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Quantitative 2D HSQC NMR determination of polymer structures by selecting suitable internal standard references
KTH, School of Chemical Science and Engineering (CHE), Fibre and Polymer Technology.
KTH, School of Chemical Science and Engineering (CHE), Fibre and Polymer Technology, Wood Chemistry and Pulp Technology.
2007 (English)In: Magnetic Resonance in Chemistry, ISSN 0749-1581, E-ISSN 1097-458X, Vol. 45, no 1, 37-45 p.Article in journal (Refereed) Published
Abstract [en]

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 T-1 and T-2 relaxations, off-resonance effects, coupling constants and homonuclear couplings are discussed. It was found that the T-2 values measured on polymeric samples with the conventional HSQC-CPMG sequence could not be used to correct the errors caused by T-2 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 T-2 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.

Place, publisher, year, edition, pages
2007. Vol. 45, no 1, 37-45 p.
Keyword [en]
NMR, HSQC, quantification, polymers, transverse relaxation (T-2), internal standards, resonance offset, dept pulse sequence, c-13 nmr, adiabatic pulses, spectroscopy, lignin, sensitivity, dependence, aggregation, improvement, inversion
URN: urn:nbn:se:kth:diva-16317DOI: 10.1002/mrc.1914ISI: 000243349900005ScopusID: 2-s2.0-33845921628OAI: diva2:334359
QC 20100525Available from: 2010-08-05 Created: 2010-08-05Bibliographically approved

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