Search NASA⌕ Search

SEARCH · Search NASA

Results for “reference material”

Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

Quote a phrase for an exact phrase match. Source license links do not imply unrestricted reuse.

At least 55 records · Page 3
All sourcesNASA NTRSDOE OSTI
DOE OSTI2023

Carbon, Nitrogen, and Sulfur Analysis of the Cetama Viognier Standard Reference Material

The Viognier sample was analyzed for C, N, and S concentrations and stable isotope compositions using an Elementar Vario Isotope Cube Elemental Analyzer (EA) that is coupled to an IsoPrime PrecisION IRMS. Powder samples were placed in tin capsules and then loaded onto a rotary autosampler. The autosampler dropped samples into the EA, and samples were combusted at 1175 °C over tungsten oxide in a continuous stream of helium carrier gas. A pulse of oxygen is added to the gas stream resulting in flash combustion of the tin capsule containing the sample, which raises the reaction temperature to approximately 1800 °C for a few seconds. The combustion reaction produces SO 2 , N 2 and CO 2 from any sulfur, nitrogen and carbon present in the sample. The resulting gases were then passed through a reduced copper reactor that was heated to 850 °C, to reduce NO x to N 2 , reduce SO 3 to SO 2 , and trap any volatile halogen compounds on silver wool. Following water removal using an adsorption tube, the N 2 , CO 2 , and SO 2 analyte gases were separated and purified using purge-trap columns. The purified gases were then carried through a thermal conductivity detector. The detector signal was passed to software that calculated elemental abundances based on integrated peak areas. The sample gases were then passed to the IRMS and stable isotope ratios were measured. Raw sample peak areas were corrected by subtracting the average peak area from blanks consisting of empty tin capsules run using the same EA analysis method. Blanks were also run following each replicate to verify that all the material was combusted. The Viognier sample was analyzed in triplicate on two days (target sample masses: 30, 60 and 90 mg). The following standards were analyzed to calibrate EA-IRMS measurements: IAEA-C6, USGS-40, USGS-41, IAEA-S1, and IAEA-S2.

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗
DOE OSTI2022

Reference surface excess isotherms for carbon dioxide adsorption on ammonium ZSM-5 at various temperatures

Abstract This work is part of the effort at the Facility for Adsorbent Characterization and Testing (FACT lab) at the National Institute of Standards and Technology (NIST) to develop reference materials, reference data, and measurement best practices for adsorption metrology. High-pressure surface excess isotherms for CO 2 adsorption on NIST Reference Material 8852 (ammonium ZSM-5) at 15 °C, 25 °C, and 35 °C are reported, expanding on a FACT Lab-organized international interlaboratory study on this sorbent/sorbate pair at 20 °C. The range of temperatures of the present study is of interest for many CO 2 adsorption measurements and applications. Measurements were made using five different adsorption instruments, both manometric and gravimetric. Excellent agreement in the measured isotherms among the instruments was found. An empirical reference equation of the form, $${n}_{ex,ref}({P}_{eq})=\frac{c}{\{{1+\mathrm{exp}[\left(-\mathrm{ln}\left(P\right)+a\right)/b ]\}}^{b }} ,$$ n e x , r e f ( P eq ) = c { 1 + exp [ - ln P + a / b ] } b , [ n ex,ref is surface excess uptake (mmol/g); P eq is equilibrium pressure (MPa); P is ( P eq )/(1 MPa)]; a , b , c are constants] and the 95% uncertainty interval were determined for the isotherms at each of the temperatures. Lastly, the isosteric heat of adsorption is estimated from absolute isotherms derived from the surface excess reference data.

Nguyen, Huong Giang T. (ORCID:0000000210527565)↗
DOE OSTI2021

New Capability at ORNL: High Precision Uranium Titration

Destructive analytical measurements establish a nuclear facility’s nuclear material inventory and inventory differences for Nuclear Material Accountancy and Control. A nuclear laboratory’s ability to perform accurate high-precision analytical measurements is key for tracking large inventories within a facility’s material balance areas and during production to track material movement through dynamic processes. For uranium, these measurements are made by using several established high-precision measurement protocols. These include isotope dilution mass spectrometry, gravimetry, and potentiometric titrations. Whatever measurement technique a nuclear lab chooses to use, reference materials (RMs) with certified attributes and accompanying uncertainties are used to calibrate measurement systems, and are the cornerstone for accurate results. In addition to calibration, RMs provide for metrological traceability, are used for method development and validation, and thus provide critical evaluations of the appropriateness and performance of analytical processes used. Evaluations may include validation that a method is fit-for-purpose, quantification of systematic and random biases, and the evaluation of long-term and short-term performance metrics. High-precision measurement techniques require that measured attributes be certified to a high degree of precision in the RMs used—ultimately, to a higher degree than that of the measurement technique itself. The US authority on the production of special nuclear material Certified Reference Materials is the NBL Program Office (NBLPO), formally known as New Brunswick Laboratory (NBL). The NBLPO is responsible for the sales and distribution of existing NBL certified reference materials (CRMs) and for the production of the next generation of nuclear RMs. To accomplish its mission, NBLPO is establishing key base capabilities within the DOE laboratory complex that formerly existed at the NBL laboratory. The Nuclear Analytical Chemistry (NAC) section within the Chemical Sciences Division (CSD) at Oak Ridge National Laboratory (ORNL) is currently working with NBLPO to set up laboratory and measurement capabilities to provide measurements and capabilities for production and/or recertification of existing and future CRMs for uranium assay. The NBL-developed high-precision titration (HPT) method is a critically-evaluated, extremely precise and accurate primary method utilized for the determination of uranium content in a variety of uranium materials. The HPT method, combined with detailed balance weighing protocols, provides for an analytical methodology that is unsurpassed in precision and one in which all sources of error have been evaluated, a requirement of CRM certification. HPT capability within the United States was lost with the closure of the labs at NBL. The NAC has been collaborating with NBLPO to stand up and demonstrate the capability to perform uranium assay via HPT at ORNL. HPT can produce results with an expanded uncertainty of approximately 0.01% for pure uranium compounds, with typical precisions of <0.006%. The major tasks required to stand up the method at ORNL were the refurbishment of a dedicated lab and equipment setup, procedure development, analyst training, establishing method-specific quality assurance, and qualification of an analyst to perform the method. This report summarizes these tasks, outlines the documents drafted, and gives the outcome of the qualification titrations.

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗
DOE OSTI2022

Coupling of nitric acid digestion and anion-exchange resin separation for the determination of methylmercury isotopic composition within organisms

Isotope ratios of methylmercury (MeHg) within organisms can be used to identify sources of MeHg that have accumulated in food webs, but these isotopic compositions are masked in organisms at lower trophic levels by the presence of inorganic mercury (iHg). To facilitate measurement of MeHg isotope ratios in organisms, we developed a method of extracting and isolating MeHg from fsh and aquatic invertebrates for compound-specifc isotopic analysis involving nitric acid digestion, batch anion-exchange resin separation, and pre-concentration by purge and trap. Recovery of MeHg was quantifed after each step in the procedure, and the average cumulative recovery of MeHg was 93.4±2.9% (1 SD, n=28) for biological reference materials and natural biota samples and 96.9±1.8% (1 SD, n=5) for aqueous MeHgCl standards. The amount of iHg impurities was also quantifed after each step, and the average MeHg purity was 97.8±4.3% (1 SD, n=28) across all reference materials and natural biota samples after the fnal separation step. Measured MeHg isotopic compositions of reference materials agreed with literature values obtained using other MeHg separation techniques, and MeHg isotope ratios of aqueous standards, reference materials, and natural biota samples were reproducible. On average, the reproducibility associated with reference material process replicates (2 SD) was 0.10‰ for δ 202 MeHg and 0.04‰ for Δ 199 MeHg. This new method provides a streamlined, reliable technique that utilizes a single sample aliquot for MeHg concentration and isotopic analysis. Furthermore, this promotes a tight coupling between MeHg concentration, %MeHg, and Hg isotopic composition, which may be especially benefcial for studying complex food webs with multiple isotopically distinct sources of iHg and/or MeHg.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2020

In Situ Oxygen Isotope Determination in Serpentine Minerals by SIMS: Addressing Matrix Effects and Providing New Insights on Serpentinisation at Hole BA1B (Samail ophiolite, Oman)

The ability to constrain the petrogenesis of multiple serpentine generations recorded at the microscale is crucial for estimating the extent and conditions of modern versus fossil serpentinisation in ophiolites. To address matrix bias effects during oxygen isotope analysis by SIMS, we present the first investigation analysing antigorite in the compositional range Mg# = 77.5–99.5 mole %, using a CAMECA IMS–1280 secondary ion mass spectrometer. Spot–to–spot homogeneity is ≤ 0.5‰ (2s) for the new antigorite reference materials. The relative bias between antigorite reference materials with different Mg/Fe ratios is described by a second order polynomial, and a maximum difference in bias of ~ 1.8‰ was measured for Mg# ~ 78 to 100. We observed a bias up to ~ 1.0‰ between lizardite and antigorite attributed to their different crystal structure. Orientation effects up to ~ 1‰ were observed in chrysotile. The new analytical protocol allowed the identification of oxygen isotope zoning up to ~ 7‰ in serpentine minerals from two serpentinites recovered from an area of active serpentinisation in the Samail ophiolite. Furthermore in situ analysis is capable of resolving isotopic heterogeneity that may directly reflect changes in the physical and chemical conditions of multiple serpentinisation events in the Samail ophiolite.

47 OTHER INSTRUMENTATION↗
DOE OSTI2021

InterCarb: A Community Effort to Improve Interlaboratory Standardization of the Carbonate Clumped Isotope Thermometer Using Carbonate Standards

Abstract Increased use and improved methodology of carbonate clumped isotope thermometry has greatly enhanced our ability to interrogate a suite of Earth‐system processes. However, interlaboratory discrepancies in quantifying carbonate clumped isotope (Δ 47 ) measurements persist, and their specific sources remain unclear. To address interlaboratory differences, we first provide consensus values from the clumped isotope community for four carbonate standards relative to heated and equilibrated gases with 1,819 individual analyses from 10 laboratories. Then we analyzed the four carbonate standards along with three additional standards, spanning a broad range of δ 47 and Δ 47 values, for a total of 5,329 analyses on 25 individual mass spectrometers from 22 different laboratories. Treating three of the materials as known standards and the other four as unknowns, we find that the use of carbonate reference materials is a robust method for standardization that yields interlaboratory discrepancies entirely consistent with intralaboratory analytical uncertainties. Carbonate reference materials, along with measurement and data processing practices described herein, provide the carbonate clumped isotope community with a robust approach to achieve interlaboratory agreement as we continue to use and improve this powerful geochemical tool. We propose that carbonate clumped isotope data normalized to the carbonate reference materials described in this publication should be reported as Δ 47 (I‐CDES) values for Intercarb‐Carbon Dioxide Equilibrium Scale.

58 GEOSCIENCES↗
DOE OSTI2020

Actinide Mixing Optimization Solver

The Actinide Mixing Optimization Solver (AMOS) is a set of programs written in MATLAB that computes theoretical mixes of different uranium, plutonium, thorium, and other actinide materials given a list of isotopic reference materials. Constraints are applied depending on the desired product and a mixture is computed to meet the specified requirements. The optimal mixture consists of a product that uses the lowest possible number of initial actinide materials and has the lowest cost. AMOS is currently applied to particular reference material requests from the sponsoring agency (NNSA) on behalf of the IAEA.

Baldwin, Aaron Taylor↗
DOE OSTI2022

Assessment of human nuclear and mitochondrial DNA qPCR assays for quantification accuracy utilizing NIST SRM 2372a

In forensic DNA casework, a highly accurate real-time quantitative polymerase chain reaction (qPCR) assay is recommended per the Scientific Working Group on DNA Analysis Methods (SWGDAM) (SWGDAM Validation Guidelines for DNA Analysis Methods [1]) to determine whether a DNA sample is of sufficient quantity and robust quality to move forward with downstream short tandem repeats (STR) or sequencing analyses. Most of these assays rely on a standard curve, referred to herein and traditionally as absolute qPCR, in which an unknown is compared, relative to that curve. However, one fundamental issue with absolute qPCR is the quantifiable concentration of commercial assay standards can vary depending on (1) origin, i.e., whether from a cell line or a human subject, (2) supplier, (3) lot number, (4) shipping method, etc. In 2018, the National Institute for Standards and Technology (NIST) released a human DNA standard reference material for evaluating qPCR quantification standards, Standard Reference Material (SRM) 2372a, Romsos et al. (2018) [2] which contains three well-characterized human genomic DNA samples: Component A) a single male1 donor, Component B) a single female 1 donor, and Component C) a 1:3 male 2 :female 2 donor, each with certification data for nDNA and informational mitochondrial DNA(mtDNA)/nuclear DNA (nDNA) ratio data. The SRM 2372a was used to assess four qPCR assays: (1) Quantifiler Trio (Thermo Fisher Scientific, Waltham, MA) for nDNA quantification, (2) NovaQUANT (EMD Millipore Corporation, San Diego, CA) for nDNA and mtDNA quantification, (3) a custom duplex mtDNA assay, and (4) a custom triplex mtDNA assay. Additionally, extracts from eighteen (18) skeletal remains were tested with the latter three assays for concordance of DNA concentration and with assays (2) and (3), for the degradation state. Our assessment revealed that an accurate, efficient, and reproducible qPCR assay is dependent on (1) the quality and reliability of the DNA standard, (2) the qPCR chemistry, and (3) the specific primers, and probes (if applicable), used in an assay. Finally, our findings indicate qPCR assays may not always quantify as expected and that performance of each lot should be verified using a well-characterized DNA standard such as the NIST SRM 2372a and adjusted if warranted.

59 BASIC BIOLOGICAL SCIENCES↗
DOE OSTI2026

ORNL Report of Analysis for the Verification of NRMP CRM U030A

In support of the Certified Reference Material (CRM) program managed by the Nuclear Reference Material Program (NRMP), the Material Signatures and Isotopic Standards (MSIS) group of Oak Ridge National Laboratory (ORNL) was asked to prepare a set of CRM U030A units for use as standards for isotopic analysis using multicollector thermal ionization mass spectrometry (TIMS) and inductively coupled plasma mass spectrometry (ICP-MS) instruments. This report documents the results of the verification measurements performed on three randomly selected units by the MSIS group’s ISO/IEC 17025:2017 accredited operating procedure CSD-AM-CIMS-IN20, Determination of Uranium and Plutonium Isotopic Composition using Thermal Ionization Mass Spectrometry [1], and in accordance with the quality assurance plan as described in QAP-X-96-CSD/RML-001, Nuclear Analytical Chemistry Laboratory Section Quality Assurance Plan [2].

Mathew, Kattathu [Oak Ridge National Laboratory (O↗
DOE OSTI2025

Boron isotopic analysis in bulk silicate materials using the Neoma MS/MS MC-ICP-MS

Boron (B) isotopes are a valuable tracer with applications ranging from geological, environmental, and nuclear studies because B isotopic fractionation is highly sensitive to chemical processes yielding distinct isotopic trends in natural and anthropogenic systems. Despite this wide applicability, there remain relatively few measurements on well-described reference materials and in some cases, poor agreement between various methods. We report a method for boron isotope ratio measurement in solution on the Neoma MS/MS MC-ICP-MS specifically targeting bulk silicates. We evaluate the performance of the method and instrument as it relates to the measurement of the absolute boron isotope ratio ( 10 B/ 11 B). The results indicate that the method produces data in agreement with literature values and that the sample–standard bracketing technique is appropriate for the Neoma MS/MS MC-ICP-MS which has been in use for decades on previous generation instruments. Careful tuning of the MS/MS lenses is required to obtain precision comparable to non MS/MS equipped MC-ICP-MS. With careful tuning, internal and external precisions of ∼0.3‰ were achieved. However, when the MS/MS is not properly tuned external precisions exceed 3‰. Nevertheless, our results for IAEA B-6, BCR-2, BHVO-2 and W-2a reference materials overlap the 1σ range of previously reported 10 B/ 11 B. Data are reported for total boron quantities down to a few tens of nanograms. Our procedure yielded blanks as low as 3 ng but up to 29 ng, making blank corrections important for small samples sizes in the few 10s of nanogram range. We report B isotope ratios for AGV-2G, SL-1G, GSC-2G, GSD-2G, GSE-2G, RLS-132, RLS-140, NKT-1G, and T1-G glass reference materials that have not been previously reported in the literature.

Scott, Sean R. [Pacific Northwest National Laborat↗
DOE OSTI2024

Fe Kα XANES, Fe Kβ HERFD XANES and EPMA flank method determinations of the oxidation state of Fe in garnet

The ferric to total iron ratios (Fe 3+ /ΣFe) of garnets can be paired with thermodynamic mineral activity models to quantify the oxygen fugacity of garnet-bearing rocks. However, techniques with a high analytical and spatial resolution are necessary to distinguish differences in garnet Fe 3+ /ΣFe ratios at the percent level and to accurately measure garnets that are zoned or contain inclusions. We acquired conventional Fe Kα and high-resolution energy fluorescence detection (HERFD) Fe Kβ X-ray absorption near edge structure (XANES) spectra and electron microprobe flank method analyses on a suite of 27 peridotitic and eclogitic garnets with Fe 3+ /ΣFe ratios previously determined by Mössbauer spectroscopy to evaluate the precision of each technique. We examined variations in the energy and intensity of three XANES spectral features as a function of Fe 3+ /ΣFe ratios: 1) the intensity ratio of two-post edge features (I-ratio; Fe Kα only); 2) the energy of the Fe edge at 90% normalized intensity (E 0.9 ; Fe Kα only) and 3) the pre-edge centroid energy (Fe Kα and HERFD Fe Kβ). In accordance with previous work, we find the energies of garnet pre-edge centroids are relatively insensitive to Fe 3+ /ΣFe ratios. The I-ratios of peridotitic and eclogitic garnets are offset from each other at low Fe 3+ /ΣFe ratios (≤0.13); I-ratio garnet XANES calibrations are composition-specific. The E 0.9 feature is independent of garnet major element composition in spectra that have been corrected for the effects of self-absorption. We produce two Fe Kα garnet XANES calibrations based on variations in the E0.9 feature; one calibration with all garnet reference materials included (Fe 3+ /ΣFe up to 1.0; “all garnet calibration”) and another calibration specific to garnets with low Fe 3+ /ΣFe ratios (“low ferric calibration”). Fe 3+ /ΣFe ratios calculated from the mean of up to 25 flank method measurements on eight garnet reference materials fall within 4% absolute of a one-to-one correlation with Fe 3+ /ΣFe ratios measured by Mössbauer. The standard error of the mean Fe 3+ /ΣFe ratio calculated from flank method approaches the Mössbauer-determined Fe 3+ /ΣFe ratio within estimated error (3%) after three analyses. Flank method precision is enhanced at higher beam current; however, the precision of the flank method does not approach the precision of XANES under any microprobe analytical condition tested here. Garnet reference materials detailed here are available by request to the Smithsonian Institution.

58 GEOSCIENCES↗
DOE OSTI2021

US-DOE and Republic of South Africa Uranium Benchmarking: Results From Los Alamos National Laboratory (Study Report)

This report details work performed at Los Alamos National Laboratory (LANL) in support of an interlaboratory uranium (U) benchmarking collaboration between LANL, Lawrence Livermore National Laboratory (LLNL), and South African Nuclear Energy Corporation (Necsa). The goal of this interlaboratory benchmarking exercise is to compare analytical methods and data obtained on uranium reference materials CUP-2 and New Brunswick Laboratory (NBL) certified reference material (CRM) 124-2. The LANL commitments for this project include performing microwave digestion of fresh CUP-2 and CRM 124-2 powders, measuring the U isotope composition of CUP-2 and CRM 124-2 by both single-collector and multi-collector inductively coupled plasma mass spectrometry (SC-ICP-MS and MC-ICP-MS, respectively), and determining trace-element abundances in CUP-2 and CRM 124-2 by inductively coupled plasma mass spectrometry (ICP-MS). This report details the methods employed by LANL in support of these objectives and presents the data obtained during this collaborative exercise.

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗
DOE OSTI2020

Toward an international practical pressure scale: A proposal for an IPPS ruby gauge (IPPS-Ruby2020)

At the 26 th AIRAPT conference in 2017, a task group was formed to work on an International Practical Pressure Scale (IPPS). This report summarizes the activities of the task group toward an IPPS ruby gauge. We have selected three different approaches to establishing the relation between pressure ( P ) and ruby R1-line shift ( Δλ ) with three groups of optimal reference materials for applying these approaches. Using a polynomial form of the second order, the recommended ruby gauge (referred as Ruby2020) is expressed by: P [ G P a ] = 1.87 ( ± 0.01 ) × 10 3 Δ λ λ 0 1 + 5.63 ( ± 0.03 ) Δ λ λ 0 , where λ 0 is the wavelength of the R1-line near 694.25 nm at ambient condition. In June of 2020, the Executive Committee of AIRAPT endorsed the proposed Ruby2020. Finally, we encourage high-pressure practitioners to utilize Ruby2020 within its applicable pressure range (up to 150 GPa), so that pressure data can be directly compared across laboratories and amended consistently as better scales emerge in the future.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2024

Tetrafluoroboric Acid Digestion for Accurate Determination of Rare Earth Elements in Coal and Fly Ash by ICP-MS Analysis

Coal and coal-related fly ash often contain rare earth elements (REEs) that have the potential to be utilized as valuable mineral resources. Accurately determining the REE content in coal and fly ash is crucial for resource evaluation. The conventional approach involves using hydrofluoric acid (HF) to dissolve silicates and release REEs, which, however, prolongs the digestion process due to the additional step of complexing fluoride ions (F−) with boric acid (H3BO3). Determining the correct amount of H3BO3 for neutralization can be challenging, and in some instances, the binding of fluoride ions with certain lanthanides (Lns) hampers the accurate determination of all 14 naturally occurring rare earth elements in a single digestion batch by inductively coupled plasma mass spectrometry (ICP-MS). In this study, we present an alternative method that achieves the accurate determination of all 14 naturally occurring REEs using tetrafluoroboric acid (HBF4) followed by ICP-MS analysis. This approach eliminates the need for an F− complexing step. We tested this method on certified REE reference materials, including NIST 1632e (coal) and NIST 1633c (fly ash), as well as the REE geological reference material USGS AGV-1 (andesite). Our results demonstrated excellent recovery rates (relative standard deviation, RSD < ±10%), with a correlation coefficient (r2) exceeding 0.99. Using this method, we investigated the concentrations of all 14 REEs in coal and fly ash samples collected from various locations in the southwestern USA. This improved digestion technique streamlines the analysis process and enhances the accuracy of REE determination, facilitating a more comprehensive evaluation of REE-rich coal and fly ash deposits for resource exploration.

58 GEOSCIENCES↗