A new decoupling method for accurate quantification of polyethylene copolymer composition and triad sequence distribution with 13C NMR

被引:78
作者
Zhou, Zhe
Kuemmerle, Rainer
Qiu, Xiaohua
Redwine, David
Cong, Rongjuan
Taha, Angela
Baugh, Dan
Winniford, Bill
机构
[1] Dow Chem Co USA, Freeport, TX 77541 USA
[2] Bruker BioSpin AG, NMR Div, CH-8117 Fallanden, Switzerland
[3] Dow Chem Co USA, Midland, MI 48667 USA
关键词
NMR; polyethylene copolymer; composition and sequence distribution; composite pulse decoupling; decoupling sidebands; waltz; bilevel;
D O I
10.1016/j.jmr.2007.05.005
中图分类号
Q5 [生物化学];
学科分类号
071010 ; 081704 ;
摘要
C-13 NMR is a powerful analytical tool for characterizing polyethylene copolymer composition and sequence distribution. Accurate characterization of the composition and sequence distribution is critical for researchers in industry and academia. Some common composite pulse decoupling (CPD) sequences used in polyethylene copolymer 13C NMR can lead to artifacts such as modulations of the decoupled 13C NMR signals (decoupling sidebands) resulting in systematic errors in quantitative analysis. A new CPD method was developed, which suppresses decoupling sidebands below the limit of detection (less than 1:40,000 compared to the intensity of the decoupled signal). This new CPD sequence consists of an improved Waltz-16 CPD, implemented as a bilevel method. Compared with other conventional CPD programs this new decoupling method produced the cleanest C-13 NMR spectra for polyethylene copolymer composition and triad sequence distribution analyses. (c) 2007 Elsevier Inc. All rights reserved.
引用
收藏
页码:225 / 233
页数:9
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