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At least 19 records

Savannah River National Laboratory Participation in the International Atomic Energy Agency CPC Interlaboratory Comparison Exercise 2

International Atomic Energy Agency Safeguards Analytical Services (IAEA-SGAS) oversees coordinating the second Controlled Potential Coulometry Quality Control Interlaboratory Comparison (CPC QC ILC) on behalf of the Nuclear Material Laboratory (NML). The purpose of the exercise is to: (1) verify the ability of participating laboratories to measure the Pu concentration in the sample solutions, and (2) estimate the method performance (repeatability and intermediate reproducibility). Sample shipping coordination was performed by IAEA-SGAS. The test sample is a plutonium nitrate solution (estimated molarity of 3-5 M), delivered in two PTFE screw-capped quartz ampoules. Each participating laboratory is to receive two ampoules. Each ampoule holds approximately 8 mL of solution containing approximately 10 mg Pu/g. The gross weights of the ampoules were provided. The test sample is assumed to have an iron content below the level of significance for the CPC. The isotopic composition of the plutonium test sample was provided; however, no analysis date was provided. In addition, IAEA-SGAS provided analytical instructions to participants. On September 20, 2022, SRNL received the samples sent by IAEA-SGAS.

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗

Interlaboratory comparison of secondary ion mass spectrometry analysis results from the 7th international technical nuclear forensics working group collaborative material exercise

A review and interlaboratory comparison of secondary ion mass spectrometry (SIMS) data obtained by laboratories participating in the International Technical Nuclear Forensics Working Group (ITWG) 7th Collaborative Material Exercise (CMX-7) has been conducted. The analyzed materials were two uranium compounds in powder form and two pieces of uranium metal. The instruments used in this comparison were a small-geometry (SG) SIMS, CAMECA IMS 7f from the Research Centre Rez, and a large-geometry (LG) SIMS, CAMECA IMS 1280 from Los Alamos National Laboratory. Despite the differences in instruments and analytical procedures, e.g., sample preparation, SIMS setups, and data post-processing, there was good agreement for the 234 U/ 238 U, 235 U/ 238 U, and 236 U/ 238 U ratios in the analyzed materials. The main difference was in the precision, which was, as expected, higher for the LG-SIMS. In addition, a comparison between the laboratories was also made for the image processing algorithms applied to raw data acquired in automated particle measurement (APM) mode. In conclusion, the result of this comparison has led to identification of best practices for setting up parameters of the APM software.

and nuclear chemistry↗

Interlaboratory comparison of fluorocarbons-11, -12, methylchloroform and nitrous oxide measurements

Measurements conducted by 19 participating laboratories were considered in the reported interlaboratory comparison study. The results show that there is considerable disagreement among laboratories regarding the absolute concentrations of all four trace gases (CCl3F, CCl2F2, H3CCl3, N2O). The magnitude of this disagreement is discussed. Laboratories in Group II showed considerable disagreement among themselves. Their results were scattered within large intervals of concentration. Laboratories in Group I (using common standards) were in excellent (+ or - 5%) agreement among themselves. A systematic disagreement was noted between Groups I and II laboratories. Generally, the mean values of concentrations determined from the measurements of Group II laboratories were lower than the mean values reported by Group I laboratories.

Rasmussen, R. A.↗

Plutonium Age Dating Interlaboratory Comparison Overview - Project Design, Sample Preparation, and Results [Slides]

Project Design – How do you validate measured Pu model age? There are no certified reference materials (CRMs) that are certified for Pu model age or purification dates. There are no Am isotopic CRMs - IRMM 0243 243 Am spike has 241 Am impurity that can be used; Community working toward "consensus ages." This project executed and evaluated results from a Pu age dating interlaboratory comparison with six IAEA NWAL participant laboratories. It also ran the first quality control evaluation of single-picogram to sub-picogram scale interlaboratory 241 Am assay measurements from cotton swipe matrices. Results are promising, with a majority of 241 Am/ 241 Pu model age results agree to within 1 to 4 years. The calculated 241 Am assay results show interlaboratory variability, expanded percent uncertainties on calculated consensus 241 Am concentrations were: PuAge-S1 = 3.1 %, PuAge-S2 = 23 %, and PuAge-S3 = 26 %. Data can be used to investigate laboratory methods and improve precision and accuracy of 241 Pu and 241 Am assay for future campaigns.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Interlaboratory comparison of chemical analysis of uranium mononitride

Analytical methods were established in which the critical variables were controlled, with the result that acceptable interlaboratory agreement was demonstrated for the chemical analysis of uranium mononitride. This was accomplished by using equipment readily available to laboratories performing metallurgical analyses. Agreement among three laboratories was shown to be very good for uranium and nitrogen. Interlaboratory precision of + or - 0.04 percent was achieved for both of these elements. Oxygen was determined to + or - 15 parts per million (ppm) at the 170-ppm level. The carbon determination gave an interlaboratory precision of + or - 46 ppm at the 320-ppm level.

Merkle, E. J.↗

An interlaboratory comparison of mid-infrared spectra acquisition: Instruments and procedures matter

Diffuse reflectance spectroscopy has been extensively employed to deliver timely and cost-effective predictions of a number of soil properties. However, although several soil spectral laboratories have been established worldwide, the distinct characteristics of instruments and operations still hamper further integration and interoperability across mid-infrared (MIR) soil spectral libraries. In this study, we conducted a large-scale ring trial experiment to understand the lab-to-lab variability of multiple MIR instruments. By developing a systematic evaluation of different mathematical treatments with modeling algorithms, including regular preprocessing and spectral standardization, we quantified and evaluated instruments' dissimilarity and how this impacts internal and shared model performance. We found that all instruments delivered good predictions when calibrated internally using the same instruments' characteristics and standard operating procedures by solely relying on regular spectral preprocessing that accounts for light scattering and multiplicative/additive effects, e.g., using standard normal variate (SNV). When performing model transfer from a large public library (the USDA NSSCKSSL MIR library) to secondary instruments, good performance was also achieved by regular preprocessing (e. g., SNV) if both instruments shared the same manufacturer. However, significant differences between the KSSL MIR library and contrasting ring trial instruments responses were evident and confirmed by a semi-unsupervised spectral clustering. For heavily contrasting setups, spectral standardization was necessary before transferring prediction models. Non-linear model types like Cubist and memory-based learning delivered more precise estimates because they seemed to be less sensitive to spectral variations than global partial least square regression. In summary, the results from this study can assist new laboratories in building spectroscopy capacity utilizing existing MIR spectral libraries and support the recent global efforts to make soil spectroscopy universally accessible with centralized or shared operating procedures.

58 GEOSCIENCES↗

An interlaboratory comparison of piston-cylinder pressure calibration using the albite-breakdown reaction.

An attempt is made to compare pressure calibration methods among several laboratories in an unbiased way to produce some indication of the bandwidth of observations on the pressure of an equilibrium reaction where sources of discrepancy not resulting from pressure calibration are likely to have been eliminated. The reaction chosen is the breakdown of albite to jadeite and quartz under pressure.

Johannes, W.↗

Spectral radiance calibrations between 165-300 nm - An interlaboratory comparison

The spectral radiance of deuterium lamps calibrated by the Max-Planck-Institut fuer Astronomie (MPI), by the U.S. National Bureau of Standards (NBS), and by the Physikalisch-Technische Bundesanstalt (PTB) are compared to check the agreement of UV radiometric scales. The NBS group used the optically thin continuum radiation from a wall-stabilized hydrogen arc as its fundamental radiometric standard, while the MPI and PTB groups used the synchrotron radiation facility in DESY. It is found that the spectral radiance scales based upon the DESY synchrotron and the NBS hydrogen arc are consistent, at least for one wavelength relative to another.

Bridges, J. M.↗

Toxicity of pyrolysis products: Influence of experimental conditions - The MSTL/UT and NASA/JSC Procedures

Ten sample materials of various polymeric composition were evaluated for toxicity of pyrolysis products utilizing two significantly different experimental methods, the MSTL/UT and NASA/JSC Procedures. A comparison of the LD(50) values obtained by the two methods for these ten samples did not yield a significant correlation. However, when the samples were ranked in order of increasing toxicity by each method independently, a comparison of their rank order toxicity improved the correlation. Because of interlaboratory variations in pyrolysis/combustion test procedures, it is suggested a series of standard materials be adopted to facilitate interlaboratory comparisons of data on pyrolysis toxicity.

Lawrence, W. H.↗

A direct time series comparison between the La Jolla and Belfast radiocarbon records

For many years it has been widely assumed that the variations in the level of atmospheric carbon-14 were due to statistical fluctuations arising from experimental error. This is understandable since the signal/noise ratio is very low and the time sequences representing the variations are strongly stochastic. Interlaboratory comparisons show that baseline variations in the absolute value of the carbon-14 concentration do exist. However, assuming linearity, the delta 14C values are independent of these. The importance of assessing the quantitive reality of the delta 14C values is based upon their expression of the interplanetary cosmic ray source function, because in the range of 100 to 1000 year periods, there appears to be no evidence that the Earth's magnetic field is the source modulating function. Therefore the modulation is either due to changes in the solar atmosphere propagated out into the solar wind, or extra-heliospheric pressure effects, but these appear to be unlikely for the periods noted here. The recent availability of the new high quality Belfast time sequence of delta 14C now permits a simple mutual assessment of the several sequences which are available. Since the La Jolla record has been a standard for many years , these two were chosen for a simple comparison. Although differences exist, the close agreement between these two sequences, one carried out on White mountain Bristlecone pines, and the other done using Irish peat bog wood, is striking. This correlation between the two strongly reinforces the statistical view that the delta 14C record is that of real interplanetary modulation of the cosmic ray source leading to the generation of atmospheric 14C.

Sonett, C. P.↗

Technical note: 21 Ne in the CoQtz-N quartz standard material

Intercomparison standards produced from mineral samples exposed to the natural cosmic ray flux are routinely used for interlaboratory comparison and normalization of measurements of the cosmogenic noble gases 3 He and 21 Ne. This effort is facilitated by the availability of multiple standard materials with a wide range of cosmogenic nuclide concentrations. The “CoQtz-N” quartz standard, which was originally produced and distributed as an intercomparison standard for cosmogenic 10 Be and 26 Al, has a significantly lower cosmogenic nuclide concentration than other mineral standards used for cosmogenic noble gas analysis and is therefore potentially useful for assessing the linearity of interlaboratory offsets across a wide range of concentrations. This paper reports 21 Ne analysis of 13 aliquots of CoQtz-N, interspersed with 14 aliquots of the commonly used CRONUS-A quartz standard, in three analytical sessions on two noble gas mass spectrometer systems. The excess 21 Ne concentration in CoQtz-N, normalized to the accepted value of 320 × 10 6 atoms g −1 for CRONUS-A, is 13.87 ± 0.24 × 10 6 atoms g −1 . Alternatively, the ratio of excess 21 Ne concentrations in CoQtz-N and CRONUS-A is 0.04330 ± 0.00077.

Balco, Greg [Lawrence Livermore National Laborator↗

Results from an international interlaboratory study on light‐ and elevated temperature‐induced degradation in solar modules

Abstract This paper reports the results of an international interlaboratory comparison study on light‐ and elevated temperature‐induced degradation (LETID) on crystalline silicon photovoltaic (PV) modules. A large global network of PV module manufacturers and PV testing laboratories collaborated to design a protocol for LETID detection and screen a large and diverse set of prototype modules for LETID. Results across labs indicate the reproducibility of LETID testing is likely within ±1% of maximum power (P MP ). In intentionally engineered LETID‐sensitive modules, mean degradation after the prescribed detection stress is roughly 6% P MP . In other module types the LETID sensitivity is smaller, and in some we observe essentially negligible degradation attributable to LETID. In LETID‐sensitive modules, both open‐circuit voltage (V OC ) and short‐circuit current (I SC ) degrade by a roughly similar magnitude. We observe, as do previous studies, that LETID affects each cell in a module differently. An investigation of the potential mismatch losses caused by nonuniform LETID degradation found that mismatch loss is insignificant compared to the estimated loss of cell I SC , which drives loss of module I SC . Overall, this work has helped inform the creation of a forthcoming standard technical specification for LETID testing of PV modules, IEC TS 63342 ED1, and should aid in the interpretation of results from that and other LETID tests.

14 SOLAR ENERGY↗

Radiochronometric discordance in cast uranium metal: a multi-laboratory intercomparison exercise

Here, the model age of a nuclear material is crucial in nuclear forensic analysis. Uranium metals with complex production histories often exhibit discordant model ages from the 230 Th– 234 U and 231 Pa– 235 U chronometers. Recent studies involving targeted uranium metal castings have enhanced our understanding of decay product behavior during casting, aiding nuclear forensic interpretation. Building on this prior work, forensics laboratories at Atomic Weapons Establishment (AWE), Lawrence Livermore National Laboratory (LLNL), and Los Alamos National Laboratory (LANL) conducted an interlaboratory comparison to investigate spatial heterogeneity in uranium metal cast under controlled conditions. Each laboratory measured samples of a mixed feedstock and its corresponding cast product. This work furthers our understanding of discordant model ages and the use of discordance as a signature to enhance confidence in interpretations of radiochronometric data for nuclear forensics.

230Th/234U↗

Round-robin analysis of highly depleted lithium for Generation IV nuclear reactor applications

Lithium reference materials containing unnaturally high abundances of 7 Li are not currently available, which poses quality control problems for highly depleted lithium materials (i.e., depleted in 6 Li) required for Generation IV nuclear reactors. This study presents an interlaboratory comparison of a lithium carbonate (NIST SRM924a) containing nominally natural isotopic abundances (~92.4 % Li-7) and a highly depleted lithium hydroxide material (~99.95 % Li-7). The natural lithium isotope abundances of NIST SRM924a are confirmed, and the 6 Li/ 7 Li ratio of the lithium hydroxide ranged from 0.000399 to 0.000436 with an average of 0.000428 ± 0.000023 (2SD, n = 9). Finally, going forward this material can be used as quality control for analytical work involving highly depleted lithium.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

R&D Outcomes of Surrogate Environmental Swipe Manufacturing Technique Method Development for Arms Control and Treaty Verification Applications

The analysis of environmental samples is a critical component of nuclear compliance verification and safeguards activities. While the associated particle analyses have benefitted from recent advances in the production of actinide-bearing particulates with uniform and well-characterized particle size, material phase, and isotopic ratios to serve as reference materials for calibration and interlaboratory comparisons, there is an outstanding need for surrogate environmental samples, which resemble field-collected samples, with the aforementioned reference particulates to support future nuclear compliance verification exercises and method development. This effort seeks to leverage the recent advances in tailored reference particle production to generate surrogate environmental swipe samples via parallel production techniques (direct and indirect) which are uniquely suited to the hydrothermal and aerosol-based synthesis routes developed at PNNL and SRNL, respectively. PNNL’s hydrothermal particle production method was used to generate surrogate reference particles for the indirect production of test swipes.

54 ENVIRONMENTAL SCIENCES↗

Product ion distributions using H 3 O + proton-transfer-reaction time-of-flight mass spectrometry (PTR-ToF-MS): mechanisms, transmission effects, and instrument-to-instrument variability

Abstract. Proton-transfer-reaction mass spectrometry (PTR-MS) using hydronium ion (H3O+) ionization is widely used for the measurement of volatile organic compounds (VOCs) both indoors and outdoors. H3O+ ionization, as well as the associated chemistry in an ion–molecule reactor, is known to generate product ion distributions (PIDs) that include other product ions besides the proton-transfer product. We present a method, using gas-chromatography pre-separation, for quantifying PIDs from PTR-MS measurements of nearly 100 VOCs of different functional types including alcohols, ketones, aldehydes, acids, aromatics, organohalides, and alkenes. We characterize instrument configuration effects on PIDs and find that reactor reduced electric field strength (E/N), ion optic voltage gradients, and quadrupole settings have the strongest impact on measured PIDs. Through an interlaboratory comparison of PIDs measured from calibration cylinders, we characterized the variability of PID production from the same model of PTR-MS across seven participating laboratories. Product ion variability was generally smaller (e.g., < 20 %) for ions with larger contributions to the PIDs (e.g., > 0.30) but less predictable for product ions formed through O2+ and NO+ reactions. We present a publicly available library of H3O+ PTR-MS PIDs that will be updated periodically with user-provided data for the continued investigation into instrument-to-instrument variability of PIDs.

Link, Michael F. (ORCID:0000000218412455)↗