I have developed a technique that improves the speed, reproducibility, and sensitivity of the measurement of degree of equilibration in ordinary chondrites. The Fast Electron Microprobe technique (FEM) technique provides a continuous quantitative scale for the amount of thermal processing a particular sample has experienced. The Fast Electron Microprobe technique (FEM) allows us to quickly collect sufficient data to determine the homogeneity and composition of olivine and low-Ca pyroxene in ordinary chondrite thin sections. I have studied several meteorites that are homogenous in olivine composition, but heterogeneous in low-Ca pyroxene composition. One of these samples (ALH 85033) has previously been classified as an L4. The FEM technique allows reproducible measurements of the degree of thermal metamorphism in ordinary chondrites, improving our understanding of thermal processing of asteroids in the early solar system.

名古屋大学年代測定総合研究センターシンポジウム報告

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Thesis advisor: Yvette D. Kuiper / The Paleoproterozoic Foxe Fold Belt (FFB) is composed of the Penrhyn Group, a Paleoproterozoic passive margin sequence, and supracrustal Archean basement. These units were interfolded and metamorphosed at amphibolite to lower granulite facies conditions during the 1883-1865 Ma Foxe orogeny, a part of the Trans-Hudson orogeny. The purpose of this study was to constrain the timing of metamorphism and deformation within the Penrhyn Group, in order to determine the role of the Foxe orogeny within the Trans-Hudson orogeny. Petrographic analysis, P-T-X pseudosections, monazite composition, and in-situ electron microprobe U-Th-Pb geochronology from sampled metapelites were used to determine the age and significance of metamorphic and deformation events related to monazite age populations. Population 1 is composed of 1926 ± 8 Ma monazite interpreted as detrital. Population 2 consists of 1892 ± 9 Ma monazite, the youngest detrital ages seen in the Penrhyn Group. Population 3 is composed of 1853 ± 5 Ma high-Y + HREE monazite predating an episode of pervasive garnet growth. Population 4 contains 1839 ± 8 Ma lower-Y + HREE monazite related to pervasive garnet growth. Population 5 is 1819 ± 16 Ma lowest-Y + HREE monazite with high LREE and Th/U, linked to the interpreted peak reaction: Bt + Sil + Pl = Grt + Crd + Kfs + melt. Monazite constraints on deformation fabrics indicate that deformation was ongoing locally as early as 1853 ± 9 Ma and continued until at least 1814 ± 14 Ma, pre- to syn-peak metamorphism. Rare 1794-1776 Ma monazite is interpreted to constrain the age of retrograde metamorphism as the Trans-Hudson orogeny waned. These data support interpreted clockwise P-T-t-D paths consistent with metamorphism initiated by crustal thickening in an orogenic belt. / Thesis (MS) — Boston College, 2013. / Submitted to: Boston College. Graduate School of Arts and Sciences. / Discipline: Earth and Environmental Sciences.

In order to evaluate the electron microprobe (EMP) method for chemical dating of monazite, we chemically analyzed selected suites of monazite grains that were previously dated by standard U/Pb isotopic methods at three laboratories each equipped with a sensitive high resolution ion microprobe (SHRIMP). Representing diverse igneous and metamorphic lithologies, these grains yielded conventional isotopic ages ranging in age from Neoarchean to Devonian. Chemical dating was performed at Virginia Tech using a Cameca SX-50 EMP in which the analytical routines and settings were specifically optimized for monazite geochronology, including correction of analytical peaks for all major spectral interferences and correction of peak intensities for local background emission. Placement of cross-grain analytical traverses was based on backscattered electron (BSE) images together with wavelength-dispersive (WD) generated X-ray maps for Y, Th, U, and Ca, which revealed the internal compositional complexity of each grain. Shorter EMP traverses were selected adjacent to each SHRIMP pit in order to provide the best possible comparison of ages obtained by the two dating methods. Synthesis protocol for key elemental measurements (Y, Th, U, and Pb) was developed utilizing the 1Ï elemental errors associated with individual analyses, providing an objective approach for data synthesis. Analytical dates were either accepted or excluded based on analytical and spatial justifications. Isotopic dating techniques utilize three independent age calculations, provided the sample is old enough to have accumulated sufficient 207Pb (i.e., ≥~1000 Ma). Similarly, the chemical dating method can utilize two independent age calculations (i.e., Th/Pb and U/Pb) and a U-Th-Pbtotal centroid age in Th/Pb vs. U/Pb space, verified independently against the calculated Th* or U* CHIME ages. Across the entire 2,200 m.y. age range represented by the sample set, the chemical ages calculated from the EMP data chemical ages are internally consistent (within 2Ï error) with the previously measured SHRIMP isotopic ages, except in one case where bulk mixing of discrete age domains within an ablation pit led to an isotopically discordant apparent age. Overall, this study illustrates that EMP chemical dating (1) represents both an accurate and precise primary method for dating monazite from igneous and polymetamorphic terrains; (2) provides superior spatial resolution for obtaining meaningful ages from small and/or irregular domains of discrete age that may be irresolvable or misinterpreted by other dating techniques that sample larger volumes; and (3) illuminates the geological meaning of isotopically discordant monazite ages obtained using conventional methods with lower spatial resolution (e.g., SHRIMP). / Ph. D.

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The Kiirunavaara mine hosts one of the world’s largest apatite-iron ore mineralisations. This ore body has been subject to large amounts of research as well as extensive mining. The ore body is situated between the syenitic foot wall and the rhyodacitic hanging wall, of which consists of differing mineralogy and characteristics. Both these rock masses contain intrusive porphyry dykes, with distinct characteristics of it own. The aim of this study was to analyse 31 samples, mainly in the form of thin sections, and determine the mineralogy and identify eventual microstructures. This was done through the use of optical mineralogy as well as EDS/WDS analysis at the National Microprobe Lab at Uppsala University. The foot wall consists of syenite-porphyry and is dominated by feldspar in both groundmass as well as phenocrysts. Characteristic for the syenite-porphyry is the rounded nodules containing actinolite, titanite, magnetite and chlorite. The hanging wall is defined as quartz-bearing porphyry. It is a rhyodacitic rock with large amounts of feldspar along with green silicates, quartz, titanite and calcite. The intrusive porphyry dyke-rocks share many similarities with the quartz-bearing porphyry, but contain a finer groundmass with larger amounts of clinopyroxene, as well as lower amounts of quartz, magnetite and titanite. Hydrothermal alteration is prevalent in all the types of rock. Alteration minerals such as actinolite, biotite and chlorite are very common within the Kiirunavaara-rocks. The quartz-bearing porphyry displays the most extensive exposure to hydrothermal fluids. The hydrothermal fluids have penetrated several samples, replacing minerals and leaving very few remnant, older minerals. The quartz-bearing porphyry contains the most prominent deformation structures, of varying extent and magnitude. Magmatic flow structures can be seen in the groundmass, as parallel alignment of feldspar and silicate grains. Evidence of solid-state deformation most commonly occurs as pressure shadows around feldspar phenocrysts. / Kiirunavaara-gruvan är belägen vid en av världens största mineraliseringar av apatit-järnmalm. Denna malmkropp har stått i fokus för både omfattande gruvdrift samt genomgripande forskning. Malmkroppen är belägen mellan den syenitiska liggväggen och den ryodacitiska hängväggen, som består av varierande mineralogi och karaktär. Båda av dessa bergmassor innehåller intrusiv gångporfyr med distinkt karaktär. Målet med denna studie var att analysera 31 prover, främst i form av tunnsliper, och bestämma dess mineralogi samt att identifiera eventuella mikrostrukturer. Detta genomfördes genom användning av optisk mineralogi och EDS/WDS-analys vid det nationella mikrosondslaboratioriet vid Uppsala Universitet. Liggväggen består av syenitporfyr och domineras av fältspat i både mellanmassa och som fenokrister. Karaktäristiskt för syenitporfyren är de rundade nodulerna, innehållandes aktinolit, titanit, magnetit och klorit. Hängväggen definieras som kvartsförande porfyr. Det är en ryodacitisk bergart med stora mängder fältspat, gröna silikater, kvarts, titanit och kalcit. Gångporfyren delar många likheter med den kvartsförande porfyren, men består av en finare mellanmassa med större mängd klinopyroxen, samt innehåller mindre mängder kvarts, magnetit och titanit. Hydrotermal omvandling är allmänt förekommande i alla bergarter i Kiirunavaara. Omvandlingsmineral så som aktinolit, biotit och klorit är väldigt vanliga hos Kiirunavaara-bergarterna. Den kvartsförande porfyren uppvisar den mest omfattande exponeringen av hydrotermala vätskor. De hydrotermala vätskorna har penetrerat ett antal prover och därigenom omvandlat mineral, med liten mängd äldre mineral kvar. Den kvartsförande porfyren innehåller de mest prominenta deformationsstrukturer, av olika omfattning och magnitud. Magmatiska flytstrukturer kan observeras i mellanmassan som parallell orientering av fältspat- och silikatkorn. Tecken av fastfasdeformation förekommer främst i form av tryckskuggor runt fältspatsfenokrister.

Hemihedrite from the Florence Lead-Silver mine in Pinal County, Arizona, USA was first described and assigned the ideal chemical formula Pb10Zn(CrO4)(6)(SiO4)(2)F-2, based upon a variety of chemical and crystal-structure analyses. The primary methods used to determine the fluorine content for hemihedrite were colorimetry, which resulted in values of F that were too high and inconsistent with the structural data, and infrared (IR) spectroscopic analysis that failed to detect OH or H2O. Our reinvestigation using electron microprobe analysis of the type material, and additional samples from the type locality, the Rat Tail claim, Arizona, and Nevada, reveals the absence of fluorine, while the presence of OH is confirmed by Raman spectroscopy. These findings suggest that the colorimetric determination of fluorine in the original description of hemihedrite probably misidentified F due to the interferences from PO4 and SO4, both found in our chemical analyses. As a consequence of these results, the study presented here proposes a redefinition of the chemical composition of hemihedrite to the ideal chemical formula Pb10Zn(CrO4)(6)(SiO4)(2)(OH)(2). Hemihedrite is isotypic with iranite with substitution of Zn for Cu, and raygrantite with substitution of Cr for S. Structural data from a sample from the Rat Tail claim, Arizona, indicate that hemihedrite is triclinic in space group P (1) over bar, a = 9.4891(7), b = 11.4242(8), c = 10.8155(7) angstrom, alpha = 120.368(2)degrees, ss = 92.017(3)degrees, gamma = 55.857(2)degrees, V = 784.88(9) angstrom(3), Z = 1, consistent with previous investigations. The structure was refined from single-crystal X-ray diffraction data to R-1 = 0.022 for 5705 unique observed reflections, and the ideal chemical formula Pb10Zn(CrO4)(6)(SiO4)(2)(OH)(2) was assumed during the refinement. Electron microprobe analyses of this sample yielded the empirical chemical formula Pb-10.05(Zn0.91Mg0.02)(Sigma) (= 0.93) (Cr5.98S0.01P0.01)(Sigma = 6.00) Si1.97O34 H-2.16 based on 34 O atoms and six (Cr + S + P) per unit cell.

Previous research indicates compositional variation of pentlandite [(Fe,Ni)9S8] and the effect this variation may have on the electrochemical behaviour of pentlandite is poorly understood. Pentlandite is the primary source of nickel and an important base metal sulfide (BMS) in the platinum industry. It hosts significant amounts of PGEs especially palladium and rhodium when compared to chalcopyrite and pyrrhotite. The aim of the project was to investigate the possible compositional variations of natural pentlandite and the effect of these variations on the electrochemical behavior thereof. To study possible compositional variations, single pentlandite particles - in the order of 100μm in size from flotation concentrates (PGM deposits) and massive samples (massive ore bodies) - from various sources were employed. Electron microprobe analysis indicated a compositional variation of the pentlandite particles hand-picked from the flotation concentrate samples. Variation was observed in the cobalt, iron and nickel content and this was independent of the deposit. A slight compositional variation was observed from the massive pentlandite samples. The effect the compositional variation may have on the electrochemical reactivity of pentlandite was investigated using electrochemical techniques, i.e. measurement of the polarisation resistance and mixed potential as well as performing linear anodic voltammetry, current density–transients and electrochemical impedance spectroscopy (i.e. capacitance). Poor electrochemical response of the pentlandite microelectrodes was observed. Pre–existing pores, deep pores, cracks and the brittle nature of pentlandite microelectrodes may have contributed to the poor electrochemical response of natural pentlandite particles hand-picked from the flotation concentrate. Slight compositional variations of the massive pentlandite sample influenced the electrochemical behaviour. In aerated solutions, iron enriched pentlandites were less reactive after progressive oxidation. The lower reactivity of the electrodes was a result of thick oxide films formed. This was illustrated by polarisation resistance and capacitance measurements. The lower reactivity of the electrodes was also related to the mechanism of the reduction of oxygen at oxidised passive electrode surfaces. It is however difficult to distinguish if the differences in the reactivity was a result of the Fe/Ni ratio or the influence of cobalt. Current density transients confirmed that the reactivity of a pentlandite electrode to be time dependent. The reactivity of the electrode decreased during oxidation. A variation in the electronic properties of the formed oxide film was observed. Slight compositional variation of pentlandite did not have a significant effect on the rest potential values as do changes in the type of sulfides (e.g. pyrite vs. pentlandite). This was confirmed by similar rest potential values of various pentlandite electrodes. The oxidation of synthetic pentlandite may be influenced by the chemical composition. In de-aerated solutions, anodic oxidation (as indicated by the linear anodic voltammogram) of synthetic pentlandite started at a potential lower than of the natural electrodes. In aerated solutions, the synthetic pentlandite was less reactive and formed thicker oxide films. Copyright / Dissertation (MEng)--University of Pretoria, 2010. / Materials Science and Metallurgical Engineering / unrestricted

Summary Serpentinites from the northern Vermont were examined for the distribution and abundance of As. XRD and electron microprobe showed the samples are composed of antigorite, chromite, magnetite, and carbonate minerals (magnesite, dolomite, calcite). The concentration in As when the samples were dissolved in H3PO4 was 10% of the concentration in As when the samples were dissolved in concentrated HF/HNO3, suggesting that As is mainly incorporated in the structure of antigorite. X-ray absorption near-edge structure spectra showed that the As is As(III) in the samples. Extended X-ray absorption fine structure spectra suggested that the As has a tetrahedral coordination and is located in the Si-site in serpentine.