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At least 703 records · Page 39

Genetic identification of avian samples recovered from solar energy installations

Renewable energy production and development will drastically affect how we meet global energy demands, while simultaneously reducing the impact of climate change. Although the possible effects of renewable energy production (mainly from solar- and wind-energy facilities) on wildlife have been explored, knowledge gaps still exist, and collecting data from wildlife remains (when negative interactions occur) at energy installations can act as a first step regarding the study of species and communities interacting with facilities. In the case of avian species, samples can be collected relatively easily (as compared to other sampling methods), but may only be able to be identified when morphological characteristics are diagnostic for a species. Therefore, many samples that appear as partial remains, or “feather spots”—known to be of avian origin but not readily assignable to species via morphology—may remain unidentified, reducing the efficiency of sample collection and the accuracy of patterns observed. To obtain data from these samples and ensure their identification and inclusion in subsequent analyses, we applied, for the first time, a DNA barcoding approach that uses mitochondrial genetic data to identify unknown avian samples collected at solar facilities to species. We also verified and compared identifications obtained by our genetic method to traditional morphological identifications using a blind test, and discuss discrepancies observed. Our results suggest that this genetic tool can be used to verify, correct, and supplement identifications made in the field and can produce data that allow accurate comparisons of avian interactions across facilities, locations, or technology types. We recommend implementing this genetic approach to ensure that unknown samples collected are efficiently identified and contribute to a better understanding of wildlife impacts at renewable energy projects.

14 SOLAR ENERGY↗

Parameter estimation by implicit sampling

© 2015 Mathematical Sciences Publishers. Implicit sampling is a weighted sampling method that is used in data assimilation to sequentially update state estimates of a stochastic model based on noisy and incomplete data. Here we apply implicit sampling to sample the posterior probability density of parameter estimation problems. The posterior probability combines prior information about the parameter with information from a numerical model, e.g., a partial differential equation (PDE), and noisy data. The result of our computations are parameters that lead to simulations that are compatible with the data. We demonstrate the usefulness of our implicit sampling algorithm with an example from subsurface flow. For an efficient implementation, we make use of multiple grids, BFGS optimization coupled to adjoint equations, and Karhunen-Loève expansions for dimensional reduction. Several difficulties of Markov chain Monte Carlo methods, e.g., estimation of burn-in times or correlations among the samples, are avoided because the implicit samples are independent.

Morzfeld, Matthias↗

Uncertainty Measurement for Trace Element Analysis of Uranium and Plutonium Samples by Inductively Coupled Plasma-Atomic Emission Spectrometry (ICP-AES) and Inductively Coupled Plasma-Mass Spectrometry (ICP-MS)

The measurement uncertainty estimation associated with trace element analysis of impurities in U and Pu was evaluated using the Guide to the Expression of Uncertainty Measurement (GUM). I this evaluation the uncertainty sources were identified and standard uncertainties for the components were categorized as either Type A or B. The combined standard uncertainty was calculated and a coverage factor k = 2 was applied to obtain the expanded uncertainty, U. The ICP-AES and ICP-MS methods used were developed for the multi-element analysis of U and Pu samples. A typical analytical run consists of standards, process blanks, samples, matrix spiked samples, post digestion spiked samples and independent calibration verification standards. The uncertainty estimation was performed on U and Pu samples that have been analyzed previously as part of the U and Pu Sample Exchange Programs. Control chart results and data from the U and Pu metal exchange programs were combined with the GUM into a concentration dependent estimate of the expanded uncertainty. Comparison of trace element uncertainties obtained using this model was compared to those obtained for trace element results as part of the Exchange programs. This process was completed for all trace elements that were determined to be above the detection limit for the U and Pu samples.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Sample Dissolution and Purification for 230 Th- 234 U Age-Dating

This is the standard operating procedure used by the Isotope Ratio Mass Spectrometry Group of the Chemical Sciences Division at LLNL for the preparation of a sample of uranium oxide or uranium metal for 230 Th- 234 U age-dating. The method described here includes the dissolution of a sample of uranium oxide or uranium metal, preparation of a secondary dilution, spiking of separate aliquots for uranium and thorium isotope dilution measurements, and purification of uranium and thorium aliquots for mass spectrometry. This SOP may be applied to uranium samples of unknown purity as in a nuclear forensic investigation, and also to well-characterized samples such as, for example, U 3 O 8 and U-metal certified reference materials. The sample of uranium is transferred to a quartz or PFA vial, concentrated nitric acid is added and the sample is heated on a hotplate at approximately 100°C for several hours until it dissolves. The sample solution is diluted with water to make the solution approximately 4 M HNO 3 and hydrofluoric acid is added to make it 0.05 M HF. A secondary dilution of the primary uranium solution is prepared. Separate aliquots for uranium and thorium isotope dilution measurements are taken and spiked with 233 U and 229 Th, respectively. The spiked aliquot for uranium isotope dilution analysis is purified using EiChrom UTEVA resin. The spiked aliquot for thorium isotope dilution analysis is purified by, first, a 1.8 mL AG1x8 resin bed in 9 M HCl on which U adsorbs and Th passes through; second, adsorbing Th on a 1 mL AG1x8 resin bed in 8 M HNO 3 and then eluting it with 9 M HCl followed by 0.1 M HCl + 0.005 M HF; and third, by passing the Th through a final 1.0 mL AG1x8 resin bed in 9 M HCl. The mass spectrometry is performed using the procedure 'Th and U Mass Spectrometry for 230 Th- 234 U Age Dating'.

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗

Analyses of HTF-48-12-20/24 (February, 2012) and Archived HTF-E-05-021 Tank 48H Slurry Samples

Personnel characterized a Savannah River National Laboratory (SRNL) archived sample of Tank 48H slurry (HTF-E-05-021) in addition to the composite of samples HTF-48-12-20 and HTF-48-12-24, which were both retrieved in February 2012. The combined February 2012 sample is referred to as HTF-48-12-20/24 in this report. The results from these analyses are compared with Tank 48H samples analyzed in 2003, 2004, and 2005. This work supports the effort to demonstrate copper-catalyzed peroxide oxidation (CCPO) of organic content in this material. The principal findings with respect to the chemical and physical characteristics of the most recent sample are: (1) The measured potassium tetraphenylborate (KTPB) solid concentration is 1.76 wt %; (2) Titanium was in line with 2004 and 2005 slurry measurements at 897 mg/L, it represents 0.1535 ± 0.0012 wt % monosodium titanate (MST); (3) The measured insoluble solids content was 1.467 wt %; (4) The free hydroxide concentration in the Tank 48H filtrate sample (1.02 ± 0.02 M) is close to the Tank 48H limit (1.0 M); (5) Carbonate reported by total inorganic carbon (TIC, 1.39 ± 0.03 M) is more than double the concentrations measured in past (2003-2005) samples; (6) The soluble potassium content (measured at 286 ± 23 mg/L) in the filtrate is in line with all past measurements; and (7) The measured 137 Cs concentration is 7.81E + 08 ± 3.9E + 07 dpm/mL of slurry (1.33 ± 5% Ci/gallon or 3.18E + 05 ± 5% curies of 137 Cs in the tank) in the slurry which is in agreement with the 2005 report of 3.14E + 05 ± 1.5% curies of 137 Cs in the tank. The filtrate 137 Cs concentration is 2.57E + 07 ± 2.6E + 05 dpm/mL. This result is consistent with previous results. Significant analytical data are summarized in Table 1.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Assessment of the Group 3-4 (HV-S1, HV-S2, IHLW-S1) Stack Sampling Probe Locations for Compliance with ANSI/HPS N13.1-1999

This document reports on a series of tests conducted to assess the proposed air sampling locations for the Hanford Tank Waste Treatment and Immobilization Plant (WTP) Group 3-4 exhaust stacks with respect to the applicable criteria regarding the placement of an air sampling probe. The HV-S1, HV-S2, and IHLW-S1 exhaust stacks were tested together as a group (Test Group 3-4) because they share a geometric attribute: the common factor in their design is that the last significant flow disturbance upstream of the air sampling probe is a jog (i.e., two conjoined bends of equal and opposite curvature resulting in a change in elevation of the duct). Federal regulations require that a sampling probe be located in the exhaust stack according to criteria established by the American National Standards Institute/Health Physics Society (ANSI/HPS) N13.1-1999, Sampling and Monitoring Releases of Airborne Radioactive Substances from the Stack and Ducts of Nuclear Facilities. These criteria address the capability of the sampling probe to extract a sample that represents the effluent stream.

Glissmeyer, John A.↗

Characterization Of Sample HTF-13-13-128

Savannah River Remediation (SRR) has requested that Savannah River National Laboratory (SRNL) characterize a sample of Tank 13 in preparation for Sludge Batch 9 (SB9). A 200 mL sample of Tank 13 was received by SRNL on July 22, 2013 (Tank Farm sample ID HTF-13-13-128). Characterization of the sample to meet the requirements of the request is complete. Results include: visual observations; slurry and supernatant density; weight percent total and insoluble solids; supernatant characterization; total alpha, total beta, and several radionuclide analyses; and elemental analyses of the dried solids. The sample was very fluid. After settling overnight, there was a small layer of solids on the bottom of the sample container (a 250 mL HDPE bottle) with the remainder being clear supernatant. To better show the sludge solids relative to the overall sample, 25 mL of slurry was placed in a graduated cylinder and allowed to settle over a weekend (approximately 90 hours). The sludge layer was at the approximately 4 mL. The small visually observed quantity of insoluble solids was confirmed with a low weight percent insoluble solids of 0.94%.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

COMPARISON OF RESULTS FOR QUARTER 3 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 March 20, 2013. Representatives from the U.S. Nuclear Regulatory Commission and the 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, and Table 1 presents 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 (ANSI N42.22). The NFS split sample report does not specify the confidence level of reported uncertainties (NFS 2013). Therefore, standard two sigma reporting is assumed and uncertainty values were divided by 1.96. In conclusion, most DER values were less than 3 and results are consistent with low (e.g., background) concentrations. The gross beta result for sample 5198W0012 was the exception. The ORAU result of 9.23 &plusmn 0.73 pCi/L from location MCD is well above NFS's result of -0.567 &plusmn 0.63 pCi/L (non-detected). NFS's data package included a detected result for U-233/234, but no other uranium or plutonium detection, and nothing that would suggest the presence of beta-emitting radionuclides. The ORAU laboratory reanalyzed sample 5198W0012 using the remaining portion of the sample volume and a result of 11.3 &plusmn 1.1 pCi/L was determined. As directed, the laboratory also counted the filtrate using gamma spectrometry analysis and identified only naturally occurring or ubiquitous man-made constituents, including beta emitters that are presumably responsible for the elevated gross beta values.

54 ENVIRONMENTAL SCIENCES↗

Analysis Of The Sludge Batch 7b (Macrobatch 9) DWPF Pour Stream Glass Sample (Rev. 1)

The Defense Waste Processing Facility (DWPF) began processing Sludge Batch 7b (SB7b), also referred to as Macrobatch 9 (MB9), in January 2012. SB7b is a blend of the heel of Tank 40 from Sludge Batch 7a (SB7a) and the SB7b material that was transferred to Tank 40 from Tank 51. SB7b was processed using Frit 418. During processing of each sludge batch, the DWPF is required to take at least one glass sample to meet the objectives of the Glass Product Control Program (GPCP), which is governed by the DWPF Waste Form Compliance Plan, and to complete the necessary Production Records so that the final glass product may be disposed of at a Federal Repository. Two pour stream glass samples were collected while processing SB7b. The samples were transferred to the Savannah River National Laboratory (SRNL) where one was analyzed and the other was archived. The following conclusions were drawn from the analytical results provided in this report: The sum of oxides for the official SB7b pour stream glass is within the Product Composition Control System (PCCS) limits (95-105 wt%); The average calculated Waste Dilution Factor (WDF) for SB7b is 2.3. In general, the measured radionuclide content of the official SB7b pour stream glass is in good agreement with the calculated values from the Tank 40 dried sludge results from the SB7b Waste Acceptance Program Specification (WAPS) sample; As in previous pour stream samples, ruthenium and rhodium inclusions were detected by Scanning Electron Microscopy-Electron Dispersive Spectroscopy (SEM-EDS) in the SB7b pour stream sample; The Product Consistency Test (PCT) results indicate that the official SB7b pour stream glass meets the waste acceptance criteria for durability with a normalized boron release of 0.8 g/L, which is an order of magnitude less than the Environmental Assessment (EA) glass; The measured density of the SB7b pour stream glass was 2.70 g/cm 3 ; The Fe 2+ /ΣFe ratio of the SB7b pour stream samples was 0.07.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

June 2011 Natural Gas and Produced Water Sampling at the Gasbuggy, New Mexico, Site

Annual natural gas and produced water monitoring was conducted for gas wells adjacent to Section 36, where the Gasbuggy test was conducted, in accordance with the draft Long-Term Surveillance and Maintenance Plan for the Gasbuggy Site, Rio Arriba County, New Mexico. Sampling and analysis were conducted as specified in the Sampling and Analysis Plan for U.S. Department of Energy Office of Legacy Management Sites (LMS/PLN/S04351, continually updated). Natural gas samples were collected for tritium and carbon-14 analyses. Produced water samples were collected and analyzed for tritium, gamma-emitting radionuclides (by high-resolution gamma spectrometry), gross alpha, and gross beta. A duplicate produced water sample was collected from well 30-039-21743. Produced water samples were not collected at locations 30-039-30161 and 30-039-21744 because of the lack of water. Samples were not collected from location 30-039-29988 because the well was shut-in.

54 ENVIRONMENTAL SCIENCES↗

Sample Results from MCU Solids Outage

Savannah River National Laboratory (SRNL) has received several solid and liquid samples from MCU in an effort to understand and recover from the system outage starting on April 6, 2014. SRNL concludes that the presence of solids in the Salt Solution Feed Tank (SSFT) is the likely root cause for the outage, based upon the following discoveries: A solids sample from the extraction contactor #1 proved to be mostly sodium oxalate; A solids sample from the scrub contactor#1 proved to be mostly sodium oxalate; A solids sample from the Salt Solution Feed Tank (SSFT) proved to be mostly sodium oxalate; An archived sample from Tank 49H taken last year was shown to contain a fine precipitate of sodium oxalate; A solids sample from ; A liquid sample from the SSFT was shown to have elevated levels of oxalate anion compared to the expected concentration in the feed. Visual inspection of the SSFT indicated the presence of precipitated or transferred solids, which were likely also in the Salt Solution Receipt Tank (SSRT). The presence of the solids coupled with agitation performed to maintain feed temperature resulted in oxalate solids migration through the MCU system and caused hydraulic issues that resulted in unplanned phase carryover from the extraction into the scrub, and ultimately the strip contactors. Not only did this carryover result in the Strip Effluent (SE) being pushed out of waste acceptance specification, but it resulted in the deposition of solids into several of the contactors. At the same time, extensive deposits of aluminosilicates were found in the drain tube in the extraction contactor #1. However it is not known at this time how the aluminosilicate solids are related to the oxalate solids. The solids were successfully cleaned out of the MCU system. However, future consideration must be given to the exclusion of oxalate solids into the MCU system. There were 53 recommendations for improving operations recently identified. Some additional considerations or additional details are provided below as recommendations. From this point on, IC-Anions analyses of the DSSHT should be part of the monthly routine analysis in order to spot negative trends in the oxalate leaving the MCU system. Care must be taken to monitor the oxalate content to watch for sudden precipitation of oxalate salts in the system; Conduct a study to optimize the cleaning strategy at ARP-MCU through decreasing the concentration or entirely eliminating the oxalic acid; The contents of the SSFT should remain unagitated. Routine visual observation should be maintained to ensure there is not a large buildup of solids. As water with agitation provided sufficient removal of the solids in the feed tank, it should be considered as a good means for dissolving oxalate solids if they are found in the future; Conduct a study to improve prediction of oxalate solubility in salt batch feed materials. As titanium and mercury have been found in various solids in this report, evaluate if either element plays a role in oxalate solubility during processing; Salt batch characterization focuses primarily on characterization and testing of unaltered Tank 21H material; however, non-typical feeds are developed through cleaning, washing, and/or sump transfers. As these solutions are processed through MCU, they may precipitate solids or reduce performance. Salt batch characterization and testing should be expanded to encompass a broader range of feeds that may be processed through ARPMCU.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Analysis of Dust Samples Collected from an Unused Spent Nuclear Fuel Interim Storage Container at Hope Creek, Delaware

In July, 2014, the Electric Power Research Institute and industry partners sampled dust on the surface of an unused canister that had been stored in an overpack at the Hope Creek Nuclear Generating Station for approximately one year. The foreign material exclusion (FME) cover that had been on the top of the canister during storage, and a second recently-removed FME cover, were also sampled. This report summarizes the results of analyses of dust samples collected from the unused Hope Creek canister and the FME covers. Both wet and dry samples of the dust/salts were collected, using SaltSmart(TM) sensors and Scotch-Brite(TM) abrasive pads, respectively. The SaltSmart(TM) samples were leached and the leachate analyzed chemically to determine the composition and surface load per unit area of soluble salts present on the canister surface. The dry pad samples were analyzed by X-ray fluorescence and by scanning electron microscopy to determine dust texture and mineralogy; and by leaching and chemical analysis to deter mine soluble salt compositions. The analyses showed that the dominant particles on the canister surface were stainless steel particles, generated during manufacturing of the canister. Sparse environmentally - derived silicates and aluminosilicates were also present. Salt phases were sparse, and consisted of mostly of sulfates with rare nitrates and chlorides. On the FME covers, the dusts were mostly silicates/aluminosilicates; the soluble salts were consistent with those on the canister surface, and were dominantly sulfates. It should be noted that the FME covers were w ashed by rain prior to sampling, which had an unknown effect of the measured salt loads and compositions. Sulfate salts dominated the assemblages on the canister and FME surfaces, and included Ca-SO 4 , but also Na-SO 4 , K-SO 4 , and Na-Al-SO 4 . It is likely that these salts were formed by particle - gas conversion reactions, either prior to, or after, deposition. These reactions involve reaction of carbonate, chloride, or nitrate salts with at mospheric SO 2 , sulfuric acid, or a mmonium sulfate to form sulfate minerals. The Na-Al-SO 4 phase is unusual, and may have formed by reaction of Na-Al containing phases in aluminum smelter emissions with SO 2 , also present in smelter emissions. An aluminum smelter is located in Camden, NJ, 40 miles NE of the Hope Creek Site.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Analysis of Tank 23H Samples in Support of Salt Batch Planning

Savannah River Remediation obtained three samples from different heights within Tank 23H. The samples were analyzed by Savannah River National Laboratory to support salt batch planning. The results from the analysis indicate the top two samples from the tank appear similar in composition. The lowest sample from the tank contained significantly more solids and a more concentrated salt solution. The filtered supernate from the bottom sample showed ~60% lower Sr-90 and Pu-238 concentrations than the decanted (unfiltered) supernate results which may indicate the presence of some small amount of entrained solid particles in the decanted sample. The mercury concentrations measured in the filtered supernate were fairly low for all three samples ranging from 11.2 to 42.3 mg/L.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Assessment of the National Research Universal Reactor Proposed New Stack Sampling Probe Location for Compliance with ANSI/HPS N13.1-1999

This document reports on a series of tests conducted to assess the proposed air sampling location for the National Research Universal reactor (NRU) complex exhaust stack, located in Chalk River, Ontario, Canada, with respect to the applicable criteria regarding the placement of an air sampling probe. Due to the age of the equipment in the existing monitoring system, and the increasing difficulty in acquiring replacement parts to maintain this equipment, a more up-to-date system is planned to replace the current effluent monitoring system, and a new monitoring location has been proposed. The new sampling probe should be located within the exhaust stack according to the criteria established by the American National Standards Institute/Health Physics Society (ANSI/HPS) N13.1-1999, Sampling and Monitoring Releases of Airborne Radioactive Substances from the Stack and Ducts of Nuclear Facilities. These criteria address the capability of the sampling probe to extract a sample that represents the effluent stream. The internal Pacific Northwest National Laboratory (PNNL) project for this task was 65167, Atomic Energy Canada Ltd. Chalk River Effluent Duct Flow Qualification. The testing described in this document was guided by the Test Plan: Testing of the NRU Stack Air Sampling Position (TP-STMON-032).

21 SPECIFIC NUCLEAR REACTORS AND ASSOCIATED PLANTS↗

Assessment of the LV-C2 Stack Sampling Probe Location for Compliance with ANSI/HPS N13.1-1999

This document reports on a series of tests conducted to assess the proposed air sampling location for the Hanford Tank Waste Treatment and Immobilization Plant (WTP) Low-Activity Waste (LAW) C2V (LV-C2) exhaust stack with respect to the applicable criteria regarding the placement of an air sampling probe. Federal regulations require that a sampling probe be located in the exhaust stack according to the criteria established by the American National Standards Institute/Health Physics Society (ANSI/HPS) N13.1-1999, Sampling and Monitoring Releases of Airborne Radioactive Substances from the Stack and Ducts of Nuclear Facilities. These criteria address the capability of the sampling probe to extract a sample that represents the effluent stream. The tests were conducted on the LV-C2 scale model system. Based on the scale model tests, the location proposed for the air sampling probe in the scale model stack meets the requirements of the ANSI/HPS N13.1-1999 standard for velocity uniformity, flow angle, gas tracer and particle tracer uniformity. Additional velocity uniformity and flow angle tests on the actual stack will be necessary during cold startup to confirm the validity of the scale model results in representing the actual stack.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Trace metal analysis by laser ablation-inductively coupled plasmamass spectrometry and x-ray K-edge densitometry of forensic samples

This dissertation describes a variety of studies on the determination of trace elements in samples with forensic importance. Laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS) was used to determine the trace element composition of numerous lipstick samples. Lipstick samples were determined to be homogeneous. Most lipstick samples of similar colors were readily distinguishable at a 95% confidence interval based on trace element composition. Numerous strands of a multi-strand speaker cable were analyzed by LA-ICP-MS. The strands in this study are spatially heterogeneous in trace element composition. In actual forensic applications, the possibility of spatial heterogeneity must be considered, especially in cases where only small samples (e.g., copper wire fragments after an explosion) are available. The effects of many unpredictable variables, such as weather, temperature, and human activity, on the retention of gunshot residue (GSR) around projectile wounds were assessed with LAICP- MS. Skin samples around gunshot and stab wounds and larvae feeding in and around the wounds on decomposing pig carcasses were analyzed for elements consistent with GSR (Sb, Pb, Ba, and Cu). These elements were detected at higher levels in skin and larvae samples around the gunshot wounds compared to the stab wounds for an extended period of time throughout decomposition in both a winter and summer study. After decomposition, radiographic images of the pig bones containing possible damage from bullets revealed metallic particles embedded within a number of bones. Metallic particles within the bones were analyzed with x-ray, K-edge densitometry and determined to contain lead, indicating that bullet residue can be retained throughout decomposition and detected within bones containing projectile trauma.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

Data Validation Package - July 2016 Groundwater Sampling at the Gunnison, Colorado, Disposal Site

Groundwater sampling at the Gunnison, Colorado, Disposal Site is conducted every 5 years to monitor disposal cell performance. During this event, samples were collected from eight monitoring wells as specified in the 1997 Long-Term Surveillance Plan for the Gunnison, Colorado, Disposal Site. 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, http://energy.gov/lm/downloads/sampling-and­ analysis-plan-us-department-energy-office-legacy-management-sites). Planned monitoring locations are shown in Attachment 1, Sampling and Analysis Work Order. A duplicate sample was collected from location 0723. Water levels were measured at all monitoring wells that were sampled and seven additional wells. 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 require additional action or follow-up.

54 ENVIRONMENTAL SCIENCES↗

Oak ridge national laboratory automated clean chemistry for bulk analysis of environmental swipe samples

To shorten the lengthy and costly manual chemical purification procedures, sample preparation methods for mass spectrometry are being automated using commercial-off-the-shelf (COTS) equipment. This addresses a serious need in the nuclear safeguards community to debottleneck the separation of U and Pu in environmental samples—currently performed by overburdened chemists—with a method that allows unattended, overnight operation. In collaboration with Elemental Scientific Inc., the prepFAST-MC2 was designed based on current COTS equipment that was modified for U/Pu separations utilizing Eichrom™ TEVA and UTEVA resins. 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. The reproducibility of the automated system was tested with samples containing 30 ng U and 15 pg Pu, which were separated in a series with alternating reagent blanks. These experiments showed very good washout of both the resin and the sample from the columns as evidenced by low blank values. Analysis of the major and minor isotope ratios for U and Pu provided values well within data quality limits for the International Atomic Energy Agency. Additionally, system process blanks spiked with 233U and 244Pu tracers were separated using the automated system after it was moved outside of a clean room and yielded levels equivalent to clean room blanks, confirming that the system can produce high quality results without the need for expensive clean room infrastructure. 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 costs by limiting personnel hours dedicated to the chemical separation.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗