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DOE OSTI2014

Biomass Compositional Analysis Laboratory (Fact Sheet)

At the Biomass Compositional Analysis Laboratory, NREL scientists have more than 20 years of experience supporting the biomass conversion industry. They develop, refine, and validate analytical methods to determine the chemical composition of biomass samples before, during, and after conversion processing. These high-quality compositional analysis data are used to determine feedstock compositions as well as mass balances and product yields from conversion processes.

09 BIOMASS FUELS↗

DOE OSTI2020

Automated Coupling of Nanodroplet Sample Preparation with Liquid Chromatography–Mass Spectrometry for High-Throughput Single-Cell Proteomics

Single-cell proteomics can provide critical biological insight into the cellular heterogeneity that is masked by bulk-scale analysis. Here, we have developed a nanoPOTS (nanodroplet processing in one pot for trace samples) platform and demonstrated its broad applicability for single-cell proteomics. However, because of nanoliter-scale sample volumes, the nanoPOTS platform is not compatible with automated LC-MS systems, which significantly limits sample throughput and robustness. To address this challenge, we have developed a nanoPOTS autosampler allowing fully automated sample injection from nanowells to LC-MS systems. We also developed a sample drying, extraction, and loading workflow to enable reproducible and reliable sample injection. The sequential analysis of 20 samples containing 10 ng tryptic peptides demonstrated high reproducibility with correlation coefficients of >0.995 between any two samples. The nanoPOTS autosampler can provide analysis throughput of 9.6, 16, and 24 single cells per day using 120, 60, and 30 min LC gradients, respectively. As a demonstration for single-cell proteomics, the autosampler was first applied to profiling protein expression in single MCF10A cells using a label-free approach. At a throughput of 24 single cells per day, an average of 256 proteins was identified from each cell and the number was increased to 731 when the Match Between Runs algorithm of MaxQuant was used. Using a multiplexed isobaric labeling approach (TMT-11plex), ~77 single cells could be analyzed per day. We analyzed 152 cells from three acute myeloid leukemia cell lines, resulting in a total of 2558 identified proteins with 1465 proteins quantifiable (70% valid values) across the 152 cells. These data showed quantitative single-cell proteomics can cluster cells to distinct groups and reveal functionally distinct differences.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2022

Analysis of DWPF Sludge Batch 6 (Macrobatch 7) Pour Stream Glass Samples

The Defense Waste Processing Facility (DWPF) began processing Sludge Batch 6 (SB6), also referred to as Macrobatch 7 (MB7), in June 2010. SB6 is a blend of the heel of Tank 40 from Sludge Batch 5 (SB5), H-Canyon Np transfers and SB6 that was transferred to Tank 40 from Tank 51. SB6 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 and to complete the necessary Production Records so that the final glass product may be disposed of at a Federal Repository. Four pour stream glass samples and two Melter Feed Tank (MFT) slurry samples were collected while processing SB6. The samples were transferred to the Savannah River National Laboratory (SRNL) where they were analyzed.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2021

Omics-Lethal Human Viruses, Influenza A Experiment IM101

The purpose of this experiment was to evaluate the host mouse response to wild-type Influenza A/Vietnam/1203/2004 (H5N1) virus, Influenza A/California/04/2009 (H1N1) virus, and Influenza A/Vietnam/1203/2004 (H5N1; "PB2-627E" and "NS1trunc124") infection. Sample data was obtained from whole mouse lung and processed for transcriptomics expression analysis. Secondary host-associated viral dataset downloads contain one or more statistically processed (normalization data transformation) quantitative dataset collections resulting in qualitative expression analyses of primary host-pathogen experimental study designs. Transcriptomics dataset downloads have a direct relationship to a primary sample submission corresponding to a specific Influenza A virus host infection.

59 BASIC BIOLOGICAL SCIENCES↗

DOE OSTI2024

Rapid measurement of soluble xylo-oligomers using near-infrared spectroscopy (NIRS) and multivariate statistics: calibration model development and practical approaches to model optimization

Rapid monitoring of biomass conversion processes using techniques such as near-infrared (NIR) spectroscopy can be substantially quicker and less labor-, resource-, and energy-intensive than conventional measurement techniques such as gas or liquid chromatography (GC or LC) due to the lack of solvents and preparation methods, as well as removing the need to transfer samples to an external lab for analytical evaluation. The purpose of this study was to determine the feasibility of rapid monitoring of a biomass conversion process using NIR spectroscopy combined with multivariate statistical modeling, and to examine the impact of (1) subsetting the samples in the original dataset by process location and (2) reducing the spectral range used in the calibration model on model performance. We develop multivariate calibration models for the concentrations of soluble xylo-oligosaccharides (XOS), monomeric xylose, and total solids at multiple points in a biomass conversion process which produces and then purifies XOS compounds from sugar cane bagasse. A single model using samples from multiple locations in the process stream showed acceptable performance as measured by standard statistical measures. However, compared to the single model, we show that separate models built by segregating the calibration samples according to process location show improved performance. We also show that combining an understanding of the sample spectra with simple multivariate analysis tools can result in a calibration model with a substantially smaller spectral range that provides essentially equal performance to the full-range model. We demonstrate that real-time monitoring of soluble xylo-oligosaccharides (XOS), monomeric xylose, and total solids concentration at multiple points in a process stream using NIR spectroscopy coupled with multivariate statistics is feasible. Segregation of sample populations by process location improves model performance. Models using a reduced spectral range containing the most relevant spectral signatures show very similar performance to the full-range model, reinforcing the importance of performing robust exploratory data analysis before beginning multivariate modeling.

09 BIOMASS FUELS↗

DOE OSTI2020

Summary Report For The Analysis Of The Sludge Batch 7b (Macrobatch 9) DWPF Pour Stream Glass Sample For Canister S04023 (Rev. 1)

In order to comply with the Defense Waste Processing Facility (DWPF) Waste Form Compliance Plan for Sluldge Batch 7b, Savannah River National Laboratory (SRNL) personnel characterized the Defense Waste Processing Facility (DWPF) pour stream (PS) glass sample collected while filling canister S04023. This report summarizes the results of the compositional analysis for reportable oxides and radionuclides and the normalized Product Consistency Test (PCT) results. The PCT responses indicate that the DWPF produced glass that is significantly more durable than the Environmental Assessment glass.

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DOE OSTI2020

Characterization Report for the MP-1 Experiment Fabrication Campaign

This report covers the results of MP 1 fuel characterization analysis to provide a detailed understanding of the as-fabricated fuel that would be irradiated in the MP 1 (Mini-Plate 1) experiment. The work was performed at Pacific Northwest National Laboratory (PNNL), Idaho National Laboratory (INL), and Los Alamos National Laboratory (LANL). Characterization of the as-fabricated fuel was performed in accordance with Characterization Plan for the Fabrication of U 10Mo for the MP 1 Experiment, hereinafter the MP 1 Characterization Plan (MAQP 2016). Under the MP 1 Characterization Plan, fuel foils at different points in the foil fabrication process (e.g., hot rolled annealed, cold rolled annealed) were studied to understand the effect of various thermomechanical processes on the fuel microstructure. Samples were sent to each of the three organizations so that testing and analysis could be performed independently using similar equipment and a standardized set of measurement and analysis procedures. The MP 1 experiment will provide an opportunity to understand the effects of processing conditions on the final fuel microstructure, to compare independently obtained results, and achieve a three-way validation. PNNL characterized 28 uranium–10 wt% molybdenum (U 10Mo) samples. Six pieces/specimens from each sample/foil were sectioned, in accordance with the MP 1 Characterization Plan. Similarly, INL and LANL also examined 24 and 17 U 10Mo specimens, respectively. These total 69 samples consist of six types of MP 1 characterization foils fabricated by Babcock and Wilcox Technologies (BWXT) from ingots produced by the Y-12 National Security Complex: • 0.047 in.-thick hot-rolled and annealed samples with and without Zr layers • 0.02 in.-thick cold-rolled and annealed samples with and without Zr layers • 0.01 in.-thick cold-rolled and annealed samples with and without Zr layers. Microstructure, chemical composition, carbide morphology, U 10Mo foil thickness, Zr thickness, mechanical properties (microhardness), and density were evaluated in both longitudinal and transverse directions for foils of the three different thicknesses.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2021

Characterization Report for the MP-1 Experiment Fabrication Campaign (Rev.1)

This report covers the results of MP 1 fuel characterization analysis to provide a detailed understanding of the as-fabricated fuel that would be irradiated in the MP 1 (Mini-Plate 1) experiment. The work was performed at Pacific Northwest National Laboratory (PNNL), Idaho National Laboratory (INL), and Los Alamos National Laboratory (LANL). Characterization of the as-fabricated fuel was performed in accordance with Characterization Plan for the Fabrication of U 10Mo for the MP 1 Experiment, hereinafter the MP 1 Characterization Plan (MAQP 2016). Under the MP 1 Characterization Plan, fuel foils at different points in the foil fabrication process (e.g., hot rolled annealed, cold rolled annealed) were studied to understand the effect of various thermomechanical processes on the fuel microstructure. Samples were sent to each of the three organizations so that testing and analysis could be performed independently using similar equipment and a standardized set of measurement and analysis procedures. The MP 1 experiment will provide an opportunity to understand the effects of processing conditions on the final fuel microstructure, to compare independently obtained results, and achieve a three-way validation. PNNL characterized 28 uranium–10 wt% molybdenum (U 10Mo) samples. Six pieces/specimens from each sample/foil were sectioned, in accordance with the MP 1 Characterization Plan. Similarly, INL and LANL also examined 24 and 17 U 10Mo specimens, respectively. These total 69 samples consist of six types of MP 1 characterization foils fabricated by Babcock and Wilcox Technologies (BWXT) from ingots produced by the Y-12 National Security Complex: (a.) 0.047 in.-thick hot-rolled and annealed samples with and without Zr layers; (b.) 0.02 in.-thick cold-rolled and annealed samples with and without Zr layers; and (c.) 0.01 in.-thick cold-rolled and annealed samples with and without Zr layers. Microstructure, chemical composition, carbide morphology, U 10Mo foil thickness, Zr thickness, mechanical properties (microhardness), and density were evaluated in both longitudinal and transverse directions for foils of the three different thicknesses.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2016

Testing of the Defense Waste Processing Facility Cold Chemical Dissolution Method in Sludge Batch 9 Qualification

For each sludge batch that is processed in the Defense Waste Processing Facility (DWPF), the Savannah River National Laboratory (SRNL) tests the applicability of the digestion methods used by the DWPF Laboratory for elemental analysis of Sludge Receipt and Adjustment Tank (SRAT) Receipt samples and SRAT Product process control samples. DWPF SRAT samples are typically dissolved using a method referred to as the DWPF Cold Chemical or Cold Chem Method (CC), (see DWPF Procedure SW4- 15.201). Testing indicates that the CC method produced mixed results. The CC method did not result in complete dissolution of either the SRAT Receipt or SRAT Product with some fine, dark solids remaining. However, elemental analyses did not reveal extreme biases for the major elements in the sludge when compared with analyses obtained following dissolution by hot aqua regia (AR) or sodium peroxide fusion (PF) methods. The CC elemental analyses agreed with the AR and PF methods well enough that it should be adequate for routine process control analyses in the DWPF after much more extensive side-by-side tests of the CC method and the PF method are performed on the first 10 SRAT cycles of the Sludge Batch 9 (SB9) campaign. The DWPF Laboratory should continue with their plans for further tests of the CC method during these 10 SRAT cycles.

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DOE OSTI2022

Testing of the Defense Waste Processing Facility Cold Chemical Dissolution Method in Sludge Batch 10 Qualification

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DOE OSTI2022

Sampling and Analysis Plan for Partial Closure of Solid Waste Management Unit #16; Addendum Part I for Delineating BH-056

On July 11, 2022, Sandia National Laboratories in California (SNL/CA) submitted a Response to Regional Water Quality Control Board Comments on Soil Sampling Results for Closure of a Portion of SWMU #16 in response to the February 16,2022 San Francisco Bay Regional Water Quality Control Board’s (SFRWQCB) letter requesting supporting information for the recommended closure of 7,700 linear feet of abandoned sewer lines. On August 18, 2022, SFRWQCB further requested a Sampling and Analysis Plan (SAP) for additional “step-out” sampling to delineate the potential presence of benzidine near borehole BH-056, which is located near the former sewer line. SNL/CA is in the process of contracting Weiss Associates (Weiss) to perform and oversee the boring, sampling, analysis, and report development to determine the potential presence and extent of benzidine. This document outlines the work that is anticipated, including the development of the SAP, to complete the investigation and submit a final report to the SFRWQCB. The work proposed by Weiss provides an estimated schedule for completing the investigation and developing the addendum Part II SAP for the project. In addition, Weiss provided a preliminary estimate of the sample locations (see Attachment A) which serve as addendum Part I of the SAP requested by the SFRWQCB. The contractor will submit the addendum Part II SAP, to satisfy the SFRWQCB requirement, before proceeding with any work.

54 ENVIRONMENTAL SCIENCES↗

DOE OSTI2018

A Review of Flow Analysis Methods for Determination of Radionuclides in Nuclear Wastes and Nuclear Reactor Coolants

The safety and security nuclear power plant operations depends on the application of the most appropriate techniques and methods of chemical analysis, where modern flow analysis methods find increasing applications. Nevetheless, the current status of development of these methods is more limited than might be expected from their authentic advantages. The main aim of this contribution is to review automated flow analysis procedures developed with various detection methods for application in the nuclear energy industry. The flow analysis methods for determination of radionuclides that have been reported to date have been primarily focused mainly on environmental applications. The needs and benefits of the application of flow methods for the monitoring of nuclear wastes and for process analysis of the primary circuit coolants of light water nuclear reactors are discussed. Application of continuous flow methods (CFA) or injection methods (FIA, SIA) of flow analysis with radiometric detection shorterns the time of analysis and improves precision of determinations due to mechanization of time-consuming operations of sample processing. The use of mass spectrometry (MS) detection enables multicomponent analyses and determination of transuranic isotopes with much better limits of detection compared to radiometric detection.

radiochemical analysis, Sequential Injection and F↗

DOE OSTI2016

The impact of alterations in lignin deposition on cellulose organization of the plant cell wall

Not Available

59 BASIC BIOLOGICAL SCIENCES↗

DOE OSTI2016

Formation of periodic interfacial misfit dislocation array at the InSb/GaAs interface via surface anion exchange

The relationship between growth temperature and the formation of periodic interfacial misfit (IMF) dislocations via the anion exchange process in InSb/GaAs heteroepitaxy was systematically investigated. The microstructural and electrical properties of the epitaxial layer were characterized using atomic force microscope, high-resolution x-ray diffraction, transmission electron microscopy, and Hall resistance measurement. The formation of interfacial misfit (IMF) dislocation arrays depended on growth temperature. A uniformly distributed IMF array was found in a sample grown at 310 °C, which also exhibited the lowest threading dislocation density. The analysis suggested that an incomplete As-for-Sb anion exchange process impeded the formation of IMF on sample grown above 310 °C. At growth temperature below 310 °C, island coalescence led to the formation of 60° dislocations and the disruption of periodic IMF array. All samples showed higher electron mobility at 300 K than at 77 K.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

DOE OSTI2016

Biosecurity through Public Health System Design.

We applied modeling and simulation to examine the real-world tradeoffs between developingcountry public-health improvement and the need to improve the identification, tracking, and security of agents with bio-weapons potential. Traditionally, the international community has applied facility-focused strategies for improving biosecurity and biosafety. This work examines how system-level assessments and improvements can foster biosecurity and biosafety. We modeled medical laboratory resources and capabilities to identify scenarios where biosurveillance goals are transparently aligned with public health needs, and resource are distributed in a way that maximizes their ability to serve patients while minimizing security a nd safety risks. Our modeling platform simulates key processes involved in healthcare system operation, such as sample collection, transport, and analysis at medical laboratories. The research reported here extends the prior art by provided two key compone nts for comparative performance assessment: a model of patient interaction dynamics, and the capability to perform uncertainty quantification. In addition, we have outlined a process for incorporating quantitative biosecurity and biosafety risk measures. Two test problems were used to exercise these research products examine (a) Systemic effects of technological innovation and (b) Right -sizing of laboratory networks.

60 APPLIED LIFE SCIENCES↗

DOE OSTI2018

Reduction Enhancement Mechanisms of a Low-Grade Iron Ore–Coal Composite by NaCl

The reduction behavior of a low iron grade with high SiO{sub 2} content ore–coal composite was investigated in the temperature range of 1143 K to 1263 K (870 °C to 990 °C). Sodium chloride was chosen as an additive to promote this reduction process. The effect of the sodium chloride addition and its mechanism was also investigated. Results showed that the added sodium chloride could enhance the reduction of wustite to iron due to the decrease of fayalite, and a higher metallization ratio of reduced sample was obtained. Thermogravimetric–differential scanning calorimeter analysis showed that sodium chloride could greatly facilitate the gasification process of coal and, thus, provide sufficient carbon monoxide to the reduction process of iron oxides. Meanwhile, sodium chloride promoted the reduction process of iron ore pellets directly as the coal gasification effect was excluded. Microstructures of reduced sample revealed that sodium chloride broke the structure of ore and enhanced the growth of newly formed iron particles. As the ore–coal composite with mol (C/Fe = 1.4) and 3 mass pct sodium chloride addition was roasted at 1233 K (960 °C) for 55 minutes, a reduced sample with metallization ration of 74.45 pct could be obtained.

36 MATERIALS SCIENCE↗

DOE OSTI2016

Gas-Phase Detection of a Multi-Complex Lanthanide Sample for Nuclear Forensics

Post-detonation nuclear forensics is an area of research that continuously necessitates progress in the reduction of sample analysis time. Rapid analysis is an essential component of the post-detonation process in order to quickly inform relevant officials of the nature and characteristics of a nuclear weapon. In order to address this issue, a new technique has been developed to more quickly isolate and quantify elements and isotopes of interest from nuclear melt glass debris. This process exploits gas-phase chemistry to identify debris constituents in a more timely fashion than currently-practiced techniques. When fully functional, this technique is expected to significantly reduce analysis time for nuclear forensic samples. (authors)

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2025

Characterization of Tank 15H Sample in Support of Preliminary Cease Waste Removal and Closure Mode Determination

The Savannah River National Laboratory (SRNL) was requested by Savannah River Mission Completion (SRMC) to provide sample preparation and analysis of Tank 15H characterization samples. These samples follow an interest in exploring avenues to condense the extensive sampling of the Tank Closure process. One such pathway would be to collect a sample during an earlier waste removal campaign for analysis to determine comparability to the later residual tank inventory determined through Residual Material sampling and characterization prior to grouting. Six Tank 15H samples (HTF-15-24-9, HTF- HTF-15-24-10, HTF-15-24-11, HTF-15-24-12, HTF15-24-13, and HTF-15-24-14) were delivered to SRNL in May of 2024. These six Tank 15H samples were taken as close as possible to the solids layer of the Tank 15H. These six Tank 15H samples were combined to form one composite sample for characterization due to the lack of sufficient solids fraction.

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