基于小型化原子磁力计的零场NMR波谱仪搭建与测试

doi:10.11938/cjmr20233060

波谱学杂志 ›› 2024, Vol. 41 ›› Issue (1): 87-98.doi: 10.11938/cjmr20233060

基于小型化原子磁力计的零场NMR波谱仪搭建与测试

付方跃^1,²,郭清乾^2,³,冯晓宇^2,³,徐佳玉^1,²,姚泽坤^1,²,胡涛^2,^3,⁴,杨晓冬^1,^2,^#(),常严^1,^2,^3,^*()

1.长春理工大学电子信息工程学院，吉林长春 130022
2.中国科学院苏州生物医学工程技术研究所，江苏苏州 215163
3.季华实验室，广东佛山 528200
4.济南国科医工科技发展有限公司，山东济南 250101

收稿日期:2023-03-26 出版日期:2024-03-05 在线发表日期:2023-06-05
通讯作者: # Tel: 18900616030, E-mail: xiaodong.yang@sibet.ac.cn; *Tel: 15895428081, E-mail: changy@sibet.ac.cn.
基金资助:
中科院科研装备研制项目(YJKYYQ20210051);苏州市基础研究试点项目(SJC2021024);山东省自然科学基金青年项目(ZR2022QF098)

Development and Validation of Zero-field NMR Spectrometer Based on Compact Atomic Magnetometer

FU Fangyue^1,²,GUO Qingqian^2,³,FENG Xiaoyu^2,³,XU Jiayu^1,²,YAO Zekun^1,²,HU Tao^2,^3,⁴,YANG Xiaodong^1,^2,^#(),CHANG Yan^1,^2,^3,^*()

1. School of Electronic and Information Engineering, Changchun University of Science and Technology, Changchun 130022, China
2. Suzhou Institute of Biomedical Engineering and Technology, Chinese Academy of Sciences, Suzhou 215163, China
3. Jihua Laboratory, Foshan 528200, China
4. Jinan Guoke Medical Technology Development Co., Ltd, Jinan 250101, China

Received:2023-03-26 Published:2024-03-05 Online:2023-06-05
Contact: # Tel: 18900616030, E-mail: xiaodong.yang@sibet.ac.cn; *Tel: 15895428081, E-mail: changy@sibet.ac.cn.

摘要/Abstract

摘要：

常规高场NMR波谱仪依托超导技术，其体积大、维护成本高，且存在样本磁化率不均匀导致的谱线展宽现象，零场或近零场NMR技术则可实现有效互补．本文自主搭建了一套基于小型原子磁力计的可移动零场NMR波谱仪，采用以多功能采集卡（National Instruments PCIe-6353）为核心的集成控制系统，仪器主磁场强度小于1 nT，可实现高分辨率的J-耦合谱采集．为实现对自旋体系的有效操控，利用样品绝热初态的单脉冲激发实现对三轴脉冲线圈的精确标定．在此基础上，使用改进的组合脉冲序列实现了在¹³C-¹H异核体系下的单自旋选择性操控，验证了零场NMR波谱仪的有效性．

关键词: 零场核磁共振, J-耦合谱, 原子磁力计, 单自旋操控

Abstract:

Conventional high-field nuclear magnetic resonance (NMR) spectrometer necessitates advanced superconducting technology, which usually involves a magnet of large volume and high maintenance cost. Moreover, strong magnet often has severe magnetic field inhomogeneity, leading to NMR line broadening. Zero- to ultralow-field (ZULF) NMR emerged as a complementary approach to traditional high-field NMR techniques. In this paper, a portable zero-field NMR spectrometer based on a compact atomic magnetometer was developed, which adopted an integrated control system based on a multi-function data acquisition card (National Instruments PCIe-6353). The spectrometer is of a main magnetic field strength less than 1 nT and enables achieving high-resolution J-spectrum under zero-field environment. Specifically, a series of single pulse excitation experiments for the initial adiabatic state was carried out to calibrate the triaxial magnetic field coils. Then a modified composite pulse sequence was developed to further validate the performance of zero-field NMR spectrometer by single-spin control experiments for the ¹³C-¹H spin system.

Key words: zero-field NMR, J-spectroscopy, atomic magnetometer, single-spin control

中图分类号:

O482.53

付方跃, 郭清乾, 冯晓宇, 徐佳玉, 姚泽坤, 胡涛, 杨晓冬, 常严. 基于小型化原子磁力计的零场NMR波谱仪搭建与测试[J]. 波谱学杂志, 2024, 41(1): 87-98.

FU Fangyue, GUO Qingqian, FENG Xiaoyu, XU Jiayu, YAO Zekun, HU Tao, YANG Xiaodong, CHANG Yan. Development and Validation of Zero-field NMR Spectrometer Based on Compact Atomic Magnetometer[J]. Chinese Journal of Magnetic Resonance, 2024, 41(1): 87-98.

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参考文献 31

[1]	BAHTI A, TELFAH A, LAMBERT J, et al. Optimal control pulses for subspectral editing in low field NMR[J]. J Magn Reson, 2021, 328: 106993. doi: 10.1016/j.jmr.2021.106993
[2]	JOHN W B, TENG WU, JAMES E, et al. Zero- to ultralow-field nuclear magnetic resonance J-spectroscopy with commercial atomic magnetometers[J]. J Magn Reson, 2020, 314: 106723. doi: 10.1016/j.jmr.2020.106723
[3]	TAYLER MICHALE C D, THOMAS T, SJOLANDER TOBIAS F, et al. Invited review article: instrumentation for nuclear magnetic resonance in zero and ultralow magnetic field[J]. Rev Sci Instrum, 2017, 88(9): 091101. doi: 10.1063/1.5003347
[4]	TOBIAS F S, JOHN W B, DMITRY B, et al. Two-dimensional single- and multiple-quantum correlation spectroscopy in zero-field nuclear magnetic resonance[J]. J Magn Reson, 2020, 318: 106781. doi: 10.1016/j.jmr.2020.106781
[5]	ALLRED J C, LYMAN R N, KORNACK T W, et al. High-sensitivity atomic magnetometer unaffected by spin-exchange relaxation[J]. Phys Rev Lett, 2002, 89(13): 130801. doi: 10.1103/PhysRevLett.89.130801
[6]	LEDBETTER M P, THEIS T, BLANCHARD J W, et al. Near-zero-field nuclear magnetic resonance[J]. Phys Rev B: Condens, 2011, 107(10): 107601.
[7]	JOHN W B, MICAH P L, THOMAS T, et al. High-resolution zero-field NMR J-spectroscopy of aromatic compounds[J]. J Am Chem Soc, 2013, 135(9): 3607-3612. doi: 10.1021/ja312239v
[8]	LIU G B, LI X F, SUN X P, et al. Ultralow field NMR spectrometer with an atomic magnetometer near room temperature[J]. J Magn Reson, 2013, 237: 158-163. doi: S1090-7807(13)00263-2 pmid: 24225528
[9]	JIANG M, ROMAN P F, WU T, et al. Magnetic gradiometer for the detection of zero- to ultralow-field nuclear magnetic resonance[J]. Phys Rev Appl, 2019, 11(2): 024005. doi: 10.1103/PhysRevApplied.11.024005
[10]	JIANG M, WU T, JOHN W B, et al. Experimental benchmarking of quantum control in zero-field nuclear magnetic resonance[J]. Sci Adv, 2018, 4(6): 6327. doi: 10.1126/sciadv.aar6327 pmid: 29922714
[11]	BIAN J, JIANG M, CUI J Y, et al. Universal quantum control in zero-field nuclear magnetic resonance[J]. Phys Rev A, 2017, 95(5): 052342. doi: 10.1103/PhysRevA.95.052342
[12]	JIANG M, BIAN J, LIU X M, et al. Numerical optimal control of spin systems at zero magnetic field[J]. Phys Rev A, 2018, 97(6): 062118. doi: 10.1103/PhysRevA.97.062118
[13]	JI Y L, BIAN J, JIANG M, et al. Time-optimal control of independent spin-1/2 systems under simultaneous control[J]. Phys Rev A, 2018, 98(6): 062108. doi: 10.1103/PhysRevA.98.062108
[14]	JIANG M, JI Y L, LI Q, et al. Multiparameter quantum metrology using strongly interacting spin systems[J]. arXiv.org, 2021, DOI: https://doi.org/10.48550/arXiv.2104.00211
[15]	DANILA A B, MICHAEL C D, IRENE M R, et al. Zero-field nuclear magnetic resonance of chemically exchanging systems[J]. Nat Commun, 2019, 10: 3002. doi: 10.1038/s41467-019-10787-9 pmid: 31278303
[16]	PIOTR P, SZYMON P, DMITRY B, et al. Zero- to ultralow-field NMR spectroscopy of small biomolecules[J]. Anal Chem, 2021, 93(6): 3226-3232. doi: 10.1021/acs.analchem.0c04738 pmid: 33448215
[17]	SAVUKOV I M, ZOTEV V S, VOLEGOV P L, et al. MRI with an atomic magnetometer suitable for practical imaging applications[J]. J Magn Reson, 2009, 199(2): 188-191. doi: 10.1016/j.jmr.2009.04.012 pmid: 19435672
[18]	SHENG D, PERRY A R, KRZYZEWSKI S P, et al. A microfabricated optically-pumped magnetic gradiometer[J]. Appl Phys Lett, 2017, 110(3): 031106. doi: 10.1063/1.4974349
[19]	SHENG J W, WAN S G, SUN Y F, et al. Magnetoencephalography with a Cs-based high-sensitivity compact atomic magnetometer[J]. Rev Sci Instrum, 2017, 88(9): 094304. doi: 10.1063/1.5001730
[20]	THEIS T, LEDBETTER M P, KERVERN G, et al. Zero-field NMR enhanced by parahydrogen in reversible exchange[J]. J Am Chem Soc, 2012, 134(9): 3987-3990. doi: 10.1021/ja2112405 pmid: 22332806
[21]	CI J, YANG X, XIN J X, et al. Preparation and lifetime studies of the singlet state of five spins in hexene molecules used to guide the preservation of the parahydrogen-induced nuclear polarization state[J]. Chinese J Magn Reson, 2023, 40(1):30-38.
	慈杰, 杨雪, 辛家祥, 等. 用于指导仲氢诱导核极化状态保存的己烯分子中五自旋的单重态制备和寿命研究[J]. 波谱学杂志, 2023, 40(1): 30-38.
[22]	BODENSTEDT S, MITCHELL M W, TAYLER M C D. Fast-field-cycling ultralow-field nuclear magnetic relaxation dispersion[J]. Nat Commun, 2021, 12: 4041. doi: 10.1038/s41467-021-24248-9 pmid: 34193862
[23]	DUDARI B B, JAMES E, JOHN W B, et al. Chemical reaction monitoring using zero-field nuclear magnetic resonance enables study of heterogeneous samples in metal containers[J]. Angew Chem Int Ed, 2020, 59(39): 17026-17032. doi: 10.1002/anie.v59.39
[24]	ZHOU Q J, XIANG J F, TANG Y L, et al. Pure shift proton NMR spectroscopy and its applications[J]. Chinese J Magn Reson, 2016, 33(3): 502-513.
	周秋菊, 向俊锋, 唐亚林, 等. 纯位移核磁共振氢谱及其应用[J]. 波谱学杂志, 2016, 33(3): 502-513.
[25]	CHEN C Q, ZHANG X, GUO Q Q, et al. Moving wearable magnetoencephalography measurement study based on optically-pumped magnetometer[J]. Chinese J Magn Reson, 2022, 39(3): 337-344.
	陈春巧, 张欣, 郭清乾, 等. 基于原子磁力计的穿戴式脑磁图动态测量研究[J]. 波谱学杂志, 2022, 39(3): 337-344.
[26]	WANG X F, ZHU M H, XIAO K D et al. Static weak magnetic field measurements based on low-field nuclear magnetic resonance[J]. J Magn Reson, 2019, 307: 106580. doi: 10.1016/j.jmr.2019.106580
[27]	BUSSANDRI S, ACOSTA R H, BULJUBASICH L. Radiofrequency encoded only parahydrogen spectroscopy[J]. J Magn Reson, 2020, 323: 106894. doi: 10.1016/j.jmr.2020.106894
[28]	ZHANG S L, CHANG Y, YANG X D. Optimization of limited amplitude radiofrequency pulse with variance evaluation[J]. Chinese J Magn Reson, 2015, 32(3):462-469.
	张树林, 常严, 杨晓冬. 方差评估在幅值限制脉冲优化中的应用[J]. 波谱学杂志, 2015, 32(3): 462-469.
[29]	江敏. 基于高灵敏度原子磁力计的超低场核磁共振研究[D]. 安徽: 中国科学技术大学, 2019.
[30]	BODENSTEDT S, MOLL D, GLOGGLER S, et al. Decoupling of spin decoherence paths near zero magnetic field[J]. J Phys Chem Lett, 2022, 13(1): 98-104. doi: 10.1021/acs.jpclett.1c03714
[31]	TIMOTHY D W C. High-resolution NMR techniques in organic chemistry[M]. Elsevier, 2009.

基于小型化原子磁力计的零场NMR波谱仪搭建与测试

Development and Validation of Zero-field NMR Spectrometer Based on Compact Atomic Magnetometer

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