Issue 20, 2003

Improved experimental setup for in situUV-vis-NIRspectroscopy under catalytic conditions

Abstract

A commercial UV-vis-NIR spectrometer (Lambda 9, PerkinElmer) equipped with an integrating sphere was supplemented with a construction to measure in situ diffuse reflectance spectra from room temperature to 723 K in the range from 250 to 2500 nm. The new construction was compared to a previously developed setup, which features a highly reflecting ceramic spacer that bridges the 12 mm between the integrating sphere and microreactor. In the new construction, the catalyst bed is in the isothermal zone of a tubular furnace and the 120 mm space between the optical quartz window of the microreactor and the integrating sphere are bridged with a specially formed light conductor made of quartz. Improvements include a stable position of the powder bed, a smaller bed volume (ca. 0.27 cm3), a reduction of thermal radiation, and a higher signal level and thus better signal-to-noise-ratio. The performance of the setup is demonstrated by two examples, (i) spectra recorded at 723 K during the activation of a zirconia sample, and (ii) spectra recorded during n-pentane isomerization over sulfated zirconia at room temperature with simultaneous gas phase analysis.

Supplementary files

Article information

Article type
Paper
Submitted
10 Apr 2003
Accepted
25 Jul 2003
First published
12 Aug 2003

Phys. Chem. Chem. Phys., 2003,5, 4366-4370

Improved experimental setup for in situ UV-vis-NIR spectroscopy under catalytic conditions

J. Melsheimer, M. Thiede, R. Ahmad, G. Tzolova-Müller and F. C. Jentoft, Phys. Chem. Chem. Phys., 2003, 5, 4366 DOI: 10.1039/B304039A

To request permission to reproduce material from this article, please go to the Copyright Clearance Center request page.

If you are an author contributing to an RSC publication, you do not need to request permission provided correct acknowledgement is given.

If you are the author of this article, you do not need to request permission to reproduce figures and diagrams provided correct acknowledgement is given. If you want to reproduce the whole article in a third-party publication (excluding your thesis/dissertation for which permission is not required) please go to the Copyright Clearance Center request page.

Read more about how to correctly acknowledge RSC content.

Social activity

Spotlight

Advertisements