Development of stopped-flow hyper-CEST NMR method on recirculating hyperpolarization system as applied to void space analysis in polymers

IF 1.8 4区 化学 Q3 CHEMISTRY, ANALYTICAL Analytical Sciences Pub Date : 2024-09-10 DOI:10.1007/s44211-024-00661-0
Hideaki Fujiwara, Hirohiko Imai, Atsuomi Kimura
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Abstract

129Xe NMR spectroscopy of polymers can provide important information on void spaces, sometimes called free volume, in polymers. Unfortunately, the spectroscopy's low sensitivity has limited its widespread use in both academic and industrial research. In order to overcome such a difficult situation, hyper-CEST method which employs hyperpolarization and CEST techniques, is examined after the introduction of recirculation and subtraction modes. Alongside the incorporated stopped-flow technique, these modes were very efficient in detecting very weak hidden signals from cellulose nanofiber (CNF) and silk fibroin (SF) films and in discussing the void space in these polymers. From the analysis of detailed saturation frequency dependence in the increment of 100 Hz, the chemical shifts of hidden peaks were successfully determined to give reasonable values for the size of void space in CNF and SF. Application on thermoplastic polyurethane film also supported our method of analysis. The subtraction mode was very efficient in judging the presence or absence of any peak at a fixed saturation frequency. These facts support that the mode will surely be useful in the future exploratory study of very weak hidden signals.

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开发应用于聚合物空隙分析的循环超极化系统停流超 CEST NMR 方法。
聚合物的 129Xe NMR 光谱可提供聚合物中空隙(有时称为自由体积)的重要信息。遗憾的是,该光谱的灵敏度较低,限制了其在学术和工业研究中的广泛应用。为了克服这一困难,我们在引入循环和减法模式后,对采用超极化和 CEST 技术的 hyper-CEST 方法进行了研究。除了采用停流技术,这些模式在检测纤维素纳米纤维(CNF)和蚕丝纤维素(SF)薄膜中非常微弱的隐藏信号以及讨论这些聚合物中的空隙空间方面非常有效。通过分析增量为 100 Hz 的详细饱和频率依赖关系,成功确定了隐藏峰的化学位移,从而给出了 CNF 和 SF 中空隙大小的合理值。在热塑性聚氨酯薄膜上的应用也支持了我们的分析方法。减法模式可以非常有效地判断在固定饱和频率下是否存在任何峰值。这些事实证明,该模式必将在未来对极弱隐藏信号的探索性研究中发挥作用。
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来源期刊
Analytical Sciences
Analytical Sciences 化学-分析化学
CiteScore
2.90
自引率
18.80%
发文量
232
审稿时长
1 months
期刊介绍: Analytical Sciences is an international journal published monthly by The Japan Society for Analytical Chemistry. The journal publishes papers on all aspects of the theory and practice of analytical sciences, including fundamental and applied, inorganic and organic, wet chemical and instrumental methods. This publication is supported in part by the Grant-in-Aid for Publication of Scientific Research Result of the Japanese Ministry of Education, Culture, Sports, Science and Technology.
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