Facilities

Our Laboratory

The NRG Lab occupies approximately 2000 sq. ft of research space in Catalysis and the Technological Institute buildings at Northwestern University. The laboratories contain extensive benchtop space, eight fume foods, ventilated storage for safe chemical handling, cooling and domestic water, and has an integrated manifold system for gas distribution. 18 MΩ water is available from a Barnstead Nanopure system. 

The laboratory is well-equipped for precision molecular, inorganic complex, and materials synthesis, and for characterization of catalyst structure and function. Synthesis facilities include standard microbalances, heaters, chillers, centrifuges, and furnaces for solids treatments and reaction temperature control. A rotary evaporator and four vacuum / inert atmosphere Schlenk lines are available for precursor and catalytic materials synthesis and the pre-treatment of solids, as is an Ar-filled LC Technologies inert atmosphere glovebox with O2 and H2O analyzer.


Laboratory Equipment

Instruments:

 TA Instruments Q500 thermogravimetric analyzer: A TGA with dual integrated mass flow controllers and evolved gas analysis furnace, its used for mass analysis and temperature programmed desorption / oxidation / reduction. Attachment of process mass spectrometer gives quantitative analysis of, for example, the evolution of H2O during reduction of oxides, giving insight into possible structures of surface oxides. 

Micromeritics ASAP 2010 surface area and porosity analyzer: This machine is currently plumbed with N2, CO2, and He and has micropore capability for comprehensive analysis. 

Shimadzu 3600 UV-visible-NIR spectrophotometer: Very low stray light is optimized for solids analysis. Also has a constant-temperature stirrer liquid cell for suspended catalysts. 

Harrick Praying Mantis diffuse reflection holder and custom reaction cell with temperature control to 400°C and gas distribution manifold. Currently plumbed with He, H2/inert, O2, CO2, and a bubbler for vapor introduction. Capable of full in situ UV-visible-NIR analysis. 

Pfeiffer Thermostar process mass spectrometer for rapid identification of desorbed species during temperature-programmed reaction (oxidation, reduction, desorption) in TGA, UV-visible-NIR spectroscopy, or standalone microreactors. 

ATAGO RX-007 Alpha Benchtop Refractometer for ultra-high precision quantification of aqueous solution concentrations. 

Malvern Instruments Nano ZS Zetasizer 

HP 6890 GC/FID, Shimadzu 2010 GC/MS, and Shimadzu 2010 GC/FID, all with automated liquid sampling.  

Reactors:

Ambient pressure, quartz U-tube, flow microreactors (4) with up to three mass flow controllers, bubblers, and controlled furnace. Fully automated flow and temperature control. Effluent detection by process mass spectrometer and/or online GC-FID/TCD.

High pressure (600 psi), Hastelloy, flow microreactors (2) each with five mass flow controllers and two liquid flow controllers, three shared pressurized liquid reservoirs and controlled furnaces. Fully automated flow and temperature control. Effluent detection by online GC-FID/TCD.

Low pressure parallel batch reactors, commercial and home-built, with temperature control and stirring or shaking. 

Medium and high pressure batch reactors. Several 100-300 mL stainless Parr autoclave reactors with magnetic stirring (3000 psi), 50 mL Hastelloy Parr autoclave reactor with overhead stirring (3000 psi, shared equipment), 100 mL Hastelloy Parr autoclave reactor with overhead stirring (3000 psi), 100 mL stainless HEL autoclave reactor (3000 psi), 4 x 190 mL Andrews glass reactors (225 psi) for batch solid/liquid reactions. Several of the reactors are specially modified to allow continuous sampling of the liquid and gas phases. 

UV sources, quartz vessels, and machined reaction blocks for photochemistry. 


Shared Facilities

Northwestern’s world-class user facilities are available for trained users in the group. Some of the more commonly-used facilities are:

• The Integrated Molecular Structure Education and Research Center: FTIR, LC-MS and standalone mass spectrometry for small molecule and materials characterization; 400 MHz and 500 MHz NMR for solutions; 300 MHz NMR for solids. 

• Quantitative Bio-element Imaging Center: ICP and microwave digesters for elemental analysis.

• Northwestern University Atomic- and Nanoscale Characterization Experimental Center: SEM, TEM, XPS, SIMS, and ESCA for visualization, elemental mapping and oxidation state analysis. 

• Keck Biophysics Facility: photoluminescence spectroscopy, circular dichroism spectrophotometry, isothermal titration calorimetry

Staffed and student-run machine and electrical shops. 

DuPont-Northwestern-Dow Collaborative Access Team at the Advanced Photon Source at Argonne National Laboratory (Station 5-BM). In addition to the station, associations with the Center for Catalysis and Surface Science make available several in situ reactors for X-ray absorption spectroscopy techniques (EXAFS, XANES). 

CleanCat user facility: New in 2010, the facility includes 4 automated Altamira BenchCAT 4000 plug flow reactor systems. All have liquid feed vaporizers and liquid traps for sampling. All reactors are routed to a bank of GC-FID/MS/TCD/NPD systems. Facility also includes two 4590 overhead stirred Parr reactors, two machines for in situ DRIFTS, N2 physisorption, a dedicated HPLC/diode-array and the AMI 200 for pulse chemisorption and TPR/TPO. An Arradiance GEMSTAR-8 is available for routine atomic layer deposition on powders.