The Certification of Standard Reference Material 1979: Powder Diffraction Line Profile Standard for Crystallite Size Analysis
Abstract not provided
Cline, James P.↗
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Ruggedness Evaluation of ASTM International Standard Test Methods for Shape Memory Materials: E3097 Standard Test Method for Mechanical Uniaxial Constant Force Thermal Cycling of Shape Memory Alloys
This paper evaluates the ruggedness testing of the newly released ASTM International E3097 Standard Test Method for Mechanical Uniaxial Constant Force Thermal Cycling of Shape Memory Alloys. The ruggedness experiment was designed with eight runs in two replicates, consisting of seven factors of strain rate (ė), heating and cooling rates (T(sub heat) and T(sub cool), respectively), upper and lower cycle temperatures (UCT and LCT, respectively), hold time (t(sub hold)), and minimum load (F(sub min)) imparted on the samples. The results indicate that the hold time factor had no effect on any result variable. The minimum load factor, alternatively, had the greatest effect on several result variables, with the greatest influence on the strains at martensite start and finish (strain variation ~0.1 percent), and the strains at the upper and lower cycle temperatures (strain variation of 0.14 percent). The UCT was found to have a large effect on the austenite and martensite finish tangent line and data intersect, denoted by A(sub f(sup *)) and M(sub f(sup*)), by ~17 and 4 °C, respectively. The testing methodology, analysis techniques, and resulting conclusions on the ruggedness of the test methods are presented.
Benafan, Othmane↗
Ruggedness Evaluation of ASTM International Standard Test Methods for Shape Memory Materials: E3097 Standard Test Method for Mechanical Uniaxial Constant Force Thermal Cycling of Shape Memory Alloys
This paper evaluates the ruggedness testing of the newly released ASTM International E3097 Standard Test Method for Mechanical Uniaxial Constant Force Thermal Cycling of Shape Memory Alloys. The ruggedness experiment was designed with eight runs in two replicates, consisting of seven factors of strain rate (ė), heating and cooling rates (Ṫ(heat) and Ṫ(cool), respectively), upper and lower cycle temperatures (UCT and LCT, respectively), hold time (thold), and minimum load (Fmin) imparted on the samples. The results indicate that the hold time factor had no effect on any result variable. The minimum load factor, alternatively, had the greatest effect on several result variables, with the greatest influence on the strains at martensite start and finish (strain variation ~0.1 percent), and the strains at the upper and lower cycle temperatures (strain variation of 0.14 percent). The UCT was found to have a large effect on the austenite and martensite finish tangent line and data intersect, denoted by Af* and Mf*, by ~17 and 4 °C, respectively. The testing methodology, analysis techniques, and resulting conclusions on the ruggedness of the test methods are presented.
shape memory alloy↗
Ruggedness Evaluation of ASTM International Standard Test Methods for Shape Memory Materials: E3098 Standard Test Method for Mechanical Uniaxial Pre-strain and Thermal Free Recovery of Shape Memory Alloys
This paper evaluates the ruggedness testing of the recently released ASTM International E3098 Standard Test Method for Mechanical Uniaxial Pre-strain and Thermal Free Recovery of Shape Memory Alloys. The ruggedness experiment was designed with eight runs in two replicates, consisting of seven factors: strain rate (ė), heating and cooling rates (Ṫ heat and Ṫ cool , respectively), upper and lower cycle temperatures (UCT and LCT, respectively), hold time (t hold ), and minimum load (F min ) imparted on the samples. The results indicate that the strain rate factor had no effect on any result variable, whereas the minimum load factor had a large effect on several result variables including the austenite start and martensite finish temperatures as well as most of the strain measurements from the thermal cycle. The lower cycle temperature factor had a large effect on the stress at maximum strain during pre-straining (e i ), denoted by S i , at ~7.2 MPa, as well as the A f , at 5.47 °C. Closely following the LCT effect, Ṫ heat was found to have a large effect on the austenite start temperature (A s ), at a value of ~2.72 °C. The testing methodology, analysis techniques, and resulting conclusions on the ruggedness of the test method are presented.
Shape memory alloys↗
Standard research materials: Feces and urine
Preparation of the standard research materials, preparation of the samples for analysis, elemental analysis, composition of standard research materials, and methodology are discussed.
Source record↗
The oxygen stable isotope composition of CRM 125-A UO 2 standard reference material
While there is a clear need for standardized reference materials for analytical calibrations and for inter-laboratory comparisons, there are not currently any for the oxygen stable isotopic composition of uranium oxides. In this paper we summarize the results from four laboratories by seven different methods of oxygen stable isotope analyses using fluorination techniques of CRM 125-A UO 2 Standard Reference Material. We synthesize these data and methods to arrive at a consensus oxygen stable isotope composition for CRM 125-A $δ$ 18 O = -9.63‰ (±0.29‰) VSMOW. We discuss methodological differences between analytical approaches, including furnace vs laser heating, fluorination using BrF 5 or ClF 3 , as well as calibration strategies. We highlight the potential effects of calibration scale compression from single-point calibrations using reference material with $δ$ 18 O values having a large relative difference from the sample being analyzed. We demonstrate how calibration scale compression can yield differences in calibrated $δ$ 18 O values up to ~2‰ for samples with ~20‰ difference from a single reference material, if the calibration slope of different analytical systems differs by 0.1. In conclusion, we suggest the use of liquid water calibration standards sealed in silver capillary tubes for multi-point calibrations of fluorination analysis systems.
07 ISOTOPE AND RADIATION SOURCES↗
STANDARD REFERENCE MATERIAL CHARPY TESTING FROM HIGH FLUENCE SURVEILLANCE CAPSULE
The Palisades Nuclear Generating Station included in its original surveillance program a surveillance capsule, designated A-60. The capsule was removed from its surveillance position in early 1995 and has been resident in the spent fuel pool since that time. It was harvested to perform characterization of surveillance specimens in this capsule in 2023. This capsule was irradiated to a fluence of 1.96x1020 n/cm2 (E> 1MeV) that is equivalent for more than 150 effective full power years for the current US reactor pressure vessel (RPV) fleet. This capsule contained several materials, including Charpy specimens of standard reference material (SRM) from Heavy-Section Steel Technology (HSST) A533-B Plate 01. To perform Charpy testing of this highly irradiated material, the new Charpy specimen transfer system was designed and implemented on Charpy impact testing machine in the hot cell to accommodate remote testing of these specimens. This new transfer system includes integrated environmental chamber to cool or heat Charpy specimens to the desired temperature. Testing of this highly irradiated material revealed very large shift of Charpy transition temperature, 188oC.
Sokolov, Mikhail [ORNL] (ORCID:0000000256373346)↗
Barium Fluoride as a Standard Reference Material for Infrared Refractometry
This work proposes a standard reference material (SRM) for measurements of refractive index in the infrared spectral region (1–12 μm). The purpose of this material is to enable cross-method comparison of refractive index data obtained through minimum deviation, ellipsometry, interferometry, and prism coupling techniques. This will allow vendors and metrology laboratories, regardless of which technique they employ, to certify that their measurements meet required levels of accuracy, precision, and repeatability. Drawing on foundational work by Tilton at the National Bureau of Standards, a figure of merit for candidate SRM materials is outlined, and three materials are selected for further evaluation. Ultimately, barium fluoride is proposed as the most suitable SRM for the infrared spectral region, based on its broad transmission range, chemical and mechanical stability, low temperature dependence of refractive index, and well-characterized dispersion behavior.
Andrew Howe↗
Corresponding Standard Reference Material Data used in Partial Least Squares Regression Models for Sugar Composition Estimates in Biomass in: Economic Impact of Yield and Composition Variation in Bioenergy Crops: Populus trichocarpa
Corresponding Standard Reference Material Data used in Partial Least Squares Regression Models for Sugar Composition Estimates in Biomass in: Economic Impact of Yield and Composition Variation in Bioenergy Crops: Populus trichocarpa (for corresponding manuscript: DOI: 10.1002/bbb.2148) PDF Files: Images of 1H NMR spectra for neutralized 2-stage acid hydrolysates of 4 NIST Standard Reference Material biomass samples (Monterey Pine 8493, Sugarcane Bagasse 8491, Wheat Straw 8494, and Eastern Cottonwood/Poplar 8492) and 2 Center for Bioenergy Innovation reference biomass samples (Poplar - Populus trichocarpa and Switchgrass - Panicum Virgatum). Suppression of the water peak was achieved using a NOESY-1D with presaturation, a recycle delay of 5 s, and a total of 64 scans. Spectra were acquired at 298 K and processed with automatic phase correction, baseline correction, and chemical shift referencing to TSP-d4. Images show all 1H data from 10 to 1ppm with inset spectra of region of interest (4.0 to 3.1 ppm). Text Files: Spectra for neutralized 2-stage acid hydrolysates of 4 NIST Standard Reference Material biomass samples (Monterey Pine 8493, Sugarcane Bagasse 8491, Wheat Straw 8494, and Eastern Cottonwood/Poplar 8492) and 2 Center for Bioenergy Innovation reference biomass samples (Poplar - Populus trichocarpa and Switchgrass - Panicum Virgatum) were converted into text files for plotting. Files contain 8192 points of raw spectral data from 12.23 to -2.78 ppm. The text file contains 4 columns of data and includes: Point number, Intensity, Hz, and ppm. Xcel Spreadsheet: HPLC measured monomeric sugar concentrations and bucketed 1H NMR data used to build monomeric sugar composition prediction models. Sugar composition in biomass determined from HPLC analyses are given in mg sugar/mg of biomass. Spectral bucketing was performed using Bruker’s AMIX software. Spectra were divided into 0.005 ppm buckets in the region of 3.10– 4.15 ppm for a total of 210 buckets. Headers for the bucketed data are the chemical shift in ppm of the center of the bucket. Bucketed data was used to build partial least squares models for subsequent predictions in The Unscrambler v. 10.5(CAMO A/S, Trondheim, Norway). The formation of methanol during hydrolysis interferes with the quantitative NMR analysis of sugars, so the methanol peak centered at 3.37 ppm and spanning four buckets (3.2925 – 3.2775 ppm) was set to zero for all spectra.
09 BIOMASS FUELS↗
Synchrotron X-ray Microdiffraction and Fluorescence Imaging of Mineral and Rock Samples
In this paper, we describe a detailed procedure for acquiring and processing x-ray microfluorescence (μXRF), and Laue and powder microdiffraction two-dimensional (2D) maps at beamline 12.3.2 of the Advanced Light Source (ALS), Lawrence Berkeley National Laboratory. Measurements can be performed on any sample that is less than 10 cm x 10 cm x 5 cm, with a flat exposed surface. The experimental geometry is calibrated using standard materials (elemental standards for XRF, and crystalline samples such as Si, quartz, or Al 2 O 3 for diffraction). Samples are aligned to the focal point of the x-ray microbeam, and raster scans are performed, where each pixel of a map corresponds to one measurement, e.g. , one XRF spectrum or one diffraction pattern. The data are then processed using the in-house developed software XMAS, which outputs text files, where each row corresponds to a pixel position. Representative data from moissanite and an olive snail shell are presented to demonstrate data quality, collection, and analysis strategies.
36 MATERIALS SCIENCE↗
Surrogate Post-Detonation Urban Debris (SPUD): Standard Reference Materials 4600 and 4601
If a terrorist nuclear explosion were to occur in the United States, high-quality (accurate and precise) legally defensible nuclear forensics measurements will be required to assure the certainty and confidence needed, for conclusions drawn from these data will be coupled with law enforcement and intelligence information for the purposes of attribution and retribution. Standard Reference Materials (SRMs)/Certified Reference Materials (CRMs) establish the traceability, accuracy, and precision of nuclear forensic measurements and provide the ability to benchmark measurement methods essential to meeting the requirements of legal scrutiny. Currently there is a critical shortage of key SRMs/CRMs required for accurate and precise measurements that are fundamental to nuclear measurements supporting pre- and post-detonation nuclear forensics. Supplies either do not exist, are not good enough, are in short supply, and/or are very expensive. The radionuclide measurement techniques and data quality objectives for pre- and post-detonation nuclear forensics are quite different than the applications for which the current suite of available SRMs/CRMs was developed. Specifically, 1) modern mass spectrometry methods have largely replaced traditional activity-based measurement methods for quantifying small quantities of long-lived radionuclides and most trace radionuclide SRMs/CRMs are certified for activity and are thus not adequate for current applications, 2) modern instrumental methods are capable of higher precision than historic measurement techniques, and in some cases exceed the precision of the available SRMs/CRMs, and 3) the quality assurance requirements for pre- and post-detonation nuclear forensics are such that the existing cadre of SRMs/CRMs does not adequately support the needs for method validation. There are numerous governmental stakeholders both within the US (DOE, DoD) and internationally (IAEA, JRC-ITU) whose missions are either directly involved with nuclear forensics measurements or rely on the forensic data obtained to make the exacting policy decisions (DOJ (FBI), DHS, CIA, DIA, DoD) associated with disrupting the production of illicit nuclear materials, interdicted nuclear materials or a nuclear/radiological detonation event. Starting in 2008 the DHS NTNFC, in collaboration with NBL and NIST, took on the production of suitable SRMs/CRMs for the pre-detonation nuclear forensics community. Two CRMs have been released since the start of this effort and two more are slated for completion in 2016. More recently, NIST, as a part of its mission as the US National Metrology Institute (NMI) to deliver standards (providing traceability) and foster homeland security, has launched the first certification campaign of a measurement traceable post nuclear detonation SRM. NIST, in cooperation with partner labs (AFIT (DoD), FBI (DOJ), and NPL) and with support from the FBI, has developed two Surrogate Post-Detonation Urban Debris (SPUD) Standard Reference Materials (SRMs) - SRM 4600 and 4601. These SRMs have been developed to simulate the expected debris mixture from the detonation of an Improvised Nuclear Device (IND) in an urban environment, which is capable of producing fresh fission as well as activation products. The elemental composition of the vitrified debris materials is a composite of minerals and metals characteristic of the concrete and steel, the building materials that would be exposed to a nuclear detonation and whose resulting activation products would be found in rubble samples collected for forensics evidence and attribution. Additionally, because post-detonation samples would also contain short-lived fission products, the debris materials have been doped with Uranium (U). To create the nuclear fission products, samples of the SPUD materials can be placed in a well-characterized nuclear reactor and exposed to a set neutron flux and energy, causing the encased U atoms to split and yield short-lived fission products. Because a known amount of U is added to the SPUD materials it is feasible to determine the concentration of the resulting fission products. The subsequent irradiated SPUD glass would be chemically similar to samples that would be generated in an actual detonation, and thus can serve as a standardized reference material for nuclear forensic post detonation measurements. (authors)
61 RADIATION PROTECTION AND DOSIMETRY↗
Retrospective Analysis of NIST Standard Reference Material 1450, Fibrous Glass Board, for Thermal Insulation Measurements
Thermal conductivity data acquired previously for the establishment of Standard Reference Material (SRM) 1450, Fibrous Glass Board, as well as subsequent renewals 1450a, 1450b, 1450c, and 1450d, are re-analyzed collectively and as individual data sets. Additional data sets for proto-1450 material lots are also included in the analysis. The data cover 36 years of activity by the National Institute of Standards and Technology (NIST) in developing and providing thermal insulation SRMs, specifically high-density molded fibrous-glass board, to the public. Collectively, the data sets cover two nominal thicknesses of 13 mm and 25 mm, bulk densities from 60 kg∙m -3 to 180 kg∙m -3 , and mean temperatures from 100 K to 340 K. The analysis repetitively fits six models to the individual data sets. The most general form of the nested set of multilinear models used is given in the following equation: λ(ρ, T) = α 0 + α 1 ρ +α 2 T + α 3 T 3 +α 4 e - ($\frac{T-a_{5}}{a_{6}}$) 2 = where λ(ρ,T) is the predicted thermal conductivity (W∙m -1 ∙K -1 ), ρ is the bulk density (kg∙m -3 ), T is the mean temperature (K) and $a_i$ (for i = 1, 2, … 6) are the regression coefficients. The least squares fit results for each model across all data sets are analyzed using both graphical and analytic techniques. The prevailing generic model for the majority of data sets is the bilinear model in ρ and T. λ(ρ, T) = α 0 + α 1 ρ +α 2 T One data set supports the inclusion of a cubic temperature term and two data sets with low-temperature data support the inclusion of an exponential term in T to improve the model predictions. Physical interpretations of the model function terms are described. Recommendations for future renewals of SRM 1450 are provided. An Addendum provides historical background on the origin of this SRM and the influence of the SRM on external measurement programs.
regression analysis↗
Addressing the Amorphous Content Issue in Quantitative Phase Analysis: The Certification of NIST Standard Reference Material 676a
A non-diffracting surface layer exists at any boundary of a crystal and can comprise a mass fraction of several percent in a finely divided solid. This has led to the long-standing issue of amorphous content in standards for quantitative phase analysis (QPA). NIST standard reference material (SRM) 676a is a corundum ({alpha}-Al{sub 2}O{sub 3}) powder, certified with respect to phase purity for use as an internal standard in powder diffraction QPA. The amorphous content of SRM 676a is determined by comparing diffraction data from mixtures with samples of silicon powders that were engineered to vary their specific surface area. Under the (supported) assumption that the thickness of an amorphous surface layer on Si was invariant, this provided a method to control the crystalline/amorphous ratio of the silicon components of 50/50 weight mixtures of SRM 676a with silicon. Powder diffraction experiments utilizing neutron time-of-flight and 25 keV and 67 keV X-ray energies quantified the crystalline phase fractions from a series of specimens. Results from Rietveld analyses, which included a model for extinction effects in the silicon, of these data were extrapolated to the limit of zero amorphous content of the Si powder. The certified phase purity of SRM 676a is 99.02% {+-} 1.11% (95% confidence interval). This novel certification method permits quantification of amorphous content for any sample of interest, by spiking with SRM 676a.
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
A thermal porosimetry method to estimate pore size distribution in highly porous insulating materials
Standard pore size determination methods such as mercury porosimetry, nitrogen sorption, microscopy, or x-ray tomography are not always applicable to highly porous, low density, and thus very fragile materials. For this kind of materials, a method based on thermal characterization is proposed. Indeed, the thermal conductivity of a highly porous and insulating medium is significantly dependent on the thermal conductivity of the interstitial gas that depends on both gas pressure and size of the considered pore (Knudsen effect). It is also possible to link the pore size with the thermal conductivity of the medium. Thermal conductivity measurements are realized on specimens placed in an enclosure where the air pressure is successively set to different values varying from 10{sup -1} to 10{sup 5} Pa. Knowing the global porosity ratio, an effective thermal conductivity model for a two-phase air-solid material based on a combined serial-parallel model is established. Pore size distribution can be identified by minimizing the sum of the quadratic differences between measured values and modeled ones. The results of the estimation process are the volume fractions of the chosen ranges of pore size. In order to validate the method, measurements done on insulating materials are presented. The results are discussed and show that pore size distribution estimated by the proposed method is coherent.
36 MATERIALS SCIENCE↗
Density functionals combined with van der Waals corrections for graphene adsorbed on layered materials
Standard density functionals like Perdew-Burke-Ernzerhof (PBE) or Strongly Constrained and Appropriately Normed (SCAN) need a correction to account for long-range van der Waals (vdW) interaction. The damped Zaremba-Kohn model (dZK) starts from a formula for the vdW interaction of a distant atom with a solid surface, both with known dielectric properties, damps this formula at short range, and then treats an adsorbed molecule or atomic layer as a collection of renormalized atoms. Here, we extend this model to graphene adsorbed on semiconducting layered materials [bulk graphite and hBN, and multilayer transition metal dichalcogenides (TMD)] by including the C 4 asymptotic term and multiple electrostatic image effects due to the two surfaces of the substrate slabs in the vdW calculations. The resulting SCAN-vdW-dZK and PBE-vdW-dZK give approximately the same results for the systems considered here, in agreement with available reference values. The predicted binding energies are roughly 25% lower than those from SCAN+rVV10 (revised Vydrov and Van Voorhis 2010), and ~15% lower than those from PBE+rVV10. Since SCAN+rVV10 usually overbinds, the predicted binding energies by SCAN-vdW-dZK and PBE-vdW-dZK are expected to be closer to the true values. The predicted equilibrium binding distances from SCAN-vdW-dZK and PBE-vdW-dZK are slightly larger (~ 0.1 Å) than those from SCAN+rVV10, and close to those from SCAN. The binding energy depends upon the number of substrate layers more strongly in vdW-dZK than in rVV10. The C 4 -term contributions can be 40% of the total vdW interactions, and the C 5 term contributes about 10%. The effects of images and the back surfaces of slabs can contribute about 4–10%. The vdW interaction energy power laws from the vdW-dZK model for graphene adsorbed on multilayer MoS 2 show slowly varying decay to the pairwise exponent –4 with increasing separation $\textit{D}$, very similar to those obtained from the random-phase approximation and renormalization group approaches by Ambrosetti et al. Both the PBE-vdW-dZK and SCAN-vdW-dZK give a greater increase in interlayer binding energy when the TMD substrate changes from monolayer to four-layer for the graphene/TMD adsorption systems. This is consistent with the relevant electron-energy-loss spectroscopy experimental results showing increased dielectric response from the substrate with increasing substrate layer number.
75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
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↗
Ultrasonic angle beam standard reflector
A method that provides an impression profile in a reference standard material utilized in inspecting critically stressed components with pulsed ultrasound is described. A die stamp having an I letter is used to impress the surface of a reference material. The die stamp is placed against the surface and struck with an inertia imparting member to impress the I in the reference standard material. Upset may appear on the surface as a result of the impression and is removed to form a smooth surface. The stamping and upset removal is repeated until the entire surface area of a depth control platform on the die stamp uniformly contacts the material surface. The I impression profile in the reference standard material is utilized for reflecting pulsed ultrasonic beams for inspection purposes.
Berry, R. F., Jr.↗
Dielectric Property Testing of Powdery Materials: A Standardized Paraffin Composite Method
Presented by NETL at Materials Science & Technology, 10/18
Tempke, Robert S.↗