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Title: Short-Pathlength, High-Pressure Flow Cell for Static and Time-Resolved Infrared Spectroscopy , suitable for Supercritical Fluid Solutions Inlcuding Hydrothermal Systems

Journal Article · · Review of Scientific Instruments
DOI:https://doi.org/10.1063/1.1150493· OSTI ID:1845974

An optical flow-cell for high pressures and temperatures is described. The use of a novel window design allows for a precise, fixed optical path length that can bee varied by use of spacers from a few micrometers to several millimeters. The cell pathlength is not affected by changes in pressure or temperature. The novel window design may be applicable to other high-pressure spectroscopic cells. The flow-cell design has a minimal sample dead volume, which is important for kinetic studies. The design eliminates the needs for frazing or a soft-sealing material for the optical windoes, thereby minimzing the number of materials in contact with the sample. Using only diamond and platinum or platinum alloys as the corrosin resistant materials, the design is optimized for the study of aqeous solutions at high temperatures. Infrared spectra of an aqueous sodium tungstate solution up to 400 degrees C and 380 bar pressure are presented. Time-resolved IR data are also presented for the UV-photolysis reaction of beta-naphthoyl azide (BNA) in supercritical carbon dioxide.

Research Organization:
Pacific Northwest National Lab. (PNNL), Richland, WA (United States)
Sponsoring Organization:
USDOE
DOE Contract Number:
AC05-76RL01830
OSTI ID:
1845974
Report Number(s):
PNNL-SA-32251
Journal Information:
Review of Scientific Instruments, Vol. 71, Issue 3; ISSN 0034-6748
Publisher:
American Institute of Physics (AIP)
Country of Publication:
United States
Language:
English

References (12)

A diamond‐window XAFS cell for studies of high‐temperature, high‐pressure aqueous solutions journal September 1996
High‐pressure, capillary x‐ray absorption fine structure cell for studies of liquid and supercritical fluid solutions journal August 1996
Optical free piston cell with constant diameter for use under high pressure journal February 1994
Vibrational Spectroscopy in Supercritical Fluids: From Analysis and Hydrogen Bonding to Polymers and Synthesis journal July 1995
CVD diamond windows for infrared synchrotron applications journal April 1998
Reliable high‐pressure seal for multiple applications journal February 1994
Infra-red absorption of HDO in water at high pressures and temperatures journal January 1967
The solubility of quartz in H2O in the lower crust and upper mantle journal November 1994
Near- and Mid-Infrared Transmission Cells for the Study of Reverse Micelle Phases in Supercritical Fluids journal July 1989
Noncatalytic Organic Synthesis Using Supercritical Water: The Peculiarity Near the Critical Point journal October 1999
Hydrogen bonding of methyl alcohol-d in supercritical carbon dioxide and supercritical ethane solutions journal October 1991
Spectroscopy of Hydrothermal Reactions. 4. Kinetics of Urea and Guanidinium Nitrate at 200−300 °C in a Diamond Cell, Infrared Spectroscopy Flow Reactor journal January 1996

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