The Effect of NMR Setting Parameters on Molecular Weight Determination of Polyether Diols

Shu-Jie Huang; Xiao-Hong Li; Ying-Feng Tu

doi:10.1007/s10118-024-3172-y

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The Effect of NMR Setting Parameters on Molecular Weight Determination of Polyether Diols

RESEARCH ARTICLE | Updated：2024-11-04

- The Effect of NMR Setting Parameters on Molecular Weight Determination of Polyether Diols
- Chinese Journal of Polymer Science Vol. 42, Issue 11, Pages: 1730-1737(2024)
- Affiliations：
  
  Jiangsu Engineering Laboratory of Novel Functional Polymeric Materials, State and Local Joint Engineering Laboratory for Novel Functional Polymeric Materials, College of Chemistry, Chemical Engineering and Materials Science, Soochow University, Suzhou 215123, China
- Author bio：
  
  lxh83@suda.edu.cn
- Funds：
- DOI：10.1007/s10118-024-3172-y
  CLC：
- Published：30 November 2024，
  
  Published Online：20 August 2024，
  
  Received：16 April 2024，
  
  Revised：12 May 2024，
  
  Accepted：22 May 2024
- Accepted：
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Huang, S. J.; Li, X. H.; Tu, Y. F. The effect of NMR setting parameters on molecular weight determination of polyether diols. Chinese J. Polym. Sci. 2024, 42, 1730–1737

Shu-Jie Huang, Xiao-Hong Li, Ying-Feng Tu. The Effect of NMR Setting Parameters on Molecular Weight Determination of Polyether Diols. [J]. Chinese Journal of Polymer Science, 2024,42(11):1730-1737.
Huang, S. J.; Li, X. H.; Tu, Y. F. The effect of NMR setting parameters on molecular weight determination of polyether diols. Chinese J. Polym. Sci. 2024, 42, 1730–1737 DOI： 10.1007/s10118-024-3172-y.

Shu-Jie Huang, Xiao-Hong Li, Ying-Feng Tu. The Effect of NMR Setting Parameters on Molecular Weight Determination of Polyether Diols. [J]. Chinese Journal of Polymer Science, 2024,42(11):1730-1737. DOI： 10.1007/s10118-024-3172-y.

摘要

We investigate the effect of liquid

H NMR setting parameters on the MW determination of polyether diols

and the optimal quantitative NMR conditions are suggested as following: 90 degree of flip angle with inverted gated

C decoupling and 30 s

Abstract

Nuclear magnetic resonance (NMR) is an advanced technique for the molecular weight (MW) determination of polymers at quantitative conditions. In this study

we investigate the effect of liquid

H-NMR instrumental setting parameters on the MW determination of polyether diols

namely poly(ethylene glycol) (PEG) and poly(tetramethylene oxide) (PTMO) diols

using hydroxymethylene groups as chain-ends. Our results show that the protons in chain-ends have larger spin-lattice relaxation time (

) than those in main chains. To let most of the excited protons relax to the equilibrium state

the delay time (

) should be much larger than

of end-groups. When

C decoupling is inactive

the relative errors can be greater than 60%

due to the

C-coupled proton satellite peaks

which can overlap with chain-end groups or be misassigned as chain-ends. The optimal quantitative NMR conditions for the MW estimation of polyethers are revealed below: standard pulse with inverted gated

C decoupling pulse sequence

32 scans

2.0 s acquisition time in 90 degree of flip angle and 30 s

. The MWs determined from

H quantitati

ve NMR are all smaller than those from SEC which are relative to polystyrene (PS) standards

since the size of polyether chains is larger than that of PS with the same MW. In addition

the MW obtained from SEC for PTMOs shows larger overestimation than PEGs

suggesting PEG chains are more flexible than PTMO’s.

关键词

Keywords

End-group analysisMolecular weightNMRPolyetherDecoupling

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