Characterization of Sn-containing polymer chain ends of polybutadiene using 1H/13C/119Sn triple-resonance 3D-NMR

Characterization of Sn-containing polymer chain ends of polybutadiene using 1H/13C/119Sn triple-resonance 3D-NMR
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DOI:
10.1021/ma991771u
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发表时间:
2000-04-04
期刊:
影响因子:
5.5
通讯作者:
Visintainer, J
Visintainer, J
中科院分区:
化学1区
文献类型:
--
作者:
Liu, WX;Saito, T;Visintainer, J

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用H-1/C-13/(119)n三重共振3D-核磁共振谱表征了有机锡聚合物n-Bu3SnPBD(PBD=聚丁二烯)中的含锡结构。当三重共振技术与脉冲Geld梯度相干性选择结合使用时,允许选择性地检测锡-119原子附近的结构碎片,同时从光谱中去除PBD主干的强烈信号。三个频率维度提供了巨大的光谱色散,使许多在1D-核磁共振光谱中看不到的信号得以分辨。三核共振的同时关联提供了大量明确的原子连接性信息。现代仪器的能力使得在没有同位素标记的情况下进行这些实验是可能的,尽管链端的浓度很低,H-1、C-13和Sn-119同位素碎片的出现也很少。
H-1/C-13/(119)n triple-resonance 3D-NMR spectroscopy is used to characterize the tin-containing structures in the organotin polymer n-Bu3SnPBD (PBD = polybutadiene). Triple-resonance techniques, when used together with pulsed Geld gradient coherence selection, permit selective detection of the structure fragments near Sn-119 atom while removing intense signals of the PBD backbone from the spectrum. Three frequency dimensions provide enormous spectral dispersion, permitting the resolution of many signals that are not observable in 1D-NMR spectra. The simultaneous correlation of resonances from three nuclei provides a large amount of unambiguous atomic connectivity information. The capabilities of modern instruments are such that it is possible to perform these experiments without the benefit of isotopic labeling, despite the low concentration of chain ends and the low occurrence of fragments with H-1,C-13,and Sn-119 isotopes.