High-Pressure, High-Temperature Spectrophotometer Cell for in Situ Catalyst Identification
A high-pressure, high-temperature spectrophotometer cell has been designed and constructed in order to examine reacting solutions at conditions which are above ambient temperature and pressure. Large windows, a variable-path length, and a relatively compact design provide considerable versatility and permit the use of the cell interchangeably among a variety of commercially available IR and UV-Visible spectrophotometers without the need for special instrument modification. The cell has been used to study solutions at a variety of reaction conditions up to 100 atmospheres of pressure at 200°C without any suggestion of window or cell failure. The design and fabrication of the cell are reported. In addition, specific applications of the cell to studies of the rhodium-catalyzed hydroformylation of olefins are described.
KeywordsCalcium Fluoride Rhodium Complex Carbonyl Band Window Material Catalyst Identification
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- 9.M. Bianchi, E. Benedetti, and F. Piacenti, Chem. Ind. (Milan), 51:613 (1969).Google Scholar
- 10.R. L. Pruett and J. A. Smith, J. Org. Chem., 34: 327 (1969).Google Scholar
- 13.R. Whyman, J. Phys. E: Sci. Instrum., 3:573 (1970).Google Scholar
- 14.Thermistor Temperature Controller, Model 7115, purchased from Yellow Spring Instrument Company, Inc., Yellow Spring, Ohio, and modified by installing a 100 0 resistor in parallel with the probe in order to expand the temperature-range. Four 50 watt heaters were sufficient to maintain 200°C.Google Scholar
- 15.Harshaw Optical Crystals, Harshaw Chemical Company, 1967, p. 15–17.Google Scholar
- 16.D. E. Morris and H. B. Tinker, presented at the Second North American Catalysis Society Meeting, Houston, Texas, February 24–26, 1971; C & E News, p. 53, March 8, 1971.Google Scholar
- 17.This equipment has been described in detail elsewhere. J. H. Craddock, A. Hershman, F. E. Paulik, and J. F. Roth, Ind. Eng. Chem. Prod. Res. Develop., 8: 291 (1969).Google Scholar