Spectroscopic set-up for simultaneous UV-Vis/(Q)EXAFS in situ and in operando studies of homogeneous reactions under laboratory conditions

被引：30

作者：

Bauer, Matthias ^{[1
]}

Heusel, Gerhard ^{[1
]}

Mangold, Stefan ^{[2
]}

Bertagnolli, Helmut ^{[1
]}

机构：

[1] Univ Stuttgart, Inst Phys Chem, D-70569 Stuttgart, Germany

[2] Forschungszentrum Karlsruhe, Angstromquelle Karlsruhe ANKA, Inst Synchrotron Radiat, D-76344 Eggenstein Leopoldshafen, Germany

来源：

JOURNAL OF SYNCHROTRON RADIATION | 2010年 / 17卷

关键词：

two-dimensional spectroscopy; QEXAFS; UV/Vis; in operando; X-RAY-ABSORPTION; EXAFS MEASUREMENTS; HETEROGENEOUS CATALYSTS; FLUORESCENCE-MODE; SAMPLE CELL; TRANSMISSION; COMPLEXES; BEHAVIOR; OXYGEN; STATE;

D O I：

10.1107/S0909049509054910

中图分类号：

TH7 [仪器、仪表];

学科分类号：

0804 ; 080401 ; 081102 ;

摘要：

A novel experimental set-up for in operando studies of homogeneous catalyzed reactions under laboratory conditions has been developed and tested. It combines time-resolved X-ray absorption spectroscopy with UV/Vis spectroscopy. The reaction solution is stirred in a vessel and pumped in a circle by a peristaltic free gear-wheel through a measurement cell. The X-ray and UV/Vis beams probe the same sample volume of the cell orthogonally. Reactants can be added to the reaction mixture in the course of the measurements and a defined gas atmosphere can be adjusted up to a pressure of 10 bar. The in situ reduction of cerium(IV) ammonium nitrate to cerium(III) by isopropanol is studied as a test reaction with quick-XANES and UV/Vis measurements with a time resolution of 60 s and 1 s, respectively.

引用

页码：273 / 279

页数：7

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