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Anion-exchange membrane water electrolysis: insights from round-robin testing

As research and industrial interest in anion-exchange membrane water electrolysis (AEMWE) grows, there is an increasing need for reliable baselines and cross-lab validation of results. The wide variety of material sets and operating conditions under consideration for AEMWE has thus far limited efforts for standardization. In this study, round-robin testing was conducted in deionized water and KOH-based supporting electrolyte by 5 institutions from academia, national laboratories, and industry to provide baseline performance data and identify sources of cross-lab variability. Baseline membrane electrode assemblies were fabricated with commercial catalysts, membranes, and transport layers using standard techniques and tested using reagent-grade electrolytes, aiming for accessibility rather than state-of-the-art performance. From all tests, the average voltage at 1 A/cm 2 was 2.72 ± 0.17 V and 1.87 ± 0.03 V in deionized water and 0.1 M KOH, respectively. The maximum in-house and cross-lab variations at this current density were 118 mV and 476 mV in water and 60 and 88 mV in 0.1 M KOH. The KOH purity, station contamination, and temperature control were identified as possible factors affecting performance between labs, with in-house specific variation attributed to sample-to-sample differences in fabrication, cell assembly, and station contamination. This work provides a commercial baseline for the field and highlights the need for improved standardization and reproducibility in AEMWE research.

08 HYDROGEN

The Seventh SeaWiFS Intercalibration Round-Robin Experiment (SIRREX-7), March 1999

This report documents the scientific activities during the seventh SeaWiFS Intercalibration Round-Robin Experiment (SIRREX-7) held at Satlantic, Inc. (Halifax, Canada). The overall objective of SIRREX-7 was to determine the uncertainties of radiometric calibrations and measurements at a single calibration facility. Specifically, this involved the estimation of the uncertainties in a) lamp standards, b) plaque standards (including the uncertainties associated with plaque illumination non-uniformity), c) radiance calibrations, and d) irradiance calibrations. The investigation of the uncertainties in lamp standards included a comparison between a calibration of a new FEL by the National Institute of Standards and Technology (NIST) and Optronic Laboratories, Inc. In addition, the rotation and polarization sensitivity of radiometers were determined, and a procedure for transferring an absolute calibration to portable light sources was defined and executed.

Hooker, Stanford B.

The Sixth SeaWiFS/SIMBIOS Intercalibration Round-Robin Experiment (SIRREX-6)

For the sixth Sea-Viewing Wide Field-of-View Sensor (SeaWiFS) Intercalibration Round-Robin Experiment (SIRREX-6), NASA personnel carried the same four Satlantic in-water radiometers to nine separate laboratories and calibrated them. Two of the sensors were seven-channel radiance heads and two were seven-channel irradiance heads. The calibration and data reduction procedures used at each site followed that laboratory's normal procedures. The reference lamps normally used for the calibration of these types of instruments by the various laboratories were also used for this experiment. NASA personnel processed the data to produce calibration parameters from the various laboratories

Riley, Thomas

Analytical Round Robin for Elastic-Plastic Analysis of Surface Cracked Plates, Phase II Results

The second phase of an analytical round robin for the elastic-plastic analysis of surface cracks in flat plates was conducted under the auspices of ASTM Interlaboratory Study 732. The interlaboratory study (ILS) had 10 participants with a broad range of expertise and experience, and experimental results from a surface crack tension test in 4142 steel plate loaded well into the elastic-plastic regime provided the basis for the study. The participants were asked to evaluate a surface crack tension test according to the version of the surface crack initiation toughness testing standard published at the time of the ILS, E2899-13. Data were provided to each participant that represent the fundamental information that would be provided by a mechanical test laboratory prior to evaluating the test result. Overall, the participant’s test analysis results were in good agreement and constructive feedback was received that has resulted in an improved published version of the standard E2899-15.

Allen, P. A.

Results from an International Measurement Round Robin of III-V Triple Junction Solar Cells under Air Mass Zero

This paper reports the results of an international measurement round robin of monolithic, triple-junction, GaInP/GaAs/Ge space solar cells. Eight laboratories representing national labs, solar cell vendors and space solar cell consumers, measured cells using in-house reference cells and compared those results to measurements made where each lab used the same set of reference cells. The results show that most of the discrepancy between laboratories is likely due to the quality of the standard cells rather than the measurement system or solar simulator used.

Jenkins, Phillip

SeaWiFS technical report series. Volume 16: The second SeaWiFS Intercalibration Round-Robin Experiment, SIRREX-2, June 1993

The results of the second Sea-viewing Wide Field-of-view Sensor (SeaWiFS) Intercalibration Round-Robin Experiment (SIRREX-2), which was held at the Center for Hydro-Optics and Remote Sensing (CHORS) at San Diego State University on 14-25 Jun. 1993 are presented. SeaWiFS is an ocean color radiometer that is scheduled for launch in 1994. The SIRREXs are part of the SeaWiFS Calibration and Validation Program that includes the GSFC, CHORS, NIST, and several other laboratories. GSFC maintains the radiometric scales (spectral radiance and irradiance) for the SeaWiFS program using spectral irradiance standards lamps, which are calibrated by NIST. The purpose of each SIRREX is to assure that the radiometric scales which are realized by the laboratories who participate in the SeaWiFS Calibration and Validation Program are correct; that is, the uncertainties of the radiometric scales are such that measurements of normalized water-leaving radiance using oceanographic radiometers have uncertainties of 5%. SIRREX-1 demonstrated, from the internal consistency of the results, that the program goals would not be met without improvements to the instrumentation. The results of SIRREX-2 demonstrate that spectral irradiance scales realized using the GSFC standard irradiance lamp (F269) are consistent with the program goals, as the uncertainty of these measurements is assessed to be about 1%. However, this is not true for the spectral radiance scales, where again the internal consistency of the results is used to assess the uncertainty. This is attributed to inadequate performance and characterization of the instrumentation. For example, spatial nonuniformities, spectral features, and sensitivity to illumination configuration were observed in some of the integrating sphere sources. The results of SIRREX-2 clearly indicate the direction for future work, with the main emphasis on instrument characterization and the assessment of the measurement uncertainties so that the results may be stated in a more definitive manner.

Hooker, Stanford B.

Sea WiFS Technical Report Series: The fourth SeaWIFS Intercalibration Round-Robin Experiment (SIRREX-4), May 1995

This report documents the fourth Sea-viewing Wide Field-of-view Sensor (SeaWiFS) Intercalibration Round-Robin Experiment (SIRREX-4), which was held at the National Institute of Standards and Technology (NIST) on 3-10 May 1995. The agenda for SIRREX-4 was established by a consensus reached at the conclusion of SIRREX-3: there should be an emphasis on training and work to foster and encourage uniform use of accepted protocols for calibrating radiometric instruments in the laboratory. The goal was to host the activity in a setting where proper techniques could be discussed and demonstrated. It seemed appealing to split the day between morning lectures and afternoon laboratory exercises or practicals. The former gave the user community a chance to present what was important to them and discuss it with acknowledged experts in radiometry, while the latter presented a unique opportunity for training and evaluation in the presence of these same experts. The five laboratory sessions were concerned with (1) determining the responsivity of a spectroradiometer and the spectral radiance of an unknown integrating sphere source, (2) demonstrating spectral field calibration procedures for an integrating sphere using three different instruments, (3) measuring spectral radiance using the plaque method, (4) setting up and aligning lamp calibration transfer standards using the NIST specifications for irradiance measurements, and (5) characterizing radiometric instruments. In addition to documenting some supplemental studies performed outside the laboratory sessions, this report includes an evaluation of the hardware that has been used during the SIRREX activities plus a critical evaluation of SIRREX objectives.

Johnson, B. Carol

SeaWiFS Postlaunch Technical Report Series: The Fifth Sea-WiFS Intercalibration Round-Robin Experiment (SIRREX-5), July 1996 - Volume 7

This report documents the fifth Sea-viewing Wide Field-of-view Sensor (SeaWiFS) Intercalibration Round-Robin Experiment (SIRREX-5), which was held at the National Institute of Standards and Technology (NIST) on 23-30 July 1996. The agenda for SIRREX-5 was established based on recommendations made during SIRREX-4. For the first time in a SIRREX activity, instrument intercomparisons were performed at field sites, which were near NIST. The goals of SIRREX-5 were to continue the emphasis on training and the implementation of standard measurement practices, investigate the calibration methods and measurement chains in use by the oceanographic community, provide opportunities for discussion, and intercompare selected instruments. As at SIRREX-4, the day was divided between morning lectures and afternoon laboratory exercises. A set of core laboratory sessions were performed: 1) in-water radiant flux measurements; 2) in-air radiant flux measurements; 3) spectral radiance responsivity measurements using the plaque method; 4) device calibration or stability monitoring with portable field sources; and 5) various ancillary exercises designed to illustrate radiometric concepts. Before, during, and after SIRREX-5, NIST calibrated the SIRREX-5 participating radiometers for radiance and irradiance responsivity. The Facility for Automated Spectroradiometric Calibrations (FASCAL) was scheduled for spectral irradiance calibrations for standard lamps during SIRREX-5. Three lamps from the SeaWiFS community were submitted and two were calibrated.

Hooker, Stanford B.

SeaWiFs Technical Report Series. Volume 34: The Third SeaWiFS Intercalibration Round-Robin Experiment (SIRREX-3), 19-30 September 1994

This report presents results of the third Sea-viewing Wide Field-of-view Sensor (SeaWiFS) Intercalibration Round- Robin Experiment (SIRREX-3), which was held at the San Diego State University (SDSU) Center for Hydro-Optics and Remote Sensing (CHORS) on 19-30 September 1994. Spectral irradiances of FEL lamps belonging to each participant were intercompared by reference to the National Institute of Standards and Technology (NIST) scale of spectral irradiance using secondary standard lamps F268, F269, and F182, with a Type A uncertainty between 1.1-1.5%. This level of uncertainty was achieved despite difficulties with lamp F269. The average spectral irradiances of FEL lamps, compared in both SIRREX-2 and SIRREX-3, differed between the two experiments by 1.5%, which probably indicates that the values assigned to the secondary standard lamp at the time of SIRREX-2 were in error. With two exceptions, spectral radiance values of integrating sphere sources were measured during SIRREX-3 with uncertainties in temporal stability of less than 0.3% and absolute uncertainties of 1.5-2.0%. This is a significant improvement over similar intercomparisons in SIRREX- I and SIRREX-2. Plaque reflectances were intercompared with an uncertainty of about 1-2%, but the absolute uncertainty is undefined. Although this is an improvement over results of previous SIRREXS, the sources and magnitude of uncertainty associated with transfers of spectral radiance using plaques requires further evaluation in future experiments.

Hooker, Stanford B.

Outdoor performance results for NBS Round Robin collector no. 1

The efficiency of a PPG flat-plate solar collector was evaluated utilizing an outdoor solar collector test facility at the NASA-Lewis Research Center, as part of the National Bureau of Standards 'round robin' collector test program. The correlation equation for collector thermal efficiency Eta curve fit of the data was: Eta = 0.666 - 1.003(Btu/hr-sq ft-F) Theta, where the parameter Theta is the difference between the average fluid temperature and the ambient temperature, all divided by the total flux impinging on the collector.

Miller, D. R.

Development of AM 1.5 global measurement procedures and international cell measurement round robin

The development of the capability for measurement under global irradiance spectral distribution is reported. The airmass 1.5 global measurement procedure is given. Also given is the procedure and justification for using the large area pulsed solar simulator (LAPSS). The status of the international round robin of reference cell measurements managed by the Commission of European Communities (CEC) is described.

Mueller, R.

The Fourth SeaWiFS HPLC Analysis Round-Robin Experiment (SeaHARRE-4)

Ten international laboratories specializing in the determination of marine pigment concentrations using high performance liquid chromatography (HPLC) were intercompared using in situ samples and a mixed pigment sample. Although prior Sea-viewing Wide Field-of-view Sensor (SeaWiFS) High Performance Liquid Chromatography (HPLC) Round-Robin Experiment (SeaHARRE) activities conducted in open-ocean waters covered a wide dynamic range in productivity, and some of the samples were collected in the coastal zone, none of the activities involved exclusively coastal samples. Consequently, SeaHARRE-4 was organized and executed as a strictly coastal activity and the field samples were collected from primarily eutrophic waters within the coastal zone of Denmark. The more restrictive perspective limited the dynamic range in chlorophyll concentration to approximately one and a half orders of magnitude (previous activities covered more than two orders of magnitude). The method intercomparisons were used for the following objectives: a) estimate the uncertainties in quantitating individual pigments and higher-order variables formed from sums and ratios; b) confirm if the chlorophyll a accuracy requirements for ocean color validation activities (approximately 25%, although 15% would allow for algorithm refinement) can be met in coastal waters; c) establish the reduction in uncertainties as a result of applying QA procedures; d) show the importance of establishing a properly defined referencing system in the computation of uncertainties; e) quantify the analytical benefits of performance metrics, and f) demonstrate the utility of a laboratory mix in understanding method performance. In addition, the remote sensing requirements for the in situ determination of total chlorophyll a were investigated to determine whether or not the average uncertainty for this measurement is being satisfied.

Hooker, Stanford B.

Results of the Second SeaWiFS Data Analysis Round Robin, March 2000 (DARR-00)

The accurate determination of upper ocean apparent optical properties (AOPs) is essential for the vicarious calibration of the Sea-viewing Wide Field-of-view Sensor (SeaWiFS) instrument and the validation of the derived data products. To evaluate the importance of data analysis methods upon derived AOP values, the Second Data Analysis Round Robin (DARR-00) activity was planned during the latter half of 1999 and executed during March 2000. The focus of the study was the intercomparison of several standard AOP parameters: (1) the upwelled radiance immediately below the sea surface, L(sub u)(0(-),lambda); (2) the downward irradiance immediately below the sea surface, E(sub d)(0(-),lambda); (3) the diffuse attenuation coefficients from the upwelling radiance and the downward irradiance profiles, L(sub L)(lambda) and K(sub d)(lambda), respectively; (4) the incident solar irradiance immediately above the sea surface, E(sub d)(0(+),lambda); (5) the remote sensing reflectance, R(sub rs)(lambda); (6) the normalized water-leaving radiance, [L(sub W)(lambda)](sub N); (7) the upward irradiance immediately below the sea surface, E(sub u)(0(-)), which is used with the upwelled radiance to derive the nadir Q-factor immediately below the sea surface, Q(sub n)(0(-),lambda); and (8) ancillary parameters like the solar zenith angle, theta, and the total chlorophyll concentration, C(sub Ta), derived from the optical data through statistical algorithms. In the results reported here, different methodologies from three research groups were applied to an identical set of 40 multispectral casts in order to evaluate the degree to which differences in data analysis methods influence AOP estimation, and whether any general improvements can be made. The overall results of DARR-00 are presented in Chapter 1 and the individual methods used by the three groups and their data processors are presented in Chapters 2-4.

Hooker, Stanford B.

SeaWiFS technical report series. Volume 26: Results of the SeaWiFS Data Analysis Round-Robin, July 1994 (DARR-1994)

The accurate determination of upper ocean apparent optical properties (AOP's) is essential for the vicarious calibration of the sea-viewing wide field-of-view sensor (SeaWiFS) instrument and the validation of the derived data products. To evaluate the role that data analysis methods have upon values of derived AOP's, the first Data Analysis Round-Robin (DARR-94) workshop was sponsored by the SeaWiFS Project during 21-23 July, 1994. The focus of this intercomparison study was the estimation of the downwelling irradiance spectrum just beneath the sea surface, E(sub d)(0(sup -), lambda); the upwelling nadir radiance just beneath the sea surface, L(sub u)(0(sup -), lambda); and the vertical profile of the diffuse attenuation coefficient spectrum, K(sub d)(z, lambda). In the results reported here, different methodologies from four research groups were applied to an identical set of 10 spectroradiometry casts in order to evaluate the degree to which data analysis methods influence AOP estimation, and whether any general improvements can be made. The overall results of DARR-94 are presented in Chapter 1 and the individual methods of the four groups are presented in Chapters 2-5. The DARR-94 results do not show a clear winner among data analysis methods evaluated. It is apparent, however, that some degree of outlier rejection is required in order to accurately estimate L(sub u)(0(sup -), lambda) or E(sub d)(0(sup -), lambda). Furthermore, the calculation, evaluation and exploitation of confidence intervals for the AOP determinations needs to be explored. That is, the SeaWiFS calibration and validation problem should be recast in statistical terms where the in situ AOP values are statistical estimates with known confidence intervals.

Hooker, Stanford B.

Round Robin Measurements of Molten Salt Properties for LiF-NaF-KF (FLiNaK) and NaCl-KCl Mixtures

The development, operation, and regulation of nuclear reactors that utilize molten salts as fuel or as heat transfer media require knowledge of the thermal properties of the salt systems and quantification of the corresponding uncertainties. Knowledge of molten salt properties is also necessary for applications in material synthesis, processing, separations, solar thermal power generation, and energy storage. A round robin was conducted with national laboratory and university participants from twenty-one laboratories in five countries to compare property measurements, to better understand uncertainties, and to identify possible best practices. Two salt mixtures, each from a common batch, were distributed to participants for evaluation: equimolar NaCl-KCl and 45.0LiF-13.7NaF-41.3KF mol % (FLiNaK). Measurements were performed to determine the major constituent composition, oxygen content, density, thermal expansivity, melting point, and thermal conductivity. Error analysis was performed on each measurement for uncertainty quantification for each type of property that was explored. Finally, the resulting discussion of the methodologies used in this work is meant to lay the groundwork for the development of standard methods and reference materials for future high-temperature property measurements on halide melts.

11 - NUCLEAR FUEL CYCLE AND FUEL MATERIALS

The Second SeaWiFS HPLC Analysis Round-Robin Experiment (SeaHARRE-2)

Eight international laboratories specializing in the determination of marine pigment concentrations using high performance liquid chromatography (HPLC) were intercompared using in situ samples and a variety of laboratory standards. The field samples were collected primarily from eutrophic waters, although mesotrophic waters were also sampled to create a dynamic range in chlorophyll concentration spanning approximately two orders of magnitude (0.3 25.8 mg m-3). The intercomparisons were used to establish the following: a) the uncertainties in quantitating individual pigments and higher-order variables (sums, ratios, and indices); b) an evaluation of spectrophotometric versus HPLC uncertainties in the determination of total chlorophyll a; and c) the reduction in uncertainties as a result of applying quality assurance (QA) procedures associated with extraction, separation, injection, degradation, detection, calibration, and reporting (particularly limits of detection and quantitation). In addition, the remote sensing requirements for the in situ determination of total chlorophyll a were investigated to determine whether or not the average uncertainty for this measurement is being satisfied. The culmination of the activity was a validation of the round-robin methodology plus the development of the requirements for validating an individual HPLC method. The validation process includes the measurements required to initially demonstrate a pigment is validated, and the measurements that must be made during sample analysis to confirm a method remains validated. The so-called performance-based metrics developed here describe a set of thresholds for a variety of easily-measured parameters with a corresponding set of performance categories. The aggregate set of performance parameters and categories establish a) the overall performance capability of the method, and b) whether or not the capability is consistent with the required accuracy objectives.

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