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The Solubilities of Significant Organic Compounds in HLW Tank Supernate Solutions

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The Solubilities of Significant Organic Compounds in HLW Tank Supernate Solutions WHC-SA-2565-FP The Solubilities of Significant Organic Compounds in HLW Tank Supernate Solutions G. S. Barney Date Published August 1994 To Be Presented at National ACS Meeting Washington, D.C. August 21-26, 1994 Prepared for the U.S. Department of Energy Office of Environmental Restoration and Waste Management Westinghouse p.o BOX 1970 ® Hanford Company Richland, Washington Hanford Operations and Engineering Contractor for the U.S. Department of Energy under Contract DE-AC06-87RL10930 Copyright License By acceptance of this article, the publisher and/or recipient acknowledges the U.S. Government's right to retain a nonexclusive, royalty-free license in and to any copyright covering this paper. Approved for Public Release ; flSffteUTIOK OF THIS OOCUMEST IS UKUffllTSl' DISCLAIMER This report was prepared as an account of work sponsored by an agency of the United States Government. Neither the United States Government nor any agency thereof, nor any of their employees, make any warranty, express or implied, or assumes any legal liability or responsibility for the accuracy, completeness, or usefulness of any information, apparatus, product, or process disclosed, or represents that its use would not infringe privately owned rights. Reference herein to any specific commercial product, process, or service by trade name, trademark, manufacturer, or otherwise does not necessarily constitute or imply its endorsement, recommendation, or favoring by the United States Government or any agency thereof. The views and opinions of authors expressed herein do not necessarily state or reflect those of the United States Government or any agency thereof. DISCLAIMER Portions of this document may be illegible in electronic image products. Images are produced from the best available original document. WHC-SA-2565-FP THE SOLUBILITIES OF SIGNIFICANT ORGANIC COMPOUNDS IN HLW TANK SUPERNATE SOLUTIONS G. S. Barney ABSTRACT Large quantities of organic chemicals used in reprocessing spent nuclear fuels at the Hanford Site have accumulated in underground high-level radioactive waste tanks. The organic content of these tanks must be known so that the potential for hazardous reactions between organic components and sodium nitrate/nitrite salts in the waste can be evaluated. The solubilities of organic compounds described in this report will help determine if they are present in the solid phases (salt cake and sludges) aswellasthe liquid phase (interstitialliquor/supernate) in the tanks. The solubilities of five significant sodium salts ofcarboxylic acids and aminocarboxylic acids [sodium oxalate, formate, citrate, nitrilotriacetate (NTA) and ethylendiaminetetraacetate (EDTA)] were measured in a simulatedsupernate solution at 25°C, 30°C, 40°C, and 50 °C. The organic compounds were selected because they are expected to exist in relatively high concentrations in the tanks. The tank supernate simulant was a 4. OM sodium nitrate - 0.97Msodium nitrite solution with sodium hydroxide concentrations ranging from 0.00003 M.to2.0M. Sodium oxalate solubilities were found to be relatively low and this compound could be expected to precipitate from some tank supernate solutions. The energy content of oxalate salts is, however, relatively small. Sodium formate, citrate, EDTA, andNTA solubilities are high and these salts are unlikely to precipitate under waste tank conditions. This conclusion is based on a comparison of measured total organic carbon (TOC) concentrations in actual tank supernates with the organic salt solubilities determined in this study. Because these organic compounds will only exist in aqueous supernate solutions, self-propagating reactions with nitrate or nitrite salts in the waste are unlikely. Also, draining the supernate from the waste tanks will lower the quantity of these organics left in the tanks. Solubilities of all the organic salts decrease with increasing sodium hydroxide concentration due to the common ion effect ofNa+. In general, increasing temperatures raised the solubilities, although for sodium citrate andNTA the temperature effect was small. iii WHC-SA-2565-FP TABLE OF CONTENTS INTRODUCTION 1 EXPERIMENTAL 2 * Materials And Equipment 2 Analyses 3 Methods 3 RESULTS AND DISCUSSION .4 Solution Densities 4 Evidence For Equilibrium 5 Solution Volume Increases 6 Sodium Oxalate Solubility 6 Sodium Formate Solubility 7 Sodium Citrate Solubility 9 Sodium EDTA Solubility 9 Sodium NTA Solubility 10 HLW Tank TOC Values 11 CONCLUSIONS... 12 REFERENCES 13 iv WHC-SA-2565-FP LIST OF FIGURES Figure 1. Solubility of sodium oxalate in 4.0 M NaN03 - 0.97 M NaN02 solutions at 25°C, 30°C, 40°C, and 50°C for various sodium hydroxide concentrations (A), and sodium oxalate solubility versus total sodium concentration at these temperatures showing linear regression lines (B) 7 Figure 2. Solubility of sodium formate in NaN03 - NaN02 solutions at 30°C, 40°C, and 50°C for various sodium hydroxide concentrations (A), and measured sodium nitrate and nitrite concentrations in the same solutions (B) 8 Figure 3. Ratios of nitrite/nitrate concentrations over 41 days averaged over all sodium hydroxide concentrations used in the formate solubility measurements at 50°C 8 Figure 4. Solubility of sodium citrate in NaN03 - NaN02 solutions at 25°C, 30°C, 40°C, and 50°C for various sodium hydroxide concentrations (A), and measured sodium nitrate and nitrite concentrations in the same solutions (B) 9 Figure 5. Solubility of sodium EDTA in NaN03 - NaN02 solutions at 25°C, 30°C, 40°C, and 50°C for various sodium hydroxide concentrations (A), and measured sodium nitrate and nitrite concentrations in the same solutions (B) 10 Figure 6. Solubility of sodium NT A in NaN03 - NaN02 solutions at 25°C, 30°C, 40°C, and 50°C for various sodium hydroxide concentrations (A), and measured sodium nitrate and nitrite concentrations in the same solutions (B) 11 Figure 7. Frequency distribution of total organic carbon (TOC) concentrations measured in supernate solutions in 61 different Hanford HLW tanks 12 WHC-SA-2565- FP LIST OF TABLES Table 1. Solubilities of organic sodium salts found in the literature .....3 Table 2. Densities of the simulated supernate solutions and supernate solutions saturated with organic salts at 25°C 5 Table 3. Average concentrations of organics versus time at 40°C over all sodium hydroxide concentrations 5 Table 4. Volume increases due to dissolution of organic salts 6 Table 5. Comparison of measured organic salt solubilities in units of molarity and total organic carbon concentrations 12 vi WHC-SA-2565-FP ACRONYMS AND TERMS DSS double-shell slurry EDTA ethylenediaminetetraacetate ED3A ethylenediaminetriacetate HEDTA N-(hydroxyethyl)ethylenediaminetriacetate HLW high-level waste NTA nitrilotriacetate TBP tributyl phosphate TOC total organic carbon vii WHC-SA-2565- FP THE SOLUBILITIES OF SIGNIFICANT ORGANIC COMPOUNDS IN HLW TANK SUPERNATE SOLUTIONS G.S.Barney Process Laboratories and Technology Westinghouse Hanford Company Richland, Washington 99352 INTRODUCTION Large quantities of organic chemicals used in reprocessing spent nuclear fuel at the Hanford Site have accumulated in underground tanks that contain high-level radioactive waste (HLW). These organic compounds can potentially react with nitrate or nitrite components of the wastes to produce heat and gaseous products. Preliminary laboratory tests (Beitel 1976a, 1976b, 1976c, and 1977) show that organic materials react violently if the organic content is in the range of 10 to 30 weight percent in mixtures with sodium nitrate. The ignition temperatures for these reactions are >400°C. Similar results (Fisher 1990) were obtained for mixtures of sodium acetate, sodium nitrite, and sodium nitrate. The mixtures deflagrate when strongly heated as long as they contain more than 10 weight percent sodium acetate and about 20 weight percent sodium nitrate/nitrite. Because of the potential for these self-propagating reactions to occur in high-level waste, the organic content of the waste tanks must be known. Very little is known about the organic content of the solids in the waste tanks. Some measurements of total organic carbon (TOC) have been performed on solids, but the identity of the specific organic compounds present are unknown, except in a few cases. The measurements described in this study will help determine if major organic components in the waste have precipitated and settled in the solid phases (saltcake and sludges) or if they remain in the liquid phase (interstitial liquor/supernate) in the tanks. If most of the organic content is in the liquid phase, a gravity drained saltcake may not contain enough organic material to allow a propagating organic-nitrate/nitrite reaction to occur. The solubilities of many significant organic compounds may be high enough in the interstitial liquor/supernate to prevent precipitation in the solid phase. Solubilities of relevant organic compounds are unknown for the conditions expected in Hanford Site high level wastes. 1 WHC-SA-2565-FP It is known that large quantities of N-(2-hydroxethyl)ethylenediaminetriacetate (HEDTA), ethylenediaminetetraacetate (EDTA), glycolate, and citric acid were added to the tanks as a result of chemical processing at B-Plant (Allen 1976). Smaller quantities of tributyl phosphate (TBP), normal paraffin hydrocarbons (NPH), oxalate, di-2-ethylhexylphosphate, and dibutylbutylphosphonate were also added, as well as small quantities of many other organic compounds. Chemical and radiolytic degradation of some of these compounds has occurred over the years
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