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DOE OSTI2023

A Progress Report for a 44-month Aging Study on Nitroplasticizer (NP) Stability - Summary of DFT and FTIR Results

In the past few years, a 44-month long aging experiment was conducted under various aging conditions. The properties of aged nitroplasticizer (NP) samples were analyzed using Fourier transform infrared spectroscopy, Karl Fischer (KF) titration, thermogravimetric analysis (TGA), liquid chromatography tandem quadrupole time of flight mass spectrometry (LC/QTOF), and ion chromatography (IC). In this progress report, some FTIR results are documented and discussed. On the theoretical front, density functional theory (DFT) calculations were carried out. Some DFT results are discussed as well.

36 MATERIALS SCIENCE↗

DOE OSTI2023

Analysis of Defense Waste Processing Facility (DWPF) Condensate Samples and Evaluation of the Glycolate Destruction Process during Nitric-Glycolic flowsheet Transition

Glycolate concentrations were measured by the Savannah River National Laboratory (SRNL) in Slurry Mix Evaporator Condensate Tank (SMECT) and Recycle Collection Tank (RCT) samples retrieved after implementation of the Nitric-Glycolic Acid flowsheet at the Defense Waste Processing Facility (DWPF). No glycolate has been detected in any sample using Ion Chromatography (IC) with a detection limit of 8 mg/L, and no glycolate has been detected using either IC or Proton Nuclear Magnetic Resonance Spectroscopy ( 1 HNMR) after a permanganate strike was performed in the RCT.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2025

Fluoride Analysis by Ion Chromatography in Support of Fast Critical Assembly (FCA) Spent Nuclear Fuel Processing

INTRODUCTION The Savannah River Site (SRS) is currently processing Fast Critical Assembly (FCA) fuel received from the Japan Atomic Energy Agency (JAEA) for disposition. Stainless steel-clad plate and rods in stainless steel containers are dissolved using electrolysis with a solution mixture of nitric acid (HNO3), potassium fluoride (KF), and gadolinium (Gd). An ion chromatography (IC) was developed and vetted to monitor fluoride at various sampling points of the process. To finalize the method, FCA test solution was analyzed to qualify the analytical method followed by real FCA process solution analysis using two different analytical columns. This presentation summarizes the development and vetting of the IC method.

White, Thomas L. [Savannah River National Laborato↗

DOE OSTI2023

Quantitative chemical assay of nanogram-level particulate matter using aerosol mass spectrometry: characterization of particles collected from uncrewed atmospheric measurement platforms

Abstract. Aerosol generation techniques have expanded the utility of aerosol mass spectrometry (AMS) for offline chemical analysis of airborne particles and droplets. However, standard aerosolization techniques require relatively large liquid volumes (e.g., several milliliters) and high sample masses that limit their utility. Here we report the development and characterization of a micronebulization AMS (MN-AMS) technique that requires as low as 10 µL of sample and can provide the quantification of the nanogram level of organic and inorganic substances via the usage of an isotopically labeled internal standard (34SO42-). Using standard solutions, the detection limits for this technique were determined at 0.19, 0.75, and 2.2 ng for sulfate, nitrate, and organics, respectively. The analytical recoveries for these species are 104 %, 87 %, and 94 %, respectively. This MN-AMS technique was applied successfully to analyze filter and impactor samples collected using miniature particulate matter (PM) samplers deployable on uncrewed atmospheric measurement platforms, such as uncrewed aerial systems (UASs) and tethered balloon systems (TBSs). Chemical composition of PM samples collected from a UAS field campaign conducted at the Department of Energy's (DOE) Southern Great Plains (SGP) observatory was characterized. The offline MN-AMS data compared well with the in situ PM composition measured by a co-located aerosol chemical speciation monitor (ACSM). In addition, the MN-AMS and ion chromatography (IC) agreed well for measurements of sulfate and nitrate concentrations in the PM extracts. This study demonstrates the utility of combining MN-AMS with uncrewed measurement platforms to provide quantitative measurements of ambient PM composition.

54 ENVIRONMENTAL SCIENCES↗

NASA NTRS1993

Characterization of Minnesota lunar simulant for plant growth

Processing of lunar regolith into a plant growth medium is crucial in the development of a regenerative life support system for a lunar base. Plants, which are the core of such a system, produce food and oxygen for humans and, at the same time, consume carbon dioxide. Because of the scarcity of lunar regolith, simulants must be used to infer its properties and to develop procedures for weathering and chemical analyses. The Minnesota Lunar Simulant (MLS) has been identified to date as the best available simulant for lunar regolith. Results of the dissolution studies reveal that appropriately fertilized MLS can be a suitable medium for plant growth. The techniques used in conducting these studies can be extended to investigate the suitability of actual lunar regolith as a plant growth medium. Dissolution experiments were conducted using the MLS to determine its nutritional and toxicity characteristics for plant growth and to develop weathering and chemical analysis techniques. Two weathering regimes, one with water and one with dilute organic acids simulating the root rhizosphere microenvironment, were investigated. Elemental concentrations were measured using inductively-coupled-plasma (ICP) emission spectrometry and ion chromatography (IC). The geochemical speciation model, MINTEQA2, was used to determine the major solution species and the minerals controlling them. Acidification was found to be a useful method for increasing cation concentrations to meaningful levels. Initial results indicate that MLS weathers to give neutral to slightly basic solutions which contain acceptable amounts of the essential elements required for plant nutrition (i.e., potassium, calcium, magnesium, sulfur, zinc, sodium, silicon, manganese, copper, chlorine, boron, molybdenum, and cobalt). Elements that need to be supplemented include carbon, nitrogen, and perhaps phosphorus and iron. Trace metals in solution were present at nontoxic levels.

Oglesby, James P.↗

NASA NTRS2000

Estimation of the oxalate content of foods and daily oxalate intake

BACKGROUND: The amount of oxalate ingested may be an important risk factor in the development of idiopathic calcium oxalate nephrolithiasis. Reliable food tables listing the oxalate content of foods are currently not available. The aim of this research was to develop an accurate and reliable method to measure the food content of oxalate. METHODS: Capillary electrophoresis (CE) and ion chromatography (IC) were compared as direct techniques for the estimation of the oxalate content of foods. Foods were thoroughly homogenized in acid, heat extracted, and clarified by centrifugation and filtration before dilution in water for analysis. Five individuals consuming self-selected diets maintained food records for three days to determine their mean daily oxalate intakes. RESULTS: Both techniques were capable of adequately measuring the oxalate in foods with a significant oxalate content. With foods of very low oxalate content (<1.8 mg/100 g), IC was more reliable than CE. The mean daily intake of oxalate by the five individuals tested was 152 +/- 83 mg, ranging from 44 to 352 mg/day. CONCLUSIONS: CE appears to be the method of choice over IC for estimating the oxalate content of foods with a medium (>10 mg/100 g) to high oxalate content due to a faster analysis time and lower running costs, whereas IC may be better suited for the analysis of foods with a low oxalate content. Accurate estimates of the oxalate content of foods should permit the role of dietary oxalate in urinary oxalate excretion and stone formation to be clarified. Other factors, apart from the amount of oxalate ingested, appear to exert a major influence over the amount of oxalate excreted in the urine.

NASA Discipline Regulatory Physiology↗

NASA NTRS1996

Chemical Characterization and Reactivity Testing of Fuel-Oxidizer Reaction Product (Test Report)

The product of incomplete reaction of monomethylhydrazine (MMH) and nitrogen tetroxide (NTO) propellants, or fuel-oxidizer reaction product (FORP), has been hypothesized as a contributory cause of an anomaly which occurred in the chamber pressure (PC) transducer tube on the Reaction Control Subsystem (RCS) aft thruster 467 on flight STS-51. A small hole was found in the titanium-alloy PC tube at the first bend below the pressure transducer. It was surmised that the hole may have been caused by heat and pressure resulting from ignition of FORP. The NASA Johnson Space Center (JSC) White Sands Test Facility (WSTF) was requested to define the chemical characteristics of FORP, characterize its reactivity, and simulate the events in a controlled environment which may have lead to the Pc-tube failure. Samples of FORP were obtained from the gas-phase reaction of MMH with NTO under laboratory conditions, the pulsed firings of RCS thrusters with modified PC tubes using varied oxidizer or fuel lead times, and the nominal RCS thruster firings at WSTF and Kaiser-Marquardt. Fourier transform infrared spectroscopy (FTIR), differential scanning calorimetry (DSC), accelerating rate calorimetry (ARC), ion chromatography (IC), inductively coupled plasma (ICP) spectrometry, thermogravimetric analysis (TGA) coupled to FTIR (TGA/FTIR), and mechanical impact testing were used to qualitatively and quantitatively characterize the chemical, thermal, and ignition properties of FORP. These studies showed that the composition of FORP is variable but falls within a limited range of compositions that depends on the fuel loxidizer ratio at the time of formation, composition of the post-formation atmosphere (reducing or oxidizing), and reaction or postreaction temperature. A typical composition contains methylhydrazinium nitrate (MMHN), ammonium nitrate (AN), methylammonium nitrate (MAN), and trace amounts of hydrazinium nitrate and 1,1-dimethylhydrazinium nitrate. The thermal decomposition reactions of FORP compositions used in this study were unremarkable, Neither the various compositions of FORP, the pure major components of FORP, nor mixtures of FORP with propellant-system corrosion products showed any unusual thermal activity when decomposed under laboratory conditions. Off-limit thruster operations were simulated by rapid mixing of liquid MMH and liquid NTO in a confined space. The test hardware was constructed with pressure- and temperature-measurement devices to determine if the expected fuel oxidizer reaction would result in increased energy release when FORP, FORP constituents, or propellant-system corrosion products were present. These tests demonstrated that FORP, MMHN, AN, or Inconel corrosion products can induce a mixture of MMH and NTO to produce component-damaging energies. The simulation-test program was not extensive enough to provide statistical probabilities for these events but did show that such events can occur. Damaging events required FORP or metal salts to be present at the initial mixing of MMH and NTO. Based on the results of these studies, it is suggested that removal or mitigation of a buildup of these materials may decrease the incidence of these high-energy, potentially damaging events.

Source record↗

DOE OSTI2026

Determining the Solubility Behavior of Kogarkoite in Simulated Nuclear Waste

Kogarkoite (Na 3 FSO 4 ) is a sparingly soluble fluoride–sulfate double salt that has been identified in high level nuclear waste sludge at the Hanford Site and, more recently, in sludge batch compilation samples at the Savannah River Site (SRS). Due to its complex dissolution behavior, which exhibits an inverse dependence on sodium ion activity, the presence of this mineral poses significant challenges to waste retrieval and processing. Incomplete dissolution during sludge washing can lead to the retention of fluoride and sulfate in the high-level waste feed, potentially causing the formation of corrosive, immiscible molten salt layers, known as "glass gall,” in vitrification melters. Current efforts to optimize flowsheet parameters and wash-water volumes are hindered by the absence of a commercially available, certified reference material, which prevents the accurate calibration of analytical methods and the verification of dissolution kinetics. To address this critical gap, this research focuses on the laboratory synthesis of pure Kogarkoite to serve as a standard for comprehensive solubility and washing performance testing. A coupled synthesis and simulant campaign was executed using an evaporative crystallization protocol designed to replicate the dynamic concentration effects observed in tank farm operations. Thirteen simulant matrices were prepared by dissolving systematically varied ratios of sodium fluoride (NaF) and sodium sulfate (Na 2 SO 4 ) in deionized water under three distinct caustic regimes: 0.0 g (control), 4.0 g (~1 M), and 12.0 g (~3 M) sodium hydroxide (NaOH). While thermodynamic equilibrium models suggest that high-caustic environments should favor the stability of the double salt7, results from this evaporative study at 25 0 C revealed a distinct kinetic divergence. Simulants with high hydroxide loading predominantly yielded large, blocky crystals of sodium sulfate decahydrate (Na 2 SO 4 .10H 2 O). Successful synthesis of pure Kogarkoite was achieved exclusively in specific NaOH-free compositional windows, where the precipitate manifested as fine, opaque granular aggregates. Ion chromatography (IC) analysis confirmed phase purity through the simultaneous stoichiometric depletion of both fluoride and sulfate from the supernatant. This successful synthesis establishes a reproducible route to generate bulk Kogarkoite, enabling the subsequent phase of quantitative dissolution testing using inhibited water to optimize sludge-batch assembly.

Sarker, Md Sharif [Florida International Univ. (FI↗

NASA NTRS2018

Characteristics of In Situ Fine Fraction Aerosol Spectra from 300-700 nm Observed Around the Korean Peninsula During KORUS-OC

In situ aerosol extinction and absorption spectra covering the 300-700 nm range at ≤ 1 nm spectral resolution were measured aboard the R/V Onnuri during the Korea U.S. – Ocean Color (KORUS-OC) cruise around the Korean Peninsula from May 21 through June 3, 2016. Total absorption spectra were obtained from aerosols collected on glass fiber filters and subsequently placed in the center of an integrating sphere (Labsphere DRA-CA-30) attached to a dual beam spectrophotometer (Cary 100 Bio UV-Visible Spectrophotometer, 0.2 nm spectral resolution). Absorption spectra from methanol and deionized water extracts of aerosols collected on Teflon filters were measured in a liquid waveguide capillary cell (World Precision Instruments LWCC- 3100, ~0.4 nm spectral resolution). Extinction spectra were measured with a custom built instrument (SpEx, ~0.8 nm spectral resolution). The measurements were obtained at a height of ~10 m above the sea surface with an inlet that limited the measured aerosols to diameters ≤ 1.3 µm. All four sets of spectra exhibit curvature in log-log space with 2nd order polynomials providing a better fit to the measured spectra than power law fits. The deionized water extracts were also analyzed with an ion chromatograph (Dionex ICS-3000 Ion Chromatography System) and with an aerosol mass spectrometer (Aerodyne Research, Inc. HR-ToF High Resolution Aerosol Mass Spectrometer) to examine chemical composition. These data indicate the optical spectra are sensitive to differing chemical properties of the measured ambient aerosols and suggest differing sources and/or atmospheric processes influence the observed optical signatures. The measured suite of spectra are combined to examine the spectral characteristics of single scattering albedo, as well as to examine the contribution of soluble absorbing chromophores to the total absorption spectra. Additional measurements made during the affiliated Korea U.S. - Air Quality (KORUS-AQ) campaign will be used to provide further insight on the observed spectral characteristics.

Jordan, Carolyn E↗

NASA NTRS2022

Source and Chemistry of Hydroxymethanesulfonate (HMS) in Fairbanks, Alaska

Fairbanks, Alaska is a subarctic city with fine-particle (PM 2.5 ) concentrations that exceed air quality regulations in winter due to weak dispersion caused by strong atmospheric inversions, local emissions, and the unique chemistry occurring under the cold and dark conditions. Here we report on observations from the winters of 2020 and 2021, motivated by our pilot study which showed exceptionally high concentrations of fine particle hydroxy methane sulfonate (HMS) or related sulfur (IV) species (e.g., sulfite and bisulfite). We deployed an online Particle-Into-Liquid Sampler-Ion Chromatography (PILS-IC) in conjunction with a suite of instruments to determine HMS precursors (HCHO, SO 2 ) and aerosol composition in general, with the goal to characterize the sources and sinks of HMS in wintertime Fairbanks. PM 2.5 HMS comprised a significant fraction of PM 2.5 sulfur (26-41%) and overall PM 2.5 mass concentration (2.8-6.8%) during pollution episodes, substantially higher than what has been observed in other regions, likely due to the exceptionally low temperatures. HMS peaked in January, with lower concentrations in December and February, resulting from changes in precursors as well as meteorological conditions. Strong correlations with inorganic sulfate and organic mass during pollution events suggest HMS is linked to processes responsible for poor air quality episodes. These findings demonstrate unique aspects of air pollution formation in cold and humid atmospheres.

Fine-particle↗

DOE OSTI2023

Total metals, carbon, nitrogen & anion concentration data; Slate River & East River floodplains, Crested Butte, CO; May 2022-October 2022

This data package includes processed and undiluted measurements for metal, total carbon, total nitrogen, and anion concentrations from pore water (groundwater) and surface water samples from the Slate River and East River floodplains of Crested Butte, CO, focus field sites for the SLAC Floodplain Hydro-Biogeochemistry SFA. The data was generated as part of the work targeting the overarching research question for the SLAC SFA: How do ubiquitous subsurface interfaces mediate molecular-scale biogeochemical processes and groundwater quality in floodplains and watersheds? Samples were collected between May and October of 2022. These measurements were all recorded at the Arizona Laboratory for Emerging Contaminants (ALEC) at the University of Arizona located in Tucson, AZ. Groundwater samples were extracted from a network of installed rhizon (Rhizosphere Research Products, part no. 19.60.21F, 0.6 micrometer mesh size) and piezometer wells within the river floodplain. All water samples were shaded from sun exposure during extraction from the subsurface and preserved at 4C until measured at ALEC.Analysis by ICP-MS (metals):Measurements for total metals were made on the Agilent 7700x ICP-MS (for total metals) – Agilent Technologies, Santa Clara, CA. The analytical QA/QC protocol was adapted from US EPA Method 200.8 for analysis by ICP-MS. Calibration standards were prepared from multi-element stock solutions (SPEX Certiprep, Metuchen, NJ). Calibration curves include at least 7 points with correlation coefficients > 0.995. The QC protocol includes a continuing calibration blank (CCB), a continuing calibration verification (CCV) solution and at least one quality control sample (QCS) to be analyzed just after calibration and again after every 12 samples and at the completion of the run. The QCS solutions are from an independent source, such as NIST SRM 1643e - Trace elements in water, or QCS solutions from High Purity Standards (Charleston, SC). Acceptable QC responses must be between 90 and 110% of the certified value. Lastly, a suitable internal standard (usually Rh, In, Ga or Ge) is added using on-line addition into the sample line and mixing tee.Analysis by Shimadzu TOC-L (TOC/TN):The TOC-L system is a combustion technique where liquid samples are injected and combusted into CO2 for carbon detection by non-dispersive infrared (NDIR) and NO for detection by chemiluminescence. A calibration curve using five standard solutions between 0.1 and 7 ppm for carbon and 0.05 and 3.5 ppm for nitrogen is made for each type of measurement with a linearity >0.99. All samples, standards, and QC’s are prepared in 24mL scintillation vials that have been baked for 4hrs at 475 Cº and made using RO water (18.2mΩ). QC’s include a calibration blank check (CCB), continuing calibration check (CCC), and a certified reference material check (CRM). All QC’s are within ±10% error and are run before and after each batch of samples. Samples are diluted and rerun if any measurement concentrations are above the highest standard.Analysis by Ion Chromatography (Anions):The instrument used is the Thermo Scientific Dionex ICS-6000 using AS+AG22 column set for anion analysis with sodium carbonate eluent. A calibration curve using five standard solutions between 5 and 250 umol/L is made with a linearity >0.99. Standards and QC’s are prepared in 15mL polypropylene conical tubes, pipetted along with the samples into 1.5mL polypropylene vials. Dilutions are made using RO water (18.2mΩ). QC’s include a calibration blank check (CCB), continuing calibration check (CCC), and a certified reference material check (CRM). All QC’s are within ±10% error and are run before and after each batch of samples. Samples are diluted and rerun if any measurement concentrations are above the highest standard.All files are in csv format.

54 ENVIRONMENTAL SCIENCES↗

NASA NTRS2015

Ion Chromatography-on-a-chip for Water Quality Analysis

We report progress towards developing a Micro-Electro-Mechanical Systems (MEMS)- based ion chromatograph (IC) for crewed spacecraft water analysis. This IC-chip is an offshoot of a NASA-funded effort to produce a high performance liquid chromatograph (HPLC)-chip. This HPLC-chip system would require a desalting (i.e. ion chromatography) step. The complete HPLC instrument consists of the Jet Propulsion Labortory's (JPL's) quadrupole ion trap mass spectrometer integrated with a state-of-the-art MEMS liquid chromatograph (LC) system developed by the California Institute of Technology's (Caltech's) Micromachining Laboratory. The IC version of the chip consist of an electrolysis-based injector, a separation column, two electrolysis pumps for gradient generation, mixer, and a built-in conductivity detector. The HPLC version of the chip also includes a nanospray tip. The low instrument mass, coupled with its high analytical capabilities, makes the LC chip ideally suitable for wide range of applications such as trace contaminant, inorganic analytical science and, when coupled to a mass spectrometer, a macromolecular detection system for either crewed space exploration vehicles or robotic planetary missions.

Kidd, R. D.↗

NASA NTRS1982

Preparation and analysis of standardized waste samples for Controlled Ecological Life Support Systems (CELSS)

The preparation and analysis of standardized waste samples for controlled ecological life support systems (CELSS) are considered. Analysis of samples from wet oxidation experiments, the development of ion chromatographic techniques utilizing conventional high pressure liquid chromatography (HPLC) equipment, and an investigation of techniques for interfacing an ion chromatograph (IC) with an inductively coupled plasma optical emission spectrometer (ICPOES) are discussed.

Carden, J. L.↗

DOE OSTI2021

Total metals & anion concentration data; Slate River floodplain, Crested Butte, CO; May 2020-September 2020

This data package includes processed and undiluted measurements for metal and anion concentrations from pore water (groundwater) samples from the Slate River floodplain of Crested Butte, CO, a focus field site for the SLAC Floodplain Hydro-Biogeochemistry SFA. The data was generated as part of the work targeting the overarching research question for the SLAC SFA: How do ubiquitous subsurface interfaces mediate molecular-scale biogeochemical processes and groundwater quality in floodplains and watersheds? Samples were collected between May and September of 2020. These measurements were all recorded at the Arizona Laboratory for Emerging Contaminants (ALEC) at the University of Arizona located in Tucson, AZ. Groundwater samples were extracted from a network of installed rhizon (Rhizosphere Research Products, part no. 19.60.21F, 0.6 micrometer mesh size) and piezometer wells within the river floodplain. All water samples were shaded from sun exposure during extraction from the subsurface and preserved at 4C until measured at ALEC.Analysis by ICP-MS:Measurements for total metals were made on the Agilent 7700x ICP-MS (for total metals) – Agilent Technologies, Santa Clara, CA.The analytical QA/QC protocol was adapted from US EPA Method 200.8 for analysis by ICP-MS. Calibration standards were prepared from multi-element stock solution (Sigma-Aldrich Multielement standard solution for ICP, St. Louis, MO) using matrix matched to sample solutions (either 2% HCl or HNO3 from AriStar Plus,grade acids from VWR Scientific). Calibration curves include at least 7 points with correlation coefficients > 0.995. The QC protocol includes a continuing calibration blank (CCB), a continuing calibration verification (CCV) solution and at least one quality control sample (QCS) to be analyzed just after calibration and again after every 12 samples and at the completion of the run. The QCS solutions are from an independent source, such as NIST SRM 1643e - Trace Elements in Water, or QCS solutions from High Purity Standards (Charleston, SC). Acceptable QC responses must be between 90 and 110% of the certified value. An internal standard (Rh) is added via on-line addition into the sample line using a mixing tee.Analysis by Ion Chromatography (Anions):The protocol follows Method 4110 in Standard Methods for Examination of Water and Wastewater.The instrument used is the Thermo Scientific Dionex ICS-6000 using AS+AG22 column set for anion analysis with isocratic method using sodium carbonate eluent. Detection is by chemical suppression of eluent conductivity. Quality control solutions and mixed analyte standards purchased from Inorganic Ventures, Christiansburg, VA.All files are in csv format.

54 ENVIRONMENTAL SCIENCES↗

DOE OSTI2025

Sulfate Conversion of Reillex HPQ Anion Exchange Resin for Disposal (Interim Report)

This report describes preliminary data to validate the Savannah River Plutonium Processing Facility’s (SRPPF) flowsheet for conversion of used Reillex HPQ anion exchange resin from the nitrate form to the sulfate form. The nitrate form is an oxidizer and therefore does not meet acceptance criteria for disposal at the Waste Isolation Pilot Plant (WIPP). The purpose of this study is to develop data to support acceptance for this disposition pathway. Due to the challenges characterizing the nitrate concentration on solid resin, the data developed to date are based upon indirect analysis of the ion exchange column effluent by ion chromatography. These challenges are discussed and two methods for quantification of nitrate directly on the resin are recommended for further development: TGA-MS and permanganate digestion followed by IC. The resin used for this work was provided in the chloride form; this is the form in which resin is supplied by the manufacturer. However, it had to be converted to the nitrate form, which is the form that will be used in SRPPF’s ion exchange process, prior to use in the sulfate conversion experiments. The chloride-form resin was characterized. A lab-scale procedure for the conversion of Reillex HPQ resin from the chloride to nitrate form was validated. The nitrate-form resin was assessed for particle size and chloride concentration to ensure it met SRPPF’s facility specifications. The baseline sulfate conversion flowsheet was tested. However, nitrate was still detectable in the effluent after approximately 10 bed volumes of 1 M sodium sulfate had been passed through the resin bed. Additional experiments were performed to assess the effect of increasing the feed volume, reducing the flowrate, the use of 2 M sulfuric acid instead of sodium sulfate, and the use of irradiated resin. The sulfuric acid test was the only one which provided a nondetectable nitrate concentration (<0.002 M) in the effluent. Detectable nitrate in the column effluent suggests that nitrate is still present on the resin itself.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗