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Improved laboratory assays of Pu and U for SRP purification and finishing processes

Description: Significant improvements have been made in routine assay techniques for uranium and plutonium as part of an effort to improve accountability at the Savannah River Plant (SRP). Emphasis was placed on input/output accountability points and key physical inventory tanks associated with purification and finishing processes. Improvements were made in existing assay methods; new methods were implemented; and the application of these methods was greatly expanded. Prior to assays, samples were validated via density measurements. Digital density meters precise to four, five, and six decimal places were used to meet specific requirements. Improved plutonium assay techniques are now in routine use: controlled-potential coulometry, ion-exchange coulometry, and Pu(III) diode-array spectrophotometry. A new state-of-the-art coulometer was fabricated and used to ensure maximum accuracy in verifying standards and in measuring plutonium in product streams. The diode-array spectrophotometer for Pu(III) measurements was modified with fiber optics to facilitate remote measurements; rapid, precise measurements made the technique ideally suited for high-throughput assays. For uranium assays, the isotope-dilution mass spectrometric (IDMS) method was converted to a gravimetric basis. The IDMS method and the existing Davies-Gray titration (gravimetric basis) have met accountability requirements for uranium. More recently, a Pu(VI) diode-array spectrophotometric method was used on a test basis to measure plutonium in shielded-cell input accountability samples. In addition, tests to measure uranium via diode-array spectrophotometry were initiated. This rapid, precise method will replace IDMS for certain key sample points.
Date: January 1, 1986
Creator: Holland, M K & Dorsett, R S
Partner: UNT Libraries Government Documents Department

Applicability of International and DOE Target Values to ALD Destructive Measurement Applications

Description: International Target values and target value applicability are a function of the nuclear material processing campaign or application for which the accountability measurement method is being applied. Safeguarding significant quantities of nuclear-grade materials requires that accountability measurements be as accurate, precise, and representative as practically possible. In general, the ITV provides a benchmark for determining generic acceptability of the performance of the various accountability measurement methods, since it represents a performance level that is accepted as highly reliable. There are cases where it is acceptable to select alternative accountability methods not specifically referenced by the ITV, or to use the recognized measurement method, even though the uncertainties are greater than the target values.
Date: December 19, 2002
Creator: Holland, M.K.
Partner: UNT Libraries Government Documents Department

MASS MEASUREMENT UNCERTAINTY FOR PLUTONIUM ALIQUOTS ASSAYED BY CONTROLLED-POTENTIAL COULOMETRY

Description: Minimizing plutonium measurement uncertainty is essential to nuclear material control and international safeguards. In 2005, the International Organization for Standardization (ISO) published ISO 12183 'Controlled-potential coulometric assay of plutonium', 2nd edition. ISO 12183:2005 recommends a target of {+-}0.01% for the mass of original sample in the aliquot because it is a critical assay variable. Mass measurements in radiological containment were evaluated and uncertainties estimated. The uncertainty estimate for the mass measurement also includes uncertainty in correcting for buoyancy effects from air acting as a fluid and from decreased pressure of heated air from the specific heat of the plutonium isotopes.
Date: March 18, 2009
Creator: Holland, M. & Cordaro, J.
Partner: UNT Libraries Government Documents Department

EVALUATING EFFECTS OF NEPTUNIUM ON THE SRS METHOD FOR CONTROLLED POTENTIAL COULOMETRIC ASSAY OF PLUTONIUM IN SULFURIC ACID SUPPORTING ELECTROLYTE

Description: A study of the impact of neptunium on the coulometric assay of plutonium in dilute sulfuric acid was performed. Weight aliquots of plutonium standard solutions were spiked with purified neptunium solution to evaluate plutonium measurement performance for aliquots with Pu:Np ratios of 50:1, 30:1, 20:1, 15:1, and 10:1. Weight aliquots of the pure plutonium standard solution were measured as controls. Routine plutonium instrument control standards were also measured. The presence of neptunium in plutonium aliquots significantly increases the random uncertainty associated with the plutonium coulometric measurement performed in accordance with ISO12183:2005.7 However, the presence of neptunium does not appear to degrade electrode performance and conditioning as aliquots of pure plutonium that were interspersed during the measurement of the mixed Pu:Np aliquots continued to achieve the historical short-term random uncertainty for the method. Lack of adequate control of the neptunium oxidation state is suspected to be the primary cause of the elevated measurement uncertainty and will be pursued in a future study.
Date: May 9, 2008
Creator: Holland, M & Sheldon Nichols, S
Partner: UNT Libraries Government Documents Department

Implementation of an Enhanced Measurement Control Program for handling nuclear safety samples at WSRC

Description: In the separation and purification of nuclear material, nuclear criticality safety (NCS) is of primary concern. The primary nuclear criticality safety controls utilized by the Savannah River Site (SRS) Separations Facilities involve administrative and process equipment controls. Additional assurance of NCS is obtained by identifying key process hold points where sampling is used to independently verify the effectiveness of production control. Nuclear safety measurements of samples from these key process locations provide a high degree of assurance that processing conditions are within administrative and procedural nuclear safety controls. An enhanced procedure management system aimed at making improvements in the quality, safety, and conduct of operation was implemented for Nuclear Safety Sample (NSS) receipt, analysis, and reporting. All procedures with nuclear safety implications were reviewed for accuracy and adequate detail to perform the analytical measurements safely, efficiently, and with the utmost quality. Laboratory personnel worked in a Deliberate Operating'' mode (a systematic process requiring continuous expert oversight during all phases of training, testing, and implementation) to initiate the upgrades. Thus, the effort to revise and review nuclear safety sample procedures involved a team comprised of a supervisor, chemist, and two technicians for each procedure. Each NSS procedure was upgraded to a Use Every Time'' (UET) procedure with sign-off steps to ensure compliance with each step for every nuclear safety sample analyzed. The upgrade program met and exceeded both the long and short term customer needs by improving measurement reliability, providing objective evidence of rigid adherence to program principles and requirements, and enhancing the system for independent verification of representative sampling from designated NCS points.
Date: January 1, 1991
Creator: Boler-Melton, C. & Holland, M.K.
Partner: UNT Libraries Government Documents Department

Implementation of an Enhanced Measurement Control Program for handling nuclear safety samples at WSRC

Description: In the separation and purification of nuclear material, nuclear criticality safety (NCS) is of primary concern. The primary nuclear criticality safety controls utilized by the Savannah River Site (SRS) Separations Facilities involve administrative and process equipment controls. Additional assurance of NCS is obtained by identifying key process hold points where sampling is used to independently verify the effectiveness of production control. Nuclear safety measurements of samples from these key process locations provide a high degree of assurance that processing conditions are within administrative and procedural nuclear safety controls. An enhanced procedure management system aimed at making improvements in the quality, safety, and conduct of operation was implemented for Nuclear Safety Sample (NSS) receipt, analysis, and reporting. All procedures with nuclear safety implications were reviewed for accuracy and adequate detail to perform the analytical measurements safely, efficiently, and with the utmost quality. Laboratory personnel worked in a ``Deliberate Operating`` mode (a systematic process requiring continuous expert oversight during all phases of training, testing, and implementation) to initiate the upgrades. Thus, the effort to revise and review nuclear safety sample procedures involved a team comprised of a supervisor, chemist, and two technicians for each procedure. Each NSS procedure was upgraded to a ``Use Every Time`` (UET) procedure with sign-off steps to ensure compliance with each step for every nuclear safety sample analyzed. The upgrade program met and exceeded both the long and short term customer needs by improving measurement reliability, providing objective evidence of rigid adherence to program principles and requirements, and enhancing the system for independent verification of representative sampling from designated NCS points.
Date: December 31, 1991
Creator: Boler-Melton, C. & Holland, M. K.
Partner: UNT Libraries Government Documents Department

ELECTRONICS UPGRADE TO THE SAVANNAH RIVER NATIONAL LABORATORY COULOMETER FOR PLUTONIUM AND NEPTUNIUM ASSAY

Description: The Savannah River Site (SRS) has the analytical measurement capability to perform high-precision plutonium concentration measurements by controlled-potential coulometry. State-of-the-art controlled-potential coulometers were designed and fabricated by the Savannah River National Laboratory and installed in the Analytical Laboratories process control laboratory. The Analytical Laboratories uses coulometry for routine accountability measurements of and for verification of standard preparations used to calibrate other plutonium measurement systems routinely applied to process control, nuclear safety, and other accountability applications. The SRNL Coulometer has a demonstrated measurement reliability of {approx}0.05% for 10 mg samples. The system has also been applied to the characterization of neptunium standard solutions with a comparable reliability. The SRNL coulometer features: a patented current integration system; continuous electrical calibration versus Faraday's Constants and Ohm's Law; the control-potential adjustment technique for enhanced application of the Nernst Equation; a wide operating room temperature range; and a fully automated instrument control and data acquisition capability. Systems have been supplied to the International Atomic Energy Agency (IAEA), Russia, Japanese Atomic Energy Agency (JAEA) and the New Brunswick Laboratory (NBL). The most recent vintage of electronics was based on early 1990's integrated circuits. Many of the components are no longer available. At the request of the IAEA and the Department of State, SRNL has completed an electronics upgrade of their controlled-potential coulometer design. Three systems have built with the new design, one for the IAEA which was installed at SAL in May 2011, one system for Los Alamos National Laboratory, (LANL) and one for the SRS Analytical Laboratory. The LANL and SRS systems are undergoing startup testing with installation scheduled for this summer.
Date: July 8, 2011
Creator: Cordaro, J.; Holland, M.; Reeves, G.; Nichols, S. & Kruzner, A.
Partner: UNT Libraries Government Documents Department

Doublet III beamline: as-built

Description: In order to fully exploit Doublet III capabilities and to study new plasma physics regimes, a Neutral Beam Injector System has been constructed. Initially, a two beamline system will supply 7 MW of heat to the plasma. The system is currently being expanded to inject approx. 20 MW of power (6 beamlines). Each beamline is equipped with two Lawrence Berkeley Laboratory type rectangular ion sources with 10 cm x 40 cm extraction grids. These sources will accelerate hydrogen ions to 80 keV, with extracted beam currents in excess of 80 A per source expected. The first completed source is currently being tested and conditioned on the High Voltage Test Stand at Lawrence Livermore Laboratory. This paper pictorially reviews the as-built Doublet III neutral beamline with emphasis on component relation and configuration relative to spatial and source imposed design constraints.
Date: March 1, 1980
Creator: Harder, C.R.; Holland, M.M.; Parker, J.W.; Gunn, J. & Resnick, L.
Partner: UNT Libraries Government Documents Department

Automated Controlled-Potential Coulometer for the IAEA

Description: An automated controlled-potential coulometer has been developed at the Savannah River Site (SRS) for the determination of plutonium for use at the International Atomic Energy Agency`s (IAEA) Safeguards Analytical Laboratory in Siebersdorf, Austria. The system is functionally the same as earlier systems built for use at the Savannah River Site`s Analytical Laboratory. All electronic circuits and printed circuits boards have been upgraded with state-of-the-art components. A higher amperage potentiostat with improved control stability has been developed. The system achieves electronic calibration accuracy and linearity of better than 0.01 percent, with a precision and accuracy better than 0.1 percent has been demonstrated. This coulometer features electrical calibration of the integration system, electrolysis current background corrections, and control-potential adjustment capabilities. These capabilities allow application of the system to plutonium measurements without chemical standards, achieving traceability to the international measurement system through electrical standards and Faraday`s constant. the chemist is provided with the capability to perform measurements without depending upon chemical standards, which is a significant advantage for applications such as characterization of primary and secondary standards. Additional benefits include reducing operating cost to procure, prepare and measure calibration standards and the corresponding decrease in radioactive waste generation. The design and documentation of the automated instrument are provided herein. Each individual module`s operation, wiring, layout, and alignment are described. Interconnection of the modules and system calibration are discussed. A complete set of prints and a list of associated parts are included.
Date: January 29, 1998
Creator: Cordaro, J.V.; Holland, M.K. & Fields, T.
Partner: UNT Libraries Government Documents Department

EXTENDING THE USEFUL LIFE OF OLDER MASS SPECTROMETERS

Description: Thermal ionization and gas mass spectrometers are widely used across the Department of Energy (DOE) Complex and contractor laboratories. These instruments support critical missions, where high reliability and low measurement uncertainty are essential. A growing number of these mass spectrometers are significantly older than their original design life. The reality is that manufacturers have declared many of the instrument models obsolete, with direct replacement parts and service no longer available. Some of these obsolete models do not have a next generation, commercially available replacement. Today's budget conscious economy demands for the use of creative funds management. Therefore, the ability to refurbish (or upgrade) these valuable analytical tools and extending their useful life is a cost effective option. The Savannah River Site (SRS) has the proven expertise to breathe new life into older mass spectrometers, at a significant cost savings compared to the purchase and installation of new instruments. A twenty-seven year old Finnigan MAT-261{trademark} Thermal Ionization Mass Spectrometer (TIMS), located at the SRS F/H Area Production Support Laboratory, has been successfully refurbished. Engineers from the Savannah River National Laboratory (SRNL) fabricated and installed the new electronics. These engineers also provide continued instrument maintenance services. With electronic component drawings being DOE Property, other DOE Complex laboratories have the option to extend the life of their aged Mass Spectrometers.
Date: June 17, 2010
Creator: Johnson, S.; Cordaro, J.; Holland, M. & Jones, V.
Partner: UNT Libraries Government Documents Department

PERFORMANCE OF THE SAVANNAH RIVER SITE COULOMETER FOR NEPTUNIUM PROCESSACCOUNTABILITY AND NEPTUNIUM OXIDE PRODUCT CHARACTERIZATION

Description: The Savannah River Site's (SRS) H-Area B-Line (HB-Line) nuclear facility is processing neptunium solutions for stabilization as an oxide. The oxide will eventually be reprocessed and fabricated into target material and the 237Np irradiated to produce {sup 238}Pu in support of National Aeronautics and Space Administration space program missions. As part of nuclear materials accountability, solution concentrations were measured using a high-precision controlled-potential coulometer developed and manufactured at the SRS for plutonium accountability measurements. The Savannah River Site Coulometer system and measurement methodology for plutonium meets performance standards in ISO 12183-2005, 'Controlled-Potential Coulometric Assay of Plutonium'. The Department of Energy (DOE) does not produce or supply a neptunium metal certified reference material, which makes qualifying a measurement method and determining accuracy and precision difficult. Testing and performance of the Savannah River Site Coulometer indicates that it can be used to measure neptunium process solutions and dissolved neptunium oxide without purification for material control and accountability purposes. Savannah River Site's Material Control and Accountability organization has accepted the method uncertainty for accountability and product characterization measurements.
Date: June 4, 2008
Creator: Holland, M; Patterson Nuessle, P; Sheldon Nichols, S; Joe Cordaro, J & George Reeves, G
Partner: UNT Libraries Government Documents Department