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RAPID DETERMINATION OF {sup 210} PO IN WATER SAMPLES

Description: A new rapid method for the determination of {sup 210}Po in water samples has been developed at the Savannah River National Laboratory (SRNL) that can be used for emergency response or routine water analyses. If a radiological dispersive device (RDD) event or a radiological attack associated with drinking water supplies occurs, there will be an urgent need for rapid analyses of water samples, including drinking water, ground water and other water effluents. Current analytical methods for the assay of {sup 210}Po in water samples have typically involved spontaneous auto-deposition of {sup 210}Po onto silver or other metal disks followed by counting by alpha spectrometry. The auto-deposition times range from 90 minutes to 24 hours or more, at times with yields that may be less than desirable. If sample interferences are present, decreased yields and degraded alpha spectrums can occur due to unpredictable thickening in the deposited layer. Separation methods have focused on the use of Sr Resin�, often in combination with 210Pb analysis. A new rapid method for {sup 210}Po in water samples has been developed at the Savannah River National Laboratory (SRNL) that utilizes a rapid calcium phosphate co-precipitation method, separation using DGA Resin� (N,N,N�,N� tetraoctyldiglycolamide extractant-coated resin, Eichrom Technologies or Triskem-International), followed by rapid microprecipitation of {sup 210}Po using bismuth phosphate for counting by alpha spectrometry. This new method can be performed quickly with excellent removal of interferences, high chemical yields and very good alpha peak resolution, eliminating any potential problems with the alpha source preparation for emergency or routine samples. A rapid sequential separation method to separate {sup 210} Po and actinide isotopes was also developed. This new approach, rapid separation with DGA Resin plus microprecipitation for alpha source preparation, is a significant advance in radiochemistry for the rapid determination of {sup 210}Po.
Date: May 22, 2013
Creator: Maxwell, S.
Partner: UNT Libraries Government Documents Department

RAPID FUSION METHOD FOR DETERMINATION OF PLUTONIUM ISOTOPES IN LARGE RICE SAMPLES

Description: A new rapid fusion method for the determination of plutonium in large rice samples has been developed at the Savannah River National Laboratory (Aiken, SC, USA) that can be used to determine very low levels of plutonium isotopes in rice. The recent accident at Fukushima Nuclear Power Plant in March, 2011 reinforces the need to have rapid, reliable radiochemical analyses for radionuclides in environmental and food samples. Public concern regarding foods, particularly foods such as rice in Japan, highlights the need for analytical techniques that will allow very large sample aliquots of rice to be used for analysis so that very low levels of plutonium isotopes may be detected. The new method to determine plutonium isotopes in large rice samples utilizes a furnace ashing step, a rapid sodium hydroxide fusion method, a lanthanum fluoride matrix removal step, and a column separation process with TEVA Resin� cartridges. The method can be applied to rice sample aliquots as large as 5 kg. Plutonium isotopes can be determined using alpha spectrometry or inductively-coupled plasma mass spectrometry (ICP-MS). The method showed high chemical recoveries and effective removal of interferences. The rapid fusion technique is a rugged sample digestion method that ensures that any refractory plutonium particles are effectively digested. The MDA for a 5 kg rice sample using alpha spectrometry is 7E-5 mBq g{sup -1}. The method can easily be adapted for use by ICP-MS to allow detection of plutonium isotopic ratios.
Date: March 1, 2013
Creator: Maxwell, S.
Partner: UNT Libraries Government Documents Department

RAPID DETERMINATION OF RADIOSTRONTIUM IN SEAWATER SAMPLES

Description: A new method for the determination of radiostrontium in seawater samples has been developed at the Savannah River National Laboratory (SRNL) that allows rapid preconcentration and separation of strontium and yttrium isotopes in seawater samples for measurement. The new SRNL method employs a novel and effective pre-concentration step that utilizes a blend of calcium phosphate with iron hydroxide to collect both strontium and yttrium rapidly from the seawater matrix with enhanced chemical yields. The pre-concentration steps, in combination with rapid Sr Resin and DGA Resin cartridge separation options using vacuum box technology, allow seawater samples up to 10 liters to be analyzed. The total {sup 89}Sr + {sup 90}Sr activity may be determined by gas flow proportional counting and recounted after ingrowth of {sup 90}Y to differentiate {sup 89}Sr from {sup 90}Sr. Gas flow proportional counting provides a lower method detection limit than liquid scintillation or Cerenkov counting and allows simultaneous counting of samples. Simultaneous counting allows for longer count times and lower method detection limits without handling very large aliquots of seawater. Seawater samples up to 6 liters may be analyzed using Sr Resin for {sup 89}Sr and {sup 90}Sr with a Minimum Detectable Activity (MDA) of 1-10 mBq/L, depending on count times. Seawater samples up to 10 liters may be analyzed for {sup 90}Sr using a DGA Resin method via collection and purification of {sup 90}Y only. If {sup 89}Sr and other fission products are present, then {sup 91}Y (beta energy 1.55 MeV, 58.5 day half-life) is also likely to be present. {sup 91}Y interferes with attempts to collect {sup 90}Y directly from the seawater sample without initial purification of Sr isotopes first and {sup 90}Y ingrowth. The DGA Resin option can be used to determine {sup 90}Sr, and if {sup 91}Y is also present, an ingrowth option ...
Date: January 16, 2013
Creator: Maxwell, S.
Partner: UNT Libraries Government Documents Department

RAPID RADIOCHEMICAL ANALYSES IN SUPPORT OF FUKUSHIMA NUCLEAR ACCIDENT

Description: There is an increasing need to develop faster analytical methods for emergency response, including emergency soil and air filter samples. The Savannah River National Laboratory (SRNL) performed analyses on samples received from Japan in April, 2011 as part of a U.S. Department of Energy effort to provide assistance to the government of Japan, following the nuclear event at Fukushima Daiichi, resulting from the earthquake and tsunami on March 11, 2011. Of particular concern was whether it was safe to plant rice in certain areas (prefectures) near Fukushima. The primary objectives of the sample collection, sample analysis, and data assessment teams were to evaluate personnel exposure hazards, identify the nuclear power plant radiological source term and plume deposition, and assist the government of Japan in assessing any environmental and agricultural impacts associated with the nuclear event. SRNL analyzed approximately 250 samples and reported approximately 500 analytical method determinations. Samples included soil from farmland surrounding the Fukushima reactors and air monitoring samples of national interest, including those collected at the U.S. Embassy and American military bases. Samples were analyzed for a wide range of radionuclides, including strontium-89, strontium-90, gamma-emitting radionuclides, and plutonium, uranium, americium and curium isotopes. Technical aspects of the rapid soil and air filter analyses will be described. The extent of radiostrontium contamination was a significant concern. For {sup 89,90}Sr analyses on soil samples, a rapid fusion technique using 1.5 gram soil aliquots to enable a Minimum Detectable Activity (MDA) of <1 pCi {sup 89,90} Sr /g of soil was employed. This sequential technique has been published recently by this laboratory for actinides and radiostrontium in soil and vegetation. It consists of a rapid sodium hydroxide fusion, pre-concentration steps using iron hydroxide and calcium fluoride precipitations, followed by Sr-Resin separation and gas flow proportional counting. To achieve a lower detection ...
Date: November 7, 2012
Creator: Maxwell, S.
Partner: UNT Libraries Government Documents Department

RAPID METHOD FOR DETERMINATION OF {sup 228}Ra IN WATER SAMPLES

Description: A new rapid method for the determination of {sup 228}Ra in natural water samples has been developed at the SRNL/EBL (Savannah River National Lab/ Environmental Bioassay Laboratory) that can be used for emergency response or routine samples. While gamma spectrometry can be employed with sufficient detection limits to determine {sup 228}Ra in solid samples (via {sup 228}Ac) , radiochemical methods that employ gas flow proportional counting techniques typically provide lower MDA (Minimal Detectable Activity) levels for the determination of {sup 228}Ra in water samples. Most radiochemical methods for {sup 228}Ra collect and purify {sup 228}Ra and allow for {sup 228}Ac daughter ingrowth for ~36 hours. In this new SRNL/EBL approach, {sup 228}Ac is collected and purified from the water sample without waiting to eliminate this delay. The sample preparation requires only about 4 hours so that {sup 228}Ra assay results on water samples can be achieved in < 6 hours. The method uses a rapid calcium carbonate precipitation enhanced with a small amount of phosphate added to enhance chemical yields (typically >90%), followed by rapid cation exchange removal of calcium. Lead, bismuth, uranium, thorium and protactinium isotopes are also removed by the cation exchange separation. {sup 228}Ac is eluted from the cation resin directly onto a DGA Resin cartridge attached to the bottom of the cation column to purify {sup 228}Ac. DGA Resin also removes lead and bismuth isotopes, along with Sr isotopes and {sup 90}Y. La is used to determine {sup 228}Ac chemical yield via ICP-MS, but {sup 133}Ba can also be used instead if ICP-MS assay is not available. Unlike some older methods, no lead or strontium holdback carriers or continual readjustment of sample pH is required.
Date: September 5, 2012
Creator: Maxwell, S.
Partner: UNT Libraries Government Documents Department

Measure Guideline: Air Sealing Attics in Multifamily Buildings

Description: This Building America Measure Guideline is intended for owners, builders, contractors, homeowners, and other stakeholders in the multifamily building industry, and focuses on challenges found in existing buildings for a variety of housing types. It explains why air sealing is desirable, explores related health and safety issues, and identifies common air leakage points in multifamily building attics. In addition, it also gives an overview of materials and techniques typically used to perform air sealing work.
Date: June 1, 2012
Creator: Otis, C. & Maxwell, S.
Partner: UNT Libraries Government Documents Department

RAPID DETERMINATION OF RA-226 IN ENVIRONMENTAL SAMPLES

Description: A new rapid method for the determination of {sup 226}Ra in environmental samples has been developed at the Savannah River Site Environmental Lab (Aiken, SC, USA) that can be used for emergency response or routine sample analyses. The need for rapid analyses in the event of a Radiological Dispersive Device or Improvised Nuclear Device event is well-known. In addition, the recent accident at Fukushima Nuclear Power Plant in March, 2011 reinforces the need to have rapid analyses for radionuclides in environmental samples in the event of a nuclear accident. {sup 226}Ra (T1/2 = 1,620 years) is one of the most toxic of the long-lived alpha-emitters present in the environment due to its long life and its tendency to concentrate in bones, which increases the internal radiation dose of individuals. The new method to determine {sup 226}Ra in environmental samples utilizes a rapid sodium hydroxide fusion method for solid samples, calcium carbonate precipitation to preconcentrate Ra, and rapid column separation steps to remove interferences. The column separation process uses cation exchange resin to remove large amounts of calcium, Sr Resin to remove barium and Ln Resin as a final purification step to remove {sup 225}Ac and potential interferences. The purified {sup 226}Ra sample test sources are prepared using barium sulfate microprecipitation in the presence of isopropanol for counting by alpha spectrometry. The method showed good chemical recoveries and effective removal of interferences. The determination of {sup 226}Ra in environmental samples can be performed in less than 16 h for vegetation, concrete, brick, soil, and air filter samples with excellent quality for emergency or routine analyses. The sample preparation work takes less than 6 h. {sup 225}Ra (T1/2 = 14.9 day) tracer is used and the {sup 225}Ra progeny {sup 217}At is used to determine chemical yield via alpha spectrometry. The rapid ...
Date: January 3, 2012
Creator: Maxwell, S.
Partner: UNT Libraries Government Documents Department

Determination of 237NP and Pu Isotopes in Large Soil Samples by Inductively Coupled Plasma Mass Spectrometry

Description: A new method for the determination of {sup 237}Np and Pu isotopes in large soil samples has been developed that provides enhanced uranium removal to facilitate assay by inductively coupled plasma mass spectrometry (ICP-MS). This method allows rapid preconcentration and separation of plutonium and neptunium in large soil samples for the measurement of {sup 237}Np and Pu isotopes by ICP-MS. {sup 238}U can interfere with {sup 239}Pu measurement by ICP-MS as {sup 238}UH{sup +} mass overlap and {sup 237}Np via {sup 238}U peak tailing. The method provides enhanced removal of uranium by separating Pu and Np initially on TEVA Resin, then transferring Pu to DGA resin for additional purification. The decontamination factor for removal of uranium from plutonium for this method is greater than 1 x 10{sup 6}. Alpha spectrometry can also be applied so that the shorter-lived {sup 238}Pu isotope can be measured successfully. {sup 239}Pu, {sup 242}Pu and {sup 237}Np were measured by ICP-MS, while {sup 236}Pu and {sup 238}Pu were measured by alpha spectrometry.
Date: July 26, 2010
Creator: Maxwell, S.
Partner: UNT Libraries Government Documents Department

RAPID SEPARATION METHOD FOR 237NP AND PU ISOTOPES IN LARGE SOIL SAMPLES

Description: A new rapid method for the determination of {sup 237}Np and Pu isotopes in soil and sediment samples has been developed at the Savannah River Site Environmental Lab (Aiken, SC, USA) that can be used for large soil samples. The new soil method utilizes an acid leaching method, iron/titanium hydroxide precipitation, a lanthanum fluoride soil matrix removal step, and a rapid column separation process with TEVA Resin. The large soil matrix is removed easily and rapidly using this two simple precipitations with high chemical recoveries and effective removal of interferences. Vacuum box technology and rapid flow rates are used to reduce analytical time.
Date: July 26, 2010
Creator: Maxwell, S.; Culligan, B. & Noyes, G.
Partner: UNT Libraries Government Documents Department

Rapid Determination of 237 Np and Pu Isotopes in Water by Inductively Coupled Plasma Mass Spectrometry and Alpha Spectrometry

Description: A new method that allows rapid preconcentration and separation of plutonium and neptunium in water samples was developed for the measurement of {sup 237}Np and Pu isotopes by inductively-coupled plasma mass spectrometry (ICP-MS) and alpha spectrometry; a hybrid approach. {sup 238}U can interfere with {sup 239}Pu measurement by ICP-MS as {sup 238}UH{sup +} mass overlap and {sup 237}Np via peak tailing. The method provide enhanced removal of uranium by separating Pu and Np initially on TEVA Resin, then moving Pu to DGA resin for additional removal of uranium. The decontamination factor for uranium from Pu is almost 100,000 and the decontamination factor for U from Np is greater than 10,000. This method uses stacked extraction chromatography cartridges and vacuum box technology to facilitate rapid separations. Preconcentration is performed using a streamlined calcium phosphate precipitation method. Purified solutions are split between ICP-MS and alpha spectrometry so that long and short-lived Pu isotopes can be measured successfully. The method allows for simultaneous extraction of 20 samples (including QC samples) in 4 to 6 hours, and can also be used for emergency response. {sup 239}Pu, {sup 242}Pu and {sup 237}Np were measured by ICP-MS, while {sup 236}Pu, {sup 238}Pu, and {sup 239}Pu were measured by alpha spectrometry.
Date: June 23, 2010
Creator: Maxwell, S.; Jones, V.; Culligan, B.; Nichols, S. & Noyes, G.
Partner: UNT Libraries Government Documents Department

RAPID SEPARATION OF ACTINIDES AND RADIOSTRONTIUM IN VEGETATION SAMPLES

Description: A new rapid method for the determination of actinides and radiostrontium in vegetation samples has been developed at the Savannah River Site Environmental Lab (Aiken, SC, USA) that can be used in emergency response situations or for routine analysis. The actinides in vegetation method utilizes a rapid sodium hydroxide fusion method, a lanthanum fluoride matrix removal step, and a streamlined column separation process with stacked TEVA, TRU and DGA Resin cartridges. Lanthanum was separated rapidly and effectively from Am and Cm on DGA Resin. Alpha emitters are prepared using rare earth microprecipitation for counting by alpha spectrometry. The purified {sup 90}Sr fractions are mounted directly on planchets and counted by gas flow proportional counting. The method showed high chemical recoveries and effective removal of interferences. The actinide and {sup 90}Sr in vegetation sample analysis can be performed in less than 8 h with excellent quality for emergency samples. The rapid fusion technique is a rugged sample digestion method that ensures that any refractory actinide particles or vegetation residue after furnace heating is effectively digested.
Date: June 1, 2010
Creator: Maxwell, S.
Partner: UNT Libraries Government Documents Department

RAPID SEPARATION METHOD FOR ACTINIDES IN EMERGENCY AIR FILTER SAMPLES

Description: A new rapid method for the determination of actinides and strontium in air filter samples has been developed at the Savannah River Site Environmental Lab (Aiken, SC, USA) that can be used in emergency response situations. The actinides and strontium in air filter method utilizes a rapid acid digestion method and a streamlined column separation process with stacked TEVA, TRU and Sr Resin cartridges. Vacuum box technology and rapid flow rates are used to reduce analytical time. Alpha emitters are prepared using cerium fluoride microprecipitation for counting by alpha spectrometry. The purified {sup 90}Sr fractions are mounted directly on planchets and counted by gas flow proportional counting. The method showed high chemical recoveries and effective removal of interferences. This new procedure was applied to emergency air filter samples received in the NRIP Emergency Response exercise administered by the National Institute for Standards and Technology (NIST) in April, 2009. The actinide and {sup 90}Sr in air filter results were reported in {approx}4 hours with excellent quality.
Date: February 3, 2010
Creator: Maxwell, S.; Noyes, G. & Culligan, B.
Partner: UNT Libraries Government Documents Department

RAPID SEPARATION METHOD FOR ACTINIDES IN EMERGENCY SOIL SAMPLES

Description: A new rapid method for the determination of actinides in soil and sediment samples has been developed at the Savannah River Site Environmental Lab (Aiken, SC, USA) that can be used for samples up to 2 grams in emergency response situations. The actinides in soil method utilizes a rapid sodium hydroxide fusion method, a lanthanum fluoride soil matrix removal step, and a streamlined column separation process with stacked TEVA, TRU and DGA Resin cartridges. Lanthanum was separated rapidly and effectively from Am and Cm on DGA Resin. Vacuum box technology and rapid flow rates are used to reduce analytical time. Alpha sources are prepared using cerium fluoride microprecipitation for counting by alpha spectrometry. The method showed high chemical recoveries and effective removal of interferences. This new procedure was applied to emergency soil samples received in the NRIP Emergency Response exercise administered by the National Institute for Standards and Technology (NIST) in April, 2009. The actinides in soil results were reported within 4-5 hours with excellent quality.
Date: November 9, 2009
Creator: Maxwell, S.; Culligan, B. & Noyes, G.
Partner: UNT Libraries Government Documents Department

RAPID DETERMINATION OF ACTINIDES IN URINE BY INDUCTIVELY-COUPLED PLASMA MASS SPECTROMETRY AND ALPHA SPECTROMETRY: A HYBRID APPROACH

Description: A new rapid separation method that allows separation and preconcentration of actinides in urine samples was developed for the measurement of longer lived actinides by inductively coupled plasma mass spectrometry (ICP-MS) and short-lived actinides by alpha spectrometry; a hybrid approach. This method uses stacked extraction chromatography cartridges and vacuum box technology to facilitate rapid separations. Preconcentration, if required, is performed using a streamlined calcium phosphate precipitation. Similar technology has been applied to separate actinides prior to measurement by alpha spectrometry, but this new method has been developed with elution reagents now compatible with ICP-MS as well. Purified solutions are split between ICP-MS and alpha spectrometry so that long- and short-lived actinide isotopes can be measured successfully. The method allows for simultaneous extraction of 24 samples (including QC samples) in less than 3 h. Simultaneous sample preparation can offer significant time savings over sequential sample preparation. For example, sequential sample preparation of 24 samples taking just 15 min each requires 6 h to complete. The simplicity and speed of this new method makes it attractive for radiological emergency response. If preconcentration is applied, the method is applicable to larger sample aliquots for occupational exposures as well. The chemical recoveries are typically greater than 90%, in contrast to other reported methods using flow injection separation techniques for urine samples where plutonium yields were 70-80%. This method allows measurement of both long-lived and short-lived actinide isotopes. 239Pu, 242Pu, 237Np, 243Am, 234U, 235U and 238U were measured by ICP-MS, while 236Pu, 238Pu, 239Pu, 241Am, 243Am and 244Cm were measured by alpha spectrometry. The method can also be adapted so that the separation of uranium isotopes for assay is not required, if uranium assay by direct dilution of the urine sample is preferred instead. Multiple vacuum box locations may be set-up to supply several ICP-MS ...
Date: May 27, 2009
Creator: Maxwell, S. & Jones, V.
Partner: UNT Libraries Government Documents Department

RAPID SEPARATION METHOD FOR EMERGENCY WATER AND URINE SAMPLES

Description: The Savannah River Site Environmental Bioassay Lab participated in the 2008 NRIP Emergency Response program administered by the National Institute for Standards and Technology (NIST) in May, 2008. A new rapid column separation method was used for analysis of actinides and {sup 90}Sr the NRIP 2008 emergency water and urine samples. Significant method improvements were applied to reduce analytical times. As a result, much faster analysis times were achieved, less than 3 hours for determination of {sup 90}Sr and 3-4 hours for actinides. This represents a 25%-33% improvement in analysis times from NRIP 2007 and a {approx}100% improvement compared to NRIP 2006 report times. Column flow rates were increased by a factor of two, with no significant adverse impact on the method performance. Larger sample aliquots, shorter count times, faster cerium fluoride microprecipitation and streamlined calcium phosphate precipitation were also employed. Based on initial feedback from NIST, the SRS Environmental Bioassay Lab had the most rapid analysis times for actinides and {sup 90}Sr analyses for NRIP 2008 emergency urine samples. High levels of potential matrix interferences may be present in emergency samples and rugged methods are essential. Extremely high levels of {sup 210}Po were found to have an adverse effect on the uranium results for the NRIP-08 urine samples, while uranium results for NRIP-08 water samples were not affected. This problem, which was not observed for NRIP-06 or NRIP-07 urine samples, was resolved by using an enhanced {sup 210}Po removal step, which will be described.
Date: August 27, 2008
Creator: Maxwell, S. & Culligan, B.
Partner: UNT Libraries Government Documents Department

RAPID METHOD FOR DETERMINATION OF RADIOSTRONTIUM IN EMERGENCY MILK SAMPLES

Description: A new rapid separation method for radiostrontium in emergency milk samples was developed at the Savannah River Site (SRS) Environmental Bioassay Laboratory (Aiken, SC, USA) that will allow rapid separation and measurement of Sr-90 within 8 hours. The new method uses calcium phosphate precipitation, nitric acid dissolution of the precipitate to coagulate residual fat/proteins and a rapid strontium separation using Sr Resin (Eichrom Technologies, Darien, IL, USA) with vacuum-assisted flow rates. The method is much faster than previous method that use calcination or cation exchange pretreatment, has excellent chemical recovery, and effectively removes beta interferences. When a 100 ml sample aliquot is used, the method has a detection limit of 0.5 Bq/L, well below generic emergency action levels.
Date: July 17, 2008
Creator: Maxwell, S. & Culligan, B.
Partner: UNT Libraries Government Documents Department

Rapid Column Extraction Methods for Urine

Description: A new fecal analysis method that dissolves plutonium oxide was developed at the Westinghouse Savannah River Site. Diphonix Resin (Eichrom Industries), is used to pre-concentrate the actinides from digested fecal samples. A rapid microwave digestion technique is used to remove the actinides from the Diphonix Resin, which effectively extracts plutonium and americium from acidic solutions containing hydrofluoric acid. After resin digestion, the plutonium and americium are recovered in a small volume of nitric acid that is loaded onto small extraction chromatography columns, TEVA Resin and TRU Resin (Eichrom Industries). The method enables complete dissolution of plutonium oxide and provides high recovery of plutonium and americium with good removal of thorium isotopes such as thorium-228.
Date: June 9, 2000
Creator: Maxwell, S.L. III
Partner: UNT Libraries Government Documents Department

Actinide Recovery Method for Large Soil Samples

Description: A new Actinide Recovery Method has been developed by the Savannah River Site Central Laboratory to preconcentrate actinides in very large soil samples. Diphonix Resin(r) is used eliminate soil matrix interferences and preconcentrate actinides after soil leaching or soil fusion. A rapid microwave digestion technique is used to remove the actinides from the Diphonix Resin(r). After the resin digestion, the actinides are recovered in a small volume of nitric acid which can be easily loaded onto small extraction-chromatography columns, such as TEVA Resin(r), U-TEVA Resin(r) or TRU Resin(r) (Eichrom Industries). This method enables the application of small, selective extraction-columns to recover actinides from very large soil samples with high selectivity, consistent tracer recoveries and minimal liquid waste.
Date: November 1998
Creator: Maxwell, S. L., III & Nichols, S.
Partner: UNT Libraries Government Documents Department

Rapid Separation Methods to Characterize Actinides and Metallic Impurities in Plutonium Scrap Materials at SRS

Description: The Nuclear Materials Stabilization and Storage Division at SRS plans to stabilize selected plutonium scrap residue materials for long term storage by dissolution processing and plans to stabilize other plutonium vault materials via high-temperature furnace processing. To support these nuclear material stabilization activities, the SRS Analytical Laboratories Department (ALD) will provide characterization of materials required prior to the dissolution or the high-firing of these materials. Lab renovations to install new analytical instrumentation are underway to support these activities that include glove boxes with simulated-process dissolution and high- pressure microwave dissolution capability. Inductively-coupled plasma atomic emission spectrometry (ICP-AES), inductively- coupled mass spectrometry (ICP-MS) and thermal-ionization mass spectrometry (TIMS) will be used to measure actinide isotopics and metallic impurities. New high-speed actinide separation methods have been developed that will be applied to isotopic characterization of nuclear materials by TIMS and ICP-MS to eliminate isobaric interferences between Pu-238 /U- 238 and Pu-241/Am-241. TEVA Resin, UTEVA Resin, and TRU Resin columns will be used with vacuum-assisted flow rates to minimize TIMS and ICP-MS sample turnaround times. For metallic impurity analysis, rapid column removal methods using UTEVA Resin, AGMP-1 anion resin and AG MP-50 cation resin have also been developed to remove plutonium and uranium matrix interferences prior to ICP-AES and ICP- MS measurements.
Date: July 1998
Creator: Maxwell, S. L., III & Jones, V. D.
Partner: UNT Libraries Government Documents Department

Analytical support for characterization of americium-curium solution at SRS

Description: Americium-Curium (Am-Cm) solution in F-Canyon was produced during the Mk 40 and Mk 41 campaigns in the mid and late 1970`s. The Savannah River Site (SRS) Central Laboratory recently characterized this important solution of nuclear material to enable assessment by Westinghouse Savannah River Company and Department of Energy of disposition options. The tank had last been sampled and analyzed in 1986. A wide range of analyses were performed to determine the tank contents. New radiochemical column separation methods were developed to fully characterize the solution for actinides, metals, anions, and isotopics to support the disposition study in a timely manner. Current disposition is to perform a vitrification process on the Am/Cm solution at SRS to produce glass canisters for safe shipment and storage of this material. The SRS Am/Cm waste solution will be converted, in effect, to a product for an outside customer. Oak Ridge National Laboratory. To support the Am/Cm vitrification processing, process support analyses are required after completion of denitration, precipitation and redissolution steps. Full elemental chemistry characterization will be required on the final melter feed solution.
Date: October 1, 1996
Creator: Maxwell, S.L. III & Nelson, M.R.
Partner: UNT Libraries Government Documents Department

Measurement of actinides and strontium-90 in high activity waste

Description: The reliable measurement of trace radionuclides in high activity waste is important to support waste processing activities at SRS (F and H Area Waste Tanks, Extended Sludge Processing (ESP) and In-Tank precipitation (ITP) processing). Separation techniques are needed to remove high levels of gamma activity and alpha/beta interferences prior to analytical measurement. Using new extraction chromatographic resins from EiChrom Industries, Inc., the SRS Central Laboratory has developed new high speed separation methods that enable measurement of neptunium, thorium, uranium, plutonium, americium and strontium-90 in high activity waste solutions. Small particle size resin and applied vacuum are used to reduce analysis times and enhance column performance. Extraction chromatographic resins are easy to use and eliminate the generation of contaminated liquid organic waste.
Date: August 1, 1994
Creator: Maxwell, S. L. III & Nelson, M. R.
Partner: UNT Libraries Government Documents Department

Improved accountability method for measuring enriched uranium in H-Canyon dissolver solution at the Savannah River Site

Description: At the Savannah River Site (SRS), accountability measurement of enriched uranium dissolved in H-Canyon is performed using isotope dilution mass spectrometry (IDMS). In the IDMS analytical method, a known quantity of uranium{sup 233} is added to the sample solution containing enriched uranium and fission products. The resulting uranium mixture must first be purified using a separation technique in the shielded analytical(``hot``) cells to lower radioactivity levels by removing fission products. Following this purification, the sample is analyzed by mass spectrometry to determine the total uranium content and isotopic abundance. The magnitude of the response of each uranium isotope in the sample solution and the response of the U{sup 233} spike is measured. By ratioing these responses, relative to the known quantity of the U{sup 233} spike, the uranium content can be determined. A hexane solvent extraction technique, used for years at SRS to remove fission products prior to the mass spectrometry analysis of uranium, has several problems. The hexone method is tedious, requires additional sample clean-up after the purified sample is removed from the shielded cells and requires the use of Resource Conservation and Recovery Act (RCRA)-listed hazardous materials (hexone and chromium compounds). A new high speed separation method that enables a rapid removal of fission products in a shielded cells environment has been developed by the SRS Central Laboratory to replace the hexone method. The new high speed column extraction chromatography technique employs applied vacuum and columns containing tri (2-ethyl-hexyl) phosphate (TEHP) solvent coated on a small particle inert support (SM-7 Bio Beads). The new separation is rapid, user friendly, eliminates the use of the RCA-listed hazardous chemicals and reduces the amount of solid waste generated by the separation method. 2 tabs. 4 figs.
Date: August 1, 1992
Creator: Maxwell, S. L. III; Satkowski, J. & Mahannah, R. N.
Partner: UNT Libraries Government Documents Department

Measurement of trace uranium-235 and plutonium-239, 240 in waste tank material at the Savannah River Site

Description: At the Savannah River Site (SRS), large quantities of radioactive liquid waste are evaporated to reduce volume before eventual processing through the In-Tank Precipitation process. Actinides in the liquid waste are only slightly soluble in the highly alkaline waste solution. Since some of the actinide isotopes are fissionable, the quantities being processed through the evaporator system are of interest. To better quantify the concentration and mass of fissionable material entering the evaporator system and eventually deposited as salt, analysis of the actinide elements were necessary. The predominant fissionable actinide isotopes of interest are U{sup 235} and Pu{sup 239}. To enable the reliable measurement of these radionuclides, the Central Laboratory has developed high speed separation techniques to measure U{sup 235} content by Isotope Dilution Mass Spectrometry and Pu{sup 239,240} by alpha spectrometry. Due to the high radioactivity levels in the samples all separations are performed in shielded analytical cells. Uranium is purified and concentrated using a high speed extraction chromatography technique that employs applied vacuum and columns containing tri (2-ethylene) phosphate solvent coated on a small particle inert support. The uranium method enables measurement of U{sup 235} concentrations to 1 {times} 10{sup {minus}4} g/L. Plutonium is purified and concentrated using a high speed anion exchange technique. The Pu method enables measurements of Pu{sup 239,240} to 2 {times} 10{sup {minus}6} g/L.
Date: August 1, 1992
Creator: Mahannah, F. N. & Maxwell, S. L. III
Partner: UNT Libraries Government Documents Department

Measurement of trace uranium-235 and plutonium-239, 240 in waste tank material at the Savannah River Site

Description: At the Savannah River Site (SRS), large quantities of radioactive liquid waste are evaporated to reduce volume before eventual processing through the In-Tank Precipitation process. Actinides in the liquid waste are only slightly soluble in the highly alkaline waste solution. Since some of the actinide isotopes are fissionable, the quantities being processed through the evaporator system are of interest. To better quantify the concentration and mass of fissionable material entering the evaporator system and eventually deposited as salt, analysis of the actinide elements were necessary. The predominant fissionable actinide isotopes of interest are U{sup 235} and Pu{sup 239}. To enable the reliable measurement of these radionuclides, the Central Laboratory has developed high speed separation techniques to measure U{sup 235} content by Isotope Dilution Mass Spectrometry and Pu{sup 239,240} by alpha spectrometry. Due to the high radioactivity levels in the samples all separations are performed in shielded analytical cells. Uranium is purified and concentrated using a high speed extraction chromatography technique that employs applied vacuum and columns containing tri (2-ethylene) phosphate solvent coated on a small particle inert support. The uranium method enables measurement of U{sup 235} concentrations to 1 {times} 10{sup {minus}4} g/L. Plutonium is purified and concentrated using a high speed anion exchange technique. The Pu method enables measurements of Pu{sup 239,240} to 2 {times} 10{sup {minus}6} g/L.
Date: January 1, 1992
Creator: Mahannah, F.N. & Maxwell, S.L. III.
Partner: UNT Libraries Government Documents Department