ULTRA-HIGH-RESOLUTION SI-29 SOLID-STATE MAS NMR INVESTIGATION OF SORBATE AND TEMPERATURE-INDUCED CHANGES IN THE LATTICE STRUCTURE OF ZEOLITE ZSM-5

被引:128
作者
FYFE, CA
STROBL, H
KOKOTAILO, GT
KENNEDY, GJ
BARLOW, GE
机构
[1] Univ of British Columbia, Vancouver,, BC, Can, Univ of British Columbia, Vancouver, BC, Can
关键词
CRYSTALS - Structure - NUCLEAR MAGNETIC RESONANCE - ORGANIC COMPOUNDS - Spectroscopic Analysis - XYLENE - Structure;
D O I
10.1021/ja00219a005
中图分类号
O6 [化学];
学科分类号
0703 ;
摘要
By preparing extremely highly crystalline, highly siliceous samples and careful optimization of all experimental parameters, it is possible to obtain **2**9Si MAS NMR spectra of zeolite ZSM-5 with line widths of 0. 06 ppm (6 Hz) at a proton frequency of 400 MHz, yielding a spectrum for the unloaded form in which up to 21 of the 24 resonances can be observed giving an unambiguous analysis. This ultra-high resolution makes it possible to clearly observe changes induced in the lattice structure by both temperature and the presence of organic sorbates. The change between the monoclinic (24 T -atoms) and orthorhombic (12 T-atoms) forms occurs between 355 and 357 degree C and in the case of p-xylene at approximately two molecules per 96 T atom unit cell.
引用
收藏
页码:3373 / 3380
页数:8
相关论文
共 45 条
[31]  
LERMER H, 1985, ZEOLITES, V5, P13
[32]   INVESTIGATION OF THE STRUCTURE OF ZEOLITES BY SOLID-STATE HIGH-RESOLUTION SI-29 NMR-SPECTROSCOPY [J].
LIPPMAA, E ;
MAGI, M ;
SAMOSON, A ;
TARMAK, M ;
ENGELHARDT, G .
JOURNAL OF THE AMERICAN CHEMICAL SOCIETY, 1981, 103 (17) :4992-4996
[33]   STRUCTURAL STUDIES OF SILICATES BY SOLID-STATE HIGH-RESOLUTION SI-29 NMR [J].
LIPPMAA, E ;
MAGI, M ;
SAMOSON, A ;
ENGELHARDT, G ;
GRIMMER, AR .
JOURNAL OF THE AMERICAN CHEMICAL SOCIETY, 1980, 102 (15) :4889-4893
[34]  
MEIER WM, 1978, ATLAS ZEOLITES STRUC
[35]   SELECTIVE EXCITATION IN FOURIER-TRANSFORM NUCLEAR MAGNETIC-RESONANCE [J].
MORRIS, GA ;
FREEMAN, R .
JOURNAL OF MAGNETIC RESONANCE, 1978, 29 (03) :433-462
[36]   CRYSTAL-STRUCTURE AND STRUCTURE-RELATED PROPERTIES OF ZSM-5 [J].
OLSON, DH ;
KOKOTAILO, GT ;
LAWTON, SL ;
MEIER, WM .
JOURNAL OF PHYSICAL CHEMISTRY, 1981, 85 (15) :2238-2243
[37]   CRYSTAL-STRUCTURE OF TETRAPROPYLAMMONIUM FLUORIDE CONTAINING PRECURSOR TO FLUORIDE SILICALITE [J].
PRICE, GD ;
PLUTH, JJ ;
SMITH, JV ;
BENNETT, JM ;
PATTON, RL .
JOURNAL OF THE AMERICAN CHEMICAL SOCIETY, 1982, 104 (22) :5971-5977
[38]   ON THE SIMILARITY OF THE HIGH-RESOLUTION SOLID-STATE SI-29 AND AL-27 SPECTRA OF SILICALITE AND DEALUMINATED ZEOLITE ZSM-5 [J].
THOMAS, JM ;
KLINOWSKI, J ;
ANDERSON, MW .
CHEMISTRY LETTERS, 1983, (10) :1555-1556
[39]   THE EVALUATION OF NON-EQUIVALENT TETRAHEDRAL SITES FROM SI-29 NMR CHEMICAL-SHIFTS IN ZEOLITES AND RELATED ALUMINOSILICATES [J].
THOMAS, JM ;
KLINOWSKI, J ;
RAMDAS, S ;
HUNTER, BK ;
TENNAKOON, DTB .
CHEMICAL PHYSICS LETTERS, 1983, 102 (2-3) :158-162
[40]   DEALUMINATED ZEOLITES [J].
THOMAS, JM .
JOURNAL OF MOLECULAR CATALYSIS, 1984, 27 (1-2) :59-69