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Testing of High S Matrix Glasses to Expand DFHLW Glass Compositional Ranges (Rev.1)

Gaps in glass composition-property data for direct-feed high-level waste (DFHLW) have recently been identified. One such gap is the region of high sulfur solubility since previous, pretreated, high-level wastes contained very little sulfur. Filling this data gap will significantly broaden the range of process flowsheet options including minimal washing and will allow for optimized waste loading in DFHLW glasses. This report summarizes the data collected during the characterization of the DFHLW High S Glass Matrix (HS24). A glass matrix of 50 glass compositions was developed to evenly cover the DFHLW composition region for high sulfur glass. Matrix glasses were designed to expand the composition region outside the current component concentration and property limits so as to reduce uncertainties at the limits. The 50 matrix glasses were fabricated and tested for properties important to the success of DFHLW vitrification including: compositions, canister centerline cooling (CCC) crystallinity and isothermal crystallinity, density, viscosity, electrical conductivity (EC), product consistency test (PCT) response, toxicity, and sulfate solubility. Melter materials corrosion testing is reported elsewhere. These glasses were intentionally designed to have high SO 3 solubilities (0.7 to 2.2 SO 3 wt%) in compositional regions that had not been previously explored. Forty-eight glasses showed the measured SO 3 content retained >80% of the target SO 3 and the densities of all the glasses ranged from 2.49 g·cm -3 to 2.74 g·cm -3 . While the model predicted nepheline formation in 5 glasses, one of the tested 50 CCC glasses formed nepheline, and 35 glasses formed Cr-containing phases such as spinels and eskolaite. Only five glasses were amorphous after CCC treatment where 44 glasses with detectable crystals contained =10 wt% crystals and only one glass had > 10 wt% crystals. None of the glasses exceeded the allowable T 2% for spinel crystal formation at 950 ºC (i.e., no glasses had >2 wt% spinel at 950 ºC) during isothermal crystal fraction tests where 10 glasses showed no crystalline phases at or below 950 ºC. All the glasses (except one which failed being slightly lower than the target) satisfied the SO 3 constraint while 98 glasses did not meet the viscosity constraints and 4 failed the EC constraints. Six quenched (Q) and six CCC glasses failed the Defense Waste Processing Facility (DWPF) Environmental Assessment (EA) glass PCT threshold and 3 Q and 4 CCC failed the PCT design constraint. One glass exceeded the WTP delisting limits for Cr via EPA Method 1311 (i.e., Toxicity Characteristic Leaching Procedure, TCLP). It should be emphasized that some of these glasses were specifically designed to approach or even exceed certain property constraints, as filling data gaps in these regions will provide the greatest benefit for future model development by improving accuracy and reducing uncertainties. These insights will ultimately support the development of more robust glass formulation strategies, enabling higher waste loading, reducing operational risks, and expanding the processing envelope.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W

Peel resistance of adhesive bonds accurately measured

Strength of adhesive bond between layers of laminated material is tested by peel force to the facing with a tensile testing machine. Testing jig has stainless steel rollers which constrain material to move horizontally while maintaining free end of facing at constant 90 deg angle.

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Ultra high vacuum adhesion testing of NERVA engine materials

The primary objective of this research program was to determine the effects of surface cleaning and deliberate gaseous contamination on the adhesion behavior of selected candidate materials for use in the NERVA nuclear rocket engine program. Using a torsion balance technique, the relationship between the normal compressive load applied to crossed rod samples and the resultant contact resistance was used to ascertain the extent of adhesion under each set of experimental conditions. In addition to an evaluation of the static adhesion behavior of selected materials combinations, the experimental apparatus was modified to permit a similar investigation relating to the effects of specific tangential displacements of the sample wires, i.e., their sliding friction behavior. During the course of this subcontract, the materials combinations 440 C vs. 440 C. pyrographite vs ZTA graphite, Nbc (graphite) vs. Nbc (graphite), and Electrolize Inconel 718 vs. Au electroplated 302 S/S were evaluated.

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Fire response test methods for aerospace materials

Fire response methods which may be suitable for materials intended for aircraft and aerospace applications are presented. They address ignitability, smolder susceptibility, oxygen requirement, flash fire propensity, fire spread, heat release, fire containment, smoke evolution, and toxic gas evolution.

Hilado, C. J.

Fire test methodology for aerospace materials. 1: Thermal and smoke toxicological assessments of graphite/bismaleimide and graphite/epoxy systems

Both materials possess a high degree of thermal stability, with total heat release values being essentially identical under piloted ignition conditions over a range of 5 to 10 W/sq cm incident heat flux. The graphite/epoxy material had a tendency to auto-ignite at a lower heat flux (about 7 W/sq cm) and produced about 23 percent higher peak heat release rates, approximately 42 percent more carbon monoxide and considerably more smoke than the graphite/bismaleimide under conditions of piloted ignition. Toxicological potencies of smoke produced from the two composites were equivalent for 30 minute exposures. Potencies were also comparable to many common materials, such as wood. There was no evidence for the formation of an "unusual toxicant" nor for any short term post-exposure toxicological effects.

Kanakia, M. D.