Facilities

Our Laboratory

The NRG Lab occupies approximately 1400 sq. ft of research space in rooms D115 and E180 of the Technological Institute at Northwestern University, approximately an additional 1000 sq. ft of shared space with another PI, and approximately 200 sq. ft of the ISEN Laboratory. The laboratories contain extensive benchtop space, nine fume foods, ventilated storage for safe chemical handling, cooling and domestic water, and has an integrated manifold system for distribution of N2, O2, Ar, He, and compressed air. 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, and furnaces for solids treatments and reaction temperature control. Six 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 O2and H2O analyzer.

Laboratory Equipment

• TA Instruments Q500 thermogravimetric analyzer with dual integrated mass flow controllers and evolved gas analysis furnace. The instrument is 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. A third external mass flow controller can be, and has previously been, added to enable more complicated temperature-programmed reaction on small volumes of catalyst. 

• 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. 

• MKS Cirrus 2 process mass spectrometer with integrated NDIR for detection of CO. Allows independent quantification of CO and N2 signals, which otherwise overlap in MS. Normally attached to a standalone flow microreactor. 

• 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. 

• Ambient pressure, quartz U-tube, flow microreactors (2) with up to three mass flow controllers and controlled furnace. Effluent detection currently by process mass spectrometer and/or online GC-FID/TCD. Can also be used as a recirculating reactor, as in prior CO2 photoreduction experiments. 

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

• Medium and high pressure batch reactors. 300 mL stainless Parr autoclave reactor with magnetic stirring (3000 psi), 2 x 50 mL Hastelloy Parr autoclave reactor with overhead stirring (3000 psi, shared equipment), 100 mL Hastelloy autoclave reactor with overhead stirring (3000 psi, shared equipment), 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. 

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

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

Shared Facilities

Northwestern’s world-class user facilities are available for trained users in the group:

• The Integrated Molecular Structure Education and Research Center: FTIR, ICP, 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. 

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

• Staffed and student-run machine 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 a dedicated HPLC/diode-array and a TPR/TPO.