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At least 379 records · Page 21
All sourcesNASA NTRSDOE OSTI
DOE OSTI2021

Solid-state NMR of unlabeled plant cell walls: high-resolution structural analysis without isotopic enrichment

Abstract Background Multidimensional solid-state nuclear magnetic resonance (ssNMR) spectroscopy has emerged as an indispensable technique for resolving polymer structure and intermolecular packing in primary and secondary plant cell walls. Isotope ( 13 C) enrichment provides feasible sensitivity for measuring 2D/3D correlation spectra, but this time-consuming procedure and its associated expenses have restricted the application of ssNMR in lignocellulose analysis. Results Here, we present a method that relies on the sensitivity-enhancing technique Dynamic Nuclear Polarization (DNP) to eliminate the need for 13 C-labeling. With a 26-fold sensitivity enhancement, a series of 2D 13 C– 13 C correlation spectra were successfully collected using the unlabeled stems of wild-type Oryza sativa (rice). The atomic resolution allows us to observe a large number of intramolecular cross peaks for fully revealing the polymorphic structure of cellulose and xylan. NMR relaxation and dipolar order parameters further suggest a sophisticated change of molecular motions in a ctl1 ctl2 double mutant: both cellulose and xylan have become more dynamic on the nanosecond and microsecond timescale, but the motional amplitudes are uniformly small for both polysaccharides. Conclusions By skipping isotopic labeling, the DNP strategy demonstrated here is universally extendable to all lignocellulose materials. This time-efficient method has landed the technical foundation for understanding polysaccharide structure and cell wall assembly in a large variety of plant tissues and species.

09 BIOMASS FUELS↗
DOE OSTI2023

R-matrix Resolved Resonance Region Evaluation of 140,142 Ce

Oak Ridge National Laboratory completed the resolved resonance region (RRR) evaluation of the two most abundant cerium isotopes, 140 Ce (88.45%) and 142 Ce (11.11%), as requested by the US Nuclear Criticality Safety Program. These evaluations are based on recent high-resolution transmission and capture measurements performed on nat Ce and highly enriched 142 Ce samples at the JRC-Geel Linear Accelerator facility, as well as measured thermal constants available from the EXFOR database. Starting from the resonance parameters of the ENDF/B-VIII.0 library followed by a preliminary R-matrix analysis, an updated set of resonance parameters and corresponding covariance information were derived by fitting these measured data using the Reich–Moore approximation of the R -matrix theory, as implemented in the SAMMY code system. The 140 Ce RRR upper energy limit was kept at 200 keV, whereas the 142 Ce resonance region was extended from 13 to 26 keV. Updated statistical properties were obtained for the new evaluations and compared to those derived from the ENDF/B-VIII.0 nuclear data library. The new evaluation work improved some of the discrepancies found in previous work, such as the capture resonance integral and stellar Maxwellian-averaged cross sections. These integral quantities were mainly derived from the fit of the latest measured data, especially the neutron capture yield data for 142 Ce isotope.

73 NUCLEAR PHYSICS AND RADIATION PHYSICS↗
DOE OSTI2021

Chromium Isotopic Evidence for Mixing of NC and CC Reservoirs in Polymict Ureilites: Implications for Dynamical Models of the Early Solar System

Nucleosynthetic isotope anomalies show that the first few million years of solar system history were characterized by two distinct cosmochemical reservoirs, CC (carbonaceous chondrites and related differentiated meteorites) and NC (the terrestrial planets and all other groups of chondrites and differentiated meteorites), widely interpreted to correspond to the outer and inner solar system, respectively. At some point, however, bulk CC and NC materials became mixed, and several dynamical models offer explanations for how and when this occurred. We use xenoliths of CC materials in polymict ureilite (NC) breccias to test the applicability of such models. Polymict ureilites represent regolith on ureilitic asteroids but contain carbonaceous chondrite-like xenoliths. We present the first 54 Cr isotope data for such clasts, which, combined with oxygen and hydrogen isotopes, show that they are unique CC materials that became mixed with NC materials in these breccias. It has been suggested that such xenoliths were implanted into ureilites by outer solar system bodies migrating into the inner solar system during the gaseous disk phase ~3–5 Myr after CAI, as in the "Grand Tack" model. However, combined textural, petrologic, and spectroscopic observations suggest that they were added to ureilitic regolith at ~50–60 Myr after CAI, along with ordinary, enstatite, and Rumuruti-type chondrites, as a result of the breakup of multiple parent bodies in the asteroid belt at this time. This is consistent with models for an early instability of the giant planets. The C-type asteroids from which the xenoliths were derived were already present in inner solar system orbits.

79 ASTRONOMY AND ASTROPHYSICS↗
NASA NTRS1972

Noble gases in the moon

The abundance and isotopic composition of helium, neon, argon, krypton, and xenon which were released by stepwise heating of lunar fines (15601.64) and (15271.65) were measured spectrometrically. The results of a composition of noble gases released from the lunar fines with noble gases in meteorites and in the earth are presented along with the isotopic composition of noble gases in lunar fines, in meteorites, and in the atmosphere. A study of two isotopically distinct components of trapped xenon in carbonaceous chondrites is also included.

Manuel, O. K.↗
NASA NTRS1972

Comparative petrology of Apollo 16 sample 68415 and Apollo 14 samples 14276 and 14310.

Petrographic and electron microprobe studies of Apollo 16 igneous rock 68415 and Apollo 14 rocks 14276 and 14310 show that all three samples differ from the mare basalts and are characterized by plagioclase as the first liquidus phase and by the abundance of plagioclase which is in part cumulate in origin. Major and minor element abundances and isotopic data prohibit the derivation of rocks like any of these samples from one another by magmatic fractionation during their crystallization. They could have originated by partial melting of an old, more Al-rich source material without isotopic equilibration with the residuum, by complete melting of three independent sources, or by contamination with old radiogenic material. The existence of such feldspathic basalts indicates that the generation of Al-rich magmas may have been an important and widespread lunar process.

Gancarz, A. J.↗
NASA NTRS1972

The organic analysis and carbon chemistry of lunar samples: Their significance for exobiology; Proceedings of the Conference, University of Maryland, College Park, Md., October 26-28, 1971.

Various methods used in the organic analysis of lunar samples are reviewed. The scope, advantages, and limitations of these methods are discussed, with particular emphasis on possible sources of contamination and experimental artifacts inherent in their use. A broad survey of the organogenic elements and compounds found in lunar samples covers the search for biogenic structures and viable organisms; the abundance and isotopic composition of various elements and compounds; the search for porphyrins, amino acids, or amino acid precursors; and the presence of heterocylics, aromatic hydrocarbons, and other organic compounds. The sources of the organogenic elements and compounds detected in lunar samples are discussed. The significance of the lunar organic analysis for exobiology is discussed in terms of its relevance to and implications for the studies of chemical evolution and terrestrial organic geochemistry. Individual items are announced in this issue.

Source record↗
NASA NTRS1972

Noble gas studies on regolith materials from Apollo 14 and 15.

Abundances and isotopic compositions of the five stable noble gases, He, Ne, Ar, Kr, and Xe in soils and breccia were determined. The samples investigated included material from a range of depths in a trench and a core tube. Noble gas determinations were performed in a 6-inch all-metal mass spectrometer of high sensitivity. The grain size separates and stepwise heating experimental methods used give results that supplement each other. Calculated concentrations of spallation Xe-126 in many of the fines and gas-rich breccia are presented in a table. Bulk soil samples obtained by Apollo 14 show an inverse correlation of spallation Xe-126 with grain size.

Bogard, D. D.↗
NASA NTRS1973

Noble gas concentrations and cosmic ray exposure ages of eight recently fallen chondrites

Abundances and isotopic compositions of He, Ne, Ar, and Xe have been measured in eight recently fallen chondrites. Ratios of concentrations of cosmic ray-produced He-3, Ne-21, Ne-22, and Ar-38 indicate that all eight samples experienced less than average cosmic ray shielding. He-3 and Ne-21 exposure ages were calculated using shielding corrected chondritic production rates and the measured Ne-22/Ne-21. Exposure ages calculated from Na-22/Ne-22 and Al-26/Ne-21 ratios and constant relative production rates show a bias between the two ages due to variations in Na-22/Al-26. Arguments are presented that this bias is due to irradiation hardness differences, and therefore the use of constant values for both the Na-22/Ne-22 and Al-26/Ne-21 production ratios is not permitted.

Bogard, D. D.↗
NASA NTRS1973

Trapped solar and cosmogenic noble gas abundances in Apollo 15 and 16 deep drill samples

Abundances and isotopic compositions of all the stable noble gases (He, Ne, Ar, Kr, Xe) were measured at different depths of the Apollo 15 and Apollo 16 deep drill cores, and in several surface fines and breccias. All samples analyzed from both drill cores were found to contain large concentrations of solar wind implanted gases. This means that even the deepest layers of both cores have experienced a lunar surface history. The Apollo 15 core data are consistent with a combined accretion plus static time of a few hundred million years, and also indicate variable pre-accretion irradiation of core material. Depth profiles of cosmogenic gases in the Apollo 16 core show considerably larger concentrations of cosmic gases below 65 cm depth than above. This pattern may be interpreted either as an accretionary process, or by a more recent deposition of regolith to the upper 70 cm of the core.

Bogard, D. D.↗
NASA NTRS1980

A post-Viking view of Martian geologic evolution

The geologic evolution of Mars is reviewed on the basis of data obtained by the Viking and previous missions. Current knowledge of the mean density and moment of inertia factor of Mars are surveyed and the constraints these data place on the structure and composition of the interior are discussed. Inferences drawn about Martian surface composition and mineralogy from lava modeling studies, in situ analyses, remote sensing observations, flow morphometry and investigations of weathering under Martian conditions are presented, and data on the topography, gravity field and structural features are considered in relation to the structure and deformational history of the crust. The temporal and spatial distribution of volcanic units are considered as a constraint on the thermal evolution of the planet, and other constraints on Martian thermal history, such as magnetic field data, are reviewed. Finally, the volatile inventory of Mars is discussed based on elemental and isotopic atmospheric abundance data and geological constraints on H2O and CO2 abundances.

Arvidson, R. E.↗
NASA NTRS1984

Rare gases in cyclosilicates and cogenetic minerals

The cyclosilicate minerals, beryl, tourmaline, and cordierite, typically contain large amounts of He-4 and Ar-40 which are not in situ radiogenic products. In the study of excess rare gases in cyclosilicates, one of the most enigmatic observations is the age effect, a qualitative tendency for geologically older samples to contain more excess He-4 and Ar-40 than younger samples. The present investigation is concerned with measurements regarding the abundance and isotopic composition of all five rare gases in a number of cyclosilicates as well as in their cogenetic minerals. The significance of the obtained data is discussed. The data indicate that cyclosilicates sample the rare gases present in the environment in which they crystallize. This 'sampling' involves major elemental fractionations which are variable but mineral specific. Cyclosilicates can, therefore, be used to probe the isotopic ratios and elemental compositions.

Saito, K.↗
NASA NTRS1986

Nitrogen and light noble gases in Shergotty

Two samples of Shergotty and a sample of EETA 79001's lithology A have been analyzed for N, He, Ne, and Ar abundances and isotopic composition. After correcting for spallogenic nitrogen, the nitrogen isotopic ratios were found to be close to that of the terrestrial atmosphere. The spallogenic noble gas data are consistent with cosmic ray irradiation of both Shergotty and EETA 79001 at shallow shielding depths. Cosmic ray exposure ages were estimated to be in the range of 0.5-0.8 Myr for EETA 79001, and of 2.0-5.2 Myr for Shergotty, depending on the choice of object size and shielding. Among the two Shergotty samples, the contents of Ar-40 differed by a factor of 3. This difference can be attributed to either a small-scale mineralogical inhomogeneity or a significant variation in the degree of degassing of minerals during shock, although the presence of trapped argon with a high Ar-40/Ar-36 ratio and its heterogeneous distribution cannot be ruled out.

Becker, R. H.↗
NASA NTRS1993

SNC meteorites and their implications for reservoirs of Martian volatiles

The SNC meteorites and the measurements of the Viking landers provide our only direct information about the abundance and isotopic composition of Martian volatiles. Indirect measurements include spectroscopic determinations of the D/H ratio of the Martian atmosphere. A personal view of volatile element reservoirs on Mars is presented, largely as inferred from the meteoritic evidence. This view is that the Martian mantle has had several opportunities for dehydration and is most likely dry, although not completely degassed. Consequently, the water contained in SNC meteorites was most likely incorporated during ascent through the crust. Thus, it is possible that water can be decoupled from other volatile/incompatible elements, making the SNC meteorites suspect as indicators of water inventories on Mars.

Jones, J. H.↗
NASA NTRS2003

AGE (Argon Geochronology Experiment): An Instrument for Geochronology on the Surface of Mars

As our knowledge of the planet Mars continues to grow, one parameter that remains elusive is the absolute chronology of the planet s geological history. Although crater counts have provided a robust relative chronology, impactor fluxes are poorly enough known that there are places on Mars where the absolute age is uncertain by a factor of two or more. To resolve these uncertainties, it will be necessary to either analyze well-documented samples returned to the Earth from the Martian surface or to perform in situ measurements with sufficient precision. Sample return is still at least a decade away, and even then it might be from a biologically interesting area that might be geologically complex. Hence an in situ measurement, within an uncertainty of 20% or better, could greatly improve our knowledge of the history of Mars. With funding from the Planetary Instrument Definition and Development Program (PIDDP), we have been working on an instrument to perform potassium-argon (K-Ar) and cosmic-ray exposure (CRE) dating in situ on the surface of Mars. For either of these techniques, it is necessary to measure the abundance of one or more major or minor elements (K in the case of KAr; all majors and minors in the case of CRE) and the abundance and isotopes composition of a noble gas (Ar in the case of K-Ar; He, Ne and Ar for CRE dating). The technology for either of these types of measurements exists, but has never before been integrated for a spacecraft. We refer to the instrument as AGE, the Argon Geochronology Experiment (although we will measure the noble gases He and Ne as well for CRE ages). We report here on the basic components that go into such an instrument, both those that use existing technology and those that had to be developed to create the integrated package.

Swindle, T. D.↗
NASA NTRS2006

Determination of Silicon in Hydrazine

Inductively coupled plasma-mass spectrometry (ICP-MS) is a highly sensitive technique sometimes used for the trace determination of silicon at a mass-to-charge (m/z) ratio of 28, the most abundant natural isotope of silicon. Unfortunately, ICP-MS is unable to differentiate between other sources of m/z 28 and false positive results for silicon will result when other sources of m/z 28 are present. Nitrogen was a major source of m/z 28 and contributes to the m/z 28 signal when hydrazine sample or nitric acid preservative is introduced into the plasma. Accordingly, this work was performed to develop a sample preparation step coupled with an ICP-MS analysis that minimized non-silicon sources of m/z 28. In the preparatory step of this method, the hydrazine sample was first decomposed predominately to nitrogen gas and water with copper-catalyzed hydrogen peroxide. In the analysis step, ICP-MS was used without nitric acid preservative in samples or standards. Glass, a potential source of silicon contamination, was also avoided where possible. The method was sensitive, accurate, and reliable for the determination of silicon in monopropellant grade hydrazine (MPH) in AF-E-332 elastomer leaching tests. Results for silicon in MPH were comparable to those reported in the literature for other studies.

McClure, Mark B.↗
NASA NTRS2009

Evolved Gas Measurements Planned for the Lower Layers of the Gale Crater Mound with the Sample Analysis at Mars Instrument Suite

The lower mound strata of Gale Crater provide a diverse set of chemical environments for exploration by the varied tools of the Curiosity Rover of the Mars Science Laboratory (MSL) Mission. Orbital imaging and spectroscopy clearly reveal distinct layers of hydrated minerals, sulfates, and clays with abundant evidence of a variety of fluvial processes. The three instruments of the MSL Sample Analysis at aMars (SAM) investigation, the Quadrupole Mass Spectrometer (QMS), the Tunable Laser Spectrometer (TLS), and the Gas Chromatograph (GC) are designed to analyze either atmospheric gases or volatiles thermally evolved or chemically extracted from powdered rock or soil. The presence or absence of organic compounds in these layers is of great interest since such an in situ search for this type of record has not been successfully implemented since the mid-60s Viking GCMS experiments. However, regardless of the outcome of the analysis for organics, the abundance and isotopic composition of thermally evolved inorganic compounds should also provide a rich data set to complement the mineralogical and elemental information provided by other MSL instruments. In addition, these evolved gas analysis (EGA) experiments will help test sedimentary models proposed by Malin and Edgett (2000) and then further developed by Milliken et al (2010) for Gale Crater. In the SAM EGA experiments the evolution temperatures of H2O, CO2, SO2, O2, or other simple compounds as the samples are heated in a helium stream to 1000 C provides information on mineral types and their associations. The isotopic composition of O, H, C, and S can be precisely determined in several evolved compounds and compared with the present day atmosphere. Such SAM results might be able to test mineralogical evidence of changing sedimentary and alteration processes over an extended period of time. For example, Bibring et al (2006) have suggested such a major shift from early nonacidic to later acidic alteration. We will illustrate through a variety of evolved gas experiments implemented under SAM-like gas flow and temperature ramp conditions on terrestrial analog minerals on high fidelity Sam breadboards the type of chemical information we expect SAM to provide.

Mahaffy, Paul↗
NASA NTRS2017

Chlorine in Lunar Basalts

In the context of the lunar magma ocean (LMO) model, it is anticipated that chlorine (and other volatiles) should have been concentrated in the late-stage LMO residual melts (i.e., the dregs enriched in incompatible elements such as K, REEs, and P, collectively called KREEP, and in its primitive form - urKREEP, [1]), given its incompatibility in mafic minerals like olivine and pyroxene, which were the dominant phases that crystallized early in the cumulate pile of the LMO (e.g., [2]). When compared to chondritic meteorites and terrestrial rocks (e.g., [3-4]), lunar samples often display heavy chlorine isotope compositions [5-9]. Boyce et al. [8] found a correlation between delta Cl-37 (sub Ap) and bulk-rock incompatible trace elements (ITEs) in lunar basalts, and used this to propose that early degassing of Cl (likely as metal chlorides) from the LMO led to progressive enrichment in remaining LMO melt in Cl-37over Cl-35- the early degassing model. Barnes et al. [9] suggested that relatively late degassing of chlorine from urKREEP (to yield delta Cl-37 (sub urKREEP greater than +25 per mille) followed by variable mixing between KREEPy melts and mantle cumulates (characterized by delta Cl-37~0 per mille) could explain the majority of Cl isotope data from igneous lunar samples. In order to better understand the processes involved in giving rise to the heavy chlorine isotope compositions of lunar samples, we have performed an in situ study of chlorine isotopes and abundances of volatiles in lunar apatite from a diverse suite of lunar basalts spanning a range of geochemical types.

Barnes, J. J.↗