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Results for “Interlaboratory study”

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.

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At least 19 records
All sourcesNASA NTRSDOE OSTI
DOE OSTI2025

Results of an interlaboratory study on the working curve in vat photopolymerization II: Towards a standardized method

The working curve measurement in photopolymer additive manufacturing is a ubiquitous measure of the cure depth of a printing resin as a function of radiant exposure of light. The fit parameters from this measurement (the depth of light penetration D p and the critical exposure E c ) are used to evaluate and report a resin’s printability, optimize processing parameters, and inform print and resin quality control. Despite its widespread use, the working curve lacks a standard measurement method. Here, following up on our paper “Results of an Interlaboratory Study on the Working Curve in Vat Photopolymerization” from last year, an interlaboratory study on the working curve was performed using calibrated, reproducible, bandpass filtered light sources. With these light sources, the variability between labs in measured working curves was dramatically reduced from the initial interlaboratory study. Aggregate data from this experiment produced reliable D p and E c measurements at 385 nm of 39.2 ± 3.7 µm and 12.3 ± 3.0 mJ cm −2 , respectively. At 405 nm the values of D p and E c are 69.3 ± 3.8 µm and 17.9 ± 2.3 mJ cm −2 , respectively. The results are agnostic to the thickness measurement tool utilized by participants, ensuring broad applicability across laboratories. We also tested the generalizability of the proposed method of using a filtered light source by filtering a commercial 405 nm light source and obtaining a working curve in agreement with the aggregate data from the interlaboratory study. This interlaboratory study provides a basis for a documentary standard for the working curve, so that the entire photopolymer additive manufacturing industry can share reproducible and interoperable working curve data.

36 MATERIALS SCIENCE↗
DOE OSTI2020

A reference high-pressure CH4 adsorption isotherm for zeolite Y: results of an interlaboratory study

Abstract This paper reports the results of an international interlaboratory study led by the National Institute of Standards and Technology (NIST) on the measurement of high-pressure surface excess methane adsorption isotherms on NIST Reference Material RM 8850 (Zeolite Y), at 25 °C up to 7.5 MPa. Twenty laboratories participated in the study and contributed over one-hundred adsorption isotherms of methane on Zeolite Y. From these data, an empirical reference equation was determined, along with a 95% uncertainty interval ( U k =2 ). By requiring participants to replicate a high-pressure reference isotherm for carbon dioxide adsorption on NIST Reference Material RM 8852 (ZSM-5), this interlaboratory study also demonstrated the usefulness of reference isotherms in evaluating the performance of high-pressure adsorption experiments.

Nguyen, H. G. T. (ORCID:0000000210527565)↗
DOE OSTI2020

Versailles Project on Advanced Materials and Standards interlaboratory study on intensity calibration for x-ray photoelectron spectroscopy instruments using low-density polyethylene

We report the results of a Versailles Project on Advanced Materials and Standards interlaboratory study on the intensity scale calibration of x-ray photoelectron spectrometers using low-density polyethylene (LDPE) as an alternative material to gold, silver, and copper. An improved set of LDPE reference spectra, corrected for different instrument geometries using a quartz-monochromated Al Kα x-ray source, was developed using data provided by participants in this study. Using these new reference spectra, a transmission function was calculated for each dataset that participants provided. When compared to a similar calibration procedure using the NPL reference spectra for gold, the LDPE intensity calibration method achieves an absolute offset of ~3.0% and a systematic deviation of ±6.5% on average across all participants. For spectra recorded at high pass energies (≥90 eV), values of absolute offset and systematic deviation are ~5.8% and ±5.7%, respectively, whereas for spectra collected at lower pass energies (<90 eV), values of absolute offset and systematic deviation are ~4.9% and ±8.8%, respectively; low pass energy spectra perform worse than the global average, in terms of systematic deviations, due to diminished count rates and signal-to-noise ratio. Differences in absolute offset are attributed to the surface roughness of the LDPE induced by sample preparation. We further assess the usability of LDPE as a secondary reference material and comment on its performance in the presence of issues such as variable dark noise, x-ray warm up times, inaccuracy at low count rates, and underlying spectrometer problems. In response to participant feedback and the results of the study, we provide an updated LDPE intensity calibration protocol to address the issues highlighted in the interlaboratory study. Finally, we also comment on the lack of implementation of a consistent and traceable intensity calibration method across the community of x-ray photoelectron spectroscopy (XPS) users and, therefore, propose a route to achieving this with the assistance of instrument manufacturers, metrology laboratories, and experts leading to an international standard for XPS intensity scale calibration.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Interlaboratory Study of Digital Volume Correlation Error Due to X-Ray Computed Tomography Equipment and Scan Parameters: an Update from the DVC Challenge

Background: The quality of Digital Volume Correlation (DVC) full-field displacement measurements depends directly on the characteristics of the X-ray Computed Tomography (XCT) equipment, and scan procedures used to acquire the tomographic images. Objective: In this work, we seek to experimentally study the effects of XCT equipment and tomographic scan procedures on the quality of these images for DVC analysis, and to survey the level of DVC error that may be achieved using standard XCT operating procedures. Methods: Six participants in an interlaboratory study acquired high-quality XCT scans of a syntactic foam before and after rigid body motion. The resulting images were correlated using commercial DVC software to quantify error sources due to random image noise, reconstruction artifacts, as well as systematic spatial or temporal distortion. Results: In the absence of rigid body motion, the standard deviation of the displacement measurements ranged from 0.012 to 0.043 voxels using a moderate subvolume size, indicating that subvoxel measurement resolution could readily be achieved with a variety of XCT equipment and scan recipes. Comparison of consecutive scans without rigid body motion showed transient dilatational displacement gradients due to self-heating of the X-ray source and/or thermal expansion of the foam. Evaluation of the scans after rigid body motion showed significant, machine-specific spatial distortion in the displacement fields of up to 0.5 voxels; new approaches to remove this error need to be developed. Conclusions: Analysis of the scan protocols used in the interlaboratory study, as well as a complementary parametric sensitivity study, showed that the DVC error was strongly influenced by the XCT equipment, but could be mitigated by adjusting the total scan duration.

47 OTHER INSTRUMENTATION↗
NASA NTRS1983

Experimental design of an interlaboratory study for trace metal analysis of liquid fluids

The accurate determination of trace metals and fuels is an important requirement in much of the research into and development of alternative fuels for aerospace applications. Recognizing the detrimental effects of certain metals on fuel performance and fuel systems at the part per million and in some cases part per billion levels requires improved accuracy in determining these low concentration elements. Accurate analyses are also required to ensure interchangeability of analysis results between vendor, researcher, and end use for purposes of quality control. Previous interlaboratory studies have demonstrated the inability of different laboratories to agree on the results of metal analysis, particularly at low concentration levels, yet typically good precisions are reported within a laboratory. An interlaboratory study was designed to gain statistical information about the sources of variation in the reported concentrations. Five participant laboratories were used on a fee basis and were not informed of the purpose of the analyses. The effects of laboratory, analytical technique, concentration level, and ashing additive were studied in four fuel types for 20 elements of interest. The prescribed sample preparation schemes (variations of dry ashing) were used by all of the laboratories. The analytical data were statistically evaluated using a computer program for the analysis of variance technique.

Greenbauer-Seng, L. A.↗
DOE OSTI2023

Round-Robin Interlaboratory Study on Rare-Earth Elements in U.S.-Based Geologic Materials

In a study funded by the U.S. Department of Energy (DOE) National Energy Technology Laboratory (NETL), the University of North Dakota (UND) Energy and Environmental Research Center (EERC) performed a first-of-its-kind round-robin interlaboratory study (RRIS) to determine lab-to-lab and method-to-method variability in analyzing the rare earth element (REE) content of domestic resources. Analyses of REEs on eleven different materials were accomplished by the laboratories using four different procedures: ASTM D6357 (Procedure A), ASTM D4503 (Procedure B), an alternate in-house procedure for digestion and REE analysis (Procedure C), and neutron activation analysis (NAA). The results of the RRIS suggest that NAA is the most accurate and reliable method for many of the REEs in these types of materials; however, the method is limited in that it is able to determining only ten of the sixteen REEs. Five of the seven labs reporting data for Procedure A and three of the five labs reporting for Procedure B showed excellent performance in terms of repeatability, reproducibility, agreement with NAA, and SRM recoveries based on AOAC International guidelines on method performance. This indicates that when strictly followed these methods are suitable for REE determination in most materials, although are subject to the overall capabilities and experience of individual laboratories.

58 GEOSCIENCES↗
DOE OSTI2023

Interlaboratory Study: Testing Reproducibility of Solid Biofuels Component Identification Using Reflected Light Microscopy

Considering global market trends and concerns about climate change and sustainability, increased biomass use for energy is expected to continue. As more diverse materials are being utilized to manufacture solid biomass fuels, it is critical to implement quality assessment methods to analyze these fuels thoroughly. One such method is reflected light microscopy (RLM), which has the potential to complement and enhance current standard testing, leading to improving fuel quality assessment and, ultimately, preventing avoidable air pollution. An interlaboratory study (ILS) was conducted to test the reproducibility of biomass fuels component identification using a reflected light microscopy technique. The exercise was conducted on thirty photomicrographs showing biomass and various undesired components (like plastics or mineral matter), which were purposely added (by the ILS organizers) to contaminate wood pellets and charcoal-based grilling fuels. Forty-six participants had various levels of difficulty identifying the marked components, and as a result, the percentage of correct answers ranged from 52.2 to 94.4%. Among the most difficult components to distinguish were petroleum products and inorganic matter. Various reasons led to the misidentification, including insufficient morphological descriptions of the components provided to participants, ambiguities of the nomenclature, limitations of the analytical and exercise method, and insufficient experience of the participants. Overall, the results indicate that RLM has the potential to enhance the quality assessment of biomass fuels. However, they also demonstrate that the petrographic classification used in this exercise requires further refinement before it can be standardized. While a new simplified classification of solid biomass fuels components was created as an outcome of this study, future research is necessary to refine the nomenclature, develop a microscopic morphological description of the components, and verify the accuracy of component identification with a follow-up ILS.

biomass↗
DOE OSTI2025

Component Identification of Solid Biomass Fuels Using Reflected Light Microscopy: Interlaboratory Study 2

As nations transition toward sustainable energy systems, biomass has become a vital component of global energy portfolios. Derived from organic materials such as wood, agricultural residues, forestry byproducts, and organic waste, biomass is a renewable energy source with significant environmental and economic benefits. Responsible biomass energy production can improve waste management, reduce emissions of greenhouse gases, and mitigate environmental pollution. However, as the diversity of biomass-derived fuels increases, robust quality assessment methods are essential to ensure their efficiency, safety, and minimal environmental impact. Reflected light microscopy (RLM) is one such technique with the potential to complement conventional physico-chemical analyses by enabling a rapid identification of material constituents and impurities. To refine this methodology and evaluate the reproducibility of solid biomass component identification using RLM, an interlaboratory study (ILS) was conducted. The study involved the recognition of 58 components across 45 photomicrographs, with the participation of 65 scientists and students from 25 countries. The participants faced high difficulty identifying some of the marked components, and as a result, the percentage of correct answers ranged from 19.0 % to 98.3 %, with an average correct identification rate of 62.7 %. The most challenging aspects of the identification process included distinguishing between woody and non-woody (agro) biomass, accurately identifying petroleum-derived materials, and differentiating agro biomass from inorganic matter. The results suggest that while RLM is an important tool for characterizing solid biomass, further development of methodology guidelines and training are necessary to enhance its effectiveness. Future research should prioritize preparing detailed, image-rich, microscopic morphological descriptions of biomass fuel components, which could improve the accuracy and reliability of using RLM in biomass fuel characterization.

09 BIOMASS FUELS↗
DOE OSTI2024

Results of an interlaboratory study on the working curve in vat photopolymerization

The working curve informs resin properties and print parameters for stereolithography, digital light processing, and other photopolymer additive manufacturing (PAM) technologies. First demonstrated in 1992, the working curve measurement of cure depth vs radiant exposure of light is now a foundational measurement in the field of PAM. Despite its widespread use in industry and academia, there is no formal method or procedure for performing the working curve measurement, raising questions about the utility of reported working curve parameters. Here, an interlaboratory study (ILS) is described in which 24 individual laboratories performed a working curve measurement on an aliquot from a single batch of PAM resin. The ILS reveals that there is enormous scatter in the working curve data and the key fit parameters derived from it. Further, the measured depth of light penetration D p varied by as much as 7x between participants, while the critical radiant exposure for gelation E c varied by as much as 70x. This significant scatter is attributed to a lack of common procedure, variation in light engines, epistemic uncertainties from the Jacobs equation, and the use of measurement tools with insufficient precision. The ILS findings highlight an urgent need for procedural standardization and better hardware characterization in this rapidly growing field.

36 MATERIALS SCIENCE↗
NASA NTRSDate not supplied

The Two-Cavity Method for Characterizing Acoustical Materials—an Interlaboratory Study

This study focuses on understanding the sound absorption characteristics of porous acoustic materials, which are determined by two key parameters independent of material thickness: characteristic impedance and propagation constant. These parameters can be characterized by testing a porous sample concept in a normal incidence impedance tube using either the two-thickness or the two-cavity method. In the two-thickness method, two samples of varying thicknesses are required. In contrast, the two-cavity method requires testing one sample at two different air cavity depths behind the porous material. This method is particularly advantageous for materials that are costly or challenging to fabricate. This interlaboratory study evaluates the variability of characteristic properties determined using the two-cavity method. Porous acoustic materials were additively manufactured and tested in the Liner Technology Facility(LTF)at NASA Langley Research Center and the Mechanics, Acoustics and Dynamics Lab (MADLab) at Michigan Technological University. The characteristic properties derived from various cavity depth combinations were used to predict the surface impedance of the sample with a rigid backing. The prediction was then compared the measured impedance spectrum. It was also found that the combinations of cavity depths can significantly influence the accuracy of the deduced properties.

acoustic liners↗
DOE OSTI2022

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↗
DOE OSTI2023

Results from an International Interlaboratory Study on Light- and Elevated Temperature-Induced Degradation (LETID) in Solar Modules

This presentation reports recently submitted results from 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. We summarize the range of observed degradation and provide initial conclusions on the reproducibility of results across labs. In LETID-sensitive modules, both open-circuit voltage (VOC) and short-circuit current (ISC) 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 direct LETID-related losses. We summarize the conclusions drawn from the study, provide an update on a forthcoming standard technical specification for LETID testing of PV modules (IEC TS 63342 ED1), and discuss unresolved questions and potential future work on LETID in PV modules.

degradation↗
DOE OSTI2024

Establishing ZIF‐8 as a reference material for hydrogen cryoadsorption: An interlaboratory study

Abstract Hydrogen storage by cryoadsorption on porous materials has the advantages of low material cost, safety, fast kinetics, and high cyclic stability. The further development of this technology requires reliable data on the H 2 uptake of the adsorbents, however, even for activated carbons the values between different laboratories show sometimes large discrepancies. So far no reference material for hydrogen cryoadsorption is available. The metal‐organic framework ZIF‐8 is an ideal material possessing high thermal, chemical, and mechanical stability that reduces degradation during handling and activation. Here, we distributed ZIF‐8 pellets synthesized by extrusion to 9 laboratories equipped with 15 different experimental setups including gravimetric and volumetric analyzers. The gravimetric H 2 uptake of the pellets was measured at 77 K and up to 100 bar showing a high reproducibility between the different laboratories, with a small relative standard deviation of 3–4 % between pressures of 10–100 bar. The effect of operating variables like the amount of sample or analysis temperature was evaluated, remarking the calibration of devices and other correction procedures as the most significant deviation sources. Overall, the reproducible hydrogen cryoadsorption measurements indicate the robustness of the ZIF‐8 pellets, which we want to propose as a reference material.

08 HYDROGEN↗
DOE OSTI2020

Interlaboratory Study for Characterizing Monoclonal Antibodies by Top-Down and Middle-Down Mass Spectrometry

The Consortium for Top-Down Proteomics (www.topdownproteomics.org) launched the present study to assess the state of top-down mass spectrometry (TD MS) and middle-down mass spectrometry (MD MS) for characterizing monoclonal antibody (mAb) primary structures, including their modifications. To meet the needs of the rapidly growing therapeutic antibody market, it is important to develop analytical strategies to characterize the heterogeneity of a therapeutic product’s primary structure reliably and reproducibly. The major objective of the present study was to determine whether current TD/MD MS technologies and protocols can add value to the more commonly employed bottom-up approaches, such as confirming protein integrity, sequencing variable domains, ruling out artefacts, and revealing modifications and their locations. A panel of three mAbs was selected and centrally provided to twenty laboratories worldwide for the analysis: Sigma mAb standard (SiLuLite), NIST mAb standard, and the therapeutic mAb Herceptin (trastuzumab). A variety of different MS instrument platforms and ion dissociation techniques were employed. Overall, the present study confirms that MD/TD MS strategies are valuable and readily available tools in laboratories worldwide. They provide complementary information to the bottom-up approach and can add unique information, which may be crucial for comprehensive mAb characterization. The current limitations, as well as possible solutions to overcome them, are also outlined. One of the limitations revealed by the results of the present study is that the expert knowledge in both experiment and data analysis is indispensable to practice TD/MD MS, but the number of TD/MD MS experts is still very low.

59 BASIC BIOLOGICAL SCIENCES↗
DOE OSTI2022

Approach to Precision and Bias Analysis of Interlaboratory Salt Study Results

An interlaboratory study of salt properties measurements was initiated in 2020 by Raluca Scarlatt of UC Berkley and Jake McMurray of Oak Ridge National Laboratory as a DOE-funded NEUP project. The objective of what is referred to as the interlaboratory salt study (ISS) was to assess the quality of molten salt property data and develop consensus standard methods for measuring key property values. Unlike many interlaboratory studies in which the precision of applying a well-defined and well-constrained method is measured, the methods used to measure property values were not specified nor were the measurement conditions controlled. Instead, the approach was to engage participants in measuring the property values of two commonly-used salt mixtures by using any desired measurement techniques. By including measurements made using the same and different methods across institutions, the precisions achieved using specific techniques can be assessed as well as the confidence in the values measured using different techniques. Details of the calibrations and uncertainty provided by the participants will be useful in establishing a best practice for the application of each technique to molten salts.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗