Users of the Environmental Molecular Sciences Laboratory (EMSL) can apply the versatile and highly sensitive Mössbauer spectrometer and associated capabilities to obtain information about the valence state, coordination number, and crystal field strengths for a wide range of samples, such as iron oxides in soils and sediments, catalysts, and iron-doped glasses.
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.
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 scientific community. Access to EMSL is governed by a proposal process. A summary of EMSL capabilities typically relevant in catalysis is given below.
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
- engine emission test Applied Process Engineering Laboratory (APEL)
- Mobile Process Engineering and Demonstration Unit
- 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 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).
- 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.
- Agilent 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.
- 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.
- Electron Spectrometers enable catalyst surfaces to be probed with a variety of complementary analysis methods including
- Microscopy instruments, including electron microscopes and scanning probe microscopes, are available. These tools are used to image a range of sample types with nanoscale—and even atomic—resolution.
- Spectroscopy equipment, including the FTIR and Mössbauer is available to study solid-, liquid-, and gas-phase sample structure and composition with remarkable resolution.
- NMR Spectrometers, with frequencies up to 900 MHz, can be used to characterize the chemical and structural environment of atoms in the catalysts or in species adsorbed at the catalyst surface.
- Computing capabilities allow 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 and deposition tools can be used to tailor surfaces, atom by atom.