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A summary of waste calcination in full-scale and pilot plant calciners has been compiled for future reference. The summary includes feed chemical composition and process operating parameters for: 1) Waste Calcining Facility (WCF) cold operation and hot campaign H-1 through H-9 from 1961 to 1981; 2) New Waste Calcining Facility (NWCF) cold operation and hot campaigns H-1 through H-4 from 1981 to 2000; and 3) smallscale feed blend tests conducted using non-radioactive simulants in various sizes of pilot plant calciners with fluidized-beds from 4 in. diameter up to 2 foot square. These summaries provide a historical record of calcination development at INTEC, give the range of feed compositions and feed additives that have been tested, and will be useful for evaluating calcinability of future wastes.In the calcination process, the liquid wastes are sprayed using air-atomizing nozzles into a fluidized bed of heated spherical calcine particles, evaporating water and nitric acid in the wastes and leaving behind solid-phase metal oxides. Heat was originally provided by re-circulating liquid eutectic sodium/potassium alloy through heat exchange tubes located in the bed. In 1970 the heat input was changed to in-bed combustion (IBC) of kerosene fuel, sprayed directly into the bed through oxygen atomized fuel nozzles, and the calcination temperature was increased to 500 o C. NWCF testing at 600°C with IBC was performed during AprilJune 1999 and April-May 2000.The successful calcination of a given waste is dependent primarily on the major chemical constituents (greater than about 0.05 molar) and the concentration (or diluteness) of dissolved solids in the waste feed. Chemical additives used for calcination have been calcium nitrate to control halide volatility, boric acid to promote amorphous alumina formation, and aluminum nitrate to dilute the sodium content in the calcine. Wastes which were difficult to calcine alone due to diluteness, inability to control particle size, or formation of agglomerates could often be calcined as blends with more amenable wastes. vi vii ACKNOWLEGEMENTS I would like to acknowledge Billie J. Newby for his years of hard work and dedication, over his 30+ years at the Idaho Chemical Processing Plant. His meticulous notes on calcination have been extremely helpful over the years. A great many others, too numerous to mention, worked on calcination development and operation over the years; and they should all be proud to have pioneered the most successful high-level radioactive waste solidification process in the Department of Energy (DOE) complex. I would also like to acknowledge R. M. Gifford for typing and preparing this report for publication.viii ix CONTENTS

This report presents the results of examination and recovery activities performed on the TRUPACT-II 157 shipping container. The container was part of a contact-handled transuranic waste shipment being transported on a truck to the Waste Isolation Pilot Plant in New Mexico when an accident occurred. Although the transport vehicle sustained only minor damage, airborne transuranic contamination was detected in air samples extracted from inside TRUPACT-II 157 at the Waste Isolation Pilot Plant. Consequently, the shipping container was rejected, resealed, and returned to the Idaho National Engineering and Environmental Laboratory where the payload was disassembled, examined, and recovered for subsequent reshipment to the Waste Isolation Pilot Plant. This report documents the results of those activities.

Methods were studied for using sugar as a feed additive for convertingthe sodium-bearingwastes stored at the Idaho Chemical ProcessingPlant into granular, free flowing solids by fluidized-bed -, calcinationat 500°C. All methods studied blended sodium-bearingwastes with Fluorinelwastes but differed in the types of sugar (sucrose or dextrose) that were added to the blend. The most promising sugar additive was determinedto be sucrose, since it is converted more completelyto inorganiccarbon than is dextrose. The effect of the feed aluminum-to-alkali metal mole ratio on calcinationof these blends with sugar was also investigated. Increasingthe aluminum-to-alkali metal ratio from 0.6 to 1.0 decreased the calcine product-to-finesratio from 3.0 to 1.0 and the attrition index from 80 to 15%. Further increasing the ratio to 1.25 had no effect.TT-CFSWB. WP/PFL/TECH i|i FINaS-6 solids rusted parts of the stainlesssteel retrieval equipment ."that would be in contact with any gases evolved from the calcine and flaked the inside of the retrievalvessel.The runs also investigatedfeed aluminum-to-alkali metal (AI/Na+K) mole ratios of 0.6, 1.0 and 1.25. Increasingthe feed AI/Na+K mole ratio from 0.6 to 1.0 decreased the calcine product-to-finesratio from 3.0 to 1.0, the product productionrate from 250 to -175 g/h, and the attrition index from 80 to -15%. Whereas, increasingthe feed AI/Na+K mole ratio from 1.0 to 1.25 had little or no effect on the calcine product-to-fines ratio, product production rate, and attrition indices. Increasingthe feed AI/Na+K mole ration from 0.6 to 1.25 had little or no effect on the behavior of chloride, fluoride, carbon, or cadmium during calcination.v"

A large number of samples are required to characterize a site contaminated with asbestos from previous mine or other industrial operations. Current methods, such as EPA Region 10's glovebox method, or the Berman Elutriator method are time consuming and costly primarily because the equipment is difficult to decontaminate between samples. EPA desires a shorter and less costly method for characterizing soil samples for asbestos. The objective of this was to design and test a qualitative asbestos sampler that operates as a fluidized bed. The proposed sampler employs a conical spouted bed to vigorously mix the soil and separate fine particulate including asbestos fibers on filters. The filters are then analyzed using transmission electron microscopy for presence of asbestos.During initial testing of a glass prototype using ASTM 20/30 sand and clay fines as asbestos surrogates, fine particulate adhered to the sides of the glass vessel and the tubing to the collection filter -presumably due to static charge on the fine particulate. This limited the fines recovery to ~5% of the amount added to the sand surrogate. A second prototype was constructed of stainless steel, which improved fines recovery to about 10%. Fines recovery was increased to 15% by either humidifying the inlet air or introducing a voltage probe in the air space above the sample. Since this was not a substantial improvement, testing using the steel prototype proceeded without using these techniques.Final testing of the second prototype using asbestos suggests that the fluidized bed is considerably more sensitive than the Berman elutriator method. Using a sand/tremolite mixture with 0.005% tremolite, the Berman elutriator did not segregate any asbestos structures while the fluidized bed segregated an average of 11.7. The fluidized bed was also able to segregate structures in samples containing asbestos at a 0.0001% concentration, while the Berman elutriator method did not detect any fibers at this concentration.Opportunities for improvement with the fluidized bed include improving reproducibility among replicates, increasing mass recovery, improving the lid gasket seal.iii CONTENTS