Process and reaction monitoring by low-field NMR spectroscopy

被引:192
作者
Dalitz, Franz [1 ]
Cudaj, Markus [2 ,3 ]
Maiwald, Michael [4 ]
Guthausen, Gisela [1 ]
机构
[1] KIT, Inst Mech Proc Engn & Mech, D-76131 Karlsruhe, Germany
[2] KIT, Inst Chem Technol & Polymer Chem, D-76128 Karlsruhe, Germany
[3] PSS Polymer Stand Serv GmbH, D-55120 Mainz, Germany
[4] BAM Fed Inst Mat Res & Testing, D-12489 Berlin, Germany
关键词
Process analysis; Low-field NMR spectroscopy; Flow-NMR; Data analysis; NUCLEAR-MAGNETIC-RESONANCE; SOLID FAT-CONTENT; PERFORMANCE LIQUID-CHROMATOGRAPHY; MULTIVARIATE CURVE RESOLUTION; HYDROGEN-INDUCED POLARIZATION; PRINCIPAL-COMPONENT ANALYSIS; SITU MAS NMR; QUANTITATIVE-ANALYSIS; WATER-SUPPRESSION; REACTION-KINETICS;
D O I
10.1016/j.pnmrs.2011.11.003
中图分类号
O64 [物理化学(理论化学)、化学物理学];
学科分类号
070304 ; 081704 ;
摘要
A study was conducted to demonstrate process and reaction monitoring by low-field nuclear magnetic resonance (NMR) spectroscopy. The study focused on the development of a robust low-field spectroscopic technique which had the potential to be widely applicable in an industrial or technical environment. The development was related to time-domain (TD-) NMR and high-field Fourier-transform (FT) NMR. Reaction monitoring by NMR had been performed inside the probe and the magnet, providing an in situ possibility for monitoring the reaction progress by diverse NMR methods. MAS-studies were also performed to observe polymerization, while heterogeneous catalytic reactions had been investigated by imaging methods. One of the most attractive features of quantitative NMR spectroscopy was that the proportionality of the peak area to the number of nuclei was essentially identical for all nuclei of the same species in a mixture.
引用
收藏
页码:52 / 70
页数:19
相关论文
共 274 条
[1]  
Abragam A., 1989, PRINCIPLES NUCL MAGN
[2]  
ACT Aachen, ACT MOB NMR SOL
[3]   Evolution of Fat Crystal Network Microstructure Followed by NMR [J].
Adam-Berret, Matthieu ;
Boulard, Marine ;
Riaublanc, Alain ;
Mariette, Francois .
JOURNAL OF AGRICULTURAL AND FOOD CHEMISTRY, 2011, 59 (05) :1767-1773
[4]   Reversible Interactions with para-Hydrogen Enhance NMR Sensitivity by Polarization Transfer [J].
Adams, Ralph W. ;
Aguilar, Juan A. ;
Atkinson, Kevin D. ;
Cowley, Michael J. ;
Elliott, Paul I. P. ;
Duckett, Simon B. ;
Green, Gary G. R. ;
Khazal, Iman G. ;
Lopez-Serrano, Joaqun ;
Williamson, David C. .
SCIENCE, 2009, 323 (5922) :1708-1711
[5]   Principal component analysis in liquid chromatography proton nuclear magnetic resonance: differentiation of three regio-isomers [J].
Airiau, CY ;
Shen, HL ;
Brereton, RG .
ANALYTICA CHIMICA ACTA, 2001, 447 (1-2) :199-210
[6]   Concentration measurement by proton NMR using the ERETIC method [J].
Akoka, S ;
Barantin, L ;
Trierweiler, M .
ANALYTICAL CHEMISTRY, 1999, 71 (13) :2554-2557
[7]  
Al Deen TS, 2002, ANAL CHIM ACTA, V474, P125, DOI 10.1016/S0003-2670(02)01017-6
[8]   Chemometric analysis of NMR spectroscopy data: A review [J].
Alam, TM ;
Alam, MK .
ANNUAL REPORTS ON NMR SPECTROSCOPY, VOL 54, 2005, 54 :41-80
[9]   Supercritical fluid chromatography proton nuclear magnetic resonance spectroscopy coupling [J].
Albert, K .
JOURNAL OF CHROMATOGRAPHY A, 1997, 785 (1-2) :65-83
[10]   ONLINE USE OF NMR DETECTION IN SEPARATION CHEMISTRY [J].
ALBERT, K .
JOURNAL OF CHROMATOGRAPHY A, 1995, 703 (1-2) :123-147