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Status Assessment of Readiness to Deploy Permanganate Treatment for Removal of Strontium and Actinides from Savannah River Site High Level Waste

Description: The current plan to dispose of high-level waste at the Savannah River Site uses monosodium titanate (MST) to remove soluble strontium and alpha-emitting radionuclides to levels acceptable for disposal in the Saltstone Production Facility. This report assesses the merits of the process using sodium permanganate, instead of monosodium titanate (MST), to remove soluble strontium and actinides from Savannah River Site high-level waste. It also describes the major elements of the recommended research and engineering.
Date: November 27, 2002
Creator: Fink, S.D.
Partner: UNT Libraries Government Documents Department

Demonstration of MST Efficacy on Removal of Actinides and Strontium in ''Bounding Alpha'' Waste

Description: Previous work at the Savannah River Site identified five microbatches of waste projected to fail to meet removal requirements for total alpha after treatment with monosodium titanate (MST) at the baseline conditions proposed for the Salt Waste Processing Facility (SWPF). This document describes an experimental demonstration that examined removal of strontium and alpha emitting radionuclides from a composite of several tanks present in the most limiting macrobatches. The work investigated the amount of MST needed to treat this ''bounding alpha'' macrobatch composite such that the separated liquid can meet the Salt Waste Processing Facility limits.
Date: February 24, 2003
Creator: Fink, S. D.
Partner: UNT Libraries Government Documents Department

Results of Analysis of Macrobatch 3 Decontaminated Salt Solution Coalescer from May 2010

Description: SRNL analyzed the Decontamination Salt Solution (DSS) coalescer from MCU by several analytical methods. This unit was removed from service in May 2010. The results of these analyses indicate that there is very little evidence of fouling via excessive solids, either from the leaching studies or X-Ray Diffraction (XRD) analysis.
Date: December 18, 2012
Creator: Peters, T. B. & Fink, S. D.
Partner: UNT Libraries Government Documents Department

Results Of Routine Strip Effluent Hold Tank, Decontaminated Salt Solution Hold Tank, And Caustic Wash Tank Samples From Modular Caustic-Side Solvent Extraction Unit During Macrobatch 4 Operations

Description: Strip Effluent Hold Tank (SEHT), Decontaminated Salt Solution Hold Tank (DSSHT), and Caustic Wash Tank (CWT) samples from several of the ?microbatches? of Integrated Salt Disposition Project (ISDP) Salt Batch (?Macrobatch?) 4 have been analyzed for {sup 238}Pu, {sup 90}Sr, {sup 137}Cs, and by inductively-coupled plasma emission spectroscopy (ICPES). Furthermore, samples from the CWT have been analyzed by a variety of methods to investigate a decline in the decontamination factor (DF) of the cesium observed at MCU. The results indicate good decontamination performance within process design expectations. While the data set is sparse, the results of this set and the previous set of results for Macrobatch 3 samples indicate generally consistent operations. There is no indication of a disruption in plutonium and strontium removal. The average cesium DF and concentration factor (CF) for samples obtained from Macrobatch 4 are slightly lower than for Macrobatch 3, but still well within operating parameters. The DSSHT samples show continued presence of titanium, likely from leaching of the monosodium titanate in Actinide Removal Process (ARP).
Date: October 25, 2012
Creator: Peters, T. B. & Fink, S. D.
Partner: UNT Libraries Government Documents Department

Sample Results From The Interim Salt Disposition Program Macrobatch 6 Tank 21H Qualification Samples

Description: Savannah River National Laboratory (SRNL) analyzed samples from Tank 21H in support of qualification of Macrobatch (Salt Batch) 6 for the Interim Salt Disposition Project (ISDP). This document reports partial results of the analyses of samples of Tank 21H. No issues with the projected Salt Batch 6 strategy are identified.
Date: December 20, 2012
Creator: Peters, T. B. & Fink, S. D.
Partner: UNT Libraries Government Documents Department

Sample Results from the Interim Salt Disposition Program Macrobatch 6 Tank 21H Qualification Samples

Description: Savannah River National Laboratory (SRNL) analyzed samples from Tank 21H in support of qualification of Macrobatch (Salt Batch) 6 for the Interim Salt Disposition Project (ISDP). This document reports partial results of the analyses of samples of Tank 21H. No issues with the projected Salt Batch 6 strategy are identified.
Date: December 11, 2012
Creator: Peters, T. B. & Fink, S. D.
Partner: UNT Libraries Government Documents Department

Thermal And Spectroscopic Analyses Of Next Generation Caustic Side Solvent Extraction Solvent Contacted With 3, 8, And 16 Molar Nitric Acid

Description: A new solvent system referred to as Next Generation Solvent or NGS, has been developed at Oak Ridge National Laboratory for the removal of cesium from alkaline solutions in the Caustic Side Solvent Extraction process. The NGS is proposed for deployment at MCU{sup a} and at the Salt Waste Processing Facility. This work investigated the chemical compatibility between NGS and 16 M, 8 M, and 3 M nitric acid from contact that may occur in handling of analytical samples from MCU or, for 3 M acid, which may occur during contactor cleaning operations at MCU. This work shows that reactions occurred between NGS components and the high molarity nitric acid. Reaction rates are much faster in 8 M and 16 M nitric acid than in 3 M nitric acid. In the case of 16 M and 8 M nitric acid, the nitric acid reacts with the extractant to produce initially organo-nitrate species. The reaction also releases soluble fluorinated alcohols such as tetrafluoropropanol. With longer contact time, the modifier reacts to produce a tarry substance with evolved gases (NO{sub x} and possibly CO). Calorimetric analysis of the reaction product mixtures revealed that the organo-nitrates reaction products are not explosive and will not deflagrate.
Date: December 7, 2011
Creator: Fondeur, F. F. & Fink, S. D.
Partner: UNT Libraries Government Documents Department

Identification And Characterization Of The Solids Found In Extraction Contactor SEP-401 In June 2012

Description: The Modular Caustic-Side Solvent Extraction Unit (MCU) recently conducted an outage that included maintenance on the centrifugal contactors. Operations personnel observed solids or deposits in two contactors and attempted to collect samples for analyses by Savannah River National Laboratory (SRNL). The residues found in Extraction Contactor SEP-401 are a mixture of amorphous silica, aluminosilicate, titanium, and debris from low alloy steel. The solids contain low concentrations of plutonium and strontium. These isotopes are associated with the titanium that came from the monosodium titanate (MST) added in the Actinide Removal Process (ARP) most likely as leached Ti from the MST that precipitated subsequently in MCU. An attempt was also made to obtain samples from the contents of Wash Contactor SEP-702. However, sampling provide ineffective.
Date: December 10, 2012
Creator: Fondeur, F. F. & Fink, S. D.
Partner: UNT Libraries Government Documents Department

CHEMICAL STABILITY OF POLYPHENYLENE SULFIDE IN THE NEXT GENERATION SOLVENT FOR CAUSTIC-SIDE SOLVENT EXTRACTION

Description: The Office of Waste Processing, within the Office of Technology Innovation and Development, is funding the development of an enhanced solvent for deployment at the Savannah River Site for removal of cesium from High Level Waste. For simplicity, this solvent is referred to as the Next Generation Solvent (NGS). The technical effort is collaboration between Oak Ridge National Laboratory (ORNL), Savannah River National Laboratory (SRNL), and Argonne National Laboratory. The initial deployment target envisioned for the technology was within the Modular Caustic-Side Solvent Extraction Unit (MCU). Deployment of a new chemical within an existing facility requires verification that the chemical components are compatible with the installed equipment. In the instance of a new organic solvent, the primary focus is on compatibility of the solvent with polyphenylene sulfide (PPS), the polymer used in the coalescers within MCU. This report provides the data from exposing PPS polymer to NGS. The test was conducted over a three month period. PPS is remarkably stable in the presence of the next generation solvent. Testing showed no indication of swelling or significant leaching. Preferential sorption of the Modifier on PPS was observed but the same behavior occurs with the baseline solvent. Therefore, PPS coalescers exposed to the NGS are expected to perform comparably to those in contact with the baseline solvent.
Date: December 8, 2011
Creator: Fondeur, F. & Fink, S.
Partner: UNT Libraries Government Documents Department

CHARACTERIZATION AND EVALUATION OF CAUSTIC WASH TANK AND SOLVENT HOLD TANK SAMPLES FROM MCU FROM AUGUST TO SEPTEMBER 2011

Description: During processing of Salt Batches 3 and 4 in the Modular Caustic-Side Solvent Extraction Unit (MCU), the decontamination efficiency for cesium declined from historical values and from expectations based on laboratory testing. This report documents efforts to analyze samples of solvent and process solutions from MCU in an attempt to understand the cause of the reduced performance and to recommend mitigations. CWT Solutions from MCU from the time period of variable decontamination factor (DF) performance which covers from April 2011 to September 2011 (during processing of Salt Batch 4) were examined for impurities using chromatography and spectroscopy. The results indicate that impurities were found to be of two types: aromatic containing impurities most likely from Modifier degradation and aliphatic type impurities most likely from Isopar{reg_sign} L and tri-n-octylamine (TOA) degradation. Caustic washing the Solvent Hold Tank (SHT) solution with 1M NaOH improved its extraction ability as determined from {sup 22}Na uptake tests. Evidence from this work showed that pH variance in the aqueous solutions within the range of 1M nitric acid to 1.91M NaOH that contacted the solvent samples does not influence the analytical determination of the TOA concentration by GC-MS.
Date: August 1, 2012
Creator: Fondeur, F. & Fink, S.
Partner: UNT Libraries Government Documents Department

THE HYDROTHERMAL REACTIONS OF MONOSODIUM TITANATE, CRYSTALLINE SILICOTITANATE AND SLUDGE IN THE MODULAR SALT PROCESS: A LITERATURE SURVEY

Description: The use of crystalline silicotitanate (CST) is proposed for an at-tank process to treat High Level Waste at the Savannah River Site. The proposed configuration includes deployment of ion exchange columns suspended in the risers of existing tanks to process salt waste without building a new facility. The CST is available in an engineered form, designated as IE-911-CW, from UOP. Prior data indicates CST has a proclivity to agglomerate from deposits of silica rich compounds present in the alkaline waste solutions. This report documents the prior literature and provides guidance for the design and operations that include CST to mitigate that risk. The proposed operation will also add monosodium titanate (MST) to the supernate of the tank prior to the ion exchange operation to remove strontium and select alpha-emitting actinides. The cesium loaded CST is ground and then passed forward to the sludge washing tank as feed to the Defense Waste Processing Facility (DWPF). Similarly, the MST will be transferred to the sludge washing tank. Sludge processing includes the potential to leach aluminum from the solids at elevated temperature (e.g., 65 C) using concentrated (3M) sodium hydroxide solutions. Prior literature indicates that both CST and MST will agglomerate and form higher yield stress slurries with exposure to elevated temperatures. This report assessed that data and provides guidance on minimizing the impact of CST and MST on sludge transfer and aluminum leaching sludge.
Date: November 11, 2010
Creator: Fondeur, F.; Pennebaker, F. & Fink, S.
Partner: UNT Libraries Government Documents Department

OXALATE MASS BALANCE DURING CHEMICAL CLEANING IN TANK 6F

Description: The Savannah River Remediation (SRR) is preparing Tank 6F for closure. The first step in preparing the tank for closure is mechanical sludge removal. Following mechanical sludge removal, SRS performed chemical cleaning with oxalic acid to remove the sludge heel. Personnel are currently assessing the effectiveness of the chemical cleaning to determine whether the tank is ready for closure. SRR personnel collected liquid samples during chemical cleaning and submitted them to Savannah River National Laboratory (SRNL) for analysis. Following chemical cleaning, they collected a solid sample (also known as 'process sample') and submitted it to SRNL for analysis. The authors analyzed these samples to assess the effectiveness of the chemical cleaning process. Analysis of the anions showed the measured oxalate removed from Tank 6F to be approximately 50% of the amount added in the oxalic acid. To close the oxalate mass balance, the author collected solid samples, leached them with nitric acid, and measured the concentration of cations and anions in the leachate. Some conclusions from this work are: (1) Approximately 65% of the oxalate added as oxalic acid was removed with the decanted liquid. (2) Approximately 1% of the oxalate (added to the tank as oxalic acid) formed precipitates with compounds such as nickel, manganese, sodium, and iron (II), and was dissolved with nitric acid. (3) As much as 30% of the oxalate may have decomposed forming carbon dioxide. The balance does not fully account for all the oxalate added. The offset represents the combined uncertainty in the analyses and sampling.
Date: July 22, 2011
Creator: Poirier, M. & Fink, S.
Partner: UNT Libraries Government Documents Department

RESULTS OF THE EXTRACTION-SCRUB-STRIP TESTING USING AN IMPROVED SOLVENT FORMULATION AND SALT WASTE PROCESSING FACILITY SIMULATED WASTE

Description: The Office of Waste Processing, within the Office of Technology Innovation and Development, is funding the development of an enhanced solvent - also known as the next generation solvent (NGS) - for deployment at the Savannah River Site to remove cesium from High Level Waste. The technical effort is a collaborative effort between Oak Ridge National Laboratory (ORNL) and Savannah River National Laboratory (SRNL). As part of the program, the Savannah River National Laboratory (SRNL) has performed a number of Extraction-Scrub-Strip (ESS) tests. These batch contact tests serve as first indicators of the cesium mass transfer solvent performance with actual or simulated waste. The test detailed in this report used simulated Tank 49H material, with the addition of extra potassium. The potassium was added at 1677 mg/L, the maximum projected (i.e., a worst case feed scenario) value for the Salt Waste Processing Facility (SWPF). The results of the test gave favorable results given that the potassium concentration was elevated (1677 mg/L compared to the current 513 mg/L). The cesium distribution value, DCs, for extraction was 57.1. As a comparison, a typical D{sub Cs} in an ESS test, using the baseline solvent formulation and the typical waste feed, is {approx}15. The Modular Caustic Side Solvent Extraction Unit (MCU) uses the Caustic-Side Solvent Extraction (CSSX) process to remove cesium (Cs) from alkaline waste. This process involves the use of an organic extractant, BoBCalixC6, in an organic matrix to selectively remove cesium from the caustic waste. The organic solvent mixture flows counter-current to the caustic aqueous waste stream within centrifugal contactors. After extracting the cesium, the loaded solvent is stripped of cesium by contact with dilute nitric acid and the cesium concentrate is transferred to the Defense Waste Processing Facility (DWPF), while the organic solvent is cleaned and recycled for further use. The ...
Date: January 9, 2012
Creator: Peters, T.; Washington, A. & Fink, S.
Partner: UNT Libraries Government Documents Department

REVIEW OF ACTINIDE AND STRONTIUM LOADING DATA FOR MST AND MMST

Description: SRNL reviewed the relevant data from MST and mMST fissile loading studies to determine if further studies were required. With respect to MST, SRNL found that the published results adequately bound the expected conditions that Small Column Ion Exchange (SCIX) process will operate under. The lack of strontium data does not represent an issue as strontium is not relevant to criticality. There is no threat to criticality safety from the lack of strontium loading data. However, SRNL proposes a single test with MST to ensure that future SCIX operations are conservatively bounded and strontium maximum loading is understood. With respect to attempts to maximally load mMST, SRNL's knowledge on actinide and strontium loading is limited to uranium behavior. mMST has a very weak affinity for uranium, and even extended contact time at high uranium concentration shows minimal loading onto mMST. This leaves questions about the ability to load plutonium, neptunium and strontium. SRNL proposes to perform two tests with mMST to ensure that questions on plutonium, neptunium, and strontium sorption are answered, as well as ensuring that future mMST operations are conservatively bounded.
Date: October 20, 2010
Creator: Peters, T.; Hobbs, D. & Fink, S.
Partner: UNT Libraries Government Documents Department

SAMPLE RESULTS FROM THE INTEGRATED SALT DISPOSITION PROGRAM MACROBATCH 4 TANK 21H QUALIFICATION SAMPLES

Description: Savannah River National Laboratory (SRNL) analyzed samples from Tank 21H to qualify them for use in the Integrated Salt Disposition Program (ISDP) Batch 4 processing. All sample results agree with expectations based on prior analyses where available. No issues with the projected Salt Batch 4 strategy are identified. This revision includes additional data points that were not available in the original issue of the document, such as additional plutonium results, the results of the monosodium titanate (MST) sorption test and the extraction, scrub strip (ESS) test. This report covers the revision to the Tank 21H qualification sample results for Macrobatch (Salt Batch) 4 of the Integrated Salt Disposition Program (ISDP). A previous document covers initial characterization which includes results for a number of non-radiological analytes. These results were used to perform aluminum solubility modeling to determine the hydroxide needs for Salt Batch 4 to prevent the precipitation of solids. Sodium hydroxide was then added to Tank 21 and additional samples were pulled for the analyses discussed in this report. This work was specified by Task Technical Request and by Task Technical and Quality Assurance Plan (TTQAP).
Date: June 22, 2011
Creator: Peters, T. & Fink, S.
Partner: UNT Libraries Government Documents Department

SAMPLE RESULTS FROM THE INTEGRATED SALT DISPOSITION PROGRAM MACROBATCH 5 TANK 21H QUALIFICATION MST, ESS AND PODD SAMPLES

Description: Savannah River National Laboratory (SRNL) performed experiments on qualification material for use in the Integrated Salt Disposition Program (ISDP) Batch 5 processing. This qualification material was a composite created from recent samples from Tank 21H and archived samples from Tank 49H to match the projected blend from these two tanks. Additionally, samples of the composite were used in the Actinide Removal Process (ARP) and extraction-scrub-strip (ESS) tests. ARP and ESS test results met expectations. A sample from Tank 21H was also analyzed for the Performance Objectives Demonstration Document (PODD) requirements. SRNL was able to meet all of the requirements, including the desired detection limits for all the PODD analytes. This report details the results of the Actinide Removal Process (ARP), Extraction-Scrub-Strip (ESS) and Performance Objectives Demonstration Document (PODD) samples of Macrobatch (Salt Batch) 5 of the Integrated Salt Disposition Program (ISDP).
Date: April 24, 2012
Creator: Peters, T. & Fink, S.
Partner: UNT Libraries Government Documents Department

SAMPLE RESULTS FROM THE INTEGRATED SALT DISPOSITION PROGRAM MACROBATCH 5 TANK 21H QUALIFICATION SAMPLES

Description: Savannah River National Laboratory (SRNL) analyzed samples from Tank 21H in support of qualification of Macrobatch (Salt Batch) 5 for the Integrated Salt Disposition Project (ISDP). This document reports partial results of the analyses of samples of Tank 21H. No issues with the projected Salt Batch 5 strategy are identified. Results of the analyses of the Tank 21H samples from this report in conjunction with the findings of the previous report, indicates that the material does not display any unusual characteristics.
Date: March 26, 2012
Creator: Peters, T. & Fink, S.
Partner: UNT Libraries Government Documents Department

Oxalate Mass Balance During Chemical Cleaning in Tank 5F

Description: The Savannah River Site (SRS) is preparing Tank 5F for closure. The first step in preparing the tank for closure is mechanical sludge removal. Following mechanical sludge removal, SRS performed chemical cleaning with oxalic acid to remove the sludge heel. Personnel are currently assessing the effectiveness of the chemical cleaning to determine whether the tank is ready for closure. SRS personnel collected liquid samples during chemical cleaning and submitted them to Savannah River National Laboratory (SRNL) for analysis. Following chemical cleaning, they collected a solid sample (also known as 'process sample') and submitted it to SRNL for analysis. The authors analyzed these samples to assess the effectiveness of the chemical cleaning process. Analysis of the anions showed the measured oxalate removed from Tank 5F to be approximately 50% of the amount added in the oxalic acid. To close the oxalate mass balance, the author collected solid samples, leached them with nitric acid, and measured the concentration of cations and anions in the leachate.
Date: July 8, 2011
Creator: Poirier, M. & Fink, S.
Partner: UNT Libraries Government Documents Department

INVESTIGATION OF PLUTONIUM AND URANIUM UPTAKE INTO MCU SOLVENT AND NEXT GENERATION SOLVENT

Description: At the request of the Savannah River Remediation (SRR) customer, the Savannah River National Laboratory (SRNL) examined the plutonium (Pu) and uranium (U) uptake into the Next Generation Solvent (NGS) that will be used at the Salt Waste Processing Facility (SWPF). SRNL examined archived samples of solvent used in Extraction-Scrub-Strip (ESS) tests, as well as samples from new tests designed explicitly to examine the Pu and U uptake. Direct radiocounting for Pu and U provided the best results. Using the radiocounting results, we found that in all cases there were <3.41E-12 g Pu/g of NGS and <1.17E-05 g U/g of NGS in multiple samples, even after extended contact times and high aqueous:organic volume phase ratios. These values are conservative as they do not allow for release or removal of the actinides by scrub, strip, or solvent wash processes. The values do not account for extended use or any increase that may occur due to radiolytic damage of the solvent.
Date: January 6, 2012
Creator: Peters, T. & Fink, S.
Partner: UNT Libraries Government Documents Department

THERMAL AND SPECTROSCOPIC ANALYSES OF NEXT GENERATION CAUSTIC SIDE SOLVENT EXTRACTION SOLVENT CONTACTED WITH 3, 8, AND 16 MOLAR NITRIC ACID

Description: A new solvent system referred to as Next Generation Solvent or NGS, has been developed at Oak Ridge National Laboratory for the removal of cesium from alkaline solutions in the Caustic Side Solvent Extraction process. NGS is proposed for deployment at MCU and at the Salt Waste Processing Facility. This work investigated the chemical compatibility between NGS and 16 M, 8 M, and 3 M nitric acid from contact that may occur in handling of analytical samples from MCU or, for 3 M acid, which may occur during contactor cleaning operations at MCU. This work shows that reactions occurred between NGS components and the high molarity nitric acid. In the case of 16 M and 8 M nitric acid, initially organo-nitrate groups are generated and attach to the modifier and that with time oxidation reactions convert the modifier into a tarry substance with gases (NO{sub x} and possibly CO) evolving. Calorimetric analysis of the organonitrate revealed the reaction products are not explosive nor will they deflagrate. NGS exposure to 3 M nitric acid resulted in much slower reaction kinetics and that the generated products were not energetic. We recommended conducting Accelerated Rate calorimetry on the materials generated in the 16 M and 8 M nitric acid test. Also, we recommend continue monitoring of the samples contacting NGS with 3 M nitric acid.
Date: September 30, 2011
Creator: Fondeur, F. & Fink, S.
Partner: UNT Libraries Government Documents Department

ANALYSIS OF SAMPLES FROM TANK 6F CHEMICAL CLEANING

Description: Savannah River Remediation (SRR) is preparing Tank 6F for closure. The first step in preparing the tank for closure is mechanical sludge removal. In mechanical sludge removal, personnel add liquid (e.g., inhibited water or supernate salt solution) to the tank to form a slurry. They mix the liquid and sludge with pumps, and transfer the slurry to another tank for further processing. Mechanical sludge removal effectively removes the bulk of the sludge from a tank, but is not able to remove all of the sludge. In Tank 6F, SRR estimated a sludge heel of 5,984 gallons remained after mechanical sludge removal. To remove this sludge heel, SRR performed chemical cleaning. The chemical cleaning included two oxalic acid strikes, a spray wash, and a water wash. SRR conducted the first oxalic acid strike as follows. Personnel added 110,830 gallons of 8 wt % oxalic acid to Tank 6F and mixed the contents of Tank 6F with two submersible mixer pumps (SMPs) for approximately four days. Following the mixing, they transferred 115,903 gallons of Tank 6F material to Tank 7F. The SMPs were operating when the transfer started and were shut down approximately five hours after the transfer started. SRR collected a sample of the liquid from Tank 6F and submitted it to SRNL for analysis. Mapping of the tank following the transfer indicated that 2,400 gallons of solids remained in the tank. SRR conducted the second oxalic acid strike as follows. Personnel added 28,881 gallons of 8 wt % oxalic acid to Tank 6F. Following the acid addition, they visually inspected the tank and transferred 32,247 gallons of Tank 6F material to Tank 7F. SRR collected a sample of the liquid from Tank 6F and submitted it to SRNL for analysis. Mapping of the tank following the transfer indicated that 3,248 ...
Date: February 2, 2010
Creator: Poirier, M. & Fink, S.
Partner: UNT Libraries Government Documents Department