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SPRUCE Deep Peat Heating (DPH) to Whole Ecosystem Warming (WEW) Metagenomes for Peat Samples Collected June 2016

This data set provides links to the results of metagenomic analyses of 44 peat samples collected on 13 June 2016 from SPRUCE experiment treatment and ambient plots. Experimental plots had received approximately 24 months of belowground warming (deep peat heating (DPH), Hanson et al. 2015) with the last 9 of those months including air warming for implementation of whole ecosystems warming (WEW – Hanson et al. 2016). The SPRUCE experiment site is located in an ombrotrophic bog forest in northern Minnesota, 40 km north of Grand Rapids, in the USDA Forest Service Marcell Experimental Forest (MEF). WEW Metagenomes: Data from these metagenomes are archived in the U.S. Department of Energy Joint Genome Institute (DOE JGI) Integrated Microbial Genomes (IMG) system and are available at the accession numbers provided below (Table 2) and in the accompanying inventory file. The easiest way to find results on IMG is at this link, https://img.jgi.doe.gov/cgi-bin/m/main.cgi, and then enter “June2016WEW” as a search term in the “Quick Genome Search:” box at the top of the page. This work was done in collaboration between ORNL, USFS and the DOE Joint Genome Institute (JGI) study that is targeting understanding the microbial metagenomes of “fungal, bacterial, and archaeal communities mediating C cycling and trace gas flux in peatland ecosystems subject to climate change” (Proposal ID: 1445).

54 ENVIRONMENTAL SCIENCES↗

Analysis of Samples Collected from the Surface of Interim Storage Canisters at Calvert Cliffs in June 2017: Revision 01.

In June 2017, dust and salt samples were collected from the surface of Spent Nuclear Fuel (SNF) dry storage canisters at the Calvert Cliffs Nuclear Power Plant. The samples were delivered to Sandia National laboratories for analysis. Two types of samples were collected: filter-backed Scotch-Brite TM pads were used to collect dry dust samples for characterization of salt and dust morphologies and distributions; and Saltsmart TM test strips were used to collect soluble salts for determining salt surface loadings per unit area. After collection, the samples were sealed into plastic sleeves for shipping. Condensation within the sleeves containing the Scotch-Brite TM samples remobilized the salts, rendering them ineffective for the intended purpose, and also led to mold growth, further compromising the samples; for these reasons, the samples were not analyzed. The SaltSmart TM samples were unaffected and were analyzed by ion chromatography for major anions and cations. The results of those analyses are presented here.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

SPRUCE Deep Peat Heat (DPH) Metagenomes for Peat Samples Collected June 2015

This data set provides links to the results of metagenomic analyses of 38 peat core samples collected on 16 June 2015 from SPRUCE experiment treatment plots after approximately one year of belowground heating. These metagenomes are archived in the U.S. Department of Energy Joint Genome Institute (DOE JGI) Integrated Microbial Genomes (IMG) system and are available at the accession numbers provided below and in the accompanying inventory file. This work was done in collaboration with the DOE Joint Genome Institute (JGI) study that is targeting understanding the microbial metagenomes of “fungal, bacterial, and archaeal communities mediating C cycling and trace gas flux in peatland ecosystems subject to climate change” (Proposal ID: 1445). The SPRUCE experiment site is an ombrotrophic bog forest in northern Minnesota, 40 km north of Grand Rapids, in the USDA Forest Service Marcell Experimental Forest (MEF).

54 ENVIRONMENTAL SCIENCES↗

TRAC Time Tags of individual particle samples collected for microscopy analysis at RMBL [AMF2] from June 2023 to August 2023

The dataset presents the time tags of individual particle samples collected on microscopy substrates during the Surface Atmosphere Integrated Field Laboratory (SAIL) campaign in Gothic, CO. A Time Resolved Aerosol Collector was deployed at the Rocky Mountain Biological Laboratory, 200 m north of AMF2 to collect ambient particles. The instrument inlet was placed 5 m above ground level. Particles are deposited on 400 mesh copper carbon-B film TEM grids (Ted Pella 01814-F). Samples are sealed and currently stored at Purdue University. A subset of the samples can be shared. Please contact dataset authors for more information. The dataset reports the sample start times in UTC and MST along with the sample ID, used to guide its location and retrieval from the storage plate. TRAC sampling started on June 17, 2023, and ended on July 31, 2023.

54 ENVIRONMENTAL SCIENCES↗

Control of the positional relationship between a sample collection instrument and a surface to be analyzed during a sampling procedure with image analysis

A system and method utilizes an image analysis approach for controlling the collection instrument-to-surface distance in a sampling system for use, for example, with mass spectrometric detection. Such an approach involves the capturing of an image of the collection instrument or the shadow thereof cast across the surface and the utilization of line average brightness (LAB) techniques to determine the actual distance between the collection instrument and the surface. The actual distance is subsequently compared to a target distance for re-optimization, as necessary, of the collection instrument-to-surface during an automated surface sampling operation.

47 OTHER INSTRUMENTATION↗

Adsorptive Films in Support of In-field UF6 Destructive Assay Sample Collection and Analysis

International Atom Energy Agency (IAEA) safeguard verification measures in gaseous centrifuge enrichment plants (GCEPs) rely on environmental sampling, non-destructive assay (NDA), and destructive assay (DA) sampling and analysis to determine uranium enrichment. UF6 bias defect measurements are made by DA sampling and analysis to assure that enrichment is consistent with declarations. DA samples are collected from a limited number of cylinders for high precision, offsite mass spectrometer analysis. Samples are typically drawn from a sampling tap into a UF6 sample bottle, then packaged, sealed, and shipped under IAEA chain of custody to an offsite analytical laboratory. Future DA safeguard measures may require improvements in efficiency and effectiveness as GCEP capacities increase and UF6 shipping regulations become increasingly more restrictive. The Pacific Northwest National Laboratory (PNNL) DA sampler concept and Laser Ablation Absorption Ratio Spectrometry (LAARS) assay method are under development to potentially provide DA safeguard tools that increase inspection effectiveness and reduce sample shipping constraints. The PNNL DA sampler concept uses a handheld sampler to collect DA samples for either onsite LAARS assay or offsite laboratory analysis. The DA sampler design will use a small sampling planchet that is coated with an adsorptive film to collect controlled quantities of UF6 gas directly from a cylinder or process sampling tap. Development efforts are currently underway at PNNL to enhance LAARS assay performance to allow high-precision onsite bias defect measurements. In this paper, we report on the experimental investigation to develop adsorptive films for the PNNL DA sampler concept. These films are intended to efficiently capture UF6 and then stabilize the collected DA sample prior to onsite LAARS or offsite laboratory analysis. Several porous material composite films were investigated, including a film designed to maximize the chemical adsorption and binding of gaseous UF6 onto the sampling planchet.

destructive assay↗

Characterization Data Package for Containerized Sludge Samples Collected from Engineered Container SCS-CON-210

This data package contains the K Basin sludge characterization results obtained by Pacific Northwest National Laboratory during processing and analysis of four sludge core samples collected from Engineered Container SCS-CON-210 in 2010 as requested by CH2M Hill Plateau Remediation Company. Sample processing requirements, analytes of interest, detection limits, and quality control sample requirements are defined in the KBC-33786, Rev. 2. The core processing scope included reconstitution of a sludge core sample distributed among four to six 4-L polypropylene bottles into a single container. The reconstituted core sample was then mixed and subsampled to support a variety of characterization activities. Additional core sludge subsamples were combined to prepare a container composite. The container composite was fractionated by wet sieving through a 2,000 micron mesh and a 500-micron mesh sieve. Each sieve fraction was sampled to support a suite of analyses. The core composite analysis scope included density determination, radioisotope analysis, and metals analysis, including the Waste Isolation Pilot Plant Hazardous Waste Facility Permit metals (with the exception of mercury). The container composite analysis included most of the core composite analysis scope plus particle size distribution, particle density, rheology, and crystalline phase identification. A summary of the received samples, core sample reconstitution and subsampling activities, container composite preparation and subsampling activities, physical properties, and analytical results are presented. Supporting data and documentation are provided in the appendices. There were no cases of sample or data loss and all of the available samples and data are reported as required by the Quality Assurance Project Plan/Sampling and Analysis Plan.

core sampling↗

Portable Automation of Static Chamber Sample Collection for Quantifying Soil Gas Flux

Quantification of soil gas flux using the static chamber method is labor intensive. The number of chambers that can be sampled is limited by the spacing between chambers and the availability of trained research technicians. An automated system for collecting gas samples from chambers in the field would eliminate the need for personnel to return to the chamber during a flux measurement period and would allow a single technician to sample multiple chambers simultaneously. This study describes Chamber Automated Sampling Equipment (FluxCASE) to collect and store chamber headspace gas samples at assigned time points for the measurement of soil gas flux. The FluxCASE design and operation is described, and the accuracy and precision of the FluxCASE system is evaluated. In laboratory measurements of nitrous oxide (N2O), carbon dioxide (CO2), and methane (CH4) concentrations of a standardized gas mixture, coefficients of variation associated with automated and manual sample collection were comparable, indicating no loss of precision. In the field, soil gas fluxes measured from FluxCASEs were in agreement with manual sampling for both N2O and CO2. Slopes of regression equations were 1.01 for CO2 and 0.97 for N2O. The 95% confidence limits of the slopes of the regression lines included the value of one, indicating no bias. Additionally, an expense analysis found a cost recovery ranging from 0.6 to 2.2 yr. Implementing the FluxCASE system is an alternative to improve the efficiency of the static chamber method for measuring soil gas flux while maintaining the accuracy and precision of manual sampling.

Davis, Morgan P.↗

Analysis of Dust Samples Collected from a Near-Marine East Coast ISFSI Site ("Site C")

In June of 2022, dust samples were collected from the surface of an in-service spent nuclear fuel dry storage canister during an inspection at an Independent Spent Fuel Storage Installation. The site is anonymous but is a near-marine or brackish water east coast location referred to here as "Site C". The purpose of the sampling was to assess the composition and abundance of the soluble salts present on the canister surface, information that provides a metric for potential corrosion risks. Following collection, the samples were delivered to Sandia National Laboratories for analysis. At Sandia, the soluble salts were leached from the dust and quantified by ion chromatography. In addition, subsamples of the dust were taken for scanning electron microscopy to determine the particle sizes, morphology, and mineralogy of the dust and salts. The results of those analyses are presented in this report.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Analysis of Dust Samples Collected from an In-Service Interim Storage System at the Maine Yankee Nuclear Site.

In July, 2016, the Electric Power Research Institute and industry partners performed a field test at the Maine Yankee Nuclear Site, located near Wiscasset, Maine. The primary goal of the field test was to evaluate the use of robots in surveying the surface of an in-service interim storage canister within an overpack; however, as part of the demonstration, dust and soluble salt samples were collected from horizontal surfaces within the interim storage system. The storage system is a vertical system made by NAC International, consisting of a steel-lined concrete overpack containing a 304 stainless steel (SS) welded storage canister. The canister did not contain spent fuel but rather greater-than-class-C waste, which did not generate significant heat, limiting airflow through the storage system. The surfaces that were sampled for deposits included the top of the shield plug, the side of the canister, and a shelf at the bottom of the overpack, just below the level of the pillar on which the canister sits. The samples were sent to Sandia National Laboratories for analysis. This report summarizes the results of those analyses. Because the primary goal of the field test was to evaluate the use of robots in surveying the surface of the canister within the overpack, collection of dust samples was carried out in a qualitative fashion, using paper filters and sponges as the sampling media. The sampling focused mostly on determining the composition of soluble salts present in the dust. It was anticipated that a wet substrate would more effectively extract soluble salts from the surface that was sampled, so both the sponges and the filter paper were wetted prior to being applied to the surface of the metal. Sampling was accomplished by simply pressing the damp substrate against the metal surface for two minutes, and then removing it. It is unlikely that the sampling method quantitatively collected dust or salts from the metal surface; however, both substrates did extract a significant amount of material. The paper filters collected both particles, trapped within the cellulose fibers of the filter, and salts, while the sponges collected only the soluble salts, with very few particles. Upon delivery to Sandia, both collection media were analyzed using the same methods. The soluble salts were leached from the substrates and analyzed via ion chromatography, and insoluble minerals were analyzed by scanning electron microscopy and energy dispersive X-ray spectroscopy. The insoluble minerals were found to consist largely of terrestrially-derived mineral fragments, dominantly quartz and biotite. Large (mm-sized) aggregates of calcium carbonate, calcium silicate, and calcium aluminum silicate were also present. The aggregates had one flat, smooth surface and one well crystallized surface, and were interpreted to be efflorescence on the inside of the overpack and in the vent, formed by seepage of cement pore fluids through joints in the steel liner of the overpack. Such efflorescence was commonly observed during the boroscope inspection of the storage system at the site. The material may have flaked off and fallen to the point where the dust was collected, or may have brushed off onto the sponges when the robot was retrieved through the inlet vent. Chemical analysis showed that the soluble salts on the shield plug were Ca- and Na-rich, with lesser K and minor Mg; the anionic component was dominated by SO 4 and Cl, with minor amounts of NO 3 . The cation composition of the soluble salts from the overpack shelf and the canister surface was similar to the filter samples, but the anions differed significantly, being dominantly NO 3 with lesser Cl and only trace SO 4 . The salts appear to represent a mixture of sea-salts (probably partially converted to nitrates and sulfates by particle-gas conversion reactions) and continental salt aerosols. Ammonium, a common component in continental aerosols, was not observed and may have been lost by degassing from the canister surface or after collection during sample storage and transportation. The demonstration at Maine Yankee has shown that the robot and sampling method used for the test can successfully be used to collect soluble salts from metal surfaces within an interim storage system overpack. The results were consistent from sample to sample, suggesting that a representative sample of the soluble salts was being collected. However, it is unlikely that the salt samples collected here represent quantitative sampling of the salts on the surfaces evaluated; for that reason, chloride densities per unit area are not presented here. It should also be noted that the relevance to storage systems at the site that contain SNF may be limited, because a heat- generating canister will result in greater airflow through the overpack, affecting dust deposition rates and possibly salt compositions.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Case Study: Systems Analysis of Y-12 Waste Sample Collection

The Environmental Management Organization has established a 90-Day Goal for characterizing, packaging, and dispositioning all waste after it has been declared. If adequate process knowledge is not available, a waste sample must be collected and analyzed. The objective of this case study is to reduce the cycle time for waste sample collection from 14.5 calendar days to 10 calendar days 95% of the time.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Analysis of Dust Samples Collected from an Inland ISFSI Site (Site A)

In September of 2020, dust samples were collected from the surface of spent nuclear fuel (SNF) dry storage canisters during an inspection at an inland Independent Spent Fuel Storage Installation. The purpose of the sampling was to assess the composition and abundance of the soluble salts present on the canister surface, information which provides a metric for potential corrosion risks. The samples were delivered to Sandia National laboratories for analysis. At Sandia, the soluble salts were leached from the dust and quantified by ion chromatography. In addition, subsamples of the dust were taken for scanning electron microscope analysis to determine the texture and mineralogy of the dust and salts. The results of those analyses are presented in this report.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Analysis of Dust Samples Collected from an Inland ISFSI Site (''Site B'').

In October of 2020, dust samples were collected from the surface of spent nuclear fuel (SNF) dry storage canisters during an inspection at an inland Independent Spent Fuel Storage Installation, the second inland site at which surface deposits have been sampled. The purpose of the sampling was to assess the composition and abundance of the soluble salts present on the canister surface, information which provides a metric for potential corrosion risks. The samples were delivered to Sandia National laboratories for analysis. At Sandia, the soluble salts were leached from the dust and quantified by ion chromatography. In addition, subsamples of the dust were taken for scanning electron microscopy to determine the texture and mineralogy of the dust and salts. The results of those analyses are presented in this report.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Wipe Sampling Collection Efficiencies and Holding Time Studies

Despite the fact that wipe sampling is commonly performed and the data produced by this technique is used to make numerous decisions, there is not an overwhelming consensus on the best method for collecting a wipe sample. It is generally agreed that, in order to produce reproducible quantitative results, consistent wetting solvents, wipe materials, sampling techniques, and sampling areas must be used. In addition, wetting solvents should be selected with consideration of the analyte of interest and wet wipes are better than dry wipes for the collection of organic chemicals. Thus, the goal of the Lawrence Livermore National Laboratory (LLNL) study was to understand factors affecting wipe sampling for specific chemical warfare agents (CWAs), including sarin (GB), soman (GD), cyclosarin (GF), distilled sulfur mustard (HD), and O-ethyl-S-(2-diisopropylaminoethyl) methylphosphonothioate (VX), and the pesticides diazinon and malathion.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Results of the Analyses of SMECT Mercury Sample Collected During Mercury Pump (MB1) Functional Check

A pump added to remove mercury from the sump of the Slurry Mix Evaporator Condensate Tank (SMECT) in DWPF was successfully tested in 2020, resulting in a sample of contaminated mercury obtained from the Mercury Purification Process (MPP) cell. The mercury in the sump of the SMECT was present as a result of steam stripping of sludge slurry in the Sludge Receipt and Adjustment Tank (SRAT) at DWPF. A schematic of the MPP system provided by DWPF personnel is shown in Appendix A. DWPF personnel supplied the following detailed description of the Hg sampling: “The sample provided is the result of DWPF extraction of mercury by means of the Mercury Pump-Water Cart. The Mercury Pump extracted the sample from the SMECT mercury sump. The pump uses pressurized water to transfer a small amount of mercury to a leachate bucket located at the Lab Mercury cell. The mercury and water were allowed to be self separated, and mercury was gravity decanted from the leachate bucket.” DWPF personnel indicate that the leachate bucket is equipped with both a top stopcock/drain and a lower/bottom stopcock/drain from which the mercury was decanted or drained out, while the separated water layer remained above the mercury during draining. The DWPF customer requested SRNL to analyze the sample for the following: gross alpha/nonvolatile beta analysis and perform a Toxicity Characteristic Leaching Procedure (TCLP) per the Environmental Protection Agency's Test Methods for Evaluating Solid Waste: Physical/Chemical Methods, SW-846. While the TCLP was preferred, a Total Metals analysis of the eight Resource Conservation and Recovery Act (RCRA) metals was deemed acceptable.2 The analytical data collected on this mercury sample will be used in planning for sample disposition as well to start a profile for future Hg disposition of Hg collected from steam stripping.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Destructive testings: dry drilling operations with TruPro system to collect samples in a powder form, from two hulls containing immobilized wastes in a hydraulic binder

The TruPro{sup R} process enables to collect a significant number of samples to characterize radiological materials. This innovative and alternative technique is experimented for the ANDRA quality-control inspection of cemented packages. It proves to be quicker and more prolific than the current methodology. Using classical statistics and geo-statistics approaches, the physical and radiological characteristics of two hulls containing immobilized wastes (sludges or concentrates) in a hydraulic binder are assessed in this paper. The waste homogeneity is also evaluated in comparison to ANDRA criterion. Sensibility to sample size (support effect), presence of extreme values, acceptable deviation rate and minimum number of data are discussed. The final objectives are to check the homogeneity of the two characterized radwaste packages and also to validate and reinforce this alternative characterization methodology. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Analysis of the Sludge Batch 9 (Macrobatch 11) DWPF Pour Stream Glass Sample Collected During the Nitric-Glycolic Acid Flowsheet Transition

A pour stream (PS) sample taken near the end of processing of Sludge Batch 9 (SB9, Macrobatch 11) during the transition to the nitric-glycolic acid (NGA) flowsheet was analyzed by the Savannah River National Laboratory (SRNL). The SB9 NGA PS sample was taken on 12/18/2022 during Melter Feed Batch 823 associated with glass canister S04773 and was transferred to SRNL in Primary Container PC0139 in February 2023.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Analysis of dust samples collected from spent nuclear fuel interim storage containers at Hope Creek, Delaware, and Diablo Canyon, California

Potentially corrosive environments may form on the surface of spent nuclear fuel dry storage canisters by deliquescence of deposited dusts. To assess this, samples of dust were collected from in-service dry storage canisters at two near-marine sites, the Hope Creek and Diablo Canyon storage installations, and have been characterized with respect to mineralogy, chemistry, and texture. At both sites, terrestrially-derived silicate minerals, including quartz, feldspars, micas, and clays, comprise the largest fraction of the dust. Also significant at both sites were particles of iron and iron-chromium metal and oxides generated by the manufacturing process. Soluble salt phases were minor component of the Hope Creek dusts, and were compositionally similar to inland salt aerosols, rich in calcium, sulfate, and nitrate. At Diablo Canyon, however, sea-salt aerosols, occurring as aggregates of NaCl and Mg-sulfate, were a major component of the dust samples. The seasalt aerosols commonly occurred as hollow spheres, which may have formed by evaporation of suspended aerosol seawater droplets, possibly while rising through the heated annulus between the canister and the overpack. The differences in salt composition and abundance for the two sites are attributed to differences in proximity to the open ocean and wave action. The Diablo Canyon facility is on the shores of the Pacific Ocean, while the Hope Creek facility is on the shores of the Delaware River, several miles from the open ocean.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗