Design and Research of the dDNP Automated Dissolution System

doi:10.11938/cjmr20243101

Abstract

Abstract:

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.

Key words: dissolution dynamic nuclear polarization, double-loop PID control algorithm, dissolution system, high temperature and high pressure

CLC Number:

O482.53

ZENG Xiangzheng, CHEN Junfei, HUANG Chongyang, PI Haiya, CAO Li, HUANG Zhen, GUO Wenlong, FENG Jiwen, LIU Chaoyang. Design and Research of the dDNP Automated Dissolution System[J]. Chinese Journal of Magnetic Resonance, 2024, 41(4): 382-392.

Figures/Tables 10

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Table 1

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每组试验次数	加入溶剂量/mL	目标压强/MPa	氦气压强/MPa	溶融出液体体积/mL	残余溶剂体积/mL
3	8.00	1.70	0.70	6.31±0.18	1.26±0.25
3	8.00	1.70	0.60	6.16±0.33	1.46±0.41
3	8.00	1.70	0.50	5.96±0.09	1.80±0.09
3	8.00	1.70	0.40	5.76±0.37	2.00±0.71
3	8.00	1.60	0.70	6.56±0.19	1.23±0.34
3	8.00	1.60	0.60	6.36±0.09	1.46±0.10
3	8.00	1.60	0.50	5.83±0.41	1.80±0.16
3	8.00	1.60	0.40	5.80±0.19	1.83±0.10
3	8.00	1.50	0.70	6.13±0.10	1.66±0.25
3	8.00	1.50	0.60	5.93±0.19	1.86±0.23
3	8.00	1.50	0.50	5.63±0.19	1.76±0.34
3	8.00	1.50	0.40	5.70±0.28	1.70±0.16
3	8.00	1.40	0.70	6.30±0.16	1.36±0.18
3	8.00	1.40	0.60	6.26±0.33	1.46±0.25
3	8.00	1.40	0.50	5.76±0.32	1.80±0.10
3	8.00	1.40	0.40	5.36±0.19	2.43±0.19