高转速下采用S-RESIDOR方法测量1H-27Al偶极偶合常数

波谱学杂志

高转速下采用S-RESIDOR方法测量¹H-²⁷Al偶极偶合常数

何义艳²，王秀梅^1,3，李芳^2*，陈雷^1*

1. 波谱与原子分子物理国家重点实验室，武汉磁共振中心(中国科学院武汉物理与数学研究所)，湖北武汉 430071； 
2. 华中师范大学化学学院，湖北武汉 430079；
3. 中国科学院大学，北京 100049

收稿日期:2012-03-14 修回日期:2012-04-23 出版日期:2013-03-05 发布日期:2013-03-05
通讯作者: 陈雷，电话：027-87199737，E-mail：chenlei@wipm.ac.cn; 李芳，电话：027-67867961，E-mail：f.li@mail.ccnu.edu.cn. E-mail:chenlei@wipm.ac.cn；f.li@mail.ccnu.edu.cn
作者简介:何义艳(1985-)，女，河南信阳人，硕士研究生，现从事固体核磁共振应用研究.
基金资助:
国家自然科学基金资助项目（10804122，31100267）.

Determination of ¹H-²⁷Al Dipolar Coupling Constant by ¹H/²⁷Al S-RESIDOR Experiment under Fast MAS

HE Yi-yan², WANG Xiu-mei^1,3, LI Fang^2*, CHEN Lei^1*

1. State Key Laboratory of Magnetic Resonance and Atomic and Molecular Physics, Wuhan Center for Magnetic Resonance (Wuhan Institute of Physics and Mathematics, Chinese Academy of Science), Wuhan 430071, China; 
2. College of Chemistry, Central China Normal University, Wuhan 430079, China; 
3. University of Chinese Academy Science, Beijing 100049, China

Received:2012-03-14 Revised:2012-04-23 Online:2013-03-05 Published:2013-03-05
Contact: Chen Lei,Tel: 027-87199737，E-mail：chenlei@wipm.ac.cn;Li Fang,Tel：027-67867961，E-mail：f.li@mail.ccnu.edu.cn. E-mail:chenlei@wipm.ac.cn；f.li@mail.ccnu.edu.cn
About author:何义艳(1985-)，女，河南信阳人，硕士研究生，现从事固体核磁共振应用研究.
Supported by:
国家自然科学基金资助项目（10804122，31100267）.

摘要/Abstract

摘要：

提出利用S-RESIDOR(Symmetry-based Resonance Echo Saturation Irradiation DOuble Resonance)方法测量¹H-²⁷Al偶极偶合常数. 通过理论模拟，讨论了四极作用常数、饱和照射脉冲功率、照射时间对¹H/²7Al S-RESIDOR实验的影响. 发现四极作用常数对¹H/²⁷Al S-RESIDOR偶极去相曲线影响较小，中等强度的饱和照射功率即能满足实验要求. 高转速下，在氢型丝光沸石上进行了¹H/²⁷Al S-RESIDOR实验，测量得到Br-nsted酸位上的 ¹H与骨架上²⁷Al的偶极偶合常数为874 Hz.

关键词: 核磁共振(NMR), S-RESIDOR, 偶极偶合常数, 丝光沸石

Abstract:

A Symmetry-based Resonance Echo Saturation Irradiation DOuble Resonance (SRESIDOR) method is proposed for measuring ¹H-²⁷Al dipolar coupling constant in zeolite. The influence of ²⁷Al C_qvalue, υ₁ (²⁷Al) and the saturation pulse length of ²⁷Al channel on the ¹H/²⁷Al S-RESIDOR experiment were discussed. Numerical simulations indicate that ¹H/²⁷Al S-RESIDOR dephasing curves are insensitive to the ²⁷Al quadrupole coupling constant, and moderate RF field can fulfill the experiment requirements. The ¹H/²⁷Al S-RESIDOR experiment was performed on H-mordenite under fast spinning speed, and the measured ¹H/²⁷Al dipolar coupling constant is 874 Hz.

Key words: NMR, S-RESIDOR, dipolar coupling constant, mordenite

中图分类号:

O482.53

何义艳，王秀梅，李芳*，陈雷*. 高转速下采用S-RESIDOR方法测量¹H-²⁷Al偶极偶合常数[J]. 波谱学杂志.

HE Yi-yan, WANG Xiu-mei, LI Fang*, CHEN Lei*. Determination of ¹H-²⁷Al Dipolar Coupling Constant by ¹H/²⁷Al S-RESIDOR Experiment under Fast MAS[J]. Chinese Journal of Magnetic Resonance.

参考文献

[1] Gullion T, Schaefer J. Rotational-echo double-resonance NMR[J]. J Magn Reson, 1989, 81: 196-200.

[2] Grey C P, Vega A G. Determination of quadrupole coupling constant of the invisible aluminum spins in zeolite HY with ¹H/²⁷Al TRAPDOR[J]. J Am Chem Soc, 1995, 117: 8 232-8 242.

[3] Gullion T. Measurement of dipolar interactions between spin-1/2 and quadrupolar nuclei by rotational-echo adiabatic-passage double-resonance NMR[J]. Chem Phys Lett, 1995, 246: 325-330.

[4] Gan Z H. Measuring multiple carbonnitrogen distances in natural abundant solids using R-RESPDOR NMR[J]. Chem Commun, 2006, 45: 4 712-4 714.

[5] Ba Y, Kao H M, Grey C P, et al. Optimizing the ¹³C-¹⁴N REAPDOR NMR experiment: a theoretical and experimental study[J]. J Magn Reson, 1998, 133: 104-114.

[6] Gullion T. Detecting ¹³C-¹⁷O dipolar interactions by rotational-echo adiabatic-passage double-resonance NMR[J]. J Magn Reson, 1995, 117: 326-329.

[7] Chopin L, Vega S, Gullion T. A MAS NMR method for measuring ¹³C-¹⁷O distances[J]. J Am Chem Soc, 1998, 120: 4 406-4 409.

[8] Ganapathy S, Kumar R, Delevoye L, et al. Identification of distinct Br-nsted acidic sites in zeolite mordenite by proton localization and ²⁷Al-¹H REAPDOR NMR[J]. Chem Commun, 2003, 16: 2 076-2 077.

[9] Kalwei M, Koller H. Quantitative comparison of REAPDOR and TRAPDOR experiments by numerical simulations and determination of H-Al distances in zeolites[J]. Solid-State NMR, 2002, 21: 145-157. 

[10] Huang W L, Vega A G, Gullion T, et al. Internuclear ³¹P-⁵¹V distance measurements in polyoxoanionic solids using rotational echo adiabatic passage double-resonance NMR spectroscopy[J]. J Am Chem Soc, 2007, 129: 13 027-13 034.

[11] Gullion T, Vega A J. Measuring hetero-nuclear dipolar couplings for S=1/2, I>1/2 spin pairs by REDOR and REAPDOR NMR[J]. Prog Nucl Magn Reson Spec, 2005, 47: 123-136. [12] Hu B W, Trébosc J, Amoureux J P. Comparison of several hetero-nuclear dipolar recoupling NMR methods to be used in MAS HMQC/HSQC[J]. J Magn Reson, 2008, 192（1）: 112-122. 

[13] Chen L, Wang Q, Hu B W, et al. Measurement of hetero-nuclear distances using symmetry- based pulse sequence in solid-state NMR[J]. Phys Chem Chem Phys, 2010, 12: 9 395-9 405.

[14] Li S H, Zheng A M, Su Y C, et al. Br-nsted/Lewis acid synergy in dealuminated HY zeolite: A combined solid-state NMR and theoretical calculation study[J]. J Am Chem Soc, 2007, 129: 11 161-11 171.

[15] Yu Z W, Zheng A M, Wang Q, et al. Insights into the dealumination of zeolite HY revealed by sensitivity-enhanced ²⁷Al DQ-MAS NMR spectroscopy at high field[J]. Angew Chem Int Edit, 2010, 49: 8 657-8 661.

[16] Hunger M, Freude D, Fenzke D, et al. ¹H solid-state NMR studies of the geometry of Br-nsted acid sites in zeolites H-ZSM-5[J]. Chem Phys Lett, 1992, 191: 391-395. 

[17] Kenaston N P, Bell A T, Reimer J A. Determination of the Al-H and H-H internuclear distances in ZSM-5 using NMR spectroscopy[J]. Chem Phys Chem, 1994, 98: 894-896. 

[18] Deng F, Yue Y, Ye C H. ¹H/²⁷Al TRAPDOR NMR studies on aluminum species in dealuminated zeolites[J]. Solid-State NMR, 1998, 10: 151-160. 

[19] Bak M, Rasmussen J T, Nielsen N C. Simpson: a general simulation program for solid-state NMR spectroscopy[J]. J Magn Reson, 2000, 147: 296-330.

[20] Bak M, Nielsen N C. Repulsion: a novel approach to efficient powder averaging in solid-state NMR[J]. J Mag Reson, 1997, 125: 132-139.

[21] Chen L, Lu X Y, Wang Q, et al. Distance measurement between a spin-1/2 and a half-integer quadrupolar nuclei by solid-state NMR using exact analytical expressions[J]. J Magn Reson, 2010, 206: 269-273.

[22] Pfeifer H, Ernst H. NMR of solid surfaces[J]. Ann Rep NMR Spectro, 1993, 5: 28-91.

[23] Hunger M. Br-nsted acid sites in zeolites characterized by multinuclear solid-state NMR spectroscopy[J]. Catal Rev-Sci Eng, 1997, 39: 345-393.

[24] Yu Zhi-wu(喻志武), Zheng An-min(郑安民), Wang Qiang(王强), et al. Acidity characterization of solid acid catalysts by solid-state NMR spectroscopy: A review on recent progresses(固体核磁共振研究固体酸催化剂酸性进展)[J]. Chinese J Magn Reson(波谱学杂志), 2010, 27(4): 485-515

[25] Vega A J. MAS NMR spin-locking of half-integer quadrupolar nuclei\[J\]. J Magn Reson, 1992, 96: 50-68.

[26] Hughes E, Gullion T, Goldbourt A, et al. Inter-nuclear distance determination of S=1, I=1/2- spin-pairs using REAPDOR NMR[J]. J Magn Reson, 2002, 156: 230-241.

[27] Goldbourt A, Vega S, Gullion T, et al. Inter-atomic distance measurement in solid-state NMR between a spin-1/2 and a spin-5/2 using a universal Reapdor curve[J]. J Am Chem Soc, 2003, 125: 11 194-11 195.

高转速下采用S-RESIDOR方法测量¹H-²⁷Al偶极偶合常数

Determination of ¹H-²⁷Al Dipolar Coupling Constant by ¹H/²⁷Al S-RESIDOR Experiment under Fast MAS

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