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Sludge Batch 6 Acceptance Evaluation: Radionuclide Concentrations in Tank 51 sb6 Qualification Sample Prepared at SRNL

Description: Presented in this report are radionuclide concentrations required as part of the program of qualifying Sludge Batch Six (SB6) for processing in the Defense Waste Processing Facility (DWPF). The SB6 material is currently in Tank 51 being 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 and is currently being processed as SB5. The radionuclide concentrations were measured or estimated in the Tank 51 SB6 Qualification Sample prepared at Savannah River National Laboratory (SRNL). This sample was prepared from the three liter sample of Tank 51 sludge slurry (HTF-51-09-110) taken on October 8, 2009. The sample was delivered to SRNL where it was initially characterized in the Shielded Cells. Under the direction of the Liquid Waste Organization it was then modified by eight washes, nine decants, an addition of Pu from Canyon Tank 16.3, and an addition of NaNO{sub 2}. 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. Determining the radionuclide concentrations in this Tank 51 SB6 Qualification Sample is part of the work requested in Technical Task Request (TTR) No. HLW-DWPF-TTR-2009-0014. The work with this qualification sample is covered by a Task Technical and Quality Assurance Plan and an Analytical Study Plan. The radionuclides included in this report are needed for the DWPF Radiological Program Evaluation, the DWPF Waste Acceptance Criteria (TSR/WAC) Evaluation, and the DWPF Solid Waste Characterization Program (TTR Task I.2). Radionuclides required to meet the Waste Acceptance Product Specifications (TTR Task II.2.) will be measured at a later date after ...
Date: May 21, 2010
Creator: Bannochie, C.; Bibler, N. & Diprete, D.
Partner: UNT Libraries Government Documents Department

Determination Of Reportable Radionuclides For DWPF Sludge Batch 7B (Macrobatch 9)

Description: The DWPF is receiving radioactive sludge slurry from HLW Tank 40. The radioactive sludge slurry in Tank 40 is a blend of the heel from Sludge Batch 7a (SB7a) and Sludge Batch 7b (SB7b) that was transferred to Tank 40 from Tank 51. The blend of sludge in Tank 40 is also referred to as Macrobatch 9 (MB9). This report develops the list of reportable radionuclides and associated activities as a function of time. Twenty-seven radionuclides have been identified as reportable for DWPF SB7b. Each of these radionuclides has a half-life greater than ten years and contributes more than 0.01% of the radioactivity on a Curie basis at some point from production through the 1100 year period between 2015 and 3115. For SB7b, all of the radionuclides in the Design Basis glass are reportable except for three radionuclides: Pd-107, Cs-135, and Th-230. At no time during the 1100- year period between 2015 and 3115 did any of these three radionuclides contribute to more than 0.01% of the radioactivity on a Curie basis. The radionuclide measurements made for SB7b are the most extensive conducted to date. Some method development/refinement occurred during the conduct of these measurements, leading to lower detection limits and more accurate measurement of some isotopes than was previously possible.
Date: December 17, 2012
Creator: Crawford, C. L. & Diprete, D. P.
Partner: UNT Libraries Government Documents Department

Determination Of Reportable Radionuclides For DWPF Sludge Batch 7B (Macrobatch 9)

Description: The Waste Acceptance Product Specifications (WAPS) 1.2 require that “The Producer shall report the inventory of radionuclides (in Curies) that have half-lives longer than 10 years and that are, or will be, present in concentrations greater than 0.05 percent of the total inventory for each waste type indexed to the years 2015 and 3115”. As part of the strategy to comply with WAPS 1.2, the Defense Waste Processing Facility (DWPF) will report for each waste type, all radionuclides (with half-lives greater than 10 years) that have concentrations greater than 0.01 percent of the total inventory from time of production through the 1100 year period from 2015 through 3115. The initial listing of radionuclides to be included is based on the design-basis glass as identified in the Waste Form Compliance Plan (WCP) and Waste Form Qualification Report (WQR). However, it is required that this list be expanded if other radionuclides with half-lives greater than 10 years are identified that may meet the greater than 0.01% criterion for Curie content. Specification 1.6 of the WAPS, International Atomic Energy Agency (IAEA) Safeguards Reporting for High Level Waste (HLW), requires that the ratio by weights of the following uranium and plutonium isotopes be reported: U-233, U-234, U-235, U-236, U-238, Pu-238, Pu-239, Pu-240, Pu-241, and Pu-242. Therefore, the complete set of reportable radionuclides must also include this set of U and Pu isotopes. The DWPF is receiving radioactive sludge slurry from HLW Tank 40. The radioactive sludge slurry in Tank 40 is a blend of the heel from Sludge Batch 7a (SB7a) and Sludge Batch 7b (SB7b) that was transferred to Tank 40 from Tank 51. The blend of sludge in Tank 40 is also referred to as Macrobatch 9 (MB9). This report develops the list of reportable radionuclides and associated activities as a function ...
Date: August 22, 2013
Creator: Crawford, C. L. & DiPrete, D. P.
Partner: UNT Libraries Government Documents Department

DETERMINATION OF REPORTABLE RADIONUCLIDES FOR DWPF SLUDGE BATCH 5 (MACROBATCH 6)

Description: The Waste Acceptance Product Specifications (WAPS) 1.2 require that ''The Producer shall report the inventory of radionuclides (in Curies) that have half-lives longer than 10 years and that are, or will be, present in concentrations greater than 0.05 percent of the total inventory for each waste type indexed to the years 2015 and 3115''. As part of the strategy to comply with WAPS 1.2, the Defense Waste Processing Facility (DWPF) will report for each waste type, all radionuclides (with half-lives greater than 10 years) that have concentrations greater than 0.01 percent of the total inventory from time of production through the 1100 year period from 2015 through 3115. The initial listing of radionuclides to be included is based on the design-basis glass as identified in the Waste Form Compliance Plan (WCP) and Waste Form Qualification Report (WQR). However, it is required that this list be expanded if other radionuclides with half-lives greater than 10 years are identified that may meet the greater than 0.01% criterion for Curie content. Specification 1.6 of the WAPS, International Atomic Energy Agency (IAEA) Safeguards Reporting for High Level Waste (HLW), requires that the ratio by weights of the following uranium and plutonium isotopes be reported: U-233, U-234, U-235, U-236, U-238, Pu-238, Pu-239, Pu-240, Pu-241, and Pu-242. Therefore, the complete set of reportable radionuclides must also include this set of U and Pu isotopes. The DWPF is receiving radioactive sludge slurry from HLW Tank 40. The radioactive sludge slurry in Tank 40 is a blend of the heel from Tank 40 (Sludge Batch 4 (SB4)), Sludge Batch 5 (SB5) that was transferred to Tank 40 from Tank 51, and H-Canyon Np transfers completed after the start of processing. The blend of sludge in Tank 40 is also referred to as Macrobatch 6 (MB6). This report develops ...
Date: February 4, 2010
Creator: Bannochie, C.; Bibler, N. & Diprete, D.
Partner: UNT Libraries Government Documents Department

DETERMINATION OF REPORTABLE RADIONUCLIDES FOR DWPF SLUDGE BATCH 6 (MACROBATCH 7)

Description: The Waste Acceptance Product Specifications (WAPS) 1.2 require that 'The Producer shall report the inventory of radionuclides (in Curies) that have half-lives longer than 10 years and that are, or will be, present in concentrations greater than 0.05 percent of the total inventory for each waste type indexed to the years 2015 and 3115'. As part of the strategy to comply with WAPS 1.2, the Defense Waste Processing Facility (DWPF) will report for each waste type, all radionuclides (with half-lives greater than 10 years) that have concentrations greater than 0.01 percent of the total inventory from time of production through the 1100 year period from 2015 through 3115. The initial listing of radionuclides to be included is based on the design-basis glass as identified in the Waste Form Compliance Plan (WCP) and Waste Form Qualification Report (WQR). However, it is required that this list be expanded if other radionuclides with half-lives greater than 10 years are identified that may meet the greater than 0.01% criterion for Curie content. Specification 1.6 of the WAPS, International Atomic Energy Agency (IAEA) Safeguards Reporting for High Level Waste (HLW), requires that the ratio by weights of the following uranium and plutonium isotopes be reported: U-233, U-234, U-235, U-236, U-238, Pu-238, Pu-239, Pu-240, Pu-241, and Pu-242. Therefore, the complete set of reportable radionuclides must also include this set of U and Pu isotopes. The DWPF is receiving radioactive sludge slurry from HLW Tank 40. The radioactive sludge slurry in Tank 40 is a blend of the heel from Sludge Batch 5 (SB5) with H-Canyon Np transfers completed after the start of processing SB5, and Sludge Batch 6 (SB6) that was transferred to Tank 40 from Tank 51. The blend of sludge in Tank 40 is also referred to as Macrobatch 7 (MB7). This report develops ...
Date: June 1, 2011
Creator: Bannochie, C. & Diprete, D.
Partner: UNT Libraries Government Documents Department

CHARACTERIZATION OF THE TANK 18F SAMPLES

Description: The Savannah River National Laboratory (SRNL) was asked by Liquid Waste Operations to characterize Tank 18F closure samples. Tank 18F slurry samples analyzed included the liquid and solid fractions derived from the 'as-received' slurry materials along with the floor scrape bottom Tank 18F wet solids. These samples were taken from Tank 18F in March 2009 and made available to SRNL in the same month. Because of limited amounts of solids observed in Tank 18F samples, the samples from the north quadrants of the tank were combined into one North Tank 18F Hemisphere sample and similarly the south quadrant samples were combined into one South Tank 18F Hemisphere sample. These samples were delivered to the SRNL shielded cell. The Tank 18F samples were analyzed for radiological, chemical and elemental components. Where analytical methods yielded additional contaminants other than those requested by the customer, these results were also reported. The target detection limits for isotopes analyzed were 1E-04 {micro}Ci/g for most radionuclides and customer desired detection values of 1E-05 {micro}Ci/g for I-129, Pa-231, Np-237, and Ra-226. While many of the minimum detection limits, as specified in the technical task request and task technical and quality assurance plans were met for the species characterized for Tank 18F, some were not met due to spectral interferences. In a number of cases, the relatively high levels of radioactive species of the same element or a chemically similar element precluded the ability to measure some isotopes to low levels. SRNL, in conjunction with the plant customer, reviewed all these cases and determined that the impacts were negligible.
Date: December 17, 2009
Creator: Oji, L.; Click, D. & Diprete, D.
Partner: UNT Libraries Government Documents Department

FINAL REPORT FOR TRITIUM WATER MONITOR

Description: The objective of this Plant Directed Research and Demonstration (PDRD) task was to develop a system to safetly analyze tritium in moisture collected from glovebox atmospheres in the Savannah River Site (SRS) Tritium Facility. In order to minimize potential radiation exposures that could occur in handling and diluting high-tritium-content water, SRS sought alternatives to liquid-scintillation counting. The proposed system determines tritium concentrations by measuring Bremsstrahlung radiation induced by low-energy beta interactions in liquid samples. Results show that, after a short counting period (30 seconds), detection limits are three orders of magnitude below the described concentration of tritiated water in the zeolite beds. Additionally, this report covers the analysis of process samples and the investigation of several cell window materials including beryllium, aluminum, and copper. Final tests reveal that alternate window materials and thicknesses can be used to obtain useful results. In particular, a window of stainless steel of moderate thickness (0.3 cm) can be used for counting relatively high levels of tritium.
Date: April 25, 2011
Creator: Sigg, R.; Ferguson, B. & DiPrete, D.
Partner: UNT Libraries Government Documents Department

APPLICATION OF COLUMN EXTRACTION METHOD FOR IMPURITIES ANALYSIS ON HB-LINE PLUTONIUM OXIDE IN SUPPORT OF MOX FEED PRODUCT SPECIFICATIONS

Description: The current mission at H-Canyon involves the dissolution of an Alternate Feedstocks 2 (AFS-2) inventory that contains plutonium metal. Once dissolved, HB-Line is tasked with purifying the plutonium solution via anion exchange, precipitating the Pu as oxalate, and calcining to form plutonium oxide (PuO{sub 2}). The PuO{sub 2} will provide feed product for the Mixed Oxide (MOX) Fuel Fabrication Facility, and the anion exchange raffinate will be transferred to H-Canyon. The results presented in this report document the potential success of the RE resin column extraction application on highly concentrated Pu samples to meet MOX feed product specifications. The original 'Hearts Cut' sample required a 10000x dilution to limit instrument drift on the ICP-MS method. The instrument dilution factors improved to 125x and 250x for the sample raffinate and sample eluent, respectively. As noted in the introduction, the significantly lower dilutions help to drop the total MRL for the analyte. Although the spike recoveries were half of expected in the eluent for several key elements, they were between 94-98% after Nd tracer correction. It is seen that the lower ICD limit requirements for the rare earths are attainable because of less dilution. Especially important is the extremely low Ga limit at 0.12 {mu}g/g Pu; an ICP-MS method is now available to accomplish this task on the sample raffinate. While B and V meet the column A limits, further development is needed to meet the column B limits. Even though V remained on the RE resin column, an analysis method is ready for investigation on the ICP-MS, but it does not mean that V cannot be measured on the ICP-ES at a low dilution to meet the column B limits. Furthermore, this column method can be applicable for ICP-ES as shown in Table 3-2, in that it trims the sample of ...
Date: March 20, 2012
Creator: Jones, M.; Diprete, D. & Wiedenman, B.
Partner: UNT Libraries Government Documents Department

CHARACTERIZATION OF TANK 19F SAMPLES

Description: The Savannah River National Laboratory (SRNL) was asked by Liquid Waste Operations to characterize Tank 19F closure samples. Tank 19F slurry samples analyzed included the liquid and solid fractions derived from the slurry materials along with the floor scrape bottom Tank 19F wet solids. These samples were taken from Tank 19F in April 2009 and made available to SRNL in the same month. Because of limited amounts of solids observed in Tank 19F samples, the samples from the north quadrants of the tank were combined into one Tank 19F North Hemisphere sample and similarly the south quadrant samples were combined into one Tank 19F South Hemisphere sample. These samples were delivered to the SRNL shielded cell. The Tank 19F samples were analyzed for radiological, chemical and elemental components. Where analytical methods yielded additional contaminants other than those requested by the customer, these results were also reported. The target detection limits for isotopes analyzed were based on detection values of 1E-04 {micro}Ci/g for most radionuclides and customer desired detection values of 1E-05 {micro}Ci/g for I-129, Pa-231, Np-237, and Ra-226. While many of the target detection limits, as specified in the technical task request and task technical and quality assurance plans were met for the species characterized for Tank 19F, some were not met. In a number of cases, the relatively high levels of radioactive species of the same element or a chemically similar element precluded the ability to measure some isotopes to low levels. SRNL, in conjunction with the plant customer, reviewed all these cases and determined that the impacts were negligible.
Date: December 17, 2009
Creator: Oji, L.; Diprete, D. & Click, D.
Partner: UNT Libraries Government Documents Department

CHARACTERIZATION OF TANK 5F VERTICAL COOLING COIL LEACHATES FOR SELECT RADIONUCLIDES 2011

Description: Two twenty-four inch samples of vertical sections of the cooling coils from Tank 5F, taken from Riser 1, were made available to SRNL by SRR for leaching and characterization of the leachates for select radionuclide trapped in the corrosion layer on the exterior of the cooling coils. One piece of cooling coil sample was obtained from a section of a vertical cooling coil located above the 45-inch elevation from the tank floor and the other also from a vertical section of a cooling coil located below the 45-inch elevation from the tank floor of Tank 5F. Analysis results from both cooling coils show that the predominant radionuclides contributing to the activity in both coils are strontium-90 and cesium-137. The activities for strontium-90 and cesium-137 in the Tank 5F vertical cooling coil located above the 45-inch elevation of the tank and designated as sample 5-R1-A45 averaged 1.34E-02 {+-} 1.12E-03 and 7.27E-04 {+-} 4.46E-05 Ci/ft{sup 2}, respectively, while the activities for the vertical cooling coil located below the 45-inch elevation of the tank and designated as sample 5-R1-B45 averaged 8.93E-03 {+-} 8.25E-04 for Sr-90 and 8.10E-04 {+-} 6.36E-05 Ci/ft{sup 2} for Cs-137. Other significant activity contributing radionuclides are americium-241 and europium-154/155. With the exception of the analysis result for Pu-241 in the 5-R1-A45 cooling coils samples, the target detection limits for the other radionuclides were met in both cooling coil samples. The detection limits for Pu-241 analyses result in coil sample 5-R1-A45 were not met consistently because of possible background changes during counting.
Date: August 17, 2001
Creator: Oji, L. & Diprete, D.
Partner: UNT Libraries Government Documents Department

REMOTE ANALYSIS OF HIGH-TRITIUM-CONTENT WATER

Description: Systems to safely analyze for tritium in moisture collected from glovebox atmospheres are being developed for use at Savannah River Site (SRS) tritium facilities. Analysis results will guide whether the material contains sufficient tritium for economical recovery, or whether it should be stabilized for disposal as waste. In order to minimize potential radiation exposures that could occur in handling and diluting high-tritium-content water, SRS sought alternatives to the process laboratory's routine analysis by liquid-scintillation counting. The newer systems determine tritium concentrations by measuring bremsstrahlung radiation induced by low-energy beta interactions. One of the systems determines tritium activity in liquid streams, the other determines tritium activity in water vapor. Topics discussed include counting results obtained by modeling and laboratory testing and corrections that are made for low-energy photon attenuation.
Date: August 7, 2007
Creator: Diprete, D; Raymond Sigg, R; Leah Arrigo, L & Donald Pak, D
Partner: UNT Libraries Government Documents Department

NEUTRON ACTIVATION ANALYSIS APPLICATIONS AT THE SAVANNAH RIVER SITE USING AN ISOTOPIC NEUTRON SOURCE

Description: NAA using {sup 252}Cf is used to address important areas of applied interest at SRS. Sensitivity needs for many of the applications are not severe; analyses are accomplished using a 21 mg {sup 252}Cf NAA facility. Because NAA allows analysis of bulk samples, it offers strong advantages for samples in difficult-to-digest matrices when its sensitivity is sufficient. Following radiochemical separation with stable carrier addition, chemical yields for a number methods are determined by neutron activation of the stable carrier. In some of the cases where no suitable stable carriers exist, the source has been used to generate radioactive tracers to yield separations.
Date: August 14, 2006
Creator: Diprete, D; C Diprete, C & Raymond Sigg, R
Partner: UNT Libraries Government Documents Department

Analysis Of The Tank 5F Final Characterization Samples-2011

Description: The Savannah River National Laboratory (SRNL) was requested by SRR to provide sample preparation and analysis of the Tank 5F final characterization samples to determine the residual tank inventory prior to grouting. Two types of samples were collected and delivered to SRNL: floor samples across the tank and subsurface samples from mounds near risers 1 and 5 of Tank 5F. These samples were taken from Tank 5F between January and March 2011. These samples from individual locations in the tank (nine floor samples and six mound Tank 5F samples) were each homogenized and combined in a given proportion into 3 distinct composite samples to mimic the average composition in the entire tank. These Tank 5F composite samples were analyzed for radiological, chemical and elemental components. Additional measurements performed on the Tank 5F composite samples include bulk density and water leaching of the solids to account for water soluble species. With analyses for certain challenging radionuclides as the exception, all composite Tank 5F samples were analyzed and reported in triplicate. The target detection limits for isotopes analyzed were based on customer desired detection limits as specified in the technical task request documents. SRNL developed new methodologies to meet these target detection limits and provide data for the extensive suite of components. While many of the target detection limits were met for the species characterized for Tank 5F, as specified in the technical task request, some were not met. In a few cases, the relatively high levels of radioactive species of the same element or a chemically similar element precluded the ability to measure some isotopes to low levels. The Technical Task Request allows that while the analyses of these isotopes is needed, meeting the detection limits for these isotopes is a lower priority than meeting detection limits for the other specified ...
Date: September 27, 2012
Creator: Oji, L. N.; Diprete, D.; Coleman, C. J. & Hay, M. S.
Partner: UNT Libraries Government Documents Department

A Compton-Vetoed Germanium Detector with Increased Sensitivity at Low Energies

Description: The difficulty to directly detect plutonium in spent nuclear fuel due to the high Compton background of the fission products motivates the design of a Gamma detector with improved sensitivity at low energies. We have built such a detector by operating a thin high-purity Ge detector with a large scintillator Compton veto directly behind it. The Ge detector is thin to absorb just the low-energy Pu radiation of interest while minimizing Compton scattering of high energy radiation from the fission products. The subsequent scintillator is large so that forward scattered photons from the Ge detector interact in it at least once to provide an anti-coincidence veto for the Ge detector. For highest sensitivity, additional material in the line-of-sight is minimized, the radioactive sample is kept thin, and its radiation is collimated. We will discuss the instrument design, and demonstrate the feasibility of the approach with a prototype that employs two large CsI scintillator vetoes. Initial spectra of a thin Cs-137 calibration source show a background suppression of a factor of {approx}2.5 at {approx}100 keV, limited by an unexpectedly thick 4 mm dead layer in the Ge detector.
Date: March 29, 2012
Creator: Friedrich, S; Bates, C; Drury, O B; Burks, M & DiPrete, D
Partner: UNT Libraries Government Documents Department

Analysis of the Tank 5F Feed and Bleed Residual Solids

Description: Savannah River Remediation (SRR) is preparing Tank 5F for closure. As part of Tank 5F Closure Mechanical Cleaning, SRR conducted a 'Feed and Bleed' process in Tank 5F. Following this 'Feed and Bleed' Mechanical Cleaning in Tank 5F, SRR collected two tank heel samples (referred to as sample 1 and sample 2) under Riser 5 to determine the composition of the material remaining in the tanks. This document describes sample analysis results. The conclusions from this analysis follow. (1) The anions measured all had a concentration less than 250 mg/kg, except for oxalate, which had a concentration of 2100-2400 mg/kg. (2) The measured cations with the highest concentration were iron (432,000-519,000 mg/kg), nickel (54,600-69,300 mg/kg), and manganese (35,200-42,100 mg/kg). All other cations measured less than 13,000 mg/kg. (3) The radionuclides present in the highest concentration are {sup 90}Sr (3.0 x 10{sup 10} dpm/g), {sup 137}Cs (6.8 x 10{sup 8} dpm/g), and {sup 241}Am (1.4 x 10{sup 8} - 1.8 x 10{sup 8} dpm/g). (4) The particle size analysis shows a large fraction of particles greater than 100 {micro}.
Date: July 7, 2011
Creator: Poirier, M.; Diprete, D.: Coleman, C. & Washington, A.
Partner: UNT Libraries Government Documents Department

DETERMINATION OF REPORTABLE RADIONUCLIDES FOR DWPF SLUDGE BATCH 4 MACROBATCH 5

Description: The Waste Acceptance Product Specifications (WAPS)1 1.2 require that 'The Producer shall report the inventory of radionuclides (in Curies) that have half-lives longer than 10 years and that are, or will be, present in concentrations greater than 0.05 percent of the total inventory for each waste type indexed to the years 2015 and 3115'. As part of the strategy to meet WAPS 1.2, the Defense Waste Processing Facility (DWPF) will report for each waste type, all radionuclides (with half-lives greater than 10 years) that have concentrations greater than 0.01 percent of the total inventory from time of production through the 1100 year period from 2015 through 3115. The initial listing of radionuclides to be included is based on the design-basis glass as identified in the Waste Form Compliance Plan (WCP)2 and Waste Form Qualification Report (WQR)3. However, it is required that this list be expanded if other radionuclides with half-lives greater than 10 years are identified that may meet the greater than 0.01% criterion for Curie content. Specification 1.6 of the WAPS, International Atomic Energy Agency (IAEA) Safeguards Reporting for High Level Waste (HLW), requires that the ratio by weights of the following uranium and plutonium isotopes be reported: U-233, U-234, U-235, U-236, U-238, Pu-238, Pu-239, Pu-240, Pu-241, and Pu-242. Therefore, the complete set of reportable radionuclides must also include this set of U and Pu isotopes. The DWPF is receiving radioactive sludge slurry from HLW Tank 40. The radioactive sludge slurry in Tank 40 is a blend of the previous contents of Tank 40 (Sludge Batch 3) and the sludge that was transferred to Tank 40 from Tank 51. The blend of sludge from Tank 51 and Tank 40 defines Sludge Batch 4 (also referred to as Macrobatch 5 (MB5)). This report develops the list of reportable radionuclides and ...
Date: May 30, 2008
Creator: Bannochie, C; Ned Bibler, N & David Diprete, D
Partner: UNT Libraries Government Documents Department

DEVELOPMENT OF ANALYTICAL METHODS FOR DETERMINING SUPPRESSOR CONCENTRATION IN THE MCU NEXT GENERATION SOLVENT (NGS)

Description: Savannah River National Laboratory (SRNL) was tasked with identifying and developing at least one, but preferably two methods for quantifying the suppressor in the Next Generation Solvent (NGS) system. The suppressor is a guanidine derivative, N,N',N"-tris(3,7-dimethyloctyl)guanidine (TiDG). A list of 10 possible methods was generated, and screening experiments were performed for 8 of the 10 methods. After completion of the screening experiments, the non-aqueous acid-base titration was determined to be the most promising, and was selected for further development as the primary method. {sup 1}H NMR also showed promising results from the screening experiments, and this method was selected for further development as the secondary method. Other methods, including {sup 36}Cl radiocounting and ion chromatography, also showed promise; however, due to the similarity to the primary method (titration) and the inability to differentiate between TiDG and TOA (tri-n-ocytlamine) in the blended solvent, {sup 1}H NMR was selected over these methods. Analysis of radioactive samples obtained from real waste ESS (extraction, scrub, strip) testing using the titration method showed good results. Based on these results, the titration method was selected as the method of choice for TiDG measurement. {sup 1}H NMR has been selected as the secondary (back-up) method, and additional work is planned to further develop this method and to verify the method using radioactive samples. Procedures for analyzing radioactive samples of both pure NGS and blended solvent were developed and issued for the both methods.
Date: July 31, 2013
Creator: Taylor-Pashow, K.; Fondeur, F.; White, T.; Diprete, D. & Milliken, C.
Partner: UNT Libraries Government Documents Department

CHARACTERIZATION OF TANK 50 SLURRY FOR SALTSTONE WASTE ACCEPTANCE CRITERIA, APRIL 2007 SAMPLES

Description: This report summarizes the results from the characterization of the second quarter April 2007 sampling of Tank 50H for the Saltstone Waste Acceptance Criteria (WAC). Six one liter samples were taken in polyethylene bottles to analyze for the WAC contaminants and a 200 mL sample was taken in a steel container for analysis of volatile organic compounds. The information from this characterization will be given to Waste Solidification Engineering personnel to qualify the transfer of aqueous waste to the Saltstone Facility. The following conclusions are drawn from the analytical results found in this report: (1) All six of the one liter samples taken in April 2007 from the mixed slurry in Tank 50 have the same compositions within the experimental uncertainty of the analyses. (2) Of the ninety-one process, chemical, and radioactive WAC target or limit contaminants listed in Revision 7 of the 'Waste Acceptance Criteria for Aqueous Waste sent to the Z-Area Saltstone Production Facility', eighty-nine had concentrations that were unequivocally less than the WAC limit or target. (3) The two contaminants whose concentrations could not be shown to be less than their WAC targets were methanol and radioactive Nb-93m. Currently the AD Section of SRNL does not have a method for measuring methanol in caustic solutions. For Nb-93m the results are ambiguous due to possible interferences in the ICP-MS analysis from Zr-93 or Mo-93. (4) Of the six additional chemical and radioactive contaminants requested in the TTR for Saltstone qualification, five were measured or calculated. These were Sb, Be, Tl, along with total beta and gamma. The AD Section does not have a method to measure the 6th contaminant which was the cyanide ion.
Date: December 7, 2007
Creator: Zeigler, K; Ned Bibler, N & David Diprete, D
Partner: UNT Libraries Government Documents Department

UNIQUE RADIOANALYTICAL PROTOCOLS FOR CHARACTERIZATION AND VERIFICATION DURING DECONTAMINATION AND DECOMMISSIONING

Description: In order to successfully decontaminate, deactivate and decommission surplus Department of Energy (DOE) facilities throughout the Savannah River Site (SRS), a variety of characterizations must be completed to sufficiently identify and quantify potential contaminants of concern. The ultimate goal is to rapidly and efficiently characterize, decontaminate (if necessary), and verify that the remnants meet specified limits established by either an industrial worker model or a groundwater model. To meet this end, the Savannah River National Laboratory (SRNL) developed a series of radioanalytical strategies and methodologies which can be used to characterize targeted facilities and prove that decontamination has been sufficient. To our knowledge, this is the first application of this novel methodology within the DOE complex. This methodology has been successfully utilized with nearly 1000 samples from over a dozen facilities. The application of this approach to just a single facility shortened the schedule by 30 days and resulted in non-labor dollar savings of over $60K. Cost savings for a second facility was determined to be $375K. Based on the success of this methodology at SRS, this approach will be valuable to other nuclear facilities in the USA and abroad involved with the decontamination and decommissioning process.
Date: January 5, 2007
Creator: Diprete, C; David Diprete, D & Wooten Simpson, W
Partner: UNT Libraries Government Documents Department

SLUDGE BATCH 5 ACCEPTANCE EVALUATION RADIONUCLIDE CONCENTRATIONS IN TANK 51 SB5 QUALIFICATION SAMPLE PREPARED AT SRNL

Description: Presented in this report are radionuclide concentrations required as part of the program of qualifying Sludge Batch Five (SB5) for processing in the Defense Waste Processing Facility (DWPF). Part of this SB5 material is currently in Tank 51 being 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 to complete the formation of SB5. The sludge slurry in Tank 40 has already been qualified for DWPF and is currently being processed as SB4. The radionuclide concentrations were measured or estimated in the Tank 51 SB5 Qualification Sample prepared at Savannah River National Laboratory (SRNL). This sample was prepared from the three liter sample of Tank 51 sludge slurry taken on March 21, 2008. The sample was delivered to SRNL where it was initially characterized in the Shielded Cells. Under direction of the Liquid Waste Organization it was then modified by five washes, six decants, an addition of Pu/Be from Canyon Tank 16.4, and an addition of NaNO2. 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 Ta Determining the radionuclide concentrations in this Tank 51 SB5 Qualification Sample is part of the work requested in Technical Task Request (TTR) No. HLW-DWPF-TTR-2008-0010. The work with this qualification sample is covered by a Task Technical and Quality Assurance Plan and an Analytical Study Plan. The radionuclides included in this report are needed for the DWPF Radiological Program Evaluation, the DWPF Waste Acceptance Criteria (TSR/WAC) Evaluation, and the DWPF Solid Waste Characterization Program (TTR Task 2). Radionuclides required to meet the Waste Acceptance Product Specifications (TTR Task 5) will be measured at ...
Date: July 28, 2008
Creator: Bannochie, C; Ned Bibler, N & David Diprete, D
Partner: UNT Libraries Government Documents Department

RAPID MEASUREMENTS OF NEPTUNIUM OXIDATION STATES USING CHROMATOGRAPHIC RESINS

Description: The Savannah River Site's (SRS) H-Canyon facility uses ceric ammonium nitrate (CAN) to separate impure neptunium (Np) from a high sulfate feed stream. The material is processed using a two-pass solvent extraction purification which relies on CAN to oxidize neptunium to Np(VI) during the first pass prior to extraction. Spectrophotometric oxidation-state analyses normally used to validate successful oxidation to Np(VI) prior to extraction were compromised by this feed stream matrix. Therefore, a rapid chromatographic method to validate successful Np oxidation was developed using Eichrom Industries TRU and TEVA{reg_sign} resins. The method was validated and subsequently transferred to existing operations in the process analytical laboratories.
Date: March 24, 2009
Creator: Diprete, D; C Diprete, C; Mira Malek, M & Eddie Kyser, E
Partner: UNT Libraries Government Documents Department

MEASUREMENT AND CALCULATION OF RADIONUCLIDE ACTIVITIES IN SAVANNAH RIVER SITE HIGH LEVEL WASTE SLUDGE FOR ACCEPTANCE OF DEFENSE WASTE PROCESSING FACILITY GLASS IN A FEDERAL REPOSITORY

Description: This paper describes the results of the analyses of High Level Waste (HLW) sludge slurry samples and of the calculations necessary to decay the radionuclides to meet the reporting requirement in the Waste Acceptance Product Specifications (WAPS) [1]. The concentrations of 45 radionuclides were measured. The results of these analyses provide input for radioactive decay calculations used to project the radionuclide inventory at the specified index years, 2015 and 3115. This information is necessary to complete the Production Records at Savannah River Site's Defense Waste Processing Facility (DWPF) so that the final glass product resulting from Macrobatch 5 (MB5) can eventually be submitted to a Federal Repository. Five of the necessary input radionuclides for the decay calculations could not be measured directly due to their low concentrations and/or analytical interferences. These isotopes are Nb-93m, Pd-107, Cd-113m, Cs-135, and Cm-248. Methods for calculating these species from concentrations of appropriate other radionuclides will be discussed. Also the average age of the MB5 HLW had to be calculated from decay of Sr-90 in order to predict the initial concentration of Nb-93m. As a result of the measurements and calculations, thirty-one WAPS reportable radioactive isotopes were identified for MB5. The total activity of MB5 sludge solids will decrease from 1.6E+04 {micro}Ci (1 {micro}Ci = 3.7E+04 Bq) per gram of total solids in 2008 to 2.3E+01 {micro}Ci per gram of total solids in 3115, a decrease of approximately 700 fold. Finally, evidence will be given for the low observed concentrations of the radionuclides Tc-99, I-129, and Sm-151 in the HLW sludges. These radionuclides were reduced in the MB5 sludge slurry to a fraction of their expected production levels due to SRS processing conditions.
Date: December 31, 2008
Creator: Bannochie, C; David Diprete, D & Ned Bibler, N
Partner: UNT Libraries Government Documents Department

ANALYSIS OF THE TANK 5F FINAL CHARACTERIZATION SAMPLES-2011

Description: The Savannah River National Laboratory (SRNL) was requested by SRR to provide sample preparation and analysis of the Tank 5F final characterization samples to determine the residual tank inventory prior to grouting. Two types of samples were collected and delivered to SRNL: floor samples across the tank and subsurface samples from mounds near risers 1 and 5 of Tank 5F. These samples were taken from Tank 5F between January and March 2011. These samples from individual locations in the tank (nine floor samples and six mound Tank 5F samples) were each homogenized and combined in a given proportion into 3 distinct composite samples to mimic the average composition in the entire tank. These Tank 5F composite samples were analyzed for radiological, chemical and elemental components. Additional measurements performed on the Tank 5F composite samples include bulk density and water leaching of the solids to account for water soluble species. With analyses for certain challenging radionuclides as the exception, all composite Tank 5F samples were analyzed and reported in triplicate. The target detection limits for isotopes analyzed were based on customer desired detection limits as specified in the technical task request documents. SRNL developed new methodologies to meet these target detection limits and provide data for the extensive suite of components. While many of the target detection limits were met for the species characterized for Tank 5F, as specified in the technical task request, some were not met. In a few cases, the relatively high levels of radioactive species of the same element or a chemically similar element precluded the ability to measure some isotopes to low levels. The Technical Task Request allows that while the analyses of these isotopes is needed, meeting the detection limits for these isotopes is a lower priority than meeting detection limits for the other specified ...
Date: August 3, 2012
Creator: Oji, L.; Diprete, D.; Coleman, C. & Hay, M.
Partner: UNT Libraries Government Documents Department