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At least 181 records · Page 10

Ion Microprobe Measurements of Comet Dust and Implications for Models of Oxygen Isotope Heterogeneity in the Solar System

The oxygen isotopic compositions of anhydrous minerals in carbonaceous chondrites reflect mixing between a O-16-rich and O-17, O18-rich reservoir. The UV photodissociation of CO (i.e. selfshielding) has been proposed as a mass-independent mechanism for producing these isotopically distinct reservoirs. Self-shielding models predict the composition for the CO gas reservoir to be O-16-rich, and that the accreting primordial dust was in isotopic equilibrium with the gaseous reservoir [1, 2]. Self-shielding also predicts that cometary water, presumed to represent the O-17, O-18-rich reservoir, should be enriched in O-17 and O-18, with compositions of 200 -1000per mille, and that the interaction with this O-17, O-18-rich H2O reservoir altered the compositions of the primordial dust toward planetary values. The bulk composition of the solar nebula, which may be an approximation to the 16O-rich gaseous reservoir, has been constrained by the Genesis results [3]. However, material representing the O-17, O-18-rich end-member is rare [4], and dust representing the original accreting primordial dust has been challenging to conclusively identify in current collections. Anhydrous dust from comets, which accreted in the distal cold regions of the nebula at temperatures below approximately 30K, may provide the best opportunity to measure the oxygen isotope composition of primordial dust. Chondritic porous interplanetary dust particles (CP-IDPs) have been suggested as having cometary origins [5]; however, until direct comparisons with dust from a known comet parent body were made, link between CP-IDPs and comets remained circumstantial. Oxygen isotope analyses of particles from comet 81P/Wild 2 collected by NASA's Stardust mission have revealed surprising similarities to minerals in carbonaceous chondrites which have been interpreted as evidence for large scale radial migration of dust components from the inner solar nebula to the accretion regions of Jupiter- family comets [6]. These studies have been largely focused on the coarse-grained terminal particles extracted from aerogel collectors; hypervelocity capture into aerogel resulted in fine-grained material that was melted and intimately mixed with the SiO2 capture medium. Hypervelocity impacts into Al foils surrounding the aerogel tiles produced impact craters that captured material from the impactor without significant oxygen contamination, allowing for analysis of both the coarse and fine-grained components of the Wild 2 dust. To date, no particles with definitive hydrated mineralogy have been observed in Stardust samples, though this may be a result of alteration due to hypervelocity capture. High-carbon hydrated CS-IDPs have been suggested as resulting from the aqueous alteration of CP-IDPs [7], and may retain evidence for interaction with O-17, O-18-enriched "cometary" water predicted by CO self-shielding. Here we present results of oxygen isotope measurements of twelve Stardust foil craters and four C-rich hydrated IDPs [8, 9], and discuss implications for models of oxygen isotope heterogeneity in the early solar system.

Snead, C. J.↗

Zirconium, hafnium, and rare earth element partition coefficients for ilmenite and other minerals in high-Ti lunar mare basalts - An experimental study

Partition coefficients were determined for Gd, Lu, Hf and Zr among ilmenite, armalcolite, and synthetic high-Ti mare basaltic melts at temperatures from 1122 deg to 1150 deg, and at oxygen fugacities of IW x 10 exp 0.5, by in situ analysis with an electron microprobe, using samples doped to present concentration levels. Coefficients for Zr were also measured for samples containing 600-1600 ppm Zr using this microprobe. In addition, coefficients were determined for Hf and Zr between chromian ulvospinel and melt, for Hf between pigeonite and melt, and for Lu between olivine and melt by microprobe analysis of samples doped to present levels. Values measured using the microprobe were in agreement with the values measured by analyzing mineral separates from the same run products by isotope dilution. Coefficient values for ilmenite are less than 0.01 for the LREE, are around 0.1 for the HREE, and are several times greater than this for Zr and Hf.

Mckay, G.↗

Calibration Issues and Operating System Requirements for Electron-Probe Microanalysis

Instrument purchase requirements and dialogue with manufacturers have established hardware parameters for alignment, stability, and reproducibility, which have helped improve the precision and accuracy of electron microprobe analysis (EPMA). The development of correction algorithms and the accurate solution to quantitative analysis problems requires the minimization of systematic errors and relies on internally consistent data sets. Improved hardware and computer systems have resulted in better automation of vacuum systems, stage and wavelength-dispersive spectrometer (WDS) mechanisms, and x-ray detector systems which have improved instrument stability and precision. Improved software now allows extended automated runs involving diverse setups and better integrates digital imaging and quantitative analysis. However, instrumental performance is not regularly maintained, as WDS are aligned and calibrated during installation but few laboratories appear to check and maintain this calibration. In particular, detector deadtime (DT) data is typically assumed rather than measured, due primarily to the difficulty and inconvenience of the measurement process. This is a source of fundamental systematic error in many microprobe laboratories and is unknown to the analyst, as the magnitude of DT correction is not listed in output by microprobe operating systems. The analyst must remain vigilant to deviations in instrumental alignment and calibration, and microprobe system software must conveniently verify the necessary parameters. Microanalysis of mission critical materials requires an ongoing demonstration of instrumental calibration. Possible approaches to improvements in instrument calibration, quality control, and accuracy will be discussed. Development of a set of core requirements based on discussions with users, researchers, and manufacturers can yield documents that improve and unify the methods by which instruments can be calibrated. These results can be used to continue improvements of EPMA.

Carpenter, P.↗

An analytical and experimental study of zoning in plagioclase

A detailed electron microprobe study has been conducted on natural and experimentally grown zoned plagioclase feldspars. Discontinuous, sector, and oscillatory chemical zoning are observed superimposed on continuous normal or reverse zoning trends. The relative accuracy of 3 element (Na, Ca, K) microprobe traverses was found statistically to be 2 mole percent. Comparison of microprobe data on natural zoned plagioclase with zoned plagioclase grown in controlled experiments has shown that it may be possible to distinguish zonal development resulting from physio-chemical changes to the bulk magma from zoning related to local kinetic control on the growth of individual crystals.

Smith, R. K.↗

Non-destructive trace element microanalysis of as-received cometary nucleus samples using synchrotron x ray fluorescence

The Synchrotron X ray Fluorescence (SXRF) microprobe at the National Synchrotron Light Source (NSLS), Brookhaven National Laboratory, will be an excellent instrument for non-destructive trace element analyses of cometary nucleus samples. Trace element analyses of as-received cometary nucleus material will also be possible with this technique. Bulk analysis of relatively volatile elements will be important in establishing comet formation conditions. However, as demonstrated for meteorites, microanalyses of individual phases in their petrographic context are crucial in defining the histories of particular components in unequilibrated specimens. Perhaps most informative in comparing cometary material with meteorites will be the halogens and trace metals. In-situ, high spatial resolution microanalyses will be essential in establishing host phases for these elements and identifying terrestrial (collection/processing) overprints. The present SXRF microprobe is a simple, yet powerful, instrument in which specimens are excited with filtered, continuum synchrotron radiation from a bending magnet on a 2.5 GeV electron storage ring. A refrigerated cell will be constructed to permit analyses at low temperatures. The cell will consist essentially of an air tight housing with a cold stage. Kapton windows will be used to allow the incident synchrotron beam to enter the cell and fluorescent x rays to exit it. The cell will be either under vacuum or continuous purge by ultrapure helium during analyses. Several other improvements of the NSLS microprobe will be made prior to the cometary nucleus sample return mission that will greatly enhance the sensitivity of the technique.

Sutton, S. R.↗

Phase transformations in 40-60-GPa shocked gneisses from the Haughton Crater (Canada): An Analytical Transmission Electron Microscopy (ATEM) study

In order to better understand phase transformations, chemical migration, and isotopic disequilibrium in highly shocked rocks, we have performed a microprobe and an ATEM study on gneisses shocked up to 60 GPa from the Haughton Crater. This study reveals the following chemical and structural characteristics: (1) SiO2 dominant areas are formed by a mixture of pure SiO2 polycrystalline quartz identified by electron diffraction pattern and chemical analysis and a silica-rich amorphous phase containing minor amounts of aluminium, potassium, and iron; (2) Areas with biotitelike composition are formed by less than 200-nm grains of iron-rich spinels embedded in a silica-rich amorphous phase that is very similar to the one described above; (3) Layers with feldsparlike composition are constituted by 100-200-nm-sized alumina-rich grains (the indexation of the crystalline structure is under progress) and the silica-rich amorphous phase; (4) Zones characterized by the unusual Al/Si ratio close to 1 are formed by spinel grains (200-nm-sized) embedded in the same silica-rich amorphous phase; and (5) The fracturated sillimanites contain domains with a lamellar structure, defined by the intercalation of 100-nm-wide lamellae of mullite crystals and of a silica-rich amorphous phase. These mullite crystals preserved the crystallographical orientation of the preshock sillimanite. All compositional domains, identified at the microprobe scale, can thus be explained by a mixture in different proportion between the following phases: (1) a silica-rich amorphous phase, with minor Al and K; (2) quartz crystals; (3) spinel crystals and alumina-rich crystals; (4) sillimanite; and (5) mullite. Such mixtures of amorphous phases and crystals in different proportions explain disturbed isotope systems in these rocks and chemical heterogeneities observed on the microprobe.

Martinez, I.↗

Characterization of Corning EPMA Standard Glasses 95IRV, 95IRW, and 95IRX

The preparation, synthesis, and characterization of Corning trace-element glasses 95IRV, 95IRW, and 95IRX by bulk chemical and electron microprobe techniques is discussed. Working values for the doped elements in the 95-series glasses are established. Blank values have been determined by both bulk chemical and electron microprobe analysis, and important x-ray interferences are highlighted. Chemical homogeneity both within a rod cross-section, and along cane length has been documented. These glasses are standard reference materials intended for use as both primary and secondary electron microprobe standards.

Carpenter, Paul K.↗

Flexible Microsensor Array for the Root Zone Monitoring of Porous Tube Plant Growth System

Control of oxygen and water in the root zone is vital to support plant growth in the microgravity environment. The ability to control these sometimes opposing parameters in the root zone is dependent upon the availability of sensors to detect these elements and provide feedback for control systems. In the present study we demonstrate the feasibility of using microsensor arrays on a flexible substrate for dissolved oxygen detection, and a 4-point impedance microprobe for surface wetness detection on the surface of a porous tube (PT) nutrient delivery system. The oxygen microsensor reported surface oxygen concentrations that correlated with the oxygen concentrations of the solution inside the PT when operated at positive pressures. At negative pressures the microsensor shows convergence to zero saturation (2.2 micro mol/L) values due to inadequate water film formation on porous tube surface. The 4-point microprobe is useful as a wetness detector as it provides a clear differentiation between dry and wet surfaces. The unique features of the dissolved oxygen microsensor array and 4-point microprobe include small and simple design, flexibility and multipoint sensing. The demonstrated technology is anticipated to provide low cost, and highly reliable sensor feedback monitoring plant growth nutrient delivery system in both terrestrial and microgravity environments.

Sathyan, Sandeep↗

Distinct Fracture Mineralogy That is Out of Equilibrium With Modern Groundwaters Provides Important Context for Subsurface Life

Rock fracture surfaces in the crust are essential habitat for microorganisms. Fracture‐groundwater interfaces provide physical substrates for biofilm growth and are sources of carbon, nutrients, and electron donors and acceptors. To better understand geochemical processes impacting fracture surfaces and the subsurface microbiome, we identified fractures in archived rock cores from the Soudan formation, which is known to host saline groundwaters and isolated microbial communities dependent on rock‐water interactions. Cores with open fractures were thin sectioned and studied via electron microprobe and synchrotron X‐ray fluorescence microprobe. Most fracture surfaces had mineralogy distinct from that of the bulk rock. Chlorite minerals were abundant on fracture surfaces and had elemental compositions suggesting deposition during late‐stage hydrothermal alteration. Fracture‐lining chlorites likely limit access to iron oxide and sulfide minerals that are active in subsurface biogeochemical cycles. Calcium‐rich rinds were also observed along fracture edges. These rinds were too thin and poorly ordered to be identified via light microscopy or X‐ray diffraction; however, Ca K‐edge micro‐X‐ray absorption near‐edge structure spectroscopy identified them as carbonates, minerals not observed in the bulk rock. Thermodynamic modeling shows that carbonate precipitation is largely unfavorable in Soudan groundwaters, indicating that fracture edge conditions differed from those in modern water samples. Because of the low carbon concentrations in Soudan groundwaters, carbonate rinds likely play an important role in subsurface carbon cycling and may mark fracture surfaces that once hosted biofilms. Overall, this study suggests that fracture alteration can both play an active role in and suppress rock‐water interactions essential to subsurface life.

36 MATERIALS SCIENCE↗

Occurrence of diopside and Cr-Zr-armalcolite on the moon.

Petrographic and electron-microprobe examination of the sample of 1 to 2 mm fines, Apollo 14166,6, has revealed a fragment with the unique lunar mineralogy of plagioclase, olivine, diopside, a Ti-Fe-Zr phase, and a trace of ilminite. The second occurrence of diopside is reported together with the third occurrence of a recently identified Ti-Fe-Zr phase. Microprobe analyses of the principal phases of the fragment studied are presented in a table. The relatively pure diopside analyses reported represent the most Mg-rich calcic pyroxene found in lunar material.

Steele, I. M.↗

Petrology of some lithic fragments from Luna 20.

Microscopic and electron microprobe studies were made of polished thin sections of part of a 30-mg sample of 250- to 500-micron lunar soil returned by Luna 20 from a point between Mare Fecunditatis and Mare Crisium. Very fine-grained lithic (crystalline) rock fragments, composing about one-fifth of the total sample, have mineralogical compositions equivalent to various types of gabbro, anorthositic gabbro, gabbroic anorthosite, and troctolite, with minor basalt. The textures now observed in these fragments are in large part metamorphic. Twenty-seven electron microprobe analyses of minerals from these fragments are presented, including olivine, plagioclase, pyroxene, spinel, nickel-iron, and a Zr-Ti-REE mineral possibly similar to 'phase B' of Lovering and Wark (1971). Analyses of seven melt inclusions and 28 defocused beam analyses of lithic fragments are also given. Some of the fragments contain 'gas' inclusions which, along with the fine grain size, are believed to indicate final crystallization under low pressure near surface conditions.

Roedder, E.↗

The Willowbar meteorite

Results of microscopic and electron microprobe analyses of a meteorite which fell near Willowbar, Okla., in December 1971. Microscopic examination confirmed the differences in structure which could be seen on the cut faces. Three distinct regions could be recognized: unblackened, blackened, and black veins. Microprobe analyses of the silicate grains in the Willowbar meteorite show that it is an L chondrite. The lack of well-defined chondrules and the large size of the maskelynite grains suggests that it is a type 6 chondrite according to the classification of Van Schmus and Wood (1967). It also has large black veins of the same composition as the matrix, and thus it might best be described as a shock-brecciated L6 chondrite.

Lange, D. E.↗

Phase chemistry of Apollo 14 soil sample 14259

Optical, X-ray-diffraction and electron-microprobe techniques were used to investigate 0.26 gm of Apollo 14 soil sample 14259. Major element microprobe analyses were made of 470 mineral grains and 388 glass grains. The mineral abundances in the soil are 45% plagioclase, 41% pyroxene, 7% olivine, 3% oxides, 2% K-feldspar; 1% nickel-iron, and less than 1% troilite. The glasses have a wide range of compositions but preferred values are evident and are interpreted as representative of rock types contributing to the soil at the Fra Mauro site. Eleven per cent of the glasses have compositions like those of mare basalts or mare soils and are believed to be mare-derived. Eighty-six per cent of the glasses are equivalent in composition to basalts that have higher Al, and lower Ca/Al and Fe/Mg ratios than mare basalts. The most abundant compositional type is named Fra Mauro basaltic glass and is subdivided into three related types. The other major glass type in the soil corresponds in composition to anorthositic gabbro.

Aitken, F. K.↗

Spinel-silicate co-crystallization relations in sample 15555

The results on the crystallization history of medium-grained mare basalt sample 15555,171, based on microprobe analyses (Dalton, 1973) of host and inclusion mineral pairs are summarized with emphasis placed on that part of the crystallization history during which chromite and ulvospinel were crystallizing. Compositional data on pyroxene olivine, chromite and ulvospinel in 15555,171 were collected using microprobe; data are based on corrected counts ratios for nine elements. It is concluded that systematic chemical relations between host and inclusion minerals suggest continuous in situ nucleation and growth of these minerals; that the data allow the possibility of some minerals, especially chromite, settling out of the melt during crystallization; and that the chromite to ulvospinel transition is correlated with a compositional change of the melt resulting from nucleation and growth of plagioclase.

Dalton, J.↗

The grape cluster, metal particle 63344,1

The grape cluster metal particle 63344,1 found in lunar coarse fines is examined using the scanning electron microscope (SEM), electron microprobe, and an optical microscope. This metal particle is approximately 0.5 cm in its largest dimension and consists of hundreds of metallic globules welded together to form a structure somewhat like a bunch of grapes. Electron microprobe analysis for Fe, Ni, Co, P, and S in the metal was carried out using wavelength dispersive detectors. No primary solidification structure is observed in the globules, and the particle is slow cooled from the solidification temperature (nearly 1300 C) taking days to probably months to reach 600 C. Two mechanisms for the formation of globules are proposed. One mechanism involves the primary impact of an iron meteorite which produces a metallic liquid and vapor phase. The second mechanism involves the formation of a liquid pool of metal after impact of an iron meteorite projectile followed by a secondary impact in the liquid metal pool.

Goldstein, J. I.↗

Three synthetic lunar glasses

Glasses have been synthesized that have the approximate compositions of lunar rocks 61156, 68415, and 77135, respectively. The glasses have been analyzed by conventional analytical and electron microprobe techniques and have been found to be highly homogeneous. They have been used successfully as electron microprobe standards and for experimental studies of crystallization and solar-wind implantation. Small amounts of these materials can be provided to investigators who would find them useful.

Minkin, J. A.↗