April 2004

DIAL's Research Highlights

Diagnostic Instrumentation & Analysis Laboratory
Mississippi State University
John Plodinec, Principal Investigator

Prepared for the U.S. Department of Energy
Office of Science and Technology
Cooperative Agreement DE-FC01-04EW54600

Task 1

Support of Closure Sites

Fernald Silos Project Monitoring and Control Integration

Instrumentation recommendations. In April, the Fernald Closure Project (FCP) invited DIAL to participate in a workshop held at the Fernald site. The intent of the workshop was to identify possible processing risks associated with the Silos Advanced Waste Retrieval (AWR) Project. DIAL was specifically asked to identify all monitoring requirements and instrumentation necessary to identify when pockets of Silos material with higher than expected radiological activities are encountered during full-scale retrieval operations. The deliverable identified by the FCP was a white paper on instrumentation and monitoring needs for the AWR Project.

A draft white paper was completed by R. Arunkumar, Brian Kauffman, and Dr. O. Perry Norton and submitted to the Fernald Silos Project Management Team. The draft white paper identified all instrumentation that was evaluated for use in the AWR process facility.

Waste stabilization formulation development. DIAL completed fabrication of the glove box component. The facility to be used for performance of the K-65 testing was prepared for the work to be initiated. Radiological monitoring instruments were placed in the facility and background radiological measurements were initiated. The ventilation system was connected to the glove boxes, the system was then sealed and tested to ensure that an adequate amount of dilution air was drawn into the boxes. The DIAL industrial health and safety officer and the Mississippi State University radiological officer performed smoke tests for verification that the glove boxes contained no leaks. Modifications were made as necessary.

The following activities are planned for the upcoming month:

• Finalize instrumentation white paper.
• Attend a follow-up workshop.
• Begin formulation testing with K-65.
• Begin the Wastewater Equilibration Study.
• Participate in the full-scale surrogate testing of the Silos Waste Retrieval System (SWRS).
• Perform real time data analysis for the full-scale surrogate testing of the SWRS.

Accelerating Phytoremediation by Monitoring Plant Status

We have been analyzing samples and data from previous experiments. We also prepared soils for the next mercury phytoremediation experiment which we expect to start in May with the arrival of ordered plants. Meanwhile, we will continue to analyze 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. This month the stereovision effort performed some experiments using camera-to-target distances comparable to Hanford tank parameters. In order to find the best resolution, we have tried different distances between the two cameras, and also different window sizes (for computing the disparity map). Testing will continue in May.

Microwave-induced plasma-cavity ringdown spectroscopy. Our major effort this month focused on improving the detection sensitivity for mercury at 254 nm using low-power microwave-induced plasma source cavity ringdown spectroscopy under atmospheric conditions. An additional effort focused on testing the temperature effect on a newly purchased compact external cavity diode laser; this laser will be used for uranium isotopic measurements at 409 nm.

Fiber optic sensors. Work this month focused on developing a LabView program to count optical emission pulses from a photodetector, such as a photomultiplier tube (PMT). In addition, we received the Hamamatsu PMT and started to connect this PMT to a computer.

Fourier transform profilometry. The blueprints provided us by Hanford have been used to generate an ACAD file of a Hanford waste tank. The design for a 4-in. riser mock-up has been completed and fabrication is underway. The riser mock-up will be utilized for FTP-probe fitting tests as well as the development of a supporting tower. For the mock-up of critical tank area near the bottom "corner" (with rounded curvature), the needed information has been extracted for a 10-ft width from the ACAD file. Fabrication of this "bottom corner" mock-up will follow completion of the FTP arm bench top optical layout and will be used to make the simulated measurements of this area. For the insertion probes engineering design work, a short three-section telescoping probe will be fabricated to work out the details; completion of required additional drawings for pulleys and bearings are underway. For the detachable elbow section of the insertion probe, work continued with component fabrication of the probe's utility light and fringe projector. Improvement of camera control and image acquisition software for the various camera models has been completed, while work for multiple camera synchronization continues.

Our efforts also included initial development of methods to correct for target distortions introduced by non-perpendicular FTP; this is necessary due to the large size of the tanks and the fact that traditional FTP assumes that the FTP system is perpendicular to the (reference) target surface. We identified that there are distortions along all three dimensions: X, Y, and Z. Initial algorithm and codes for corrections have been completed. Initial experimental results with a simulated target demonstrated that the proposed correction approach works well, with correct heights and shapes restored. Further development to improve the restoration, which shows some missing data ("black holes") with the current approach, will continue.

Information sifting. Currently the information sifting effort is working on and has almost completed a view feature in the tool. Using this feature, a user will be able to view a graphical representation of any spectrum in the library. A feature has also been added that will let users contact the administrator of the website.

Process Chemistry and Operations Planning for Hanford Waste Alternatives

Work continued on measuring solubilities and developing and distributing data bases and on the application of ESP to Hanford waste operations.

A series of experiments were begun to examine the solubility of aluminum in the presence of different anions such as nitrate, phosphate, and carbonate. Initial measurements for the pure component aluminum system resulted in considerably larger aqueous phase concentrations than those predicted by ESP using either the Weslow database or the Public database alone. Consequently, a series of studies were developed to follow the equilibration as a function of time. These efforts involved the initial preparations of about 100 g of solution at a given starting sodium aluminate concentration, followed by immediately splitting the solution into a control and into a fraction that would be sampled regularly. After six weeks the aqueous phase aluminum concentrations are continuing to decrease indicating that equilibrium has not been attained. Extrapolation of the available data indicates that equilibration times of between four and five months will be required.

ESP calculations have been started for the dissolution and retrieval of the waste in Hanford tank 241-S-102. Data from the best basis inventory has been downloaded and is being examined with respect to spatial variations within the core samples. Once the compositions of the waste in the tank is set the dissolution simulations will proceed followed by evaluations of the resulting streams at the operating conditions of the 242-A evaporator.

ESP simulations have also begun in an attempt to analyze the pilot-scale salt cake dissolution experiments conducted at FIU in fiscal year 2003. Current efforts are aimed at matching the chemical compositions within the column following simulant preparation, column loading, and interstitial draining.

Flexible Scintillating Optical Fiber Sensor for Determination of Liquid Level

The photomultiplier tube assembly to serve as the detection system for the scintillating fiber optic sensor was received during this reporting period. Upon receipt of the Hamamatsu HC135-11, the entire detection system including the power supply, computer, and photomultiplier tube/micro controller were wired together. In addition, the photomultiplier tube assembly was temporarily mounted in a black box for the initial testing period. This configuration will permit the control code to be written with only minimum exposure of the photocathode to light. This is critical as the detection mechanism of the photomultiplier tube can be permanently damaged if exposed to room light for even short periods of time. Programming of the photomultiplier tube will be conducted during the next reporting period.

Tank Leak Detection and Monitoring System

The major effort this month was focused on the elimination of the optical feedback effect of the system. Due to the unavailability of the wedged ringdown mirrors, one of the non-wedged ringdown mirrors aligned in the gas cell was pulled out and installed on a separate mirror mount. In this way, the flexible free space of the mirror mount allows us to achieve a particular alignment of the laser beam to reduce the feedback effect. A much improved ringdown signal was obtained. This testing indicates that the optical feedback can be overcome by utilizing a pair of wedged ringdown mirrors in the final version of the system. Since all electronics and optical parts were loaded in a single rubber cart, the system mobility was also tested. With this initial integrated system (in the rubber cart), the atmospheric concentrations of moisture can be determined at any point where the system is located. The future developments include the vibration testing, temperature effects, and procurement of a pair of wedged ringdown mirrors.

Task 3

Disposition of Idaho HLW Calcine

Support of INEEL Calcine Disposition Project

The ICP-SP3 (new name of INEEL) has down-selected three stabilizers: Fe-P ceramic, hydroceramic cement, and grout cement.

DIAL/MSU prepared a first draft of the test plan. The draft will undergo further review. Drs. Tom Thomas and Walt Tisdale will visit DIAL May 18 - 20 to complete the test plan review.

Task 4

Support of SRS Salt Disposition and Other SRS Alternatives

Support for SRS Salt Disposition Alternatives

Work on the evaluation of the dissolution behavior of SRS salt cake simulant from tank 38H was begun. A formula for the simulant was developed, prepared, aged, and DASR experiments were performed. Analyses of the chemical composition of the fractions resulting from the experiments were then compared to ESP simulations. An unusual trend was noted for the phosphate, aluminum and nitrite concentrations. At the weight percent dissolution of 16 through 27 an increase in concentration was discovered and samples were resubmitted for analysis to determine the validity of the numbers obtained. The samples were almost identical in number. Results were compiled and presented at an SRS POW meeting. A second experiment was started and samples are under analysis. A new batch of the 38H stimulant was prepared and flow through experiments will be conducted for porosity and permeability determinations.

Efforts for development of the NAS database were begun by collecting the relevant data for the aluminum and aluminum silicate systems. Workers at SRTC previously commissioned OLI Systems Inc. to develop a similar database and this source was distributed here. Current efforts involve comparing the available data with that incorporated in the SRTC zeolite database and thereafter determining what upgrades will be needed.

On-line Analysis for Defense Waste Processing Facility

The process of making glass samples for LIBS calibration has been delayed because the glass group was working on the Fernald project. To avoid the cross contamination, they need to finish all the work for the Fernald project before making glass samples for LIBS calibration. A paper entitled "Analysis of Defense Waste Processing Facility Sludge and Slurry Products with Laser Induced Breakdown Spectroscopy" was presented at the 106th American Ceramic Society Annual Meeting. The pellets with different heating times were tested to see the effects of moisture of the samples on the LIBS signal. Testing different data analysis techniques for improving LIBS accuracy and precision continued. We are also in the process of getting sludge samples from DWPF for the initial sludge sample test.

Support of Production of High Waste Loading Glasses in the DWPF

Following up on last month's visit, Drs. John Plodinec and Adriana Giordana prepared a new plan of research that has been approved by Drs. David Peeler and Sharon Marra at SRS. The new plan of research entails a detailed investigation of the cold cap dynamics. SRS will send some simulant samples to DIAL.

Task 5

HEPA Filter Performance Assurance

Regenerable HEPA Filter Performance Testing

During the month of April, abstracts for three papers were submitted to the 23rd Annual Conference of the American Association for Aerosol Research for review. These abstracts discussed the development of the DIAL large scale particle generator, the DIAL HEPA test stand, and the performance of HEPA filters under a variety of challenge conditions. Work continued in the HEPA laboratory on the set up for preliminary DOP testing. A review of literature associated with testing methods and DOE standards for HEPA filters was underway.

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