dDNP溶融系统的自动化设计与研究
收稿日期: 2024-03-18
网络出版日期: 2024-04-16
基金资助
国家自然科学基金重大科研仪器研制项目(22327901);国家重点研发计划项目(2022YFF0707001);国家自然科学基金青年项目(22204168);国家自然科学基金青年项目(12205352);曙光计划项目(2022010801020130);中国科学院B类先导专项(XDB0540301)
Design and Research of the dDNP Automated Dissolution System
Received date: 2024-03-18
Online published: 2024-04-16
溶融动态核极化(dDNP)是一种将分子样品在超低温、强磁场以及微波照射下高度极化,然后经高温高压溶剂快速溶解后立即转移至NMR/MRI系统进行检测的灵敏度增强技术.溶融系统是实现这一过程的关键部分,其性能直接影响样品的溶融、转移效率以及样品极化度的保留程度.本文提出了基于双闭环PID控制算法的自动化溶融系统的控制方案,可在9 min以后达到目标压强1.7 MPa左右并使内部压强被动控制在1.5%以内.将研制的自动化溶融系统集成于自主开发的5 T dDNP仪器系统,可将-271℃的低温样品快速溶融,并于4 s内将其转移到距离11.2 m处的7 T NMR系统进行检测,获得了[1-13C]-丙酮酸钠在溶融态下13C NMR信号9 050倍的增强.自动化溶融系统简化了操作步骤,提高了实验的安全性和一致性.
关键词: 溶融动态核极化; 双闭环PID控制算法; 溶融系统; 高温高压
曾祥政 , 陈俊飞 , 黄重阳 , 皮海亚 , 曹丽 , 黄臻 , 郭文龙 , 冯继文 , 刘朝阳 . dDNP溶融系统的自动化设计与研究[J]. 波谱学杂志, 2024 , 41(4) : 382 -392 . DOI: 10.11938/cjmr20243101
Dissolution dynamic nuclear polarization (dDNP) involves polarizing the sample under microwave irradiation at a low-temperature and strong-magnetic field, dissolving it by solvent of high-temperature and high-pressure, then injecting it rapidly into an NMR/MRI for detection. The dissolution system serves as a pivotal component in the dissolving and injecting process, with its performance directly affecting the melting and transfer efficiency and the high polarization retention. We present an automated dissolution system using a dual-loop proportional-integral-derivative (PID) control algorithm that can reach the target pressure of ~1.7 MPa after 9 min and control the internal pressure within 1.5%. The system can dissolve a solid sample of -271 ℃ in the self-developed 5 T dDNP polarizer and transfer it to the 7 T NMR system at a distance of 11.2 m for detection in 4 s, yielding a 9050-fold enhancement of 13C NMR signal of sodium [1-13C]-pyruvate at the solvated state. In summary, this work developed an automated dissolution system that simplifies the operation steps, ensures detection consistency, and improves experimental safety.
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