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At least 451 records · Page 25

The development and application of the stirred‐reactor coupon analysis (SRCA) test method

A new technique, termed the stirred‐reactor coupon analysis (SRCA) method, has been developed to measure the rate of glass dissolution in forward‐rate conditions. Monolithic glass coupons are partially masked with an inert material before placement in a large volume of well‐mixed solution with known chemistry and temperature for a predetermined duration. After the test, the mask is removed, and the difference in step height between the protected area and the exposed corroded portions of the sample coupon is measured to determine the extent of glass dissolution. The step height is converted to a rate measurement using the test duration and glass density. Test parameters such as sample surface preparation and test duration were evaluated to determine their effects on the measured rates. Additionally, results from an interlaboratory study (ILS) consisting of 12 laboratories from 11 different institutions are presented, where each laboratory performed 12 independent tests. When removing experimental outlier data, the 95% reproducibility limits for the SRCA method has no statistical difference with previously published standardized test methods used to determine the forward rate of glass dissolution. Overall, this paper describes steps necessary to perform the test method and provides the statistical calculations to evaluate test accuracy.

chemical durability↗

In-plasma photo-assisted etching of Si with chlorine aided by an external vacuum ultraviolet source

Photo-assisted etching of p-type Si was previously found to occur in a chlorine-containing, Faraday-shielded, inductively coupled plasma (ICP), and this was attributed to the vacuum ultraviolet (VUV) light generated by the plasma. Other causes for the very high etching rates were ruled out, including ion bombardment. In the present study, the substrate in the main Cl2/Ar ICP was subjected to extra VUV light that was generated in an independently controlled, auxiliary Ar/He ICP in tandem with the main ICP. The ICPs were separated by a tungsten mesh and a bundle of high-aspect-ratio quartz tubes in a honeycomb configuration. There was no measurable perturbation of the main plasma by the auxiliary plasma. The etching rate was found to be enhanced by 11%–51% with the additional VUV light provided by the auxiliary ICP. With absolute measurements of the auxiliary ICP photon flux at the sample surface, as described elsewhere, incredibly large etching yields of 90–240 Si atoms per photon were obtained. It is argued that etching is not a result of electron–hole pair formation but is instead ascribed to a photocatalytic chain reaction.

42 ENGINEERING↗

Ellipsometry: dielectric functions of anisotropic crystals and symmetry

The optical functions of anisotropic materials can be determined using generalized ellipsometry, which can measure the cross-polarization coefficients (CPs) of the sample surface reflections. These CPs have several symmetry relations with respect to the symmetry of the crystal. This paper explores the symmetry relations of these CPs for uniaxial, orthorhombic, and monoclinic crystals and the requirements for generalized ellipsometry. Several ellipsometry measurement configurations are examined, including the requirements for the accurate measurements of the dielectric functions of anisotropic crystals.

Jellison, Gerald E.↗

Uranium Processing Signatures for Nuclear Forensics (NA22 End of FY23 Report)

A vacuum induction melting (VIM) furnace was used to produce an ~120 kg depleted uranium (DU) rod in November 2021 from well characterized feedstock to investigate the separation of thorium (Th) and protactinium (Pa) from uranium (U) during U metal casting and quantify the behavior of the 230 Th/ 234 U and 231 Pa/ 235 U radiochronometry systems. This work suggested that while 234 Th, measured by gamma spectrometry, appears to segregate to the top and surface of the rod, the concentration of 230 Th determined by isotope dilution mass spectrometry (IDMS) in drill turnings from multiple locations in the rod, including the hot top, is relatively consistent. To evaluate whether Th is potentially enriched at only the very outer surface of the cast DU rod relative to the bulk material in the cast rod, thin surface samples were collected from the cast DU rod. Locations sampled included the inner diameter (ID) and outer diameter (OD) of the bottom of the casting and the ID, OD, and top face of the hot top (very top of the casting). The locations are shown in Figure 1. Four samples were taken from each location at different depths in the cast material. Each cut took approximately 0.03 – 0.05” off of the casting.

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗

An Improved Method for Extracting, Sorting, and AMS Dating of Pollen Concentrates From Lake Sediment

High-resolution chronologies are crucial for paleoenvironmental reconstructions, and are particularly challenging for lacustrine records of terrestrial paleoclimate. Accelerator Mass Spectrometry (AMS) radiocarbon measurement of terrestrial macrofossils is the most common technique for building age models for lake sediment cores, but relies on the presence of terrestrial macrofossils in sediments. In the absence of sufficient macrofossils, pollen concentrates represent a valuable source of dates for building high-resolution chronologies. However, pollen isolation and dating may present several challenges, as has been reported by different authors in previous work over the last few decades. Here we present an improved method for extracting, purifying and radiocarbon-dating pollen concentrates using flow cytometry to improve the extraction efficiency and the purity of the pollen concentrates. Overall, the nature of the sediments and the abundance of the pollen represent major considerations in obtaining enough pollen grains and, consequently, enough carbon to be dated. Further, the complete separation of pollen from other forms of organic matter is required to ensure the accuracy of the dates. We apply the method to surface samples and sediment cores recovered from two contrasting lake basins on the eastern side of the Sierra Nevada (California), and describe the variations that may be used to optimize pollen preparation from a variety of sediments.

58 GEOSCIENCES↗

Effects of high-pressure hydrogen on storage vessel materials

Tensile tests on welded plates of three grades of steel indicate an appreciable decrease of tensile strength and ductility of notched specimens and a decrease in ductility of unnotched samples. Surface cracking, evident in unnotched specimens, is conducive to breakdown in tensile strength and ductility.

Chandler, W. T.↗

Extraterrestrial life detection.

Sequential analyses of planetary surface sample for extraterrestrial life detection, discussing chemistry, morphology, growth and metabolism for life attributes

Young, R. S.↗

Apollo 12 soil and breccia

Apollo 12 lunar soil and breccia core tube and surface samples optical and electron microscope and microprobe analysis, relating data to geologic processes

Clanton, U. S.↗

Effect of metallurgical structure and properties on adhesion and friction behavior of cobalt alloys

The metallurgical structure and some of the mechanical properties of two cobalt alloys, cobalt-50% iron and cobalt-25% molybdenum-10% chromium, were determined under various heat treated conditions. The mechanical properties of the bcc disordered Co-50Fe alloy, which was found to be very brittle, indicated an exceedingly low fracture strength, low hardness, and very weak grain boundary strength. Ordering by suitable heat treatment only produced a more brittle material with a lower fracture strength and a slightly higher hardness value. Work hardening was found to produce a finer grain structure and a greater grain boundary strength. Tensile properties were examined. It was found that the Co-25Mo-10Cr alloy was difficult to place in the alpha Co solid solution condition, which limited the ability to use precipitation as a hardening reaction. Over two hundred adhesion cycles from zero contact load, to maximum load, to fracture were conducted between couples for each of the above alloys in an ultrahigh vacuum system which would permit the sample surfaces to be cleaned of all contaminant layers. In the Co-50Fe case, the calculated fracture stress from the adhesion tests showed values in the range of 80 to 150 k.s.i., which is about ten times greater than the values from tension tests.

Keller, D. V., Jr.↗

Spacecraft orientation and exposure to environment, Appendix A

Material removed from the spacecraft and returned to earth remained on the lunar surface for 31.9 lunations. None of the returned parts received the maximum 10,686 hours of exposure because of shadowing by the planar array antenna, solar panel, thermal control compartments, or other parts of the spacecraft. To determine the actual exposure of specific parts to sunlight, six series of photographs were taken. A one-fifth-scale model spacecraft was oriented to a collimated light source simulating the orientation of Surveyor with the sun. Three cameras were set up to view different parts of the spacecraft. The data obtained from these photographs permitted an evaluation of the effects of exposure to solar radiation on the camera and its parts, the surface sampling scoop, and the strut from the radar altimeter and Doppler velocity sensor.

Nickle, N. L.↗

Infrared absorptivities of transition metals at room and liquid-helium temperatures.

Evaluation of experimental data concerning the normal spectral absorptivities of the transition metals, nickel, iron, platinum, and chromium, at both room and liquid-helium temperatures in the wavelength range from 2.5 to 50 microns. The absorptivities were derived from reflectivity measurements made relative to a room-temperature vapor-deposited gold reference mirror. The absorptivity of the gold reference mirror was measured calorimetrically, by use of infrared laser sources. Investigation of various methods of sample-surface preparation resulted in the choice of a vacuum-annealing process as the final stage. The experimental results are discussed on the basis of the anomalous-skin-effect theory modified for multiple conduction bands. As predicted, the results approach a single-band model toward the longer wavelengths. Agreement between theory and experiment is considerably improved by taking into account the modification of the relaxation time due to the photon-electron-phonon interaction proposed by Holstein (1954) and Gurzhi (1958); but, particularly at helium temperatures, the calculated curve is consistently below the experimental results.

Jones, M. C.↗

Alpha particles in solar cosmic rays over the last 80,000 years.

Present-day (1967 to 1969) fluxes of alpha particles from solar cosmic rays, determined from satellite measurements, were used to calculate the production rates of cobalt-57, cobalt-58, and nickel-59 in lunar surface samples. Comparisons with the activities of nickel-59 (half-life, 80,000 years) measured in lunar samples indicate that the long-term and present-day fluxes of solar alpha particles are comparable within a factor of approximately 4.

Lanzerotti, L. J.↗

Effects of atmospheric moisture on rock resistivity.

This study examines the changes in resistivity of rock samples as induced by atmospheric moisture. Experiments were performed on samples of hematitic sandstone, pyrite, and galena. The sandstone underwent a change in resistivity of four orders of magnitude when it was measured in a vacuum of 500 ntorr and in air of 37% relative humidity. Pyrite and galena showed no variations in resistivity when they were measured under the same conditions. These results, plus others obtained elsewhere, indicate that rocks of the resistive type are affected in their electrical properties by atmospheric moisture, whereas rocks of the conductive type are not. The experimental evidence obtained is difficult to reconcile with a model of aqueous electrolytic conduction on the sample surface. It is instead suggested that adsorbed water molecules alter the surface resistivity in a manner similar to that observed in semiconductors and insulators.

Alvarez, R.↗

A theoretical model for lunar surface material thermal conductivity.

This paper presents a theoretical thermal conductivity model for the uppermost layer of lunar surface material under the lunar vacuum environment. The model assumes that the lunar soil can be simulated by spherical particles in contact with each other and that the effective thermal conductivity is a function of depth, temperature, porosity, particle dimension, and mechanical-thermal properties of the solid particles. Two modes of heat transport are considered, conduction and radiation - with emphasis on the contact resistance between particles. The model gives effective conductivity values that compare favorably with the experimental data from lunar surface samples obtained on Apollo 11 and 12 missions.

Khader, M. S.↗

Development study of the X-ray scattering properties of a group of optically polished flat samples

Four optically polished flat samples were tested at wavelengths of 8.34 A, 13.3 A, and 44 A and 0.5 deg, 0.92 deg, 1.5 deg, 2.0 deg and 4.0 deg angle of incidence. The four samples were also tested at 8.34 A and 0.92 deg angle of incidence for three additional angular orientations about an axis normal to the sample surface: 45 deg, 90 deg and 180 deg from the 0 deg position. The tests indicate that the scattering was greater at 44 A than at 13.3 A and 8.34 A. The orientation tests indicated that no great irregularities were present.

Froechtenigt, J. F.↗