Field trip guide to kaolinite geodes in Hamilton, Illinois, USA

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Porosity and permeability determination of organic-rich Posidonia shales based on 3-D analyses by FIB-SEM microscopy

The goal of this study is to better understand the porosity and permeability in shales to improve modelling fluid and gas flow related to shale diagenesis. Two samples (WIC and HAD) were investigated, both mid-Jurassic organic-rich Posidonia shales from Hils area, central Germany of different maturity (WIC R0 0.53 % and HAD R0 1.45 %). The method for image collection was focused ion beam (FIB) microscopy coupled with scanning electron microscopy (SEM). For image and data analysis Avizo and GeoDict was used. Porosity was calculated from segmented 3-D FIB based images and permeability was simulated by a Navier Stokes–Brinkman solver in the segmented images. Results show that the quantity and distribution of pore clusters and pores (≥  40 nm) are similar. The largest pores are located within carbonates and clay minerals, whereas the smallest pores are within the matured organic matter. Orientation of the pores calculated as pore paths showed minor directional differences between the samples. Both samples have no continuous connectivity of pore clusters along the axes in the x, y, and z direction on the scale of 10 to 20 of micrometer, but do show connectivity on the micrometer scale. The volume of organic matter in the studied volume is representative of the total organic carbon (TOC) in the samples. Organic matter does show axis connectivity in the x, y, and z directions. With increasing maturity the porosity in organic matter increases from close to 0 to more than 5 %. These pores are small and in the large organic particles have little connection to the mineral matrix. Continuous pore size distributions are compared with mercury intrusion porosimetry (MIP) data. Differences between both methods are caused by resolution limits of the FIB-SEM and by the development of small pores during the maturation of the organic matter. Calculations show no permeability when only considering visible pores due to the lack of axis connectivity. Adding the organic matter with a background permeability of 1 × 10−21 m2 to the calculations, the total permeability increased by up to 1 order of magnitude for the low mature and decreases slightly for the overmature sample from the gas window. Anisotropy of permeability was observed. Permeability coefficients increase by 1 order of magnitude if simulations are performed parallel to the bedding. Our results compare well with experimental data from the literature suggesting that upscaling may be possible in the future as soon as maturity dependent organic matter permeability coefficients can be determined

Plasma Spraying of Kaolinite for Preparing Reactive Alumino-Silicate Glass Coatings

Thermally treated kaolinite is used to develop a range of alumino-silicate-based precursor materials but its behavior during plasma spraying has not been well-researched. In this study, two types of kaolinite samples were investigated in the form of low defect (KGa-1b) and high defect (KGa-2) varieties. The extreme temperatures of the plasma stream (up to 20 000 K) induced flash melting to produce a highly porous alumino-silicate glass without any crystallization of new Al−Si oxide minerals. The glass is comprised largely of intact or deformed spheres (average diameters 1.14–1.44 μm), which indicates rapid quenching and solidification before impact. The subspherical structures contain up to 40 % closed pore space caused by the rapid escape of water during melting. The low-density, porous alumino-silicate glass coatings with predicted specific surface areas (>0.95 m2/g) and hardnesses >1.8 GPa represent a potentially reactive but physically stable substrate ideal for further chemical functionalization

Simulating permeability reduction by clay mineral nanopores in a tight sandstone by combining computer X-ray microtomography and focussed ion beam scanning electron microscopy imaging

Computer X-ray microtomography (µXCT) represents a powerful tool for investigating the physical properties of porous rocks. While calculated porosities determined by this method typically match experimental measurements, computed permeabilities are often overestimated by more than 1 order of magnitude. This effect increases towards smaller pore sizes, as shown in this study, in which nanostructural features related to clay minerals reduce the permeability of tight reservoir sandstone samples. Focussed ion beam scanning electron microscopy (FIB-SEM) tomography was applied to determine the permeability effects of illites at the nanometre scale, and Navier–Stokes equations were applied to calculate the permeability of these domains. With these data, microporous domains (porous voxels) were defined using microtomography images of a tight reservoir sample. The distribution of these domains could be extrapolated by calibration against size distributions measured in FIB-SEM images. For this, we assumed a mean permeability for the dominant clay mineral (illite) in the rock and assigned it to the microporous domains within the structure. The results prove the applicability of our novel approach by combining FIB-SEM with X-ray tomographic rock core scans to achieve a good correspondence between measured and simulated permeabilities. This methodology results in a more accurate representation of reservoir rock permeability in comparison to that estimated purely based on µXCT images

Porosity and distribution of water in perlite from the island of Milos, Greece

A perlite sample representative of an operating mine in Milos was investigated with respect to the type and spatial distribution of water. A set of different methods was used which finally provided a consistent view on the water at least in this perlite. Infrared spectroscopy showed the presence of different water species (molecular water and hydroxyl groups / strongly bound water). The presence of more than 0.5 mass% smectite, however, could be excluded considering the cation exchange capacity results. The dehydration measured by thermal analysis occurred over a wide range of temperatures hence confirming the infrared spectroscopical results. Both methods point to the existence of a continuous spectrum of water binding energies. The spatial distribution of water and/or pores was investigated using different methods (CT: computer tomography, FIB: scanning electron microscopy including focused ion beam technology, IRM: infrared microscopy). Computer tomography (CT) showed large macropores (20 – 100 μm) and additionally revealed a mottled microstructure of the silicate matrix with low density areas up to a few μm in diameter. Scanning electron microscopy (FIB) confirmed the presence of μm sized pores and IRM showed the filling of these pores with water. In summary, two types of pores were found. Airfilled 20 – 100 μm pores and μm-sized pores disseminated in the glass matrix containing at least some water. Porosity measurements indicate a total porosity of 26 Vol%, 11 Vol% corresponding to the μm-sized pores. It remains unsolved wether the water in the μm-sized pores entered after or throughout perlite formation. However, the pores are sealed and no indications of cracks were found which indicated a primary source of the water, i.e. water was probably entrapped by quenching of the lava. The water in these pores may be the main reason for the thermal expandability which results in the extraordinarily porous expanded perlite building materials

Illite in the Lower Paleozoic of the Illinois Basin: Origin, age, and polytype quantification

Illite was first named in 1937 in Illinois by Ralph Grim, one of the founders of clay mineralogy. Illite is the most abundant clay mineral on the earth's surface. However, we know very little about the origin of illite in Illinois. This dissertation focuses on two aspects of illite in the Lower Paleozoic of the Illinois Basin: (1) illite polytype quantification, which explains the anomalies of the distribution of illite and smectite in the Illinois Basin, and (2) the origin and age of diagenetic illite, which is used to link illitization to fluid migration.Illite polytype quantification allows the differentiation of diagenetic and detrital illite. In Paleozoic shales from the Illinois Basin three polytypes 1M\rm\sb{d}, 1M, and 2M\sb1 are observed. 1M\rm\sb{d} and 1M are of diagenetic origin and 2M\sb1 of detrital origin. All three polytypes were quantified by mixing single polytypes and comparing the experimental XRD traces with traces calculated using WILDFIRE$\copyright.$Illite polytype quantification of different size fractions combined with K/Ar dates allows the extrapolation to apparent ages of detrital and diagenetic end-members. The extrapolated age of the diagenetic end-members dates episodes of diagenesis. Results show that the Upper Ordovician Maquoketa Group shales contain diagenetic illite (dominantly 1M\rm\sb{d} with minor 1M) with an age of $\sim$360 Ma, that was not formed solely by burial diagenesis but mainly through either a hydrothermal or K-rich brine event. Ordovician and Cambrian shale partings and sandstones, older than the Maquoketa Group, contain diagenetic illite (1M\rm\sb{d} in shales and 1M in sandstones) having an age of 300 Ma. This late Paleozoic age falls within the span of the Alleghanian orogeny.The conclusion is that the diagenetic illite of the Maquoketa Group and that of the underlying formations formed from different precursors in different hydrologic systems. The diagenetic illite in the Maquoketa Group formed mainly during a hydrothermal or K-rich brine event ($\le$100\sp\circC) from smectite or kaolinite. During the Alleghanian orogeny the Maquoketa Group served as an aquitard to fluids ($\le$140\sp\circC) that precipitated the diagenetic illite in the older and more permeable sandstones and carbonates.U of I OnlyETDs are only available to UIUC Users without author permissio

In situ measurements of the hydration behavior of compacted Milos (SD80) bentonite by wet-cell X-ray diffraction in an Opalinus clay pore water and a diluted cap rock brine

: Compacted bentonite is currently being considered as a suitable backfill material for sealing underground repositories for radioactive waste as part of a multi-barrier concept. Although showing favorable properties for this purpose (swelling capability, low permeability, and high adsorption capacity), the best choice of material remains unclear. The goal of this study was to examine and compare the hydration behavior of a Milos (Greek) Ca-bentonite sample (SD80) in two types of simulated ground water: (i) Opalinus clay pore water, and (ii) a diluted saline cap rock brine using a confined volume, flow-through reaction cell adapted for in situ monitoring by X-ray diffraction. Based on wet-cell X-ray diffractometry (XRD) and calculations with the software CALCMIX of the smectite d(001) reflection, it was possible to quantify the abundance of water layers (WL) in the interlayer spaces and the amount of non-interlayer water uptake during hydration using the two types of solutions. This was done by varying WL distributions to fit the CALCMIX-simulated XRD model to the observed data. Hydrating SD80 bentonite with Opalinus clay pore water resulted in the formation of a dominant mixture of 3- and 4-WLs. The preservation of ca. 10% 1-WLs and the apparent disappearance of 2-WLs in this hydrated sample are attributed to small quantities of interlayer K (ca. 8% of exchangeable cations). The SD80 bentonite of equivalent packing density that was hydrated in diluted cap rock brine also contained ca. 15% 1-WLs, associated with a slightly higher concentration of interlayer K. However, this sample showed notable suppression of WL thickness with 2- and 3-WLs dominating in the steady-state condition. This effect is to be expected for the higher salt content of the brine but the observed generation of CO2 gas in this experiment, derived from enhanced dissolution of calcite, may have contributed to the suppression of WL thickness. Based on a comparison with all published wet-cell bentonite hydration experiments, the ratio of packing density to the total layer charge of smectite is suggested as a useful proxy for predicting the relative amounts of interlayer and non-interlayer water incorporated during hydration. Such information is important for assessing the subsequent rates of chemical transport through the bentonite barrier

A talc-based cement-poor concrete for sealing boreholes in rock

Deep investigation boreholes in crystalline rock for site selection of repositories for high-level radioactive waste are proposed to be sealed by installing a series of dense concrete and clay plugs. These should prevent radionuclides from leaking canisters at depth to migrate to the biosphere through the holes. The concrete seals will be installed where the holes intersect water-bearing fracture zones to serve as stable and low-permeable supports for adjacent clay plugs. Low porosity and microstructural stability must be guaranteed for many thousands of years and ordinary Portland cement with organic superplastizer will not fulfil the requirements since the high pH will cause degradation of contacting clay and the organic additive can produce colloids with a capacity to carry radionuclides up to the biosphere. Very cement-poor concrete (<8 %) based on low-pH cement and with talc as plasticizer is an option but it matures more slowly, which requires that the construction of seals is made so that sufficient bearing capacity for carrying overlying clay seals is reached.Validerad; 2013; 20130104 (mohhat