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DOE OSTI2016

Defense Waste Processing Facility Simulant Chemical Processing Cell Studies for Sludge Batch 9

The Savannah River National Laboratory (SRNL) received a technical task request from Defense Waste Processing Facility (DWPF) and Saltstone Engineering to perform simulant tests to support the qualification of Sludge Batch 9 (SB9) and to develop the flowsheet for SB9 in the DWPF. These efforts pertained to the DWPF Chemical Process Cell (CPC). CPC experiments were performed using SB9 simulant (SB9A) to qualify SB9 for sludge-only and coupled processing using the nitric-formic flowsheet in the DWPF. Two simulant batches were prepared, one representing SB8 Tank 40H and another representing SB9 Tank 51H. The simulant used for SB9 qualification testing was prepared by blending the SB8 Tank 40H and SB9 Tank 51H simulants. The blended simulant is referred to as SB9A. Eleven CPC experiments were run with an acid stoichiometry ranging between 105% and 145% of the Koopman minimum acid equation (KMA), which is equivalent to 109.7% and 151.5% of the Hsu minimum acid factor. Three runs were performed in the 1L laboratory scale setup, whereas the remainder were in the 4L laboratory scale setup. Sludge Receipt and Adjustment Tank (SRAT) and Slurry Mix Evaporator (SME) cycles were performed on nine of the eleven. The other two were SRAT cycles only. One coupled flowsheet and one extended run were performed for SRAT and SME processing. Samples of the condensate, sludge, and off-gas were taken to monitor the chemistry of the CPC experiments.

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DOE OSTI2019

Selection of glasses in support of the Sludge Batch 9 variability study for coupled operation with the Salt Waste Processing Facility

Prior to the processing of Sludge Batch 9 (SB9) with Frit 803 at the Defense Waste Processing Facility (DWPF), assessments and experimental glass work were completed to support the qualification of SB9 coupled processing with streams from the Actinide Removal Process (ARP) and Modular Caustic Side Solvent Extraction Unit (MCU). This previous work did not address coupled processing with streams from the Salt Waste Processing Facility (SWPF) because the Product Composition Control System (PCCS) models limited the TiO 2 concentration in glass to 2 weight percent (wt.%). These high activity streams from SWPF include monosodium titanate (MST) and sludge solids from the Sludge Solids Receipt Tank as well as Cs-containing strip effluent. The incorporation of these SWPF streams is expected to reach TiO2 concentrations in glass greater than 2 wt.% based on an MST addition of 0.4 g MST/L of salt solution. If double strike operation is required, then the MST addition is increased to 0.8 g MST/L of salt solution. Therefore, revisions to the models contained in PCCS were completed to allow the evaluation of glasses containing greater than 2 wt.% TiO 2 , but less than 6 wt.%. To support the implementation of the revised PCCS for SB9 – Frit 803 processing at DWPF prior to SWPF startup, the applicability of the new durability models for the SB9 variability study glasses was verified. Since the initial SB9 qualification for ARP-MCU coupled operation, additional Tank 40 analyses have been completed, which served as the basis for an updated projection of the SB9 blend composition in Tank 40. To identify a frit optimized for SB9 coupled operation with SWPF, the Savannah River National Laboratory (SRNL) performed a paper-study by utilizing Measurement Acceptance Region (MAR) assessments with DWPF PCCS. Based on these MAR assessment results, Frit 625 was recommended for processing both single and double MST strike scenarios. Savannah River Remediation (SRR) requested that SRNL perform a variability study with both Frit 803 and Frit 625 for SB9 coupled operation with SWPF. The objective of the variability study is to demonstrate that the Product Consistency Test (PCT) responses of the glasses are acceptable relative to the chemical durability of the Environmental Assessment (EA) reference glass and predictable by the current DWPF PCCS models for durability. This report documents the development of a test matrix that will support the variability study. To provide operational flexibility prior to SWPF startup, the predictability of glasses within the glass region for Frit 625-SB9 coupled operation with ARP-MCU was also confirmed.

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DOE OSTI2023

Measurement Acceptance Region (MAR) Assessment Results Based on Confirmation Sample Sludge Batch 10 Projections

The Defense Waste Processing Facility (DWPF) is currently preparing to initiate processing of Sludge Batch 10 (SB10), which is comprised of material from Tanks 11H, 13H, 15H, 26F, 40H (heel only), and Alternate Feed Stock-2 and Sodium Reactor Experiment material from H-Canyon. Frit 473 was recommended for sludge-only (SO) and coupled processing with the Salt Waste Processing Facility (SWPF) based on previous assessments of SB10 projections with the DWPF Product Composition Control System (PCCS) glass property models and their associated Measurement Acceptance Region (MAR) constraints. Savannah River Mission Completion (SRMC) subsequently pursued Wash Cycle Y to further reduce the total sulfur in the sludge batch and increase processing flexibility at DWPF. In October 2022, SRMC System Planning provided an updated SB10 Tank 40H blend baseline projection based on the Tank 51 confirmation sample results. Due to the reduced Na concentration relative to previous SB10 projections, two additional projections based on the addition of 7,000 gallons of caustic were provided in November 2022.

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DOE OSTI2015

Integrated sampling and data flow for Hanford vitrification - 15337

The Hanford Tank Waste Treatment and Immobilization Plant (WTP) is a one-of-a-kind nuclear facility being designed, built, and commissioned for the U.S. Department of Energy (DOE) by Bechtel National, Inc. and its subcontractor URS Corporation. The WTP facilities are under construction to complete the design and construction, as well as planning to support the startup, commissioning, and operation for vitrifying the radioactive waste stored in aging underground tanks at the Hanford Site. The work progress includes development of waste feed acceptance and qualification program, including methodologies for processing feed batches. Qualification data from staged feed samples will support the verification that waste acceptance criteria (WAC) and processability requirements are met. This verification is required to ensure safe operation of WTP processes for vitrifying the waste, while establishing specific campaign and batch sheets to comply with glass form acceptance requirements. Sampling and data integration are critical for process control and monitoring of the feed through unit operations. Data collection begins with process knowledge of staged feed for determining the required WAC analyses and testing for unit operations. The waste feed qualification data form the baseline information for WTP operation. The qualification data will be tracked and compared with sample analyses at different steps in vitrification operation. All aspects of data life cycle will be managed by the WTP Plant Engineering organization. The data management approach is established in this manner to allow maintaining campaign traceability through glass production records, while safely processing the corresponding feed campaigns and complying with permitting requirements. (authors)

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DOE OSTI2016

Sludge batch 9 (SB9) acceptance evaluation. Radionuclide concentrations in tank 51 SB9 qualification sample prepared at SRNL

Presented in this report are radionuclide concentrations required as part of the program of qualifying Sludge Batch 9 (SB9) for processing in the Defense Waste Processing Facility (DWPF). The SB9 material is currently in Tank 51 and has been washed and prepared for transfer to Tank 40. The acceptance evaluation needs to be completed prior to the transfer of the material in Tank 51 to Tank 40. The sludge slurry in Tank 40 has already been qualified for DWPF processing and is currently being processed as Sludge Batch 8 (SB8). The radionuclide concentrations were measured or estimated in the Tank 51 SB9 Washed Qualification Sample prepared at Savannah River National Laboratory (SRNL). This sample was prepared from a three liter sample of Tank 51 sludge slurry (HTF-51-15-81) taken on July 23, 2015. The sample was delivered to SRNL where it was initially characterized in the Shielded Cells. Under the direction of Savannah River Remediation (SRR) it was then adjusted per the Tank Farm washing strategy as of October 20, 2015. This final slurry now has a composition expected to be similar to that of the slurry in Tank 51 after final preparations have been made for transfer of that slurry to Tank 40.

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DOE OSTI2016

Sludge batch 9 (SB9) accepance evaluation: Radionuclide concentrations in tank 51 SB9 qualification sample prepared at SRNL

Presented in this report are radionuclide concentrations required as part of the program of qualifying Sludge Batch 9 (SB9) for processing in the Defense Waste Processing Facility (DWPF). The SB9 material is currently in Tank 51 and has been washed and prepared for transfer to Tank 40. The acceptance evaluation needs to be completed prior to the transfer of the material in Tank 51 to Tank 40. The sludge slurry in Tank 40 has already been qualified for DWPF processing and is currently being processed as Sludge Batch 8 (SB8). The radionuclide concentrations were measured or estimated in the Tank 51 SB9 Washed Qualification Sample prepared at Savannah River National Laboratory (SRNL). This sample was prepared from a three liter sample of Tank 51 sludge slurry (HTF-51-15-81) taken on July 23, 2015. The sample was delivered to SRNL where it was initially characterized in the Shielded Cells. Under the direction of Savannah River Remediation (SRR) it was then adjusted per the Tank Farm washing strategy as of October 20, 2015. This final slurry now has a compositioniv expected to be similar to that of the slurry in Tank 51 after final preparations have been made for transfer of that slurry to Tank 40.

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DOE OSTI2017

Multi-criteria group decision-making based sustainability measurement of wastewater treatment processes

There are various processes which can be used for wastewater treatment (WT), and the selection of the most sustainable one among different processes is a hard task. This study aims at helping the decision-makers (DM) to address this by developing an intuitionistic fuzzy set (IFS) theory based group multi-attribute decision analysis (MADA) method. Ten criteria in environment, economy, society-politic, and technology dimensions were employed to achieve sustainability measurement (SM) of WT processes. The multi-criteria sustainability assessment method developed in this study allow different experts to attend the SM, and enable the participants to employ the natural language/words to depict their intuitionistic opinions. Accordingly, the proposed method can achieve group SM under uncertainties. An illustrative case including four processes for wastewater treatment, namely Anaerobic-Anoxic-Oxic (AAO) process, Triple Oxidation Ditch (TOD) process, Anaerobic single-ditch oxidation (ASD) process, and Sequencing batch reactor activated sludge process (SBR), has been studied, and the results reveal that this method can determine sustainability sequence of different WT processes.

54 ENVIRONMENTAL SCIENCES↗

DOE OSTI2022

Purification and Concentration of 99 Mo from a UREX raffinate

The medical isotope 99m Tc ( t ½ = 6.0 h) accounts for over 80% of isotopes used in diagnostic nuclear medicine today and is normally derived from its transient equilibrium parent 99 Mo ( t ½ = 66 h). To reduce U.S. dependence on 99 Mo derived from HEU by foreign suppliers, the NNSA/M3 program—under the American Medical Isotope Production Act—has been tasked with facilitating the work of domestic 99 Mo suppliers that do not utilize HEU. Superconducting electron linear accelerators with high-Z converter targets can generate bremsstrahlung photons and neutron fluxes that can induce photonuclear reactions and LEU fission. After sufficient production intervals, targets can be rotated out and processed while another batch is irradiated. The process flow chemistry is shown in Figure 1. The irradiated U 3 O 8 targets are retrieved and dissolved in HNO 3 ; the volatile fission products are expelled and captured during this step. The HNO 3 liquor bearing the uranyl, fission and activation products is injected into the UREX suite of liquid-liquid extraction banks. The uranyl is partitioned in typical fashion using tri-$\textit{n}$-butyl phosphate (TBP) in a hydrocarbon diluent. The raffinate—comprising mainly 99 Mo and fission products—is then injected into the MoLLE (Molybdenum Liquid-Liquid Extraction) flowsheet, where the Mo is selectively extracted by an organophosphorous acid extractant such as di-(2-ethylhexyl phosphoric acid) (HDEHP). Trace amounts of Nb, Zr, Np, I, and Te are co-extracted. The Mo is stripped using acetohydroxamic acid (AHA) and fed onto an anion exchange column. Following a series of hydroxide, HCl, and oxalic acid wash steps, the Mo can be recovered in NaOH/NaCl. A manuscript describing this process chemistry in more detail was recently published.

07 ISOTOPE AND RADIATION SOURCES↗

DOE OSTI2016

Results of Hg speciation testing on DWPF SMECT-8, OGCT-1, AND OGCT-2 samples

The Savannah River National Laboratory (SRNL) was tasked with preparing and shipping samples for Hg speciation by Eurofins Frontier Global Sciences, Inc. in Seattle, WA on behalf of the Savannah River Remediation (SRR) Mercury Task Team. The sixteenth shipment of samples was designated to include a Defense Waste Processing Facility (DWPF) Slurry Mix Evaporator Condensate Tank (SMECT) sample from Sludge Receipt and Adjustment Tank (SRAT) Batch 738 processing and two Off-Gas Condensate Tank (OGCT) samples, one following Batch 736 and one following Batch 738. The DWPF sample designations for the three samples analyzed are provided. The Batch 738 ‘End of SME Cycle’ SMECT sample was taken at the conclusion of Slurry Mix Evaporator (SME) operations for this batch and represents the fourth SMECT sample examined from Batch 738. Batch 738 experienced a sludge slurry carryover event, which introduced sludge solids to the SMECT that were particularly evident in the SMECT-5 sample, but less evident in the ‘End of SME Cycle’ SMECT-8 sample.

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DOE OSTI2014

Sample Results from MCU Solids Outage

Savannah River National Laboratory (SRNL) has received several solid and liquid samples from MCU in an effort to understand and recover from the system outage starting on April 6, 2014. SRNL concludes that the presence of solids in the Salt Solution Feed Tank (SSFT) is the likely root cause for the outage, based upon the following discoveries: A solids sample from the extraction contactor #1 proved to be mostly sodium oxalate; A solids sample from the scrub contactor#1 proved to be mostly sodium oxalate; A solids sample from the Salt Solution Feed Tank (SSFT) proved to be mostly sodium oxalate; An archived sample from Tank 49H taken last year was shown to contain a fine precipitate of sodium oxalate; A solids sample from ; A liquid sample from the SSFT was shown to have elevated levels of oxalate anion compared to the expected concentration in the feed. Visual inspection of the SSFT indicated the presence of precipitated or transferred solids, which were likely also in the Salt Solution Receipt Tank (SSRT). The presence of the solids coupled with agitation performed to maintain feed temperature resulted in oxalate solids migration through the MCU system and caused hydraulic issues that resulted in unplanned phase carryover from the extraction into the scrub, and ultimately the strip contactors. Not only did this carryover result in the Strip Effluent (SE) being pushed out of waste acceptance specification, but it resulted in the deposition of solids into several of the contactors. At the same time, extensive deposits of aluminosilicates were found in the drain tube in the extraction contactor #1. However it is not known at this time how the aluminosilicate solids are related to the oxalate solids. The solids were successfully cleaned out of the MCU system. However, future consideration must be given to the exclusion of oxalate solids into the MCU system. There were 53 recommendations for improving operations recently identified. Some additional considerations or additional details are provided below as recommendations. From this point on, IC-Anions analyses of the DSSHT should be part of the monthly routine analysis in order to spot negative trends in the oxalate leaving the MCU system. Care must be taken to monitor the oxalate content to watch for sudden precipitation of oxalate salts in the system; Conduct a study to optimize the cleaning strategy at ARP-MCU through decreasing the concentration or entirely eliminating the oxalic acid; The contents of the SSFT should remain unagitated. Routine visual observation should be maintained to ensure there is not a large buildup of solids. As water with agitation provided sufficient removal of the solids in the feed tank, it should be considered as a good means for dissolving oxalate solids if they are found in the future; Conduct a study to improve prediction of oxalate solubility in salt batch feed materials. As titanium and mercury have been found in various solids in this report, evaluate if either element plays a role in oxalate solubility during processing; Salt batch characterization focuses primarily on characterization and testing of unaltered Tank 21H material; however, non-typical feeds are developed through cleaning, washing, and/or sump transfers. As these solutions are processed through MCU, they may precipitate solids or reduce performance. Salt batch characterization and testing should be expanded to encompass a broader range of feeds that may be processed through ARPMCU.

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DOE OSTI2022

Characterization of Tank 9H Salt Dissolution Batch 2B in Support of Tank Closure Cesium Removal (TCCR) 1A Batch 2 Preparations

Savannah River Mission Completion (SRMC) is currently preparing the second batch of material to be processed through the Tank Closure Cesium Removal (TCCR) 1A system. The feed for TCCR 1A consists of dissolved saltcake from Tank 9H. The second batch of salt to make up processing Batch 2 (Batch 2B) has recently been dissolved in Tank 9H and transferred to Tank 10H where it was composited with the first part of the batch (Batch 2A) in preparation for processing through the TCCR 1A unit. Savannah River National Laboratory (SRNL) received samples from the recent batch (2B) of dissolved salt for characterization. Two samples from Batch 2B were received for characterization, a surface sample and a variable depth sample (VDS). Neither sample contained significant solids, although the VDS appeared slightly cloudy as compared to the surface sample. The sodium concentrations of both the surface and VDS filtrate samples were approximately 5.8 M, and the 137 Cs activity was 9.8E+07 dpm/mL in the surface sample and 9.5E+07 dpm/mL in the VDS. The total Cs concentrations were 2.5 mg/L and 2.4 mg/L in the surface sample and VDS, respectively, using the gamma activity and the Cs isotopic ratios determined by ICP-MS. The alpha activity was below the detection limit in both samples. Nitrate was the dominant anion present, and the samples were primarily concentrated sodium nitrate solutions with hydroxide, nitrite, and carbonate present at 0.1 – 0.2 M. In general, the Batch 2B samples were more dilute than the previously characterized Batch 2A samples.

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DOE OSTI2022

Characterization of Tank 9h Salt Dissolution Batch 2C In Support of Tank Closure Cesium Removal (TCCR) 1A Batch 2 Preparations

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2022

Measurement Acceptance Region (MAR) Assessment Results Based On Sludge Batch 10 Projections from December 2021, February 2022 and August 2022

The Defense Waste Processing Facility (DWPF) is currently preparing to initiate processing of Sludge Batch 10 (SB10), which is comprised of material from Tanks 11H, 13H, 15H, and 26F, Alternate Feed Stock-2 and Sodium Reactor Experiment material from H-Canyon. Frit 473 (8B 2 O 3 -8Li 2 O-5Na 2 O-79SiO 2 , in weight percent) was recommended for sludge-only (SO) and coupled processing with the Salt Waste Processing Facility (SWPF) based on previous assessments of SB10 projections with the DWPF Product Composition Control System (PCCS) glass property models and their associated Measurement Acceptance Region (MAR) constraints. Due to the lower processing rate of Sludge Batch 9 (SB9), the heel in Tank 40 is anticipated to be greater than 40 inches at the projected start of SB10 processing to meet the upcoming Accelerated Basin Deinventory addition dates in Tank 51 for Sludge Batch 11. In December 2021 and February 2022, Savannah River Remediation System Planning provided updated SB10 Tank 40 blend projections based on heels of 74 inches, 84 inches, 94 inches and 103.4 inches. Savannah River Mission Completion (SRMC) subsequently pursued Wash Cycle Y to further reduce the total sulfur in the sludge batch and increase processing flexibility at DWPF. In August 2022, SRMC System Planning provided an updated SB10 Tank 40 blend projection with a 76 inch-heel representing Decant Y2 and 60 kilogallons of bearing water inleakage that is anticipated during the Tank 51 to Tank 40 transfer. The objectives of this task were to: • Determine the impact on the operating windows for SO and coupled processing • Determine whether any composition gaps exist between the already completed SB10 variability study and the reprojected SB10 glass composition region • Compare the SB10 reprojected glass composition region to the DWPF PCCS model development and validation ranges to ensure that compositional gaps do not exist between the data sets. This report documents the results of these evaluations. Calculation-based frit assessments were performed using the DWPF PCCS glass property models and their associated MAR constraints. Evaluated parameters for coupled processing included the following transfer volumes per Sludge Receipt and Adjustment Tank batch: 5700 gallons of Tank 40 sludge, 2400-4500 gallons of the SWPF monosodium titanate (MST) and sludge solids stream, and 15,000 gallons of strip effluent. Based on these MAR assessment results, Frit 473 remains viable for SB10 processing. A target waste loading (WL) of 36% is possible for SO operation and single strike (0.4 g/L MST) coupled processing up to 600 mg/L of SB9 insoluble sludge solids at a nominal transfer volume of ~2800 gallons. Increasing the single strike transfer volume to 4500 gallons may reduce the maximum WL below 40%. Operating windows are 12 percentage points for SO processing and 14-16 percentage points for coupled processing. Frit 625 allows for a target WL of 36% and is acceptable for use during the SB9 to SB10 transition to deplete remaining inventory as needed. Operating windows are 8 percentage points for SO processing and 12-14 percentage points for coupled processing. Predictive PCCS evaluations performed at DWPF will provide insight into batch-specific acceptability at desired WLs for compositions having expected oxide ratios during processing versus the extreme vertices (corner points) evaluated in this study. The reprojected SB10 glass composition region generally overlaps the previously evaluated SB10 variability study composition region. Thus, the minor composition shift of these updated SB10 projections indicates that no additional glasses are necessary to demonstrate acceptability relative to the chemical durability of the Environmental Assessment benchmark glass and predictability using the current PCCS models for durability. Based on a comparison of the PCCS model development and validation data to the reprojected SB10 glass composition region, the viscosity and liquidus temperature models will reliably predict SB10 compositions. No additional glasses are necessary to demonstrate predictability of these models.

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DOE OSTI2019

Frit 625 Manufacturability Study

Based on the anticipated higher sodium concentration salt stream coming to the Defense Waste Processing Facility (DWPF) from the Salt Waste Processing Facility (SWPF), there may be a future need to reduce the alkali concentration in the frit depending on the composition of the sludge in Tank 40. SWPF is projected to start operating in late 2019. Thus, a lower alkali frit is beneficial for Sludge Batch (SB9) processing. Lower alkali frits may also be needed for Sludge Batch 10 (SB10) and later batches to ensure that the composition of the material in the Slurry Mix Evaporator (SME) is acceptable relative to the Product Composition Control System (PCCS) models.

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DOE OSTI2017

Preliminary Analysis of Facility Design for Pyro-processing Safeguardability

The deployment of advanced nuclear energy systems can assure sustainable energy use worldwide. For some of these systems, nuclear fuel will be fabricated in remotely-handled facilities in which batch-type processing will occur in heavily-shielded hot cells. Because special nuclear material is in both different physical and chemical form than that of the contemporary fuel cycle, new challenges have arisen in terms of safeguards, safety, and security, integrated with facility design; i.e., safeguardability. There is a need to develop models that can quantitatively assess safeguardability from a design-driven perspective. Previously, the first build of a material throughput model was established using discrete event simulation (DES) for the fuel fabrication process. Results showed that the DES model potentially can detect diversion attempts. This paper continues the study by further developing the the model. We test the use of the probability of the false alarm; i.e., the Type I error, as a metric for safeguardability assessment. Initiating events leading to a false alarm arise from aspects of safeguards, safety, and security. Different conceptual facility designs could exhibit different frequencies for the Type I error, and this could provide a measure of the safeguardability of each design. A quantitative assessment for safeguardable facility designs has not been developed in this manner. Much of the research into safeguardability has been qualitative. Engineering design approaches for a safeguardable facility are now needed. As there are not accepted metrics for safeguardability assessment, our motivation is to develop this design facet of safeguardability further.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2015

Enrichment Meter Dataset from High-Resolution Gamma Spectroscopy Measurements of U3O8 Enrichment Standards and UF6 Cylinder Wall Equivalents

The Enrichment Meter Principle (EMP) is the basis for a commonly used standard test method for the non-destructive assay of 235 U enrichment in bulk compounds [1]. The technique involves determining the net count rate in the direct 186 keV peak using medium or high energy gamma-ray spectrometry in a fixed geometry. With suitable correction for wall attenuation, compound type, rate loss (live time), and peaked background (if significant), the atom fraction of 235 U may be obtained from the counting rate from a linear relationship through the origin. The widespread use of this method for field verification of enrichment [2,3] together with the fact that the response function rests on fundamental physics considerations (i.e., is not represented by a convenient but arbitrary form) makes it an interesting example of uncertainty quantification, one in which one can expect a valid measurement model can be applied. When applied using NaI(Tl) and region of interest analysis, the technique is susceptible to both interference error and bias [2-4]. When implemented using high-resolution gamma-ray spectroscopy, the spectrum interpretation is considerable simplified and more robust [5]. However, a practical challenge to studying the uncertainty budget of the EMP method (for example, to test linearity, extract wall corrections and so forth using modern methods) is the availability of quality experimental data that can be referenced and shared. To fill this gap, the research team undertook an experimental campaign [6]. A measurement campaign was conducted to produce high-resolution gamma spectroscopy enrichment meter data comparable to UF 6 cylinder measurements. The purpose of this report is to provide both an introduction to and quality assurance (QA) of the raw data produced. This report is intended for the analyst or researcher who uses the raw data. Unfortunately, the raw data (i.e., the spectra files) are too voluminous to include in this report but can be requested from Steven Croft of the Safeguards & Security Technology Group (scroft@ornl.gov 865-241-2834). The complete processed data are tabulated in Appendix A. The analysis techniques used to produce the QA data presented in this report [e.g., three regions-ofinterest (ROI) peak extraction and batch analysis processes] are not the most sophisticated techniques available; analysts are encouraged to reanalyze the raw data using more sensitive techniques and to improve upon the results presented here. With that being said, the analysis techniques used here are more than adequate to present and inspect the quality of the data.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

DOE OSTI2021

Raman Spectroscopy Based On-Line, Real-Time Monitoring to Reduce Composition Uncertainties: Enhanced sensitivity through optimization of Raman Parameters

Optical spectroscopy-based on-line monitoring of Hanford processing streams can enable real-time characterization of chemical composition of process streams and batches, ultimately enabling and enhancing process control. It can provide immediate feedback on process conditions and has the potential to reduce the needed number of grab sample collections, thereby reducing times and costs associated with laboratory processing. Here we discuss the utilization of Raman spectroscopy to quantify multiple target analytes that are common within Hanford tanks and waste processing streams. Analytes include: nitrate, nitrite, carbonate, chromate, sulfate, phosphate, hydroxide, oxalate, ammonia, and aluminate. Most notably in this work, Raman applications to low-concentration streams are explored and optimized. Raman instrument specifications are compared; specifically, the impact of utilizing three different Raman excitation wavelengths, 405, 532, and 671 nm, is discussed. Also, Raman data collection parameters such as collection time and spectral averaging are measured and discussed. Finally, optical libraries of chemical targets were collected using optimized collection parameters and chemometric models were built to automate quantification of chemical targets. These models were validated through application to simulants and real Hanford process samples. Chemometric models performed well on both training and validation sets, suggesting these approaches can be successfully applied to on-line and real-time monitoring of low concentration Hanford processing streams. The use of the combine Raman wave lengths with the enhanced chemometric models for the low concentration streams significantly improved the chemical detection levels and significantly reduced uncertainties of those measurements.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

DOE OSTI2016

Actual Waste Demonstration of the Nitric-Glycolic Flowsheet for Sludge Batch 9 Qualification

For each sludge batch that is processed in the Defense Waste Processing Facility (DWPF), the Savannah River National Laboratory (SRNL) performs qualification testing to demonstrate that the sludge batch is processable. Testing performed by the Savannah River National Laboratory has shown glycolic acid to be effective in replacing the function of formic acid in the DWPF chemical process. The nitric-glycolic flowsheet reduces mercury, significantly lowers the catalytic generation of hydrogen and ammonia which could allow purge reduction in the Sludge Receipt and Adjustment Tank (SRAT), stabilizes the pH and chemistry in the SRAT and the Slurry Mix Evaporator (SME), allows for effective rheology adjustment, and is favorable with respect to melter flammability. In order to implement the new flowsheet, SRAT and SME cycles, designated SC-18, were performed using a Sludge Batch (SB) 9 slurry blended from SB8 Tank 40H and Tank 51H samples. The SRAT cycle involved adding nitric and glycolic acids to the sludge, refluxing to steam strip mercury, and dewatering to a targeted solids concentration. Data collected during the SRAT cycle included offgas analyses, process temperatures, heat transfer, and pH measurements. The SME cycle demonstrated the addition of glass frit and the replication of six canister decontamination additions. The demonstration concluded with dewatering to a targeted solids concentration. Data collected during the SME cycle included offgas analyses, process temperatures, heat transfer, and pH measurements. Slurry and condensate samples were collected for subsequent analysis

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