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NASA NTRS1972

Petrographic and electron microprobe study of the Monturaqui impactite.

Study of Monturaqui-crater impactite specimens attempting to determine the type of shock features present, shock intensities, type of meteorite projectile, and environmental conditions of impactite formation, by means of petrographic and electron microprobe techniques. The specimens were found to contain shocked and unshocked mineral and rock fragments together with Ni-Fe-Co-P spherules tightly bound in a partly devitrified matrix of clear, green or brown glass. Shock effects range from lightly shocked to intensely shocked. Observed and simulated shock effects are discussed.

Bunch, T. E.↗

NASA NTRS1972

Ion microprobe mass analyzer.

A useful future in many areas of solid material research is shown to exist for the ion microprobe mass analyzer, in the light of the quantitative analyses and other application examples described for illustration. The potentialities and limitations of the instrument are defined.

Andersen, C. A.↗

NASA NTRS1973

Pb-207/Pb-206 ages of individual mineral phases in Luna 20 material by ion microprobe mass analysis.

Ion microprobe analyses of returned lunar material have helped to demonstrate that U, Th, and radiogenic Pb are concentrated in small accessory mineral phases. It is possible to measure the isotopic composition of this Pb and obtain a radiometric Pb-207/Pb-206 age for the mineral. The ages so derived compare favorably with crystallization ages determined by conventional methods. A grain mount (22003,2/6) of Luna 20 material was searched for such accessory mineral phases, and two were found. One of these phases give an age of 4.12 plus or minus 0.04 b.y. and the other an age of 4.42 plus or minus 0.11 b.y. Ages of minerals dated by the ion probe in Apollo samples 14310 and 15555 are given for comparison. Data on the upper limit for Pb concentration in the outermost surface layers of free lunar soil particles are also given.

Andersen, C. A.↗

NASA NTRS1973

Preparation of ultra small samples for optical and microprobe analysis

This paper describes a simple but satisfactory new method for the preparation of tiny, varied and specialized specimens for electron or ion-microprobe analysis developed over the past five years. Microtektites, individual chondrules, single grains, blebs from lunar samples and meteoritic minerals have been prepared by this technique. A description of the preparation of these usually difficult samples from the initial mounting through the various polishing steps to their final polish is presented in detail. The procedures used to prevent any contamination of these specimens by the polishing agents and to prevent cross contamination to the other samples used for geochronology studies are presented.

Inman, C. S.↗

NASA NTRS1973

Rapid correction of electron microprobe data for multicomponent metallic systems

This paper describes an empirical relation for the correction of electron microprobe data for multicomponent metallic systems. It evaluates the empirical correction parameter, a for each element in a binary alloy system using a modification of Colby's MAGIC III computer program and outlines a simple and quick way of correcting the probe data. This technique has been tested on a number of multicomponent metallic systems and the agreement with the results using theoretical expressions is found to be excellent. Limitations and suitability of this relation are discussed and a model calculation is also presented in the Appendix.

Gupta, K. P.↗

NASA NTRS1974

The electron microprobe as a metallographic tool

The electron microprobe (EMP) is shown to represent one of the most powerful techniques for the examination of the microstructure of materials. It is an electron optical instrument in which compositional and topographic information is obtained from regions smaller than 1 micron in diameter on a specimen. Photographs of compositional and topographic changes in 1-sq-mm to 20-sq-micron areas on various types of specimens can also be obtained. These photographs are strikingly similar to optical photomicrographs. Various signals measured in the EMP (X-rays, secondary electrons, backscattered electrons, etc.) are discussed, along with their resolution and the type of information they may help obtain. In addition to elemental analysis, solid state detecting and scanning techniques are reviewed. Various techniques extending the EMP instrument capabilities, such as deconvolution and soft X-ray analysis, are also described.

Goldstein, J. I.↗

NASA NTRS1976

Microprobe and oxygen fugacity study of armalcolite

The stability of synthetic armalcolite was determined as a function of oxygen fugacity with particular regard to the oxidation state of iron and titanium. The equilibrium pseudobrookite (armalcolite) composition was measured at 1200 C under various conditions of oxidation typical of the lunar environment. These data, when compared with published descriptions of mare basalts, provide information about the conditions of crystallization of armalcolite-bearing lunar rocks. Some information about the crystal chemistry of armalcolite was obtained from X-ray diffraction and electron microprobe analyses of synthetic armalcolite and Zr-armalcolite. Further data were gathered from a comparison of the Mossbauer spectra of a phase pure stoichiometric armalcolite and one containing appreciable amounts of trivalent titanium.

Friel, J. J.↗

NASA NTRS1979

Magnesium isotopic variations in hibonite from the Murchison meteorite - An ion microprobe study

Ion microprobe measurements show that some hibonite crystals from refractory-rich inclusions in Murchison contain isotopically anomalous Mg. The observed effects include: (1) the largest mass fractionation ever observed in nature for this element, about 10% per mass unit; (2) small Mg-26 excesses; (3) isotopic variability on a scale of microns or less in individual grains. These observations are corroborative evidence for the primitiveness of the Murchison inclusions. More importantly, they indicate that the types of Mg isotopic anomalies previously observed in Allende and Leoville inclusions are not confined to CV meteorites.

Macdougall, J. D.↗

NASA NTRS1978

Ion microprobe analyses of aluminous lunar glasses - A test of the 'rock type' hypothesis

Previous soil survey investigations found that there are natural groupings of glass compositions in lunar soils and that the average major element composition of some of these groupings is the same at widely separated lunar landing sites. This led soil survey enthusiasts to promote the hypothesis that the average composition of glass groupings represents the composition of primary lunar 'rock types'. In this investigation the trace element composition of numerous aluminous glass particles was determined by the ion microprobe method as a test of the above mentioned 'rock type' hypothesis. It was found that within any grouping of aluminous lunar glasses by major element content, there is considerable scatter in the refractory trace element content. In addition, aluminous glasses grouped by major elements were found to have different average trace element contents at different sites (Apollo 15, 16 and Luna 20). This evidence argues that natural groupings in glass compositions are determined by regolith processes and may not represent the composition of primary lunar 'rock types'.

Meyer, C., Jr.↗

NASA NTRS1979

Scanning Auger Microprobe and atomic absorption studies of lunar volcanic volatiles

Results on lunar volatile transport processes have been obtained by studying green and brown glass droplets, orange and black core tube samples and the surface sample 74241 with the Scanning Auger Microprobe (SAM) and by Flameless Atomic Absorption Analysis (FLAA). SAM analyses show that the most dominant volatiles in the top few atomic layers of droplets are Zn and S, confirming that the surface Zn and S are good indicators of pyroclastic origin, and they are not entirely present as ZnS. In addition, FLAA thermal release profiles show that almost all the Zn and Cd are on grain surfaces, indicating that Zn and Cd were completely outgassed from lava fountain products during the volcanic eruption, were recondensed during or after the eruptions, and are thus present as surface coating.

Cirlin, E. H.↗

NASA NTRS1980

Ion microprobe analysis and petrogenetic interpretations of Li, Mg, Ti, K, Sr, Ba in lunar plagioclase

The ion microprobe employed in the considered investigation utilizes a focused primary ion beam to sputter a tiny volume of a sample. A small fraction of the sputtered atoms is ionized and extracted from the sample region for subsequent analysis with a mass spectrometer. A systematic study was conducted to determine which elements can be detected and analyzed in lunar Ca-rich plagioclase. Attention is given to the method of quantitative determination, the selected samples, and aspects of data presentation. A number of general conclusions are discussed. All minor elements in plagioclases from anorthosites from several lunar sites show a restricted range consistent with a common origin. The simplest interpretation is that the anorthosites developed from a moon-wide event, or at least from closely-related events. A moon-wide magma ocean would satisfy this condition.

Steele, I. M.↗

NASA NTRS1980

Controlled cooling and crystallization of a eucrite - Microprobe studies

The paper presents microprobe data on controlled cooling experiments on the eucrite meteorite Stannern, with emphasis on pyroxene zoning and chemistry, development of immiscible liquids in the mesostasis, and compositional boundary layer development adjacent to crystals. Controlled cooling rate experiments on melted samples of the meteorite yield a variety of petrographic textures that can be related to the cooling rate. Textures of clasts in Stannern suggest natural cooling rates of .1 to 100 C/hr for various clasts in the meteorite. Residual liquids are found to unmix at temperatures below about 990 C at moderate cooling rates. Results indicate that Stannern's pyroxenes have evidently undergone subsolidus internal cation exchange, thereby removing Fe-Mg variation in pyroxenes, lowering Al contents, and promoting exosolution.

Powell, M. A.↗

NASA NTRS1982

New oxidation features in NiCrAl-Zr revealed by an Auger microprobe

A NiCrAl-0.5 (wt %) Zr alloy, oxidized in air for 1 h at 1180 C was studied using a 30-nm resolution Auger microprobe. Depth analysis was achieved using crater edge profiling. This first application of AES to these alloys enabled several new observations of the chemical composition of microstructural features in the corrosion layer. The external oxide was rough, about 2-3 microns thick, and contained Ni, Cr, Al, and O. It was discovered that stoichiometric Al2O3 was restricted to a homogeneous layer about 300-nm thick between the oxide and the base metal. The metal immediately beneath this Al2O3 layer was found to be depleted in Al and roughly ten times richer in Zr than the bulk alloy. These observations are compared with the predictions of current models of the oxidation of MCrAl alloys.

Larson, L. A.↗

NASA NTRS1982

Electron microprobe analysis of trace elements in minerals at 10 PPM concentrations

An improved technique is developed for measuring backgrounds during trace element analysis of crystals and glass using electron microprobes. This technique overcomes major difficulties encountered with conventional techniques, such as the problem of obtaining the net X-ray intensity of the characteristic emission line of interest with sufficient precision and accuracy, as well as the error due to the inability to directly measure the intensity at the wavelength of the characteristic line on the sample being analyzed. It is shown that this technique can yield reproducible results to within 4 ppm in olivine, and has a minimum uncertainty and detection limit of 10 ppm Nd in olivine.

Mckay, G. A.↗

NASA NTRS1983

FUN with PANURGE - High mass resolution ion microprobe measurements of Mg in Allende inclusions

Isotopic ratios have been determined, at a precision level approaching that of counting statistics using beam switching, by employing PANURGE, a modified CAMECA IMS3F ion microprobe at a mass resolving power of 5000. This technique is used to determine the isotopic composition of Mg and Si and the atomic ratio of Al/Mg in minerals from the Allende inclusion WA and the Allende FUN inclusion C1. Results show enrichment in Mg-26 of up to 260 percent. Results of Mg and Al/Mg measurements on cogenetic spinel inclusion and host plagiclase crystals show Mg-Al isochrons in excellent agreement with precise mineral isochrons determined by thermal emission mass spectrometry. The measurements are found to confirm the presence of substantial excess Mg-26 in WA and its near absence in C1. Data is obtained which indicates a metamorphic reequilibrium of Mg in Allende plagioclase at least 0.6 my after WA formation. Ion probe measurements are obtained which confirm that the Mg composition in Allende C1 is highly fractionated and is uniform among pyroxene, melilite, plagioclase, spinel crystals, and spinel included in melilite and plagioclase crystals.

Huneke, J. C.↗

NASA NTRS1983

Ion microprobe zircon geochronology of the Uivak Gneisses: Implications for the evolution of early terrestrial crust in the North Atlantic Craton

Ion microprobe U-Pb results for zircons from three Uivak I gneisses and one specimen of Uivak II gneiss, from the Saglek-Hebron area of Northern Labrador are reported. These results are compared with interpretations based on published conventional U-Pb zircon results and with conclusions about crustal evolution in the NAC derived from Rb-Sr, Sm-Nd and Pb-Pb isotopic studies.

Collerson, K. D.↗

NASA NTRS1984

Ion microprobe magnesium isotope analysis of plagioclase and hibonite from ordinary chondrites

Ion and electron microprobes were used to examine Mg-26 excesses from Al-26 decay in four Al-rich objects from the type 3 ordinary hibonite clast in the Dhajala chondrite. The initial Al-26/Al-27 ratio was actually significantly lower than Al-rich inclusions in carbonaceous chondrites. Also, no Mg-26 excesses were found in three plagioclase-bearing chondrules that were also examined. The Mg-26 excesses in the hibonite chondrites indicated a common origin for chondrites with the excesses. The implied Al-26 content in a proposed parent body could not, however, be confirmed as a widespread heat source in the early solar system.

Hinton, R. W.↗

NASA NTRS1984

Experimental determination of the partitioning of gallium between solid iron metal and synthetic basaltic melt Electron and ion microprobe study

The distribution of Ga between solid Fe metal and synthetic basaltic melt is investigated experimentally at temperatures of 1190 and 1330 C, and over a narrow range of oxygen fugacities. Metal-silicate reversal experiments were conducted, indicating a close approach to equilibrium. The analysis of the partitioned products was performed using electron and ion microprobes. At one bar total pressure, the solid metal/silicate melt partition coefficient D(Ga) is used to evaluate metal-silicate fractionation processes in the earth, moon, and Eucrite Parent Body (EPB). It is found that the depletion of Ga abundances in the EPB is due to the extraction of Ga into a metallic core. Likewise, the depletion of Ga in the lunar mantle is consistent with the extraction of Ga into a smaller lunar core if Ga was originally present in a subchondritic concentration. The relatively high Ga abundances in the earth's mantle are discussed, with reference to several theoretical models.

Drake, M. J.↗