Equipment & Facilities
The IIC is a virtual organization that facilitates collaborative synergistic research among scientists and engineers across the Pacific Northwest National Laboratory campus and around the globe. In that context, IIC facilitates the deployment of a range of facilities controlled, managed and supported by other organizations (see our flier Experimental and Computational Capabilities for 21st Century Catalysis Research [pdf, 364kb]). Among these is a powerful and extensive portfolio of leading-edge experimental and computational resources for catalysis research located in the Environmental Molecular Sciences Laboratory (EMSL), a DOE BER-supported national scientific user facility on the PNNL campus. These resources are available for collaborative, independent, and proprietary research by the external scientific community of universities, other federal laboratories, and industry, as well as the internal PNNL staff. Access to these facilities is governed by a proposal process administered by EMSL. For more information, potential users should access the EMSL website. A summary of EMSL capabilities typically relevant in catalysis is given below. More detailed listing can be found on the EMSL website.
In numerous other locations across the PNNL campus, the catalysis science and engineering facilities include a range of reactor systems for scale-up (bench-to-pilot scale):
- Chemical Engineering Laboratory
- Chemical Process Development Laboratory
- Process Development Laboratory-East
Additional applied catalysis research work, including catalyst synthesis, bench-scale testing, and catalytic process development, is conducted throughout the Laboratory:
- Chemical and Biological Process Development
- Advanced Processing and Applications
- engine emission test Applied Process Engineering Laboratory (APEL)
- Mobile Process Engineering and Demonstration Unit
- Physical Sciences Laboratory
- Combinatorial Catalyst Lab at PSL
- Advanced Photon Source. PNNL is a member of the Advanced Photon Source PNC-CAT beamline (Sector 20) at the Argonne National Laboratory. The experimental capabilities of the beamline include in-situ X-ray absorption fine structure (XAFS), X-ray scattering, reflectivity, and imaging. The X-ray scattering will include application of the diffraction anomalous fine structure (DAFS) and X-ray resonant inelastic scattering (XRIS) techniques.
Summary of capabilities in EMSL, a DOE national scientific user facility:
- ASDI RXM-100 Catalyst Testing and Characterization Standard is a multifunctional instrument used for performing chemisorption, physisorption, temperature programmed characterization (TPR, TPO, and TPD), kinetics and reaction mechanisms, isotopic tracer and transient studies on practical and high surface area catalysts.
- UHV Surface Science/High Pressure Catalysis System is capable of studying catalytic reactions over model, often single-crystal, catalyst materials at elevated temperatures to gas mixtures of one atmosphere or below in a reactor situated just below an ultrahigh vacuum (UHV) chamber. Pre- and post-high pressure reaction surface analysis with LEED, AES, TPD, and XPS and ion scattering (ISS) spectroscopies can be performed.
- Molecular Beam-Surface Scattering and Kinetics Instrumentation is a powerful experimental tool for studying the dynamics and kinetics of the interaction of molecules with model catalyst surfaces.
- Zeton Altamira Reactor Test Stand comprises three types of reactors generally utilized in bench-scale testing of catalysts—a fixed bed reactor, Rotoberty reactor, and continuous stirred tank reactor (CSTR).
- Photochemical Reactor allows photochemical studies such as water splitting.
- Gas Chromatography-Mass Spectrometer-Infra Red Spectrometer (GC-MS-IR) consists of an HP 5890 gas chromatograph hyphenated with an HP 5972 mass spectrometer, and a Bio-Rad infrared detector. The system is an excellent qualitative analysis tool and can be used for quantitative analysis of complex organic gas and liquid samples.
- High Performance Liquid Chromatography (HPLC) equipped with a Waters 2690 separations module, a 996 Photodiode Array detector (PDA), and Millennium32 chromatography software, and can be used for quantitative analysis of UV absorbing organic compounds.
- Agilent 6890N Gas Chromatograph with an O.I. Analytical 5380 Pulsed Flame Photometric Detector (PFPD) can handle both gas phase and liquid phase samples with detectivity for sulfur <1 pgS/sec.
- Hewlett-Packard (HP) 4500 Series Inductively Coupled Plasma Mass Spectrometer (ICP-MS) is available for analyzing trace metals in catalyst samples
- Total Organic Carbon Analyzer is available for analyzing total carbon (TC), inorganic carbon (IC), total organic carbon (TOC), purgeable organic carbon (POC), and non-purgeable organic carbon (NPOC) on catalyst samples.
- Micromeritics TriStar 3000 uses gas sorption techniques to generate high-speed surface area and pore size data.
- Micromeritics AutoPore Mercury Porosimeters uses mercury intrusion to determine total pore volume, pore size distribution, percent porosity, density, and transport properties.
- Particle Sizing System AccuSizer C770 measures the size distribution of particles based on the principle of light extinction.
- Netzsch STA409 simultaneous TGA-DTA/DSC with a Bruker Vector 22 infrared detector and a Balzers mass spectrometer
- Isothermal titration calorimeter and potentiometric titrator – can be used to precisely measure the thermal or surface charge change due to the binding between probe molecules and catalyst surface.
- Nikon TE-300 Inverted Optical Microscope is available for general optical microscopic imaging as well as confocal optical microscopic imaging of samples with resolution down to 0.3 μm.
- Electron Microscopes allow visual observations of catalyst particles as small as single atom and can perform elementary analysis of small spots on the surface of catalysts
- Philips X-Ray Diffraction Systems can perform analysis of crystalline catalyst samples from -193 to 1000°C
- Electron Spectrometers enable catalyst surfaces to be probed with a variety of complementary analysis methods including
- Scanning Probe System is capable of imaging catalyst surface in gas or liquid environments
- Variable Temperature Scanning Probe Microscope – state-of-the art surface science tool comprising multiple complementary probes of surface phenomena.
- Topometrix Scanning Probe Microscope (SPM) involving atomic force microscopy (AFM) and scanning tunneling microscopy (STM) – can provide atomic resolution images of catalyst surface.
- DI Nanoscope IIIa Atomic Force Microscope (AFM) – can be used to probe catalyst surface morphology; defects; and electrostatic, magnetic, and mechanical properties of conducting and non-conducting catalytic materials.
- Spectrometers, including vibrational spectroscopies, can be used to provide detailed structural information on high surface area porous catalysts.
- NMR Spectrometers, including high-field NMRs, can be used to characterize the chemical and structural environment of atoms in the catalysts or in species adsorbed at the catalyst surface.
- NMR Spectrometer, Bruker Avance 500 MHz WB (Imaging)
- NMR Spectrometer, CMX 300 MHz WB for Solids (and Liquids)
- NMR Spectrometer, CMX 500 MHz NB for Liquids (and Solids)
- NMR Spectrometer, Varian Infinity Plus 400 MHz WB
- NMR Spectrometer, VarianInova 600 MHz NB
- NMR Spectrometer, VarianInova 750 MHz NB
- NMR Spectrometer, VarianInova 800 MHz (18.8 Tesla)
- NMR Spectrometer, Varian Unity 600 MHz NB
- NMR Spectrometer, Varian Unity Plus 300 MHz WB
- NMR Spectrometer, Varian Unity Plus 500 MHz NB
- NMR Spectrometer, Varian Unity Plus 500 MHz WB
- Non-Thermal Interfacial Reactions Instrumentation
- Molecular Science Computing Facility allows remote and onsite access to the high-performance supercomputer and associated integrated software for a variety of applications such as modeling of chemistry on porous sites, molecular thermodynamics, kinetics, and prediction of excited states.
- Microfabrication Equipment supports a variety of microprocessing activities that include thin film deposition, thermal treatments, microphotolithography, chemical etching, inspection and characterization, bonding and packaging, and test and measurement.
