ONLINE COUPLING OF SUPERCRITICAL-FLUID CHROMATOGRAPHY AND PROTON HIGH-FIELD NUCLEAR-MAGNETIC-RESONANCE SPECTROSCOPY

被引:40
作者
ALBERT, K
BRAUMANN, U
TSENG, LH
NICHOLSON, G
BAYER, E
SPRAUL, M
HOFMANN, M
DOWLE, C
CHIPPENDALE, M
机构
[1] INST ORGAN CHEM,D-72076 TUBINGEN,GERMANY
[2] BRUKER ANALYT MESSTECH GMBH,D-76287 RHEINSTETTEN,GERMANY
[3] ICI PLC,WILTON MAT RES CTR,MIDDLESBROUGH TS90 85E,CLEVELAND,ENGLAND
[4] ZENECA SPECIALTIES,MANCHESTER M9 3DA,LANCS,ENGLAND
关键词
D O I
10.1021/ac00091a009
中图分类号
O65 [分析化学];
学科分类号
070302 ; 081704 ;
摘要
The direct on-line coupling of supercritical fluid chromatography and proton high-field nuclear magnetic resonance spectroscopy is demonstrated. For this purpose, a specially designed pressure-proof continuous-flow probe head has been developed, from which a signal line width of 1.5 Hz can be obtained in the supercritical state. A separation of phthalates is carried out under supercritical conditions with carbon dioxide as eluent and is monitored on-line with H-1 NRIR on a 400-MHz NMR instrument. All the components can be identified from their NMR spectra. The advantage of carbon dioxide as eluent is that the whole spectral range of the H-1 NMR spectra can be observed and no solvent suppression techniques are necessary to obtain the MMR spectre. Continuous-flow H-1 NMR spectra acquired under supercritical conditions are of the same quality as those recorded in liquids.
引用
收藏
页码:3042 / 3046
页数:5
相关论文
共 14 条
[1]   REVERSED-PHASE HIGH-PERFORMANCE LIQUID-CHROMATOGRAPHY NUCLEAR MAGNETIC-RESONANCE ONLINE COUPLING WITH SOLVENT NON-EXCITATION [J].
ALBERT, K ;
KUNST, M ;
BAYER, E ;
SPRAUL, M ;
BERMEL, W .
JOURNAL OF CHROMATOGRAPHY, 1989, 463 (02) :355-363
[2]   HIGH-PERFORMANCE LIQUID-CHROMATOGRAPHY - NUCLEAR MAGNETIC-RESONANCE ONLINE COUPLING [J].
ALBERT, K ;
BAYER, E .
TRAC-TRENDS IN ANALYTICAL CHEMISTRY, 1988, 7 (08) :288-293
[3]  
ALBERT K, 1988, THESIS TUBINGEN U
[4]  
ALBERT K, 1989, ANAL CHEM, V61, P775
[5]  
Albert K, 1992, HPLC DETECTION NEWER, P197
[6]   DIRECT MONITORING OF SUPERCRITICAL FLUIDS AND SUPERCRITICAL CHROMATOGRAPHIC SEPARATIONS BY PROTON NUCLEAR MAGNETIC-RESONANCE [J].
ALLEN, LA ;
GLASS, TE ;
DORN, HC .
ANALYTICAL CHEMISTRY, 1988, 60 (05) :390-394
[7]   ONLINE COUPLING OF LIQUID-CHROMATOGRAPHY AND HIGH-FIELD NUCLEAR MAGNETIC-RESONANCE SPECTROMETRY [J].
BAYER, E ;
ALBERT, K ;
NIEDER, M ;
GROM, E ;
WOLFF, G ;
RINDLISBACHER, M .
ANALYTICAL CHEMISTRY, 1982, 54 (11) :1747-1750
[8]   ONLINE COUPLING OF HIGH-PERFORMANCE LIQUID-CHROMATOGRAPHY AND NUCLEAR MAGNETIC-RESONANCE [J].
BAYER, E ;
ALBERT, K ;
NIEDER, M ;
GROM, E .
JOURNAL OF CHROMATOGRAPHY, 1979, 186 (DEC) :497-507
[9]  
DORN HC, 1984, ANAL CHEM, V56, P747
[10]  
HOFMANN M, 1993, LABOR PRAXIS, V10, P36