January 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

During January, our efforts have concentrated upon analyzing Fourier transform profilometry (FTP) data of corrosion pits inside the Oak Ridge Research Reactor (ORRR) pool. The data was acquired by DIAL's submergible FTP probe system during our December 9, 2005 deployment into the ORRR pool. During the week of December 5 - 10, 2005, a team of five DIAL researchers (Ping-Rey Jang, Walter Okhuysen, Arun Kumar, Melissa Mott, and David Monts) traveled to Oak Ridge, completed essential training, and after extensive review of the deployment equipment and plan, obtained permission for deployment into the ORRR pool. Setup of equipment occurred on December 7 and 8 and actual deployment of the submergible FTP system occurred on December 9. A preliminary report of the results has been sent to Oak Ridge; the final report for this initial deployment is nearing completion.

Also during January, the majority of the equipment was retrieved from ORNL; some of the equipment (the submergible box itself and the scraping tool) were retained by ORNL as potentially radiologically contaminated. After the December deployment, the equipment was left at ORNL in order to give ORNL radiation technology personnel sufficient time to radiologically survey the equipment. Planning for the next deployment into the ORRR pool has begun.

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

In January, we finally received the three mercury contaminated soil samples from the Oak Ridge site. In our previous study, we identified some problems of the analytical method developed by Revis, et al., (1989), at Oak Ridge Research Institute when it is applied to a wide range of contaminated soils. We started a detailed method study on improving extraction of mercury sulfide form in soils and sediments.

In February, we will start a series of measurements and experiments to study mercury forms and binding in field contaminated Oak Ridge samples. We will also continue the method study on improving extraction of mercury sulfide form.

Accelerating Phytoremediation by Monitoring Plant Status

During the month of January, we began preparation for a new round of phytoremediation experiments. We planted some vegetation species including Indian mustard and some native Oak Ridge grass species. Pot-study will start once the plants reach three to four weeks old. Meanwhile, we have been analyzing samples and data from previous experiments.

Task 2

Support of Hanford Single Shell Tank Waste Disposition

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

Stereovision. The stereovision effort has been comparing different approaches, such as SAD (sum of absolute differences), SSD (sum of squares of differences), and other matching algorithms, such as NCC (normalized cross correlation coefficient) and global matching.

Computational cost (time) and matching quality are being compared. Both experimental images from our lab and some ground-truth images published by others are being used for these comparisons. These results will allow us to determine the optimum approach for utilization of stereovision in Hanford waste tanks.

Laser-induced fluorescence-spectral imaging. During January, we have experienced problems with operation of our camera system. We are currently diagnosing the problem.

Microwave-induced plasma-cavity ringdown spectroscopy. Efforts this month focused on investigating the feasibility of detecting inductively couple plasma laser-induced fluorescence (ICP-LIF) of uranium using blue diode laser excitation. ICP-LIF has been successfully performed in this laboratory in the past using the frequency doubled output of a dye laser pumped by a Nd:YAG laser. ICP-LIF and ICP-CRDS results were directly compared. In order to perform a similar analysis with ICP-CRDS blue diode laser uranium data, the experimental ICP-CRDS configuration was modified to accommodate this new approach. Multiple experimental parameters, including the plasma height and power as well as the position of the grating, were examined to obtain uranium fluorescence signal. No LIF signal has been observed so far.

Fiber optic sensors. This month, a literature research on scintillating technology for neutron detection has been conducted. Techniques for converting neutron to gamma radiation are presently our concern. It is expected that our scintillating optical fiber will be used to detect the resulting gamma radiation. We are also preparing a new liquid core scintillating optical fiber to test with our newly packed photomultiplier tube (PMT).

Fourier transform profilometry. During January, the FTP group initiated bi-weekly phone calls with our collaborators at Hanford. Hanford has provided us with information essential for planning a side-by-side comparison of Hanford’s existing video referencing technique with FTP; the side-by-side comparison will be performed at DIAL. Hanford is currently checking on the availability of a camera system that can be lent to DIAL for the side-by-side comparison and to enable DIAL to gain hands-on familiarity with a Hanford approved camera system so that we better plan how to modify our FTP system so that it can be deployed utilizing camera systems previously accepted by Hanford.

Process Chemistry and Operations Planning for Hanford Waste Alternatives

A second approach to the development of training sets is being investigated. Previous work in these laboratories involved ESP modeling of salt cake core sample dissolutions conducted at the Hanford site. These data spanned a wide range of salt cake compositions and are expected to provide a framework for the development of a self-consistent neural network model. Additional modeling of the compositions for BY-102 and BY-106 are in progress. Additional waste compositions will be sequentially added to create the training set which will then be tested against compositions from the Best Basis Inventory.

Separation and analysis of the aluminum hydroxide solutions continues. Equilibrium has been established for solutions prepared in 1-m and 3-m caustic. The data will be analyzed within the ESP Bromley framework and then folded in to the DBLSLTDB database.


Task 3

Disposition of Idaho HLW Calcine

Support of CH2M-WG Calcine Disposition Project

The compressive strength results of the most recent 1:.5:.5 formulation tests are given below.

7-Day Compressive Strength

Stirred 10 Minutes
Stirred 30 Minutes
125 psi
144 psi
108 psi
139 psi
131 psi
162 psi

28-Day Compressive Strength

Stirred 10 Minutes
Stirred 30 Minutes
1695 psi
1230 psi
1098 psi
1500 psi
1230 psi
1570 psi

Those tested at 28-days obviously have passed the compressive strength test and are far stronger than the 7-day results. This formulation tested very well early last year, but more recently has not been very strong. We need to figure out just what the difference(s) is(are) among these various samples. We may need to send samples out for phase analysis by x-ray diffraction (XRD).

After some reflection and discussion (and before the results given above were in), we'd decided to make some larger batches of the 1:1:1 formulation. We'll make two batches of six, half of each to be tested at 7-days and half at 28-days. One batch will be made (as usual) with sodium sulfide and the other without. (We still have some concern about the presence of the sulfide, so we'll try this experiment to see if it adds to either the strength or TCLP behavior of the material.) The 1:1:1 formulation has been very watery in consistency which is very desirable from a processing perspective. If we are to consider (as we believe we probably should) waste loadings between this formulation (at about 17%) and the 1:.5:.5 formulation (about 34%), we should try to maintain the watery rheology.

We have begun to craft the test plan and are examining the options for a one-tenth scale pilot facility.


Task 4

Support of SRS Salt Disposition and Other SRS Alternatives

Modeling and Experimental Support for High-level SRS Waste Disposition

Modeling and Experimental Support for High-level SRS Waste Disposition

All potassium nitrate/sodium hydroxide and cesium nitrate/sodium hydroxide systems have been sent for analysis. Analytical results have been received and several samples have been resubmitted. Solids analysis has been completed. KNO3 and CsNO3 crystals found in the caustic concentrations were observed to contain misshaped formations. New solubility experiments for KNO3 and CsNO3 mixtures in 1 and 3-m caustic are currently being examined for the next series of experiments.

The DASR small column experiment using SRS 38H simulant with 3% by weight sludge is complete. The experiment was stopped at approximately 77% dilution by weight and a total of 35 fractions were collected. The remaining heel will be used for another experiment. All fraction samples, including the solids, have been submitted for analysis.

FIU analytical results have been received and modeling of the SRS 41H aged simulant tall column experiment is underway. We are still awaiting the corrected analysis for the carbonate and oxalate concentrations.

Process Improvements for the Defense Waste Processing Facility (DWPF)

Work continued on collecting calibration data for simulated melter feed. The simulated melter feed was prepared in our laboratory by acidifying the sludge batch then adding the proper amount of frit. Initially, we recorded Li calibration with a broadband Echelle spectrometer detection system and found that sample splashing due to laser-induced shock wave is quite serious due to relatively long data acquisition time. To reduce the consumption of the limited slurry resource, we chose a narrow band detection system (20-nm spectral coverage) that can perform much faster data acquisition than with the Echelle detection system. Li calibration data were recorded with this system and compared with the data previously collected with the Echelle system. The Li calibration obtained from this system is linear and has better sensitivity at low Li concentration as compared with the Echelle spectrometer system. To obtain the calibration data for Na, we added various amounts of frit and pure Na2CO3 to the acidified sludge batch. Slurry samples containing Na concentrations from 3 to 9% were prepared. The strong Na D-lines are not suitable for LIBS calibration because of the self-absorption problems at this concentration level. By using a non-resonant Na line, we have obtained a linear calibration curve for Na in slurry.

Glass melting. A series of experiments has been set up to examine the evolution of interactions between frits 200 and 320 and the SRAT Case 7d waste simulant. The experiments have been run over a temperature range of 600°C to 800°C for times of 15, 30 and 60 minutes. Optical microscopy and differential scanning calorimetry (DSC) of the resulting samples will be completed during February.


Task 5

Support of the Fernald Silos Project

Fernald Silos Project - Remediation Process Support

Waste disposition. Activities for disposing of the remaining Fernald K-65 material, the grout samples, the laboratory trash, and the building trash were completed. Nine drums of material were delivered back to the Fernald site for treatment and disposal. Decontamination of the glove boxes was initiated. Dismantlement will commence following the decontamination activities.

The following activities are planned for the upcoming months:

  • Make a site visit in order to discuss the completion of the Fernald waste treatment activities and D&D operations.
  • Package and ship surrogate loop equipment and instrumentation to Fernald.

Task 6

HEPA Filter Performance Assurance

Regenerable HEPA Filter Performance Testing

In January, we received the repaired laser particle counter from Particle Measuring Systems. The instrument was found by us to be fully functional and preparations have been made to resume media velocity testing.


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