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Subsurface Science & Technology Group

Equipment

Anaerobic ChamberAnaerobic Chamber
(Coy Laboratory Products)
Location: 331 Building, Lab 170
Contact: Wooyong Um (509) 372-6227

The Geosciences group maintains three controlled-atmosphere glove bags. Two of these units can be used to maintain inert atmospheres for experiments involving radioactive materials.

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The three units are routinely used as platforms to perform experiments under tightly controlled redox conditions. These include batch and column flow through experiments under anaerobic conditions, synthesis of reductive materials, as well as experiments studying the biogeochemical impacts of anaerobic microorganisms on contaminant fate and transport.

Carbon AnalyzerCarbon Analyzer
(Shimadzu TOC-Vcsn Total Organic Carbon Analyzer)
Location: 331 Building, Lab 166
Contact: Steven Baum (509) 372-6616

The Shimadzu carbon analyzer can be used to measure total carbon, inorganic carbon, organic carbon, non-purgeable organic carbon, and purgeable organic carbon in solid and solution matrices.

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The carbon in the sample is burned in a combustion tube to form carbon dioxide. A carrier gas is used to sweep the carbon dioxide into a non-dispersive infrared gas analyzer. The instrument can be used to analyze non-rad and radiologically controlled samples.

High Pressure Reactor SystemsHigh Pressure Reactor Systems
Location: 331 Building, Lab 311
Contact: Kirk Cantrell (509) 371-7175

Eight Parr high pressure/pressure vessels, each with its own heater and pressure/temperature controllers. Agilent 8453 diode-array spectrophotometer with a custom-designed high-pressure vessel equipped with integral 1.27-cm-diameter quartz windows on opposite sides to allow the light beam to pass through the vessel.

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The spectrophotometer is controlled by a computer with Agilent ChemStation software. The temperature of the vessel is regulated with a controller (Parr Model 4848) that supplies power to an embedded cartridge heater based on the response of a thermocouple suspended inside the vessel. The vessel was also equipped with a magnetic drive and a stir shaft to allow mixing.

Isco Model 500D syringe pump for transfer of CO2 to the vessels and to pressurize the vessels.

Inductively Coupled-Plasma Mass SpectrometryInductively Coupled-Plasma Mass Spectrometry
(Thermo Scientific X Series 2 ICP-MS)
Location: 331 Building, Lab 113
Contact: Eirik Krogstad (509) 372-4923

These highly sensitive instruments are capable of detecting a range of trace elements and radionuclides at the low to sub parts per trillion (ppt) range in a multitude of matrices.

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The ELAN's Dynamic Reaction Cell™ (DRC) uses chemical resolution and the X-Series uses H2/He collision cell technology to eliminate plasma-based polyatomic species and improve detection limits for difficult elements, such as Fe, Ca, K, Mg, As, Se, Cr, V.

Inductively Coupled Plasma-Optical Emission SpectrometryInductively Coupled Plasma-Optical Emission Spectrometry
(Perkin Elmer Optima 8300 DV ICP-OES)
Location: 331 Building, Lab 113
Contact: Eirik Krogstad (509) 372-4923

The Environmental Sciences Laboratory (ESL) houses a full suite of scientific instrumentation and technologies designed to analyze various types of organic and inorganic samples in liquid and solid forms.

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These analytical instruments provide valuable characterization data that help researchers advance their capability to deliver science and technology solutions. The ESL's two Optima 8300 Dual View inductively coupled plasma optical emission spectrometers are used to analyze a multitude of samples, including waters, biological materials, inorganic materials, and environmental and geological samples. One of the instruments can be used to analyze radiologically controlled samples. Detection capabilities span the periodic table of elements, with detection limits in the low to mid parts per billion (ppb) range.

Ion ChromatographIon Chromatograph
(Dionex DX-600 IC, radiological sample capable)
Location: 331 Building, Lab 164
Contact: Keith Geiszler (509) 372-6402

The instruments can be used to measure anions and cations, carbohydrates, organic acids, amino acids, proteins, peptides, oxyhalides, carboxylates, polyphosphates, fatty acids, metals, and phenols in a variety of matrices.

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The DX-600 instrument can be used to analyze radioactively controlled samples. Typical detection limits span the ppb to ppm range.

Laser Ablation SystemLaser Ablation System
(PERKIN ELMER ELAN DRC II)
Location: 331 Building, Lab 113
Contact: Eirik Krogstad (509) 372-4923

The Applied Spectra J-100 is a tandem laser ablation and laser induced breakdown spectroscopy (LIBS) tool. It uses a Nd:YAG laser quadrupled in frequency at a wavelength of 266nm to ablate material from solids in an ablation cell that is flooded by a He sweep gas.

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The ablation process is used in two ways: (1) the emission of photons from the ca. 100,000°K fireball created by the laser pulse above the surface of a sample material is quantified by a CCD spectrometer, with the intensity of specific lines being proportional to the concentration of elements, and (2) the ablated material is swept into the plasma of the ICP-MS (either quadrupole or HR-ICP-MS) and analyzed for either concentration or isotopic compositions. This combination allows concentrations to be simultaneously determined at the 100 to 0.01% level (LIBS) and 1000 to 0.001 ppm (LA-ICP-MS) from the same site. The LIBS capability allows determination of concentrations of various elements that do not lend themselves to LA-ICP-MS analysis, such as H, F, N, O, etc.

Laser Diffraction SystemLaser Diffraction System
(Horiba Laser Diffraction La950v2)
Location: 331 Building, Lab 170
Contact: Michelle Snyder (509) 372-6388

The Horiba Laser-Scatter particle size analyzer (LA-950V2) measures the angles and intensity of light diffracted off the surface of soil particles to provide a distribution of particle size in sediments <2 mm in size.

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Using <1 gram of sediment and only a fraction of time compared to the traditional method of hydrometer and sieving, the particle size analyzer is a time saving alternative to provide particle size distribution for sediments.

Mass SpectrometryMass Spectrometry
(Dionex ICS 5000 IC with MSQ mass spectrometer)
Location: 331 Building, Lab 164
Contact: Keith Geiszler (509) 372-6402

The instruments can be used to measure anions and cations, carbohydrates, organic acids, amino acids, proteins, peptides, oxyhalides, carboxylates, polyphosphates, fatty acids, metals, and phenols in a variety of matrices.

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The DX-600 instrument can be used to analyze radioactively controlled samples. Typical detection limits span the ppb to ppm range.

Pressurized Unsaturated Flow InstrumentPressurized Unsaturated Flow Instrument
Location: 331 Building, Lab 148
Contact: Ben Williams (509) 372-6397

This instrument has the capability to measure contaminant retardation with flow-through columns operating at unsaturated water conditions. The PUF test is a unique capability at PNNL that allows us to investigate the behavior of wast forms.

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The PNNL patented device is designed to vary the volumetric water content from saturation down to 20% of saturation; minimize the flow rate to increase liquid residence time; and operate at a maximum temperature of 90°C. The instruments have been used to conduct multi-year tests needed to develop corrosion rates of glass materials in support of performance assessment calculations. The units can also be used to evaluate the leaching and migration of contaminants of concern (e.g., Tc, U, I, Cr) in simulated disposal environments.

Sample Preparation EquipmentSample Preparation Equipment
Fluxer Instrument (Claisse Gas M430)
Vibration Grinding Mill and Pellet Press (Herzog Automation Grinding Hsm100h)
Location: 331 Building, Lab 164
Contact: Eirik Krogstad (509) 372-4923

The Claisse fluxer instrument is used to help digest samples of solid material for ICP or XRF analysis. Sample powders are mixed with a flux to lower the melting temp of materials.

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The mixture is then placed in noble metal crucibles (up to three at a time), and automatically heated over a flame until it reaches the temperature of ca. 1100°C. the crucibles are stirred while heating, resulting in a well-mixed, molten sample. This sample is then either poured into (1) forms for cooling into XRF-ready disks or (2) dilute nitric acid for solution-based analysis by ICP. The Herzog grinding mill is used to prepare powder samples for XRF analysis, either as bulk powders or as XRF-ready pressed pellets.

Subsurface Science & Technology