April 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

Construction of a new submergible box has begun. It is necessary because during our initial deployment of the submergible Fourier transform profilometry (FTP) system into the Oak Ridge Research Reactor (ORRR) pool in December, a detectable amount of radioactive materials were deposited onto the metal box containing our instrumentation; consequently, ORNL has retained the original metal box. Efforts have begun to improve FTP spatial resolution by using higher resolution cameras. An engineer with experience in uncertainty analysis has joined this effort in order to provide us with a more rigorous and detailed analysis of the measurement uncertainties. Planning for the next deployment into the ORRR pool continues.

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

In April, we finished characterization of mercury-contaminated field soils from the Oak Ridge site. We have processed the data from the study on extraction of mercury sulfide from soils and sediments. We are in the process of summarizing the data from experiments on dynamics and kinetics of mercury speciation and transformation in Oak Ridge soils at three redox conditions. We began writing a couple of journal manuscripts from these studies. In May, we expect to have the first drafts of these manuscripts.

Accelerating Phytoremediation by Monitoring Plant Status

During the month of April, we harvested 70 pots of Indian mustard. The objective of this experiment is to compare uptake and phytoremediation efficiency of mercury from mercury-contaminated Oak Ridge soils by two varieties of Indian mustard (Giant and Broadleaf). We monitored plants by both plant physiological enzyme activities and spectral reflectance. In May, we will continue all soil and plant tissue analyses.

Task 2

Support of Hanford Single Shell Tank Waste Disposition

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

Stereovision. During April, we submitted one conference paper and one scientific journal paper. A series of experiments have begun to characterize the stereovision performance of the new cameras (SONY FCB-EX78B) which have greater zoom capability; different zooms and different objects are being used. Some difficulty was experienced with one of the new cameras; efforts are ongoing to solve the identified problems.

Laser-induced fluorescence-spectral imaging. During April, our survey of currently available camera systems continued in preparation for purchase of a new camera system. Our efforts to utilize a currently available camera system in the interim continue.

Microwave-induced plasma-cavity ringdown spectroscopy. A prototype instrument case that houses the optical components has been developed and the system is being tested for pressure control and optical alignment. The purpose of the development of this instrument system is to transform lab-level technology into a site-deployable system. Without a wide tunable light source, the system will be initially tested with a single diode laser for a few chemical compounds that have spectral absorption in the near infrared; these chemical compounds are of interest because they occur among the gases found in the Hanford waste tanks.

Fiber optic sensors. During this month, we tested our liquid core waveguide (LCW) scintillating optical fiber for detection of gamma radiation by using MSU's 137Cs gamma source. The preliminary results indicate that one of our ZnS/CdSe quantum dot solution-filled LCW scintillating optical fibers can be used to detect gamma radiation.

Fourier transform profilometry. A multi-stage side-by-side comparison of our Fourier transform profilometry (FTP) system and the imaging method currently used by Hanford, video camera/CAD modeling system (CCMS) has begun. The side-by-side comparison is being performed at ICET, using an available classroom. One of the walls of the classroom is being utilized to simulate the bottom of a C-200 series Hanford waste tank. The test involves determinations of the volumes of both objects with (at least some) known dimensions and of nondescript objects (with unknown dimensions). These are viewed by the cameras from nine different combinations of distance and angle. The volumes (and associated uncertainties) of the nondescript objects have been determined using traditional volume determination methods. An engineer with expertise in uncertainty analysis has joined our team in order to better characterize the uncertainties associated with the FTP technique and to use the insights of uncertainty analysis in developing the optimum deployment system for Hanford waste tanks. A video of the test objects was recorded for use by CCMS under direction of Hanford personnel via a Webcast. FTP measurements have begun. During this first stage of testing, the test objects are located on a flat surface and determinations are made using single images; future testing will involve stitching together results from different images and the use of a "bowl-like tank floor."

Process Chemistry and Operations Planning for Hanford Waste Alternatives

Porting of the DBLSLTDB database to ESP version 7.0 is nearing completion. Additional simulations in support of the neural network development effort were run on eight candidate salt cake compositions. These are the same wastes that were initially modeled using ESP and subsequently compared to experimental results obtained in the 222-S laboratories at Hanford during the 1998 - 2003 time frame. Results for all of the waste compositions look reasonable and follow the typical dissolution/dilution curves except for the composition from the TX-113 core sample. The normal behavior of increasing concentration followed by an exponential decay was not approached for TX-113 and efforts are currently in progress to identify why the normal behavior was not observed.

The aluminum solubility experiments have been completed and data is being worked up. The initial goal is to fit the data according to the ESP framework and then include the results in a later version of the DBLSLTDB database.


Task 3

Disposition of Idaho HLW Calcine

Support of CH2M-WG Calcine Disposition Project

The Final Stabilizer Development Report has been issued.

We have begun obtaining estimates for equipment for the mock-up and have started discussing among ourselves just what the equipment ought to do and how it all fits into a test plan. We should be on time to meet the various schedule milestones. Informal estimates for the feeding equipment for the mock-up seem high, so we will be adjusting our specifications for the official request for bid to see about obtaining a lower price. A request for bids on the feeder equipment for the pilot scale test has been issued.

Compressive testing of 28-day samples was done. These are from the large-sized batch of materials made in March:

17A: 1237 psi. 17B: 1370 psi. 17C: 1340 psi.
17D: 1545 psi. 17E: 1315 psi. 17F: 1295 psi.

*All 17% WL were still green-tinged on sides and bottom.

34A: 2817 psi. 34B: 2827 psi. 34C: 2625 psi.
34D: 2465 psi. 34E: 2950 psi.

On the large samples we made last month, there are areas of different colors. It is thought that this is simply the result of a degree of curing and moisture content, but to be sure we have done a chemical analysis of the various areas. These analyses showed that there were no significant differences in composition.


Task 4

Support of SRS Salt Disposition and Other SRS Alternatives

Modeling and Experimental Support for High-level SRS Waste Disposition

Modeling of the 38H simulant containing three percent sludge by weight was first attempted using ESP version 6.5 in order to include the redox for the 8F sludge simulant preparation. Due to problems associated with these redox equations within 6.5, the modeling has been switched to version 7.0 using the ICET/double salt, Zeolite, and public databases. Results of these simulations and comparisons to the experiment will be presented at the Hanford Technology Exchange in May.

Results from the 50°C CsNO3 and KNO3 in caustic were delayed due to instrument problems. Results of the 25°C experiments for these systems have been determined and both should be ready to present next month. New simulations for CsNO3 - KNO3 - (0, 1 and 3 m) NaOH are currently underway.

Process Improvements for the Defense Waste Processing Facility (DWPF)

On-line slurry analysis. Work continued on conducting slurry measurements with the narrow band spectrometer for Na and Mg calibration. Previous studies have shown that by reducing the laser frequency from 10 Hz to 5 Hz, the relative standard deviation of slurry measurements reduced almost four times. This is because the slurry surfaces are less frequently disturbed by laser-induced shock waves. We conducted the slurry measurements by putting the sample on a rotating stage, and we found no significant difference in the signal intensity and measurement standard deviation from the data recorded with and without rotation during data acquisition. The recorded slurry spectra were analyzed by using peak height, full peak area and half peak area. We found, when using the resonant Mg and Na lines, the peak height seems to give better accuracy than with the other two methods. We will test these methods for some non-resonant analyte lines. Testing of the Echelle spectrometer with the new software was completed. The new program allows us to effectively control laser firing and only record the defined region of interest during the data acquisition. We will set up the Echelle spectrometer for slurry measurements again.

Improvement of waste throughput. A series of experiments has been run to examine the evolution of interactions between frits 200 and 320 and the SRAT Case 7d waste simulant. The experiments encompassed a temperature range of 600 to 800°C and times of 15, 30 and 60 minutes. Differential scanning calorimetry (DSC) of the resulting samples has been completed. These data have now been reviewed in preparation for a site visit during the month of May 2006. Further analyses of these experiments and plans for future work will be discussed at that time.

Task 5

Support of the Fernald Silos Project

Fernald Silos Project - Remediation Process Support

Waste disposition. The interior of the gloveboxes was decontaminated to the extent possible in preparation for dismantlement. Dismantlement and disposition are planned for the month of May. Bionomics will provide the disposal containers and ICET personnel will perform the disposition activities. The following activities are planned for the upcoming months:

  • package and ship surrogate loop equipment and instrumentation to Fernald;
  • dismantle and dispose of the gloveboxes.

Task 6

HEPA Filter Performance Assurance

Two manuscripts, "Lifetime Testing of Sintered Metal and Ceramic Membrane Regenerable Filter Media" and "Evaluation of Glass Fiber HEPA Filters as a Function of Media Velocity," were finalized and accepted for publication in the proceedings of the International Conference on Incineration and Thermal Treatment Technologies, to be held in May 2006. The oral presentations associated with the papers were assembled.

An abstract was submitted for presentation at the Nuclear Air Cleaning Conference to be held in Cincinnati, OH, July 17 - 19. The scope of this presentation will also concern the function of HEPA filters at elevated media velocities, but will additionally compare ACFM vs. the standard SCFM derived media velocities.


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
Email: icet@icet.msstate.edu