在的各种类型的羟基。紫丁香基、愈创木基和对羟基苯基游离酚基，以及伯羟基和仲羟基（属于芳基甘油 β-O-4 醚结构的各个赤式和苏式形式）可以通过 P-31 NMR 实验定量测定。这是通过用 1,3,2 二氧磷酰氯对木质素进行亚磷酰化，然后在弛豫试剂（乙酰丙酮铬）和内标存在下进行 P-31 NMR 光谱来实现的。讨论了导致该技术发展的各个方面以及与该方法的再现性和定量有效性相关的统计信息。这种简单而新颖的光谱形式可能成为木质素化学家的宝贵资源，因为它可以提供有关可溶性木质素样品结构的详细定量信息。
A novel quantitative method has been developed for the determination of the various types of hydroxyl groups present in lignins. The syringyl, guaiacyl and p-hydroxyphenyl free phenolic groups, as well as the primary, and the secondary hydroxyl groups (belonging to individual erythro and threo forms of the arylglycerol beta-O-4 ether structures) can be quantitatively determined from a P-31 NMR experiment. This is made possible by phosphitylating lignins with 1,3,2 dioxaphospholanyl chloride, followed by P-31 NMR spectroscopy, in the presence of a relaxation reagent (chromium acetylacetonate) and an internal standard. The various aspects leading to the development of this technique are discussed together with relevant statistical information pertaining to the reproducibility and quantitative validity of the method. This simple and novel form of spectroscopy may become a valuable resource to the lignin chemist, because it can supply detailed quantitative information about the structure of a soluble lignin sample.