Quantitative 2D HSQC NMR determination of polymer structures by selecting suitable internal standard references

• Published in: Magnetic resonance in chemistry Vol. 45; no. 1; pp. 37 - 45
• Main Authors: Zhang, Liming, Gellerstedt, Göran
• Format: Journal Article
• Language: English
• Published: Chichester, UK John Wiley & Sons, Ltd 01.01.2007
• Subjects: Acetylation; adiabatic pulses; aggregation; Anisoles - chemistry; c-13 nmr; Cellulose - analogs & derivatives; Cellulose - chemistry; Chloroform - chemistry; dependence; dept pulse sequence; HSQC; improvement; internal standards; inversion; lignin; Lignin - chemistry; Magnetic Resonance Spectroscopy - methods; Magnetic Resonance Spectroscopy - standards; NMR; polymers; Polymers - chemistry; quantification; Reference Standards; resonance offset; sensitivity; spectroscopy; transverse relaxation (T-2); transverse relaxation (T2)
• ISSN: 0749-1581; 1097-458X; 1097-458X
• DOI: 10.1002/mrc.1914

A new analytical method based on the 2D HSQC NMR sequence is presented, which can be applied for quantitative structural determination of complicated polymers. The influence of T1 and T2 relaxations, off‐resonance effects, coupling constants and homonuclear couplings are discussed. It was found that the T2 values measured on polymeric samples with the conventional HSQC‐CPMG sequence could not be used to correct the errors caused by T2 relaxations during the polarization transfer delay. A unique way of selecting the proper internal standard reference signal(s) is therefore proposed to eliminate the major errors caused by T2 relaxations, resonance offsets, coupling constant deviations and homonuclear couplings. Two polymer samples, a cellulose triacetate and an acetylated lignin, have been used to illustrate the principles. The methodology developed in this work is robust to instrument miss‐setting and it can find wide‐spread applications in areas where a quantitative analysis of structurally complicated polymers is necessary. Copyright © 2006 John Wiley & Sons, Ltd.