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DOE OSTI2012

Analytical Results of MOX Colemanite Concrete Samples Poured August 29, 2012

The Mixed Oxide Fuel Fabrication Facility (MFFF) will use colemanite bearing concrete neutron absorber panels credited with attenuating neutron flux in the criticality design analyses and shielding operators from radiation. The Savannah River National Laboratory is tasked with measuring the total density, partial hydrogen density, and partial boron density of the colemanite concrete. Samples poured 8/29/12 were received on 9/20/2012 and analyzed. The average total density of each of the samples measured by the ASTM method C 642 was within the lower bound of 1.88 g/cm 3 . The average partial hydrogen density of samples 8.6.1, 8.7.1, and 8.5.3 as measured using method ASTM E 1311 met the lower bound of 6.04E-02 g/cm 3 . The average measured partial boron density of each sample met the lower bound of 1.65E-01 g/cm 3 measured by the ASTM C 1301 method. The average partial hydrogen density of samples 8.5.1, 8.6.3, and 8.7.3 did not meet the lower bound. The samples, as received, were not wrapped in a moist towel as previous samples and appeared to be somewhat drier. This may explain the lower hydrogen partial density with respect to previous samples.

36 MATERIALS SCIENCE↗

DOE OSTI2012

Analytical Results of MOX Colemanite Concrete Samples Poured August 29, 2012

36 MATERIALS SCIENCE↗

DOE OSTI2012

Comparison of Results for Quarter 1 Surface Water Split Samples Collected at the Nuclear Fuel Services Site, Erwin, Tennessee

Oak Ridge Associated Universities (ORAU), under the Oak Ridge Institute for Science and Education (ORISE) contract, collected split surface water samples with Nuclear Fuel Services (NFS) representatives on August 22, 2012. Representatives from the U.S. Nuclear Regulatory Commission and Tennessee Department of Environment and Conservation were also in attendance. Samples were collected at four surface water stations, as required in the approved Request for Technical Assistance number 11-018. These stations included Nolichucky River upstream (NRU), Nolichucky River downstream (NRD), Martin Creek upstream (MCU), and Martin Creek downstream (MCD). Both ORAU and NFS performed gross alpha and gross beta analyses. The comparison of results using the duplicate error ratio (DER), also known as the normalized absolute difference. A DER ≤ 3 indicates that, at a 99% confidence interval, split sample results do not differ significantly when compared to their respective one standard deviation (sigma) uncertainty. The NFS split sample report does not specify the confidence level of reported uncertainties. Therefore, standard two sigma reporting is assumed and uncertainty values were divided by 1.96. A comparison of split sample results, using the DER equation, indicates one set with a DER greater than 3. A DER of 3.1 is calculated for gross alpha results from ORAU sample 5198W0003 and NFS sample MCU-310212003. The ORAU result is 0.98 ± 0.30 pCi/L (value ± 2 sigma) compared to the NFS result of -0.08 ± 0.60 pCi/L. Relatively high DER values are not unexpected for low (e.g., background) analyte concentrations analyzed by separate laboratories, as is the case here. It is noted, however, NFS uncertainties are at least twice the ORAU uncertainties, which contributes to the elevated DER value. Differences in ORAU and NFS minimum detectable activities are even more pronounced. comparison of ORAU and NFS split samples produces reasonably consistent results for low (e.g., background) concentrations.

54 ENVIRONMENTAL SCIENCES↗

DOE OSTI2013

Rheology and TIC/TOC Results of ORNL Tank Samples

The Savannah River National Laboratory (SRNL)) was requested by Oak Ridge National Laboratory (ORNL) to perform total inorganic carbon (TIC), total organic carbon (TOC), and rheological measurements for several Oak Ridge tank samples. As received slurry samples were diluted and submitted to SRNL-Analytical for TIC and TOC analyses. Settled solids yield stress (also known as settled shear strength) of the as received settled sludge samples were determined using the vane method and these measurements were obtained 24 hours after the samples were allowed to settled undisturbed. Rheological or flow properties (Bingham Plastic viscosity and Bingham Plastic yield stress) were determined from flow curves of the homogenized or well mixed samples. Other targeted total suspended solids (TSS) concentrations samples were also analyzed for flow properties and these samples were obtained by diluting the as-received sample with de-ionized (DI) water.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2015

Analysis of Tank 35H Samples in Support of Salt Batch Planning

Savannah River Remediation obtained three samples from different heights within Tank 35H. The samples were analyzed by Savannah River National Laboratory to support Salt Batch planning. The results from the analysis indicate the compositions of the three samples show increasing concentrations for most analytes going from HTF-35-15-17 through HTF-35-15-19 corresponding to successively deeper sampling locations. The data indicate some stratification within the tank. The plutonium and Sr-90 concentrations measured in the filtered samples were slightly lower than in the decanted (unfiltered) samples. The difference in the results for the filtered and unfiltered samples likely lies within the expected uncertainty for the measurement, but may indicate that filtration removed a small amount of suspended material from the samples.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2015

SNS Sample Activation Calculator Flux Recommendations and Validation

The Spallation Neutron Source (SNS) at Oak Ridge National Laboratory (ORNL) uses the Sample Activation Calculator (SAC) to calculate the activation of a sample after the sample has been exposed to the neutron beam in one of the SNS beamlines. The SAC webpage takes user inputs (choice of beamline, the mass, composition and area of the sample, irradiation time, decay time, etc.) and calculates the activation for the sample. In recent years, the SAC has been incorporated into the user proposal and sample handling process, and instrument teams and users have noticed discrepancies in the predicted activation of their samples. The Neutronics Analysis Team validated SAC by performing measurements on select beamlines and confirmed the discrepancies seen by the instrument teams and users. The conclusions were that the discrepancies were a result of a combination of faulty neutron flux spectra for the instruments, improper inputs supplied by SAC (1.12), and a mishandling of cross section data in the Sample Activation Program for Easy Use (SAPEU) (1.1.2). This report focuses on the conclusion that the SAPEU (1.1.2) beamline neutron flux spectra have errors and are a significant contributor to the activation discrepancies. The results of the analysis of the SAPEU (1.1.2) flux spectra for all beamlines will be discussed in detail. The recommendations for the implementation of improved neutron flux spectra in SAPEU (1.1.3) are also discussed.

43 PARTICLE ACCELERATORS↗

DOE OSTI2016

Results of Hg speciation testing on tank 39 and 1Q16 tank 50 samples

The Savannah River National Laboratory (SRNL) was tasked with preparing and shipping samples for Hg speciation by Eurofins Frontier Global Sciences, Inc. in Seattle, WA on behalf of the Savannah River Remediation (SRR) Mercury Task Team.i,ii The seventeenth shipment of samples was designated to include two Tank 39 samples and the 1Q16 Tank 50 Quarterly WAC sample. The surface Tank 39 sample was pulled at 262.1” from the tank bottom, and the depth Tank 39 sample was pulled at 95” from the tank bottom. The 1Q16 Tank 50 WAC sample was drawn from the 1-L variable depth sample received by SRNL.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2016

K West Basin Sand Filter Backwash Sample Analysis

A sand filter is used to help maintain water clarity at the K West Basin where highly radioactive sludge is stored. Eventually that sand filter will require disposal. The radionuclide content of the solids trapped in the sand filter will affect the selection of the sand filter disposal pathway. The Pacific Northwest National Laboratory (PNNL) was contracted by the K Basin Operations & Plateau Remediation Project (operations contractor CH2M Hill) to analyze the radionuclide content of the solids collected from the backwash of the K West Basin sand filter. The radionuclide composition in the sand filter backwash solids will be used by CH2M Hill to determine if the sand filter media and retained sludge solids will be designated as transuranic waste for disposal purposes or can be processed through less expensive means. On October 19, 2015, K Basin Operations & Plateau Remediation Project staff backwashed the sand filter into the North Load-Out Pit (NLOP) and immediately collected sample slurry from a sampling tube positioned 24 in. above the NLOP floor. The 764 g sand filter backwash slurry sample, KW-105 SFBW-001, was submitted to PNNL for analysis on October 20, 2015. Solids from the slurry sample were consolidated into two samples (i.e., a primary and a duplicate sample) by centrifuging and measured for mass (0.82 g combined – wet centrifuged solids basis) and volume (0.80 mL combined). The solids were a dark brown/orange color, consistent with iron oxide/hydroxide. The solids were dried; the combined dry solids mass was 0.1113 g, corresponding to 0.0146 weight percent (wt%) solids in the original submitted sample slurry. The solids were acid-digested using nitric and hydrochloric acids. Insoluble solids developed upon dilution with 0.5 M HNO 3 , corresponding to an average 6.5 wt% of the initial dry solids content. The acid digestate and insoluble solids were analyzed separately by gamma spectrometry. Nominally, 7.7% of the 60 Co was present in the insoluble solids; less than 1% of other gamma-emitters (i.e., 137 Cs, 154/155 Eu, and 241 Am) were present in the insoluble solids. Aliquots of the acid digestate were analyzed directly using gamma energy analysis (GEA) and after separations for 238 Pu, 239+240 Pu, 237 Np, and 241 Am radioisotopes using alpha energy analysis (AEA). The 90 Sr was measured by liquid scintillation counting (LSC) on the Sr-separated fraction. The plutonium isotopic distribution of the acid digestate was analyzed following Pu separations by thermal ionization mass spectrometry (TIMS). A table summarizes the results for the primary and duplicate samples. The 239+240 Pu concentration (µCi/g dry) relative to 90 Sr and to 137 Cs concentrations (µCi/g dry) was examined. The K West Basin sludge has a 239+240 Pu/ 90 Sr ranging from 0.1 to 1.2 and the 239+240 Pu/ 137 Cs ratio ranging from 0.10 to 0.47. In contrast, the sand filter backwash solids 239+240 Pu/ 90 Sr ratio was 10.6 and the 239+240 Pu/ 137 Cs ratio was 2.0. The ratio differences indicate a relative enhancement of the Pu concentration in the sand filter solids relative to the 137 Cs and 90 Sr sludge concentrations currently in the K West Basin. A dose-to-curie radioisotope evaluation of the sand filter waste form may need to consider this dissimilarity.

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DOE OSTI2016

GoAmazon 2014/15 Particle Sampling Field Campaign Report

As a part of the GoAmazon 2014/15 field deployments, samples of atmospheric particles were collected at the T3 field site (3° 12' 46.70" S, 60° 35' 53.0, Manacapuru, Brazil) established in the Amazonian region. The site was located downwind from Manaus and therefore, experienced clean conditions when winds were from northwest and polluted conditions when winds were from Manaus. During the second intensive operational period of GoAmazon 2014/15 (09/06/2014-10/02/2014), multiple samples of particles were collected using a cascade Multi-Orifice Uniform Deposition Impactor (MOUDI-110). Size-resolved samples by MOUDI (0.056-0.1, 0.1-0.18, 0.18-0.32, 0.32-0.56, 0.56-1.0, 1.0-1.8 μm) were collected for 6-12 hours. A variety of substrates, compatible with different spectro-microscopy methods of analysis, were arranged on the impactor stages. Collected aerosol samples are now stored pending laboratory analysis using multi-modal methods of chemical imaging. Our approach is to analyze only the samples of specific interest. We use the field campaign records and data on meteorology, as well as in situ measurements of gases and aerosols, to select the subset of samples for the in-depth laboratory analysis for selected episodes where changes in chemical composition of particles can be correlated with other data recorded at the site. Hence, we do not expect to perform detailed measurements on all samples—rather, only those samples with the greatest potential to provide scientific insight into aerosol chemistry.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2015

California GAMA Special Study. Development of a Capability for the Analysis of Krypton-85 in Groundwater Samples

A capability for the analysis of krypton-85 ( 85 Kr) in groundwater samples was developed at LLNL. Samples are collected by extracting gas from 2000-4000 L of groundwater at the well, yielding approximately 0.2 cm 3 STP krypton. Sample collection takes 1 to 4 hours. Krypton is purified in the laboratory using a combination of molecular sieve and activated charcoal traps, and transferred to a liquid scintillation vial. The 85 Kr activity is measured by liquid scintillation on a Quantulus 1220 liquid scintillation counter from PerkinElmer. The detection limit for a typical 0.2 cm 3 Kr sample size is 11% of the present day activity in air, corresponding to the decay corrected activity in air in 1987. The typical measurement uncertainty is below 10% for recently recharged samples. Six groundwater samples were collected, purified and counted. 85 Kr was not detected in any of the samples counted at LLNL. 85 Kr was detected by the low level counting laboratory of Bern University in all samples between 1.5 and 6.6 decays per minute per cm 3 krypton, corresponding to decay corrected activities in air between 1971 and 1985. The new capability is an excellent complement to tritium-helium, expanding the existing suite of age dating tools available to the GAMA program ( 35 S, 3 H/ 3 He, 14 C and radiogenic helium). 85 Kr can replace 3 H/ 3 He in settings where 3 H/ 3 He ages are impossible to determine (for example where terrigenic helium overwhelms tritiogenic helium) and provides additional insight into travel time distributions in complex mixed groundwater systems.

54 ENVIRONMENTAL SCIENCES↗

DOE OSTI2016

Data Validation Package: April 2016 Groundwater Sampling at the Falls City, Texas, Disposal Site

Nine groundwater samples were collected at the Falls City, Texas, Disposal Site as specified in the March 2008 Long-Term Surveillance Plan for the US Department of Energy Falls City Uranium Mill Tailings Disposal Site, Falls City, Texas (DOE-LM/1602-2008). Sampling and analyses were conducted as specified in the Sampling and Analysis Plan for US Department of Energy Office of Legacy Management Sites (LMS/PRO/S04351, continually updated). The wells sampled included the cell performance monitoring wells (0709, 0858, 0880, 0906, and 0921) and the groundwater monitoring wells (0862, 0886, 0891, 0924, and 0963). A duplicate sample was collected from location 0891. Water levels were measured at each sampled well. Historically, cell performance monitoring wells 0908 and 0916 have not produced water and were confirmed as dry during this sampling event. These wells are completed above the saturated interval in the formation. Notable observations for time-concentration graphs in this report include: (1) uranium concentrations in well 0891 continue to increase; (2) the uranium concentration in well 0880 is higher than the 2015 value and lower than the 2014 value, and it remains within the range of historical values; and (3) uranium concentrations in the other sampled wells are below 2 mg/L and consistent with previous results.

54 ENVIRONMENTAL SCIENCES↗

DOE OSTI2016

Data Validation Package - June 2016 Groundwater and Surface Water Sampling at the Green River, Utah, Disposal Site

This event included annual sampling of groundwater and surface water locations at the Green River, Utah, Disposal Site. Sampling and analyses were conducted as specified in Sampling and Analysis Plan for US. Department of Energy Office of Legacy Management Sites (LMS/PRO/S04351, continually updated, http://energy.gov/lrnldownloads/sampling-and- analysis-plan-us-department-energy-office-legacy-management-sites). Samples were collected from 15 monitoring wells and two surface locations at the disposal site as specified in the draft 2011 Ground Water Compliance Action Plan for the Green River, Utah, Disposal Site. Planned monitoring locations are shown in Attachment 1, Sampling and Analysis Work Order. A duplicate sample was collected from location 0179. One equipment blank was collected during this sampling event. Water levels were measured at all monitoring wells that were sampled. See Attachment 2, Trip Reports for additional details. The analytical data and associated qualifiers can be viewed in environmental database reports and are also available for viewing with dynamic mapping via the GEMS (Geospatial Environmental Mapping System) website at http://gems.lm.doe.gov/#. No issues were identified during the data validation process that requires additional action or follow-up.

54 ENVIRONMENTAL SCIENCES↗

DOE OSTI2015

Data Validation Package - June 2015 Groundwater and Surface Water Sampling at the Green River, Utah, Disposal Site

Groundwater samples were collected during the 2015 sampling event from point-of-compliance (POC) wells 0171, 0173, 0176, 0179, 0181, and 0813 to monitor the disposition of contaminants in the middle sandstone unit of the Cedar Mountain Formation. Groundwater samples also were collected from alluvium monitoring wells 0188, 0189, 0192, 0194, and 0707, and basal sandstone monitoring wells 0182, 0184, 0185, and 0588 as a best management practice. Surface locations 0846 and 0847 were sampled to monitor for degradation of water quality in the backwater area of Brown’s Wash and in the Green River immediately downstream of Brown’s Wash. The Green River location 0801 is upstream from the site and is sampled to determine background-threshold values (BTVs). Sampling and analyses were conducted as specified in Sampling and Analysis Plan for U.S. Department of Energy Office of Legacy Management Sites (LMS/PRO/S04351, continually updated, http://energy.gov/lm/downloads/sampling-and- analysis-plan-us-department-energy-office-legacy-management-sites). Water levels were measured at each sampled well. The analytical data and associated qualifiers can be viewed in environmental database reports and are also available for viewing with dynamic mapping via the GEMS (Geospatial Environmental Mapping System) website at http://gems.lm.doe.gov/#. All six POC wells are completed in the middle sandstone unit of the Cedar Mountain Formation and are monitored to measure contaminant concentrations for comparison to proposed alternate concentration limits (ACLs), as provided in Table 1. Contaminant concentrations in the POC wells remain below their respective ACLs.

54 ENVIRONMENTAL SCIENCES↗

DOE OSTI2016

Data Validation Package, July 2016 Groundwater Sampling at the Shirley Basin South, Wyoming, Disposal Site November 2016

Sampling Period: July 14-15, 2016 The 2004 Long-Term Surveillance Plan for the Shirley Basin South (UMTRCA Title II) Disposal Site, Carbon County, Wyoming, requires annual monitoring to verify continued compliance with the pertinent alternate concentration limits (ACLs) and Wyoming Class III (livestock use) groundwater protection standards. Planned monitoring locations are shown in Attachment 1, Sampling and Analysis Work Order. Point-of-compliance (POC) wells 19-DC, 5-DC, and 5-SC, and monitoring wells 10-DC, 110-DC, 112-DC, 113-DC, 40-SC, 54-SC, 100-SC, 102-SC, and K.G.S.#3 were sampled. POC well 51-SC and downgradient well 101-SC were dry at the time of sampling. The water level was measured at each sampled well. See Attachment 2, Trip Report for additional details. Sampling and analyses were conducted in accordance with the Sampling and Analysis Plan for the U S. Department of Energy Office of Legacy Management Sites (LMS/PRO/S04351, continually updated, http://energy.gov/lm/downloads/sampling-and analysis-plan-us-department-energy-office-legacy-management-sites). ACLs are approved for cadmium, chromium, lead, nickel, radium-226, radium-228, selenium, thorium-230, and uranium in site groundwater. Time-concentration graphs of the contaminants of concern in POC wells are included in Attachment 3, Data Presentation. The only ACL exceedance in a POC well was radium-228 in well 5-DC where the concentration was 30.7 picocuries per liter (pCi/L), exceeding the ACL of 25.7 pCi/L. Concentrations of sulfate and total dissolved solids continue to exceed their respective Wyoming Class III groundwater protection standards for livestock use in wells 5-DC, 5-SC, and 54-SC as they have done throughout the sampling history; however, there is no livestock use of the water from these aquifers at the site, and no constituent concentrations exceed groundwater protection standards at the wells near the site boundary.

Carbon County, Wyoming↗

DOE OSTI2017

Solvent hold tank sample results for MCU-16-1488-1493 (December 2016), MCU-17-86-88 (January 2017), and MCU-17-119-121 (February 2017): Quarterly Report

A trend summary of three Solvent Hold Tank (SHT) monthly samples; MCU-16-1488-1493 (December 2016), MCU-17-86-88 (January 2017), and MCU-17-119-121 (February 2017) are reported. Analyses indicate that the modifier (CS-7SB) and the extractant (MaxCalix) concentrations are at their nominal recommended levels (169,000 mg/L and 46,300 mg/L respectively). The suppressor (TiDG) level has decreased to a steady state level of 673 mg/L well above the minimum recommended level (479 mg/L). This analysis confirms the Isopar™ addition to the solvent in January 18, 2017. This analysis also indicates the solvent did not require further additions. Based on the current monthly sample, the levels of TiDG, Isopar™L, MaxCalix, and modifier are sufficient for continuing operation but are expected to decrease with time. Periodic characterization and trimming additions to the solvent are recommended. No impurities above the 1000 ppm level were found in this solvent by the Semi-Volatile Organic Analysis (SVOA). No impurities were observed in the Hydrogen Nuclear Magnetic Resonance (HNMR). Another impurity observed in the samples was mercury. Up to 38 ± 8 micrograms of mercury per mL of solvent was detected in these samples (the average of the CV-AA and XRF methods). The higher mercury concentration in the solvent (as determined in the last three monthly samples) is possibly due to the higher mercury concentration in Salt Batches 8 and 9 (Tank 49H) or mixing of previously undisturbed areas of high mercury concentration in Tank 49H. The gamma level (0.21E5 dpm/mL) measured in the February SHT sample was one order of magnitude lower than the gamma levels observed in the December and January SHT samples. The February gamma level is consistent with the solvent being idle (since January 10, 2017). The gamma levels observed in the December and January SHT samples were consistent with previous monthly measurements where the process operated normally. The laboratory will continue to monitor the quality of the solvent in particular for any new impurities or degradation of the solvent components.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2018

Results for the First Quarter Calendar Year 2017 Tank 50H Salt Solution Sample

In this memorandum, the chemical and radionuclide contaminant results from the First Quarter Calendar Year 2017 (CY17) sample of Tank 50 H salt solution are presented in tabulated form. The First Quarter CY17 Tank 50H samples [a 200 mL sample obtained 6” below the surface (HTF-50-17-7) and a 1 L sample obtained 66” from the tank bottom (HTF-50-17-8)] were obtained on January 15, 2017 and received at Savannah River National Laboratory (SRNL) on January 16, 2017. Prior to obtaining the samples from Tank 50H, a single pump was run at least 4.4 hours and the samples were pulled immediately after pump shut down. All volatile organic analysis (VOA) and semi-volatile organic analysis (SVOA) were performed on the surface sample and all other analyses were performed on the variable depth sample. The information from this characterization will be used by Savannah River Remediation (SRR) for the transfer of aqueous waste from Tank 50H to the Saltstone Production Facility, where the waste will be treated and disposed of in the Saltstone Disposal Facility.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2018

Results for the Third Quarter Calendar Year 2017 Tank 50 Salt Solution Sample

In this memorandum, the chemical and radionuclide contaminant results from the Third Quarter Calendar Year 2017 (CY17) sample of Tank 50 salt solution are presented in tabulated form. The Third Quarter CY17 Tank 50 samples [a 200 mL sample obtained 6” below the surface (HTF-50-17-62) and a 1 L sample obtained 66” from the tank bottom (HTF-50-17-63)] were obtained on July 17, 2017 and received at Savannah River National Laboratory (SRNL) on July 17, 2017. Prior to obtaining the samples from Tank 50, a single pump was run at least 4.4 hours and the samples were pulled immediately after pump shut down. All volatile organic analysis (VOA) and semi-volatile organic analysis (SVOA) were performed on the surface sample and all other analyses were performed on the variable depth sample. The information from this characterization will be used by Savannah River Remediation (SRR) for the transfer of aqueous waste from Tank 50 to the Saltstone Production Facility, where the waste will be treated and disposed of in the Saltstone Disposal Facility.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2018

Automated Clean Chemistry for Bulk Analysis of Environmental Swipe Samples – Final Report

Sample preparation methods for mass spectrometry are being automated using commercial-off-the-shelf (COTS) equipment to shorten lengthy and costly manual chemical purification procedures. This development addresses a serious need in the International Atomic Energy Agency’s (IAEA) Network of Analytical Laboratories (NWAL) to increase efficiency in the Bulk Analysis of Environmental Samples for Safeguards program with a method that allows unattended, overnight operation. In collaboration with Elemental Scientific Inc. (ESI), the prepFAST-MC2 was designed based on COTS equipment. It was modified for uranium/plutonium separations using renewable columns packed with Eichrom TEVA® and UTEVA® resins, with a chemical separation method based on the Oak Ridge National Laboratory (ORNL) NWAL chemical procedure. Initial verification of individual columns yielded small elution volumes with consistent elution profiles and good recovery. Combined column calibration demonstrated ample separation without crosscontamination of the eluent. Automated packing and unpacking of the built-in columns initially showed >15% deviation in resin loading by weight, which can lead to inconsistent separations. Optimization of the packing and unpacking methods led to a reduction in the variability of the packed resin to less than 5% daily. Based on the initial experience at ORNL with the prepFAST-MC2, a second-generation model, the prepFAST-SR, was built by ESI. The newly designed prepFAST-SR has several upgrades compared with the original prepFAST-MC2. The upgrades largely addressed issues with the reliability of unpacking the Eichrom columns and with ventilation to ensure adequate removal of acid vapors. Both systems are currently installed in the Ultra-Trace Forensics Science Center at ORNL. Separations of mixed uranium and plutonium samples containing certified reference materials were analyzed by multi-collector inductively coupled plasma mass spectrometry and yielded good results. Current efforts have demonstrated a wider applicability of the prepFAST system. Near-quantitative removal of metal interferences was achieved with the system in both uranium and plutonium separated fractions. Successful system validation was completed with several archived samples. Isotopic results from archived samples and certified reference materials were well within data quality limits for the IAEA NWAL. Additional COTS equipment has been evaluated for its potential to aid the prepFAST-SR system in reducing the time allotments and cleanroom infrastructure requirements for accurate separations. Overall, these efforts help ensure continued efficient and effective operation of the NWAL. Comparison of the amount of personnel time necessary for successful manual vs. automated chemical separations showed a significant decrease in hands-on time from 9.8 hours to 35 minutes for seven samples, respectively. This documented time savings and reduced labor translates to a significant cost savings per sample. Overall, the system will enable faster sample reporting times at reduced cost by limiting personnel hours dedicated to the chemical separation.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗