Scanning mass spectrometer for quantitative reaction studies on catalytically active microstructures.
We describe an apparatus for spatially resolving scanning mass spectrometry which is able to measure the gas composition above catalytically active microstructures or arrays of these microstructures with a lateral resolution of better than 100 mum under reaction conditions and which allows us to quantitatively determine reaction rates on individual microstructures. Measurements of the three-dimensional gas composition at different vertical distances and separations between active structures allow the evaluation of gas phase mass transport effects. The system is based on a piezoelectrically driven positioning substage for controlled lateral and vertical positioning of the sample under a rigidly mounted capillary probe connecting to a mass spectrometer. Measurements can be performed at pressures in the range of <10(-2)-10 mbars and temperatures between room temperature and 450 degrees C. The performance of the setup is demonstrated using the CO oxidation reaction on Pt microstructures on Si with sizes between 100 and 300 mum and distances in the same order of magnitude, evaluating CO(2) formation and CO consumption above the microstructures. The rapidly decaying lateral resolution with increasing distance between sample and probe underlines the effects of (lateral) gas transport in the room between sample and probe. The reaction rates and apparent activation energy obtained from such measurements agree with previous data on extended surfaces, demonstrating the feasibility of determining absolute reaction rates on individual microstructures.
Roos
M
M
Institute of Surface Chemisty and Catalysis, Ulm University, D-89069, Ulm, Germany.
Kielbassa
S
S
Schirling
C
C
Häring
T
T
Bansmann
J
J
Behm
R J
RJ
D002384:Catalysis; D004867:Equipment Design; D019544:Equipment Failure Analysis; D017022:Flow Injection Analysis / Q000295:instrumentation* / Q000379:methods; D005740:Gases / Q000032:analysis / Q000737:chemistry*; D013058:Mass Spectrometry / Q000295:instrumentation* / Q000379:methods; D008832:Microchemistry / Q000295:instrumentation* / Q000379:methods; D018625:Microscopy, Atomic Force / Q000295:instrumentation* / Q000379:methods; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D013048:Specimen Handling / Q000295:instrumentation* / Q000379:methods
D005740:Gases