PROTON NMR CHARACTERIZATION OF POLY(ETHYLENE GLYCOLS) AND DERIVATIVES

被引:165
作者
DUST, JM [1 ]
FANG, ZH [1 ]
HARRIS, JM [1 ]
机构
[1] UNIV ALABAMA,DEPT CHEM,HUNTSVILLE,AL 35899
关键词
D O I
10.1021/ma00218a005
中图分类号
O63 [高分子化学(高聚物)];
学科分类号
070305 ; 080501 ; 081704 ;
摘要
Derivatives of poly(ethylene glycol) (PEG) are of importance in a variety of applications. Often it is difficult to determine the identity of the end groups and the purity of these derivatives. In the present work we show that proton NMR spectra of PEGs dissolved in deuterated dimethyl sulfoxide (but not other solvents) reveal a hydroxyl peak at 4.56 (±0.02) ppm, which does not shift or broaden with variation in concentration of the PEG, water, or impurities and which is well separated from the large backbone resonance. The hydroxyl resonance in other solvents does not show this independence, and thus it is difficult to locate and utilize. The PEG hydroxyl resonance for samples in dimethyl sulfoxide is, therefore, well suited for quantifying percent substitution and molecular weight of PEG and derivatives. Use of this method is illustrated. © 1990, American Chemical Society. All rights reserved.
引用
收藏
页码:3742 / 3746
页数:5
相关论文
共 53 条
[1]  
ABUCHOWSKI A, 1977, J BIOL CHEM, V252, P3578
[2]  
Andrade J. D., 1987, ASAIO J, V10, P75
[3]  
BARELLE M, 1982, ORG MAGN RESONANCE, V19, P102
[4]  
BAYER E, 1982, POLYM BULL, V8, P585
[5]  
BAYER E, 1983, POLYM BULL, V10, P231
[6]   INSITU REACTIONS OF AMINES AND AMINO-ALCOHOLS AND THEIR APPLICATION TO STRUCTURAL ASSIGNMENT BY H-1-NMR SPECTROSCOPY [J].
BUDESINSKY, M ;
SAMEK, Z ;
TICHY, M .
COLLECTION OF CZECHOSLOVAK CHEMICAL COMMUNICATIONS, 1980, 45 (10) :2784-2803
[7]   STYRAGEL AS PACKING FOR AQUEOUS GEL-PERMEATION CHROMATOGRAPHY [J].
CHOW, CD .
JOURNAL OF CHROMATOGRAPHY, 1975, 114 (02) :486-487
[8]   EFFECT OF END GROUP AND SOLVENT ON GEL-PERMEATION CHROMATOGRAPHY OF OLIGO(OXYETHYLENE) COMPOUNDS [J].
CRAVEN, JR ;
TYRER, H ;
LI, SPL ;
BOOTH, C ;
JACKSON, D .
JOURNAL OF CHROMATOGRAPHY, 1987, 387 :233-240
[9]   FRAGMENTATION OF 2-METHOXYETHANOL DERIVATIVES [J].
DALE, J ;
FREDRIKSEN, SB .
ACTA CHEMICA SCANDINAVICA SERIES B-ORGANIC CHEMISTRY AND BIOCHEMISTRY, 1985, 39 (06) :511-512
[10]   H-1 AND C-13 RELAXATION FOR THE RESOLVED CRYSTALLINE AND AMORPHOUS PHASES OF POLYETHYLENE OXIDE [J].
DECHTER, JJ .
JOURNAL OF POLYMER SCIENCE PART C-POLYMER LETTERS, 1985, 23 (05) :261-266