(click for enlarged version)
2 L Parr Reactor
Micromeritics ASAP 2020 (with chemisorption option)
Catalyst Pretreatment Rig
300 mL Parr Reactor
Gas Analysis GC/FID & GC/TCD
FTIR (with 10 cm gas cell installed)
|Microcalorimeter Vacuum Rig
|50 mL Parr Reactors
|Liquid Autoinjector GC/FID
Facilities, Equipment and Other
-Liquid Phase Flow Reactors-
We have built and tested several liquid phase flow reaction kinetics apparatus for the
catalytic upgrading of water-soluble, biomass-derived organic molecules. The catalyst is
loaded in 1/4 or 1/2 inch stainless steel reactors. HPLC pumps are used to supply
the reactor with liquid feed. Hydrogen or (or other) gas can also be fed
to the reactor. The system operates at pressures up to 1000 psig (the pressure
is controlled by the backpressure regulator). The liquid effluent from the
reactor is collected in a gas-liquid separator. The effluent gas stream is analyzed on-line
by GC. The separator is periodically drained and the organic and liquid phases
are analyzed off-line using GC and HPLC.
-Parr Batch Reactors-
We currently have five 50 mL, two 300-mL, two 500-mL, and one 2-L stirred batch Parr Reactors. The reactors
are capable of operating at temperatures up to 490 K and pressures up to 3000
psig, and one is configured to operate at temperatures up to 573 K. The 50-mL reactors are stirred with magnetic stirrers (0-600 rpm), and the larger reactors are stirred using motor-driven impellers. Each has a
liquid sampling valve so that samples can be withdrawn during operation.
Reaction products are identified by GC or HPLC. Additionally, one 50-mL Parr Reactor is configured to accept an ATR-IR probe, allowing in-situ monitoring of reactions.
-Glass Batch Reactors-
We have configured several hot plates with oil baths that accept 10-mL glass batch reactors for small-volume reaction studies. The reactors are capable of operating at temperatures up to 443 K. They are stirred magnetically (0-1000 rpm). Reaction products are identified by GC or HPLC.
We currently have several Tian-Calvet type heat-flux calorimeters for
studies of adsorption processes on supported metal catalysts. For example, we
have an automated Setaram C-80 calorimeter for determination of heats of
adsorption at temperatures from 300 to 570 K, and we have a Setaram BT-215
low-temperature calorimeter that can be used at temperatures between 77 to 470
We have a Thermo Nicolet 6700 FTIR spectrometer. We
have constructed FTIR cells that allow in-situ studies over a range of
temperatures from 77 to 800 K. We also have an in-situ Attenuated Total
Reflectance (ATR) cell that allows us to study the surface properties of metal
oxides or supported metal catalysts in aqueous environments at temperatures up
to 470 K and pressures up to 600 psig. This cell is connected to an apparatus
similar to our reaction kinetics units, which allows ATR-IR
spectra to be collected with the sample under flowing liquid samples at reaction temperatures and pressures.
A number of electron microscopes are available for this research through the
Material Science Center at the University of Wisconsin, including a Phillips CM
200 high resolution transmission electron microscope (TEM), a HB 501 scanning
transmission electron microscope (STEM) equipped with a X-ray microanalysis,
electron energy loss spectroscopy and micro-diffraction, and a LEO Gemini field
emission scanning electron microscope (SEM) equipped with X-ray microanalysis.
In collaboration with Professor Kuech in the Department of Chemical Engineering,
we have a UHV system fitted with the Omicron Multiprobe S model STM, with liquid
He/N2 cooling and resistive heating over a temperature range of 50-900K. An
Omicron EA 125 HR U5 electronic spectroscopy unit provides XPS and AES
capabilities. The apparatus is equipped with an Inficon Transpector 2 residual
gas analyzer for temperature programmed desorption and reaction measurements. An
attached preparation chamber is outfitted with a SPECS USA Model 11/35 Ar-ion
sputter gun for UHV sample cleaning and an Oxford Applied Research model EGN4
evaporator for sequential deposition of up to four metals, monitored by quartz
crystal deposition controller. Structural characterization of samples can be
accomplished with a Staib Instruments RHEED 15 electron diffraction system. Both
chambers are fitted with Pfeiffer TMU 261 turbopumps, Varian Vaclon Plus ion
pumps, and titanium sublimation pumps, for base pressures below 10-10 torr. We
also have built a sample chamber that allows samples to be pretreated under
controlled conditions (pressures up to 1 atm and temperatures up to 770 K),
followed by transfer to the vacuum chamber for analysis without exposure to air.
We have various gas chromatographs (GC) which have a variety of detectors
including thermal conductivity detectors (TCD), flame ioniziation detectors
(FID) and a mass spectrometry detector (MS). The GCs contain on-line sampling
valves as well as injection ports for off-line analysis.
We currently have four high performance liquid chromatographs (Waters 2695
separations module) with autosamplers, Refractive Index detectors (410
Differential Refractometer), and UV detectors (2998 Photodiode Array).
We have access to a total organic carbon (TOC) analysis instrument (Shimadzu
TOC-6001 with autosampler) in the Water Chemistry Department at the University
of Wisconsin-Madison. This unit allows us to analyze the aqueous phase products
of our reactions for total carbon content.
We have access to eight different NMR spectrometers at the Magnetic Resonance
Facility in the Chemistry Department of the University of Wisconsin-Madison,
allowing us to perform routine and non-routine 1H and 13C experiments for
identification of reaction products.
-Other Catalyst Characterization Equipment-
Most of the techniques typically used in catalyst characterization studies are
available at the UW-Madison. These techniques include chemisorption, X-ray
diffraction, magnetic susceptibility, BET surface area measurement, X-ray
photoelectron spectroscopy, thermo-gravimetric analysis and laser Raman