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Facilities

The Water Science and Engineering Laboratory provides facilities for the following user groups:

Facilities in the Water Science & Engineering Laboratory for the Environmental Chemistry and Technology Area

Laboratory and Office Facilities:

The Environmental Chemistry and Technology Area occupies over 10,000 sq ft of office and laboratory space in the Water Science and Engineering Laboratory. Our facilities include faculty, staff and graduate student offices, a 400 sq ft Conference Room, 40-seat Classroom, 300 sq ft Computer/Work Room, and over 8,000 sq ft devoted to research in aquatic chemistry and biogeochemistry. The laboratories are designed for analyses and experiments dealing with metals, major elements, and organic chemicals. Modern shop facilities (electronics/mechanical) located in our building allows fabrication of specialized equipment tailored to the particular field and laboratory research needs.

Facilities for Trace Metal and Biogeochemistry Research:

Our group has excellent facilities and equipment for research on trace metals in natural waters and environmental systems. Facilities include several dedicated clean rooms for trace metal and mercury sample processing and analysis, unique equipment for collecting and processing samples in the field under clean conditions, and highly sensitive instrumentation for trace-level analysis of mercury and other metals. Through recent research, our QA/QC procedures have been reviewed and approved by the EPA. Our research technical support staff have many years of experience in all phases of environmental trace analysis. We also have significant collaborative relationships with researchers from the USGS and other universities.

Mercury Laboratory: The Mercury Laboratory is dedicated to the analysis of low-level Hg in aquatic samples. Incoming air to the room is filtered through an activated carbon filter (to remove organics, CH3Hg, etc.), followed by a large particle filter, a gold-coated cheesecloth (to remove Hg0) and a HEPA filter unit. Additionally, air within the room is filtered through HEPA units on laminar flow hoods and clean benches. The Envirco Model 430 laminar flow hood is used for standard and reagent preparation, assembly and packaging of ultra-clean sampling equipment, drying of miscellaneous clean sampling components and storage of sample bottles immediately before analysis. Sample preparation such as reduction and bubbling is conducted under several large vertical-flow Class-100 clean benches. We have three analytical systems equipped with atomic fluorescence detectors. Two, dedicated to analysis of total Hg, use Brooks Rand Model II detectors; one is equipped with an automated sample injector. A third, dedicated to analysis of methyl mercury, uses a Tekran Model 2500 detector. We employ a small and large volume all-Teflon distillation apparatus for preparation of methyl mercury samples (Horvat, Bloom and Liang, 1993). Two Teflon nitric acid baths (Lufran Inc, Macedonia, OH) are located outside of the mercury room for preparation of Teflon sample bottles for field and laboratory use. Two Teflon stills (Savillex Inc, Minnetonka, MN) are used to purify contaminant-prone reagents such as the BrCl oxidant and HCl sample preservative.

Trace Metal Clean Lab: The Water Chemistry Program maintains a dedicated state-of-the-art trace-metal clean lab in addition to the dedicated Hg clean lab. The 350 sq ft facility was built specifically for trace metal research for non-metallic materials. Particle counts of <10 per cubic foot of air @ 0.3 µm (better than CLASS 10) are maintained with over 160 air exchanges per hour. The lab is equipped with a dedicated high purity water system, two laminar-flow clean benches, and one HEPA filtered, polypropylene, exhausting fume hood.

Inductively Coupled Plasma Mass Spectrometer: Our ICP-MS is located in another HEPA filtered trace metal dedicated clean room at the State Lab of Hygiene. In early 1999 this instrument and analytical support equipment was moved into a new 1000 sq ft facility, designed explicity for environmental trace metal analysis. The ICP-MS is a VG PlasmaQuad II Plus running with Maglev turbo pumps and high performance interface. When operated with pneumatic aspiration, this instrument will give 20 to 30 million counts per ppm of any given isotope. The sensitivity is further increased 5 to 15 fold, depending on the isotope, when interfaced with an ultrasonic nebulizer (CETAC 5100AT). A recently acquired microconcentric nebulizer (CETAC MCN6000) allows us to work with very small samples and serves as an ideal interface for coupled on-line techniques (HPLC-ICP-MS and chelex-ICP-MS). Typically data is acquired in peak jumping mode for maximum sensitivity and precision. Multiple isotopes of each metal are monitored where practical, and particularly with Pb, isotope ratios routinely reported. We have nearly 6 years of experience with the ICP-MS running trace level analyses and in addition to participation in several intercalibration studies, have run extensive comparison studies with established multiple-pipetting z-GFAA methods. Data generated in this study is subject to an extensive QA/QC program.

Major equipment germane to trace metal studies in addition to the Inductively Coupled Plasma Mass Spectrometer (VG PlasmaQuad II+) include an Inductively Coupled Plasma Emission Spectrometer (PE Optima 4300 DV); Voltammetry System (Radiometer Trace Lab 50 /HDME/SMDE/DME and 6mm RDE); High Performance Liquid Chromatography System (Waters 600 with 991 diode array); Fourier Transform Infrared Spectrometer (Nicolet 60SX with 680DSP); Carbon analyzers (Shimadzu TOC-5000 with SSM); Trace Sulfur analyzer (APS instruments); Electrophoresis system (PenKem 3000); Particle counter/sizers (Brinkman time of transition analyzer and Brookhaven BI-2030-AT); Ultracentrifuge (Beckman L8-80M). We also have access to high performance NMR spectrometers, SEMs, TEMs, and STEMs on campus.

Field Study Capabilities: We have demonstrated capability to project both large and small scale trace metal related studies anywhere in the United States. Field-based studies have been conducted in the Florida Everglades, Northern Minnesota, Northeastern Upper Peninsula of Michigan, Lower Michigan, Indiana, and Ohio. Our facility has specialized equipment and highly qualified personnel dedicated to field geochemical studies. The laboratory and department are staffed by chemists, limnologists, and geochemists with decades of experience in designing field-based studies, and interpreting environmental geochemical data.

Facilities for the Environmental Organic Chemistry Research Area:

Facilities for the Environmental Technology Research Area:

The Environmental Technology Program actively studies the synthesis and characterization of novel nanoparticulate oxides (including fundamental colloid chemistry studies of suspensions of these materials) as well as several applications of these materials. These applications include, but are not limited to: thermal catalysis and photocatalysis, separations (both liquid and gas phase separations as well as proton exchange membranes in fuel cells), energy storage devices (as ultracapacitors and thin film batteries), and sensors. Available equipment is often used in several different research areas but will be listed under the area of primary use.

Oxide Synthesis and Characterization: Because this research area provides the core studies that underlie all of our application efforts, this area receives the most support in terms of available equipment. Key instruments used in these studies are a Nicolet Magna 750 FTIR spectrometer with accessories for diffuse reflectance studies of solid-gas interfaces and attenuated total reflectance studies of solid-liquid interfaces, a Brookhaven Instruments B2100 correlator for both dynamic and static light scattering studies associated with particle sizing and stability, a Micromeritics ASAP 2010 micropore analyzer with chemisorption accessory for determining specific surface areas and pore size distributions in microporous solids as well as adsorption densities of selected gases in porous solids, a Netzsch Model STA 409 / 3 / 410 thermogravimetric and differential thermal analysis unit for studying phase changes and weight loss or gain during the sintering process, and a Malvern Zetasizer 3000 for determining particle sizes and mobilities in dilute suspensions. We also utilize rheology instrumentation for measuring sol viscosities, and temperature programmed furnaces for sintering. A glove box is available for synthesizing materials that require water or air sensitive precursors.

Thermal Catalysis and Photocatalysis: We have fabricated a variety of reactors for studying thermal catalytic and photocatalytic processes as well as two reaction manifolds that allow us to control the mixing and flow of gas phase reactants. Identification and quantitation of reactants and products of gas phase reactions are facilitated by using a Hewlett-Packard Model 5890 Series II gas chromatograph equipped with a Porapak R column and flame ionization and thermal conductivity detectors as well as a capillary column Hewlett-Packard GCD gas chromatograph equipped with an electron ionization detector. Both of these GCs include data stations and are interfaced with the reaction manifolds mentioned above. We also utilize a Hewlett-Packard Model 5890A gas chromatograph with a flame ionization detector, a capillary column, and an integrator to analyze directly injected gas samples. An Oriel 1000 Watt light source, optical table, and coupling lenses are available for liquid phase studies. We employ a Shimadzu TOC-5000 total organic carbon analyzer, a Waters ion chromatograph, a Hewlett-Packard Model 8452A UV-Visible spectrometer, and occasionally a capillary column Hewlett-Packard Model 5890A gas chromatograph with an electron capture detector and a data station for sample analysis in liquid phase studies. Several photometers are available for measuring the irradiance of the light sources used in our photocatalysis studies.

Separations: We utilize several dip coating devices to fabricate nanoporous ceramic membranes for use in both liquid and gas phase separations. One dip coater is housed in a laminar flow hood to minimize dust accumulation on the membranes. This laminar flow hood also contains a Headway spin coater as used in the microelectronics industry. A second laminar flow hood is also available for coating. We have a Digital Instruments Nanoscope III atomic force microscope to study surface smoothness and porosities of deposited and fired thin films as well as a Gaertner variable angle ellipsometer to determine porosities and thickness of deposited and fired thin films. However, both of these instruments require flat supports for effective analysis. We have fabricated systems to measure permeabilities through flat and tubular ceramic membranes as a function of applied pressure in order to determine which of these membranes have minimal microscopic defects (cracks and pinholes) and so can be used for further studies. We use an Olympus BX40 reflection microscope to visually characterize membranes of all types. In addition, we have access to XRD, SEM, TEM and XPS equipment in the Materials Science Program to assist in these studies.

Energy Storage Devices: We characterize these thin-film devices using an EG&G Instruments Model 6310 Electrochemical Impedance Analyzer to perform cyclic voltammetry and impedance spectroscopy studies, a Solartron SI 1260 Impedance/Gain-Phase Analyzer and SI 1287 Electrochemical Interface for impedance spectroscopy studies at higher frequencies than the EG&G unit, and an IBM EC/225 voltammetric analyzer for simple voltage and current control. We also have built systems to study discharge from these devices at constant current or constant potential. A Denton Vacuum Desk II sputter coating system is available for depositing metallic coatings on supports and devices when needed.

Proton Exchange Membranes: We are developing a new set of porous oxide electrolyte membranes to be employed in proton exchange membrane fuel cells. These materials require that we characterize the proton conductivity using the Solartron SI 1260 Impedance/Gain-Phase Analyzer in chambers that can maintain fixed temperatures (25-150°C) and humidities (10-100%).

Photoelectrochemical Electrodes: When we coat electrodes with our photocatalytic materials, we need to characterize the fundamental photoelectrochemical properties of the resulting photoelectrodes using several techniques to measure flat-band potentials, overpotentials, etc. To perform these studies, we employ light benches that allow us to control the wavelength of the radiation (e.g., the Oriel light source) at given applied potentials in three electrode photo-electrochemical cells utilizing either the Solartron or the EG&G potentiostat.

Sensors: We conduct research in the area of chemical sensing of gases in conjunction with Professor Craig Grimes at the University of Kentucky. The majority of this work is based on magnetoelastic sensing technology. Experiments are conducted using a magnetoelastic resonance meter fabricated at the University of Kentucky. Specific components of this device include a drive coil, a pick-up coil, a Wavetek 10 MHz DDS function generator (Model 29), a Kepco bipolar operational power supply/amplifier, a Stanford Research Systems SR830 DSP lock-in amplifier, a Mackie M 1400 power amplifier, an Earthworks LAB1 preamp, and a data station. In addition, we have added a gas-tight sensor chamber, a temperature controlled drying chamber, and a dedicated manifold for our specific gas sensing studies.

Facilities for Air Pollution Chemistry Research

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