August 2006

Monthly Research Progress


Institute for Clean Energy Technology
(formerly Diagnostic Instrumentation & Analysis Laboratory)
Mississippi State University
Roger King, Interim Director


Prepared for the U.S. Department of Energy
Office of Science and Technology
Cooperative Agreement DE-FC01-06EW07040


Task 1

Support of Oak Ridge Site Closure

Characterization of Corrosion for Closure of Oak Ridge Research Reactor

The new submergible instrument box has been leak tested. The FTP simulated pool target measurements using a 10-gallon aquarium have begun. Because of lack of funds for the rest of the federal fiscal year, our Oak Ridge collaborators are unable to provide the required support to enable deployment into the Oak Ridge Research Reactor (ORRR) pool during September; a revised deployment date is being sought.

Bio-availability and Speciation of Mercury in the Oak Ridge Ecosystem

In August, we finished further characterization (solution phase) of field contaminated Oak Ridge soils. Soil solution pH, soluble Ca, Mg, Fe, Al, K, Na, Cl, NO3, PO4, SO4, dissolved organic carbon have been determined. The solution phase characterization will be used to determine the solution phase mercury speciation in Oak Ridge soils. At this time, a soil freshly contaminated with HgS has been prepared to study bioavailability of HgS under controlled chamber conditions. In September and October, we will begin the chamber study on bioavailability of HgS under the controlled study.

The abstract on "Stability and Bioavailability of Mercury Sulfide in Oak Ridge Soils" has been submitted to the 2007 Waste Management Symposium.

Accelerating Phytoremediation by Monitoring Plant Status

During the month of August, we started a new round of mercury phytoremediation experiments with Indian mustard and Chinese brake fern. Aged soils from previous experiments were re-mixed and re-sampled before use in the current experiment. This experiment will be finished in the following months.

Task 2

Support of Hanford Single Shell Tank Waste Disposition

In-tank/At-tank Characterization for Closure of Hanford Tanks

Stereovision. During the month of August, we performed more experiments with the FTP target board in the classroom. We tried different stereo matching approaches with images acquired at different working distances to get better results. The "grid" projection from the FTP Ronchi filters does help to overcome the textureless problem associated with white board background and targets. With the projected "grid," even the basic sum-of-absolute-differences (SAD) stereo matching algorithm produces better results (i.e., comparable results to much more computationally expensive algorithms). We will continue to search for optimum experimental parameters as well as stereo matching parameters (such as window size, matching range, etc.) for application to Hanford waste tanks.

Laser-induced fluorescence-spectral imaging. We have installed the optics to separate the 266-nm fourth harmonic of the Nd:YAG laser from the Nd:YAG fundamental and other harmonics. The Nd:YAG currently only produces a few millijoules of 266-nm radiation. New flash lamps have been ordered for the Nd:YAG laser; these flash lamps may be able to significantly increase the amount of 266-nm radiation generated. LIF experiments using 266-nm excitation and simple uranium compounds will be performed during September.

Microwave-induced plasma-cavity ringdown spectroscopy. Mercury vapors (Hg) from three types of mercury-spiked aqueous solution and soil have been measured using cavity ringdown spectroscopy. Data processing is being carried out this month.

Fiber optic sensors. During August, we designed a package for an optical fiber-compatible ultraviolet/visible (UV/Vis) spectrometer (model SD2000, Ocean Optics) in order to use the spectrometer to record the scintillating emission spectra from our scintillating optical fibers. This package will shield stray light in the working environment from entering the UV/Vis spectrometer. This shielding is critical for detecting very weak scintillating emission signals from a scintillating optical fiber. Information about the emission spectrum of a scintillating optical fiber is important in deciding what kind of photodetector will be used in designing a scintillating optical fiber system for application at Hanford.

Fourier transform profilometry. In August, we continued our efforts to prepare a report describing the results from the first stage of simulation testing. In order to test the ability of critical FTP optical components (Ronchi filter, diffuser, SONY 78B camera) to withstand gamma radiation, we have initiated radiation testing using MSU's Cs-137 gamma irradiator. The procedure is to record every five minutes an image that includes the Ronchi filter, the diffuser, and a portion of a thin stainless steel plate that simulates the FTP probe wall. We have developed software that automatically analyzes multiple regions-of-interest (ROI) and records the results in a form that can be imported into a spreadsheet for trend analysis. The use of wireless communication to transfer image files from the gamma irradiator room to ICET proved unreliable. A LAN line has been installed in the gamma irradiator room and is now used for transfer of files to ICET. By the end of August, the FTP components have been subjected to a total of ~ 17,000 R with very little noticeable change in the camera performance.

Process Chemistry and Operations Planning for Hanford Waste Alternatives

 Discussions were held with Hanford personnel regarding the ICET work scope for 2006. Additional talks were held with workers at OLI, Inc. regarding the license costs for the ESP and Stream Analyzer software and about the perceived future of their thermodynamic models. As noted previously, ICET has expended tremendous resources in the development of the DBLSLTDB database. The work has included the determination of solubilities in the laboratory followed by fitting the data to the OLI employed Helgeson framework. Seeing as how the compiled database depends on the ESP Public database along with the frequency of software upgrades, it has become necessary to investigate whether the alternate OLI framework, known as the mixed electrolyte model (MSE), will be more robust than the current model. Details of the MSE model were supplied by OLI and the framework is currently being evaluated. The proposed work elements for CY 07 were routed to Hanford for comment.

Task 3

Disposition of Idaho HLW Calcine

Support of CH2M-WG Calcine Disposition Project

The orders were placed in July for the feeding systems and mixer for the pilot scale system. The lead times for both are 10 - 12 weeks. Recent contact with the vendors has the shipping date for the feeders to be September 15. We expect to begin shakedown testing of the mock-up in October/November 2006. Two 55-gallon drums of calcine simulant (non-hazardous) will be shipped from INL in early September. We expect to receive them by the end of September.


Task 4

Support of SRS Salt Disposition and Other SRS Alternatives

Modeling and Experimental Support for High-level SRS Waste Disposition

Two similar sets of solutions containing the system, KNO3-NaNO3-Water at 50°C, have been prepared. One set will be sampled weekly for approach to equilibrium. Once equilibrium is established, the second set will undergo analysis for concentration and solids identification. Additional calculations for these components in caustic and an additional system (CsNO3-NaNO3-Water, caustic) are complete and these solutions will be prepared in September.

Modeling of the 1.5% by weight 8F sludge simulant incorporation for a second DASR experiment containing the 38H salt simulant is nearing completion and will be compared to the two previous DASR experiments employing the same salt simulant. Discussions were held with SRS engineers and the prospective work scope for CY 07 was sent to the site engineers and site DOE personnel. Following the receipt of comments, the work elements will be combined with the budget and collected in the overall ICET DOE HQ proposal.

Process Improvements for the Defense Waste Processing Facility (DWPF)

On-line slurry analysis. The work on evaluating powder samples with LIBS for SRNL's new project has just started. The batch powder sample was prepared by mixing various chemicals provided by SRNL. Various amounts of binder were added to the batch powder sample and pressed into pellets. The effects of the amount of binder on the pellet were studied. The effects of laser energy, detection windows, and lens-to-sample distance on the LIBS signal of these pellets were also investigated. The calibration data were then recorded by using the pellets made with optimum binder concentration and under the optimum experimental parameters. Five power samples of different compositions were made for the LIBS calibration. These data are being analyzed.

Improvement of waste throughput. Experiments run so far to examine the relative reaction rates of the two frits have not provided the information expected. These tests have been done both with a dried version of the Case 7d SRAT as well as with the slurry. It appears that in both sets of experiments, Frit 200 reacts more rapidly (at lower temperatures) than Frit 320, and that's not what has been observed in practice. The products of these experiments are now being evaluated by differential scanning calorimetry and optical microscopy.

More experiments have been run this month to establish a reason for the above discrepancy. A paper is being prepared for the October meeting of the American Ceramic Society. A shipment of SB4 simulant Frit 503 and Frit 418 was received this month. We have begun chemical and thermal characterization of these materials. The budget and statement of work for CY 07 have been drafted and are in negotiation.

Task 5

Support of the Fernald Silos Project

Fernald Silos Project - Remediation Process Support

Final decontamination and disposition of the Fernald building and the associated systems is ongoing. Communication with the Fernald Management Team will continue through project completion.

Task 6

HEPA Filter Performance Assurance

Media velocity testing of Camfil Farr AG-1 nuclear grade HEPA filters was initiated. The filters were first characterized over the flow rate range of 175-435 SCFM with regard to initial differential pressure, downstream particle counts due to blow off from the filter media, and test stand static pressure. Test were conducted loading with 30% KCl at media velocities ranging from 3 - 7.5 ft/min. Tests were conducted with the cyclone in place and with no cyclone to compare filter performance during loading with differing particle sizes and mass loading rates. Of particular interest is the effect filtration media velocity on the filter MPPS (measured downstream with the PMS LPC), filtration efficiency, and mass loading rate vs. differential pressure. Media velocity testing will continue into September.


Inquiries may be addressed to:

Dr. Roger King, Interim Director
205 Research Blvd.
Starkville, MS 39762-5932


Phone: 662-325-2105
FAX: 662-325-8465