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At least 37 records · Page 2

Sealed container sampling device

Sampling device, by means of a tapered needle, pierces a sealed container while maintaining the seal and either evacuates or pressurizes the container. This device has many applications in the chemical, preservative and battery-manufacturing industries.

Hennigan, T. J.↗

Preliminary Study of Microfluidic Chip as Sample Containment for Quantitative hiRX Measurements

This is a preliminary report on the development and testing of a microfluidic sample chip for the hiRX prototype instrument test slated for FY14. We used an in-house manufacturing laser-based tool at LANL. This allowed us to change experimental parameters rapidly and generate desired features as needed. The finished product was not a polished commercial grade specimen; however we were able to make these relatively easily and quite rapidly. The performance of these handmade devices was surprisingly good with about 5% RSD for a 1 microliter sample volume.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Resonant ultrasound spectroscopy for crystalline samples containing initial strain

Resonant ultrasound spectroscopy (RUS) is a mature and robust technique for the nondestructive characterization of the elastic properties of solids capable of providing the elastic constants of anisotropic crystalline solids. The traditional method is based on assuming that the solid is linear elastic and, therefore, obeys a linearized Hookean constitutive relationship (Hooke’s law). In this work, an alternative constitutive law is provided that allows for an initial strain or prestrain to be present stemming from residual stress. Then, the constitutive relationship is integrated into the RUS framework. The model is demonstrated using a realistic prestrain field obtained by simulating shot-peening processing of a polycrystalline Cu sample. The sensitivity of the resonances to the developed prestrain is established and discussed. This work allows researchers to consider the influence of initial strain or residual stress in their samples and the potential influence on accurate elastic constant estimates. The model also supports the potential of RUS for the nondestructive characterization of prestrain in materials.

42 ENGINEERING↗

Accelerated 133 Xe Quantification in Samples Containing Significant 133 mXe

The quantification of 133 Xe in the presence of its mother radionuclide 133 mXe requires the full quantification of both to perform the ingrowth correction for 133 Xe. Due to the nature of both of these radionuclides, the 133 mXe requires significantly more time to quantify by High Purity Germanium (HPGe) detectors due to lower production yields, lower gamma emission probabilities, and lower detection efficiencies. This work shows that 133 Xe and 133 mXe quantification can be accelerated by measuring the 133m:133 activity ratio for a large batch of material and applying this activity ratio to assays of lower activity subsamples of the same batch of material. Included in this report are derivations of the required decay correction equations, and experiments using actual samples to validate the performance of these equations. A detector calibration method is also shown that leverages this method as an alternative to existing calibration methods for 133 mXe quantification.

133mXe↗

Percentage of Water Retained in Icy Lunar Regolith Simulant During Transfer into a Sample Container

We now know that water ice exists on the lunar surface thanks to the findings of multiple lunar missions such as LRO and LCROSS. However, before we develop systems that can utilize this precious resource at a useful scale, we need to acquire more data about the concentration of water in the lunar regolith and how it may vary by depth and location. The OVEN (Optimized Volatile Extraction Node) system is designed to determine the concentration of water as part of an instrument called WAVE (Water Analysis & Volatile Extraction) which can be deployed during a lunar resource prospecting mission. Experiments were carried out at the Johnson Space Center in order to better understand the potential losses of water that may occur during a prospecting mission when a sample is transferred from a drill to the OVEN. A description of the experiment as well as the results will be presented here.

ISRU↗

Preparation of Mo-Re-C samples containing Mo{sub 7}Re{sub 13}C with the β-Mn-type structure by solid state reaction of planetary-ball-milled powder mixtures of Mo, Re and C, and their crystal structures and superconductivity

Mo-Re-C compounds containing Mo{sub 7}Re{sub 13}C with the β-Mn structure were synthesized with high-melting-temperature metals Mo, Re, and C powders using a conventional solid state method with a planetary ball milling machine instead of the arc melting method. Use of the ball milling machine was necessary to obtain Mo{sub 7}Re{sub 13}C with the β-Mn structure using the solid state method. Almost single-phase Mo{sub 7}Re{sub 13}C with a trace of impurity were obtained using the synthesis method. By XRF and lattice parameter measurements on the samples, Fe element existed in the compound synthesized using the planetary ball milling machine with a pot and balls made of steel, though Fe element was not detected in the compound synthesized using a pot and balls made of tungsten carbide. The former compound containg the Fe atom did not show superconductivity but the latter compound without the Fe atom showed superconductivity at 6.1 K. - Graphical abstract: Temperature dependence of the magnetic susceptibility measured under 10 Oe for the superconducting PBM-T samples without Fe element and non-superconducting PBM-S with Fe element. The inset is the enlarged view of the data for the PBM-S sample.

36 MATERIALS SCIENCE↗

Activation product analysis in a mixed sample containing both fission and neutron activation products

Activation analysis of gold (Au) is used to estimate neutron fluence resulting from a criticality event; however, such analyses are complicated by simultaneous production of other gamma-emitting fission products. Confidence in neutron fluence estimates can be increased by quantifying additional activation products such as platinum (Pt), tantalum (Ta), and tungsten (W). This work describes a radiochemical separation procedure for the determination of these activation products. Anion exchange chromatography is used to separate anionic forms of these metals in a nitric acid matrix; thiourea is used to isolate the Au and Pt fraction, followed by removal of the Ta fraction using hydrogen peroxide. W, which is not retained on the first anion exchange column, is transposed to an HCl/HF matrix to enhance retention on a second anion exchange column and finally eluted using HNO3/HF. Chemical separations result in a reduction in the minimum detectable activity by a factor of 287, 207, 141, and 471 for 182Ta, 187W, 197Pt, and 198Au respectively, with greater than 90% recovery for all elements. These results represent the highest recoveries and lowest minimum detectable activities for 182Ta, 187W, 197Pt, and 198Au from mixed fission-activation product samples to date, enabling considerable refinement in the measurement uncertainties for neutron fluences in highly complex sample matrices.

anion exchange↗

Monte Carlo simulations of channeling spectra recorded for samples containing complex defects

The main aim of the present paper is to describe the current status of the development of McChasy, a Monte Carlo simulation code, to make it suitable for the analysis of dislocations and dislocation loops in crystals. Such factors like the shape of the bent channel and geometrical distortions of the crystalline structure in the vicinity of dislocation has been discussed. Several examples of the analysis performed at different energies of analyzing ions are presented. The results obtained demonstrate that the new procedure applied to the spectra recorded on crystals containing dislocation yields damage profiles which are independent of the energy of the analyzing beam.

Carlo↗

Dual reactor for in situ/operando fluorescent mode XAS studies of sample containing low-concentration 3d or 5d metal elements

Transition metal elements are the most important elements of heterogeneous catalysts used for chemical and energy transformations. Many of these catalysts are active at a temperature higher than 400 °C. For a catalyst containing a 3d or 5d metal element with a low concentration, typically their released fluorescence upon the K-edge or L-edge adsorption of X-rays is collected for the analysis of chemical and coordination environments of these elements. However, it is challenging to perform in situ/operando X-ray absorption spectroscopy (XAS) studies of elements of low-energy absorption edges at a low concentration in a catalyst during catalysis at a temperature higher than about 450 °C. Here a unique reaction system consisting two reactors, called a dual reactor system, was designed for performing in situ or operando XAS studies of these elements of low-energy absorption edges in a catalyst at a low concentration during catalysis at a temperature higher than 450 °C in a fluorescent mode. This dual-reactor system contains a quartz reactor for preforming high-temperature catalysis up to 950 °C and a Kapton reactor remaining at a temperature up to 450 °C for collecting data in the same gas of catalysis. With this dual reactor, chemical and coordination environments of low-concentration metal elements with low-energy absorption edges such as the K-edge of 3d metals including Ti, V, Cr, Mn, Fe, Co, Ni, and Cu and L edge of 5d metals including W, Re, Os, Ir, Pt, and Au can be examined through first performing catalysis at a temperature higher than 450 °C in the quartz reactor and then immediately flipping the catalyst in the same gas flow to the Kapton reactor remained up to 450 °C to collect data. The capability of this dual reactor was demonstrated by tracking the Mn K-edge of the MnO x /Na 2 WO 4 catalyst during activation in the temperature range of 300-900 °C and catalysis at 850 °C.

47 OTHER INSTRUMENTATION↗

A Comparative Study of Single-pulse and Double-pulse Laser-Induced Breakdown Spectroscopy with Uranium-containing Samples

Laser-induced breakdown spectroscopy (LIBS) holds potential advantages in special nuclear material (SNM) sensing and nuclear forensics which require rapid analysis, minimal sample preparation and stand-off distance capability. SNM, such as U, however, result in crowded emission spectra with LIBS, and characteristic emission lines are challenging to discern. It is well-known that double-pulse LIBS (DPLIBS) improves the signal intensity for analytes over conventional single-pulse LIBS (SPLIBS). This study investigates U signal in a glass matrix using DPLIBS and compares to signal features obtained using SPLIBS. DPLIBS involves sequential firing of 1.06 µm Nd:YAG pre-pulse and 10.6 µm TEA CO2 heating pulse in near collinear geometry. Optimization of experimental parameters including inter-pulse delay and energy follows identification of characteristic lines and signals for bulk analyte Ca and minor constituent analyte U for both DPLIBS and SPLIBS. Spatial and temporal coupling of the two pulses in the proposed DPLIBS technique yields improvements in analytical merits with negligible further damage to the sample compared to SPLIBS. Subsequently, the study discusses optimum plasma emission conditions of U lines and relative figures of merit in both SPLIBS and DPLIBS. Investigation into plasma characteristics also addresses plausible mechanisms related to observed U analyte signal variation between SPLIBS and DPLIBS.

Skrodzki, P. J.↗

Finding Interstellar Particle Impacts on Stardust Aluminium Foils: The Safe Handling, Imaging, and Analysis of Samples Containing Femtogram Residues

Impact ionisation detectors on a suite of spacecraft have shown the direction, velocity, flux and mass distribution of smaller ISP entering the Solar System. During the aphelion segments of the Stardust flight, a dedicated collector surface was oriented to intercept ISP of beta = 1, and returned to Earth in January 2006. In this paper we describe the probable appeareance and size of IS particle craters from initial results of experimental impacts and numerical simulation, explain how foils are being prepared and mounted for crater searching by automated acquisition of high magnification electron images (whilst avoiding contamination of the foils) and comment on appropriate analytical techniques for Preliminary Examination (PE).

Kearsley, A. T.↗

Long-term material compatibility testing system

System includes procedure for hermetically sealing solid materials and fluids in glass ampoule and use of temperature-controlled facility containing sample holder, which permits sample containers to be retrieved safely and conveniently. Solid material and fluid are sealed within chemically-clean glass ampoule according to highly detailed procedure.

Toth, L. R.↗

Analysis of Mixed Aryl/Alkyl Esters by Pyrolysis Gas Chromatography-Mass Spectrometry in the Presence of Perchlorate

Mars is an important target for Astrobiology. A key goal of the MSL mission was to determine whether Mars was habitable in the past, a que-tion that has now been definitely determined to be yes. Another key goal for Mars exploration is to understand the origin and distribution of organic material on Mars; this question is being addressed by the SAM instrument on MSL, and will also be informed by two upcoming Mars exploration missions, ExoMars and Mars 2020. These latter two missions have instrumentation capable of detecting and characterize organic molecules. Over the next decade, these missions will analyze organics in surface, near-surface and sub-surface samples. Each mission has the capability to analyze organics by different methods (pyrolysis gas chromatography-mass spectrometry [py-GC-MS]; laser desorption and thermal volatilization GC-MS; and Raman spectroscopy). Plausibly extraterrestrial organics were recently discovered by the Mars Science Laboratory (MSL), providing an important first step towards understanding the organic inventory on Mars [1]. The compounds detected were chlorobenzenes and chloroalkanes, but it was argued that chlorination of these compounds occurred during pyrolysis of samples containing unchlorinated organics in the presence of perchlorate. A recent report analyzed a suite of aromatic (benzene, toluene, benzoic acid, phthalic acid, and mellitic acid) and aliphatic (acetic acid, propane, propanol, and hexane) by pyrolysis under SAM-like conditions in the presence of perchlorate to attempt to constrain possible precursor molecules for the organic molecules detected on Mars. For aromatic compounds, the aromatic acids all readily produced SAM-relevant chlorobenzes, whereas benzene and toluene did not. This observation suggests that the chlorobenzene detected on Mars could have derived from compounds like mellitic acid, consistent with the previous hypothesis by Benner et al. [3]. Among the aliphatic molecules, it was shown that pyrolysis of alkanes and alcohols in the presence of perchlorates produced polychlorine containing chloro-alkanes similar to what was observed on Mars. Surpris-ingly, however, similar treatment of acetic acid pro-duced chloroketones, instead, and no chloroalkanes were reported. This suggests that the chloroalkanes detected in the Sheepbed mudstone were not derived from aliphatic carboxylic acids, but instead were from more reduced alcohols or even alkanes, or perhaps were degradation products of more complicated organic material. Because organics analyses on mars will rely heavily on py-GC-MS of perchlorate-containing samples over the next decade, it is important to understand the fate of organic molecules of biotic and abiotic origin under such conditions. In this work we begin a series of experiments to improve our understanding of products generated during py-GC-MS of increasingly complex organic molecules (esters, amides, peptides, nucleic acids, fatty acids) in the presence of perchlorate.

Burton, A. S.↗

Recovery, Transportation and Acceptance to the Curation Facility of the Hayabusa Re-Entry Capsule

The "Hayabusa" re-entry capsule was safely carried into the clean room of Sagamihara Planetary Sample Curation Facility in JAXA on June 18, 2010. After executing computed tomographic (CT) scanning, removal of heat shield, and surface cleaning of sample container, the sample container was enclosed into the clean chamber. After opening the sample container and residual gas sampling in the clean chamber, optical observation, sample recovery, sample separation for initial analysis will be performed. This curation work is continuing for several manths with some selected member of Hayabusa Asteroidal Sample Preliminary Examination Team (HASPET). We report here on the 'Hayabusa' capsule recovery operation, and transportation and acceptance at the curation facility of the Hayabusa re-entry capsule.

Abe, M.↗