Analytical electron microscopy of fine-grained phases in primitive interplanetary dust particles and carbonaceous chondrites

In order to describe the total mineralogical diversity within primitive extraterrestrial materials, individual interplanetary dust particles (IDPs) collected from the stratosphere as part of the JSC Cosmic Dust Curatorial Program were analyzed using a var ...

The clay-size fraction of CI chondrites Alais and Orgueil : an AEM study

CI chondrites are used pervasively in the meteorite literature as a cosmochemical reference point for bulk compositions[1], isotope analyses[2] and, within certain models of meteorite evolution, as an important component of an alteration sequence within the carbonaceous chondrite subset[3]. More recently, the chemical variablity of CI chondrite matrices (which comprise >80% of the meteorite), has been cited in discussions about the "chondritic" nature of spectroscopic data from P/comet Halley missions[4] and of chemical data from related materials such as interplanetary dust particles[5]. Most CI chondrites have been studied as bulk samples(e.g. major and trace element abundances)and considerable effort has also been focussed on accessory phases such as magnetites, olivine, sulphates and carbonates [6-8]. A number of early studies showed that the primary constituents of CI matrices are layer silicates and the most definitive structural study on powdered samples identified two minerals: montmorillonite and serpentine[9]. In many cases, as with the study by Bass[9],the relative scarcity of most CI chondrites restricts such bulk analyses to the Orgueil meteorite. The electron microprobe/SEM has been used on petrographic sections to more precisely define the "bulk" composition of at least four CI matrices[3], and as recently summarised by McSween[3], these data define a compositional trend quite different to that obtained for CM chondrite matrices. These "defocussed-beam" microprobe analyses average major element compositions over matrix regions ~lOOµm in diameter and provide only an approximation to silicate mineral composition(s) because their grain sizes are much less than the diameter of the beam. In order to (a) more precisely define the major element compositions of individual mineral grains within CI matrices, and (b)complement previous TEM studies [11,12], we have undertaken an analytical electron microscopy (AEM) study of Alais and Orgueil matrices.

Grain size distributions of Magneli phases and metallic titanium in chondritic porous interplanetary dust particles

A mineralogical survey of chondritic interplanetary dust particles (IDPs)showed that these micrometeorites differ significantly in form and texture from components of carbonaceous chondrites and contain some mineral assemblages which do not occur in any meteorite class1. Models of chondritic IDP mineral evolution generally ignore the typical (ultra-) fine grain size of consituent minerals which range between 0.002-0.1µm in size2. The chondritic porous (CP) subset of chondritic IDPs is probably debris from short period comets although evidence for a cometary origin is still circumstantial3. If CP IDPs represent dust from regions of the Solar System in which comet accretion occurred, it can be argued that pervasive mineralogical evolution of IDP dust has been arrested due to cryogenic storage in comet nuclei. Thus, preservation in CP IDPs of "unusual meteorite minerals", such as oxides of tin, bismuth and titanium4, should not be dismissed casually. These minerals may contain specific information about processes that occurred in regions of the solar nebula, and early Solar System, which spawned the IDP parent bodies such as comets and C, P and D asteroids6. It is not fully appreciated that the apparent disparity between the mineralogy of CP IDPs and carbonaceous chondrite matrix may also be caused by the choice of electron-beam techniques with different analytical resolution. For example, Mg-Si-Fe distributions of Cl matrix obtained by "defocussed beam" microprobe analyses are displaced towards lower Fe-values when using analytical electron microscope (AEM)data which resolve individual mineral grains of various layer silicates and magnetite in the same matrix6,7. In general, "unusual meteorite minerals" in chondritic IDPs, such as metallic titanium, Tin01-n(Magneli phases) and anatase8 add to the mineral data base of fine-grained Solar System materials and provide constraints on processes that occurred in the early Solar System.

Trace phases in CI chondrites Alais and Orgueil

Minor phases in meteorites are important indicators of parent-body processing conditions. For example, Kerridge and others (1, 2) have shown that the presence of sulphates and carbonates in CI chondrites provides evidence for aqueous alteration on the parent body. Carbonates and sulphates are relatively prominent components of CI chondrites (e.g., -11.6 wt.% of total mass' and> 10 um diameter) compared to minor phases in most other classes of meteorite and thus, have been amenable to macro scale characterisation using optical petrography and electron microprobe analysis. These minor phases account for significant accumulations of low abundance elements, such as Na, S, K, Ca, and Ni within the bulk meteorite. The fine grained matrix, which consists mostly oflizardite- and montmorillonite-like clays (3), is the...

Fresh water and acid sensitivity of authigenic clays in sandstone reservoirs

Authigenic illite-smectite and chlorite in reservoir sandstones from several Pacific rim sedimentary basins in Australia and New Zealand have been examined using an Electroscan Environmental Scanning Electron Microscope (ESEM) before, during, and after treatment with fresh water and HCl, respectively. These dynamic experiments are possible in the ESEM because, unlike conventional SEMs that require a high vacuum in the sample chamber (10-6 torr), the ESEM will operate at high pressures up to 20 torr. This means that materials and processes can be examined at high magnifications in their natural states, wet or dry, and over a range of temperatures (-20 to 1000 degrees C) and pressures. Sandstones containing the illite-smectite (60-70% illite interlayers) were flushed with fresh water for periods of up to 12 hours. Close examination of the same illite-smectite lines or filled pores, both before and after freshwater treatments, showed that the morphology of the illite-smectite was not changed by prolonged freshwater treatment. Chlorite-bearing sandstones (Fe-rich chlorite) were reacted with 1M to 10M HCl at temperatures of up to 80 degrees C and for periods of up to 48 hours. Before treatment the chlorites showed typically platy morphologies. After HCl treatment the chlorite grains were coated with an amorphous gel composed of Ca, Cl, and possibly amorphous Si, as determined by EDS analyses on the freshly treated rock surface. Brief washing in water removed this surface coating and revealed apparently unchanged chlorite showing no signs of dissolution or acid attack. However, although the chlorite showed no morphological changes, elemental analysis only detected silicon and oxygen.

Micrinite in Southern Hemisphere sub-bituminous and bituminous coals : redefined as fine grained kaolinite

A range of complementary analytical techniques including SEM/EDS, TEM/EDS and conventional optical microscopy has been rigorously applied to precisely defined areas of micrinite in polished coal samples from Australia and New Zealand. Elemental analyses of micrinite regions showed a high abundance of Al, Si and O and high resolution images of micrinite revealed a grain size < 1μm. Electron diffraction and elemental analyses from individual grains within the optically and electron-optically correlated micrinite regions are consistent with the occurence of fine-grained kaolinite. The optical properties of "dark clay" and "micrinite" (i.e. fine-grained kaolinite) can be understood in terms of the diffuse scattering of visible light from the surfaces of materials with different grain sizes in single-phase or multi-phase mixtures.

A multi-stage history for carbonaceous material in extraterrestrial chondritic porous aggregate W7029*A and a new cosmothermometer

A new set of primitive extraterrestrial materials collected in the Earth's stratosphere include Chondritic Porous Aggregates (CPA's) [1]. CPAs have a complex and variable mineralogy [1-3] that include 'organic compounds' [4,5] and poorly graphitised carbon (PGC)[6]. This study presents a continuation of our detailed Analytical Electron Microscope study on carbon-rich CPA W7029*A from the JSC Cosmic Dust Collection. This CPA is an uncontaminated sample that survived atmospheric entry without appreciable alteration [7] and which contains ~44% carbonaceous material. The carbonaceous composition of selected particles was confirmed by Electron Energy Loss Spectroscopy and Selected Area Electron Diffraction (SAED). Possible carbonaceous contaminants introduced by specimen preparation techniques are easily recognised from indigenous CPA carbon particles [8] and do not bias our interpretations.

Freshwater sensitivity of corrensite and chlorite/smectite in hydrocarbon reservoirs - an ESEM study

An Environmental Scanning Electron Microscope (ESEM) has been used to investigate the freshwater sensitivity of secondary corrensite (regularly interstratified chlorite/smectite) and chlorite-rich chlorite/smectite in order to determine whether hydrocarbon reservoirs hosting these clays should be regarded as freshwater sensitive. ESEM experiments involved an examination and close comparison of selected clay areas in three samples at high magnification before, during and after prolonged freshwater treatments. Corrensite and chlorine/smectite in the samples did not visibly swell when immersed in fresh water. After soaking in fresh water for up to three months, these clays retained their original morphology and associated porosity. Hence, the presence of corrensite or chlorite/smectite in a hydrocarbon reservoir need not indicate that the reservoir is freshwater sensitive. © 1994.

Integrated TEM, XRD and electron-microprobe investigation of mixed-layer chlorite smectite from the Point-Sal ophiolite, California

Five basalt samples from the Point Sal ophiolite, California, were examined using HRTEM and AEM in order to compare observations with interpretations of XRD patterns and microprobe analyses. XRD data from ethylene-glycol-saturated samples indicate the following percentages of chlorite in mixed-layer chlorite-smectite identified for each specimen: (i) L2036 almost-equal-to 50%, (ii) L2035 almost-equal-to 70 and 20%, (iii) 1A-13 almost-equal-to 70%, (iv) 1B-42 almost-equal-to 70%, and (v) 1B-55 = 100%. Detailed electron microprobe analyses show that 'chlorite' analyses with high Si, K, Na and Ca contents are the result of interlayering with smectite-like layers. The Fe/(Fe + Mg) ratios of mixed-layer phyllosilicates from Point Sal samples are influenced by the bulk rock composition, not by the percentage of chlorite nor the structure of the phyllosilicate. Measurements of lattice-fringe images indicate that both smectite and chlorite layers are present in the Point Sal samples in abundances similar to those predicted with XRD techniques and that regular alternation of chlorite and smectite occurs at the unit-cell scale. Both 10- and 14-angstrom layers were recorded with HRTEM and interpreted to be smectite and chlorite, respectively. Regular alternation of chlorite and smectite (24-angstrom periodicity) occurs in upper lava samples L2036 and 1A-13, and lower lava sample 1B-42 for as many as seven alternations per crystallite with local layer mistakes. Sample L2035 shows disordered alternation of chlorite and smectite, with juxtaposition of smectite-like layers, suggesting that randomly interlayered chlorite (< 0.5)-smectite exists. Images of lower lava sample 1B-55 show predominantly 14-angstrom layers. Units of 24 angstrom tend to cluster in what may otherwise appear to be disordered mixtures, suggesting the existence of a corrensite end-member having thermodynamic significance.