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Results for “Journal of Magnetic Resonance”

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USGS2018

KG²B, a collaborative benchmarking exercise for estimating the permeability of the Grimsel granodiorite - Part 2: modeling, microstructures and complementary data

Measuring and modelling the permeability of tight rocks remains a challenging task. In addition to the traditional sources of errors that affect more permeable formations (e.g. sample selection, non-representative specimens, disturbance introduced during sample acquisition and preparation), tight rocks can be particularly prone to solid–fluid interactions and thus more sensitive to the methods, procedures and techniques used to measure permeability. To address this problem, it is desirable to collect, for a single material, measurements obtained by different methods and pore fluids. For that purpose, a benchmarking exercise involving 24 laboratories was organized for measuring and modelling the permeability of a single low-permeability material, the Grimsel granodiorite. The objectives of the benchmark were: (i) to compare the results for a given method, (ii) to compare the results between different methods, (iii) to analyse the accuracy of each method, (iv) to study the influence of experimental conditions (especially the nature of pore fluid), (v) to discuss the relevance of indirect methods and models and finally (vi) to suggest good practice for low-permeability measurements. To complement the data set of permeability measurements presented in a companion paper, we focus here on (i) quantitative analysis of microstructures and pore size distribution, (ii) permeability modelling and (iii) complementary measurements of permeability anisotropy and poroelastic parameters. Broad ion beam—scanning electron microscopy, micro-computerized tomography, mercury injection capillary pressure (MICP) and nuclear magnetic resonance (NMR) methods were used to characterize the microstructures and provided the input parameters for permeability modelling. Several models were used: (i) basic statistical models, (ii) 3-D pore network and effective medium models, (iii) percolation model using MICP data and (iv) free-fluid model using NMR data. The models were generally successful in predicting the actual range of measured permeability. Statistical models overestimate the permeability because they do not adequately account for the heterogeneity of the crack network. Pore network and effective medium models provide additional constraints on crack parameters such as aspect ratio, aperture, density and connectivity. MICP and advanced microscopy techniques are very useful tools providing important input data for permeability estimation. Permeability measured—orthogonal to foliation is lower that—parallel to foliation. Combining the experimental and modelling results provide a unique and rich data set.

Geophysical Journal International↗

USGS1998

Rocky 7 prototype Mars rover field geology experiments: 1. Lavic Lake and Sunshine volcanic field, California

Experiments with the Rocky 7 rover were performed in the Mojave Desert to better understand how to conduct rover-based, long-distance (kilometers) geological traverses on Mars. The rover was equipped with stereo imaging systems for remote sensing science and hazard avoidance and 57 Fe Mössbauer and nuclear magnetic resonance spectrometers for in situ determination of mineralogy of unprepared rock and soil surfaces. Laboratory data were also obtained using the spectrometers and an X ray diffraction (XRD)/XRF instrument for unprepared samples collected from the rover sites. Simulated orbital and descent image data assembled for the test sites were found to be critical for assessing the geologic setting, formulating hypotheses to be tested with rover observations, planning traverses, locating the rover, and providing a regional context for interpretation of rover-based observations. Analyses of remote sensing and in situ observations acquired by the rover confirmed inferences made from orbital and simulated descent images that the Sunshine Volcanic Field is composed of basalt flows. Rover data confirmed the idea that Lavic Lake is a recharge playa and that an alluvial fan composed of sediments with felsic compositions has prograded onto the playa. Rover-based discoveries include the inference that the basalt flows are mantled with aeolian sediment and covered with a dense pavement of varnished basalt cobbles. Results demonstrate that the combination of rover remote sensing and in situ analytical observations will significantly increase our understanding of Mars and provide key connecting links between orbital and descent data and analyses of returned samples.

Journal of Geophysical Research E: Planets↗

USGS2020

Sample mounting for organic petrology: No thermal effects from transient exposure to elevated temperatures

For sample mounting, organic petrology laboratories typically use cold-setting epoxy-resin (e.g., 40 °C, used by Oklahoma Geological Survey, OGS) or heat-setting thermoplastic (e.g., 180 °C, used by U.S. Geological Survey, USGS). Previous workers have suggested a systematic huminite/vitrinite reflectance (VR o ) increase was associated with the thermoplastic preparation process, relative to epoxy mounting, which was possibly attributed to moisture loss from organic matter due to the transient high temperatures of plastic mounting. In this study, we evaluated thermal effects to low thermal maturity organic matter from transient exposure to elevated temperatures. A subbituminous coal sample was subjected to long-term (4 to 38 weeks) exposure to temperatures of 85 to 120 °C and afterward evaluated by multiple approaches to test thermal advance [elemental analyses, Rock-Eval pyrolysis, Fourier transform infrared spectroscopy (FTIR), nuclear magnetic resonance (NMR), pyrolysis gas chromatography, and petrographic analyses, including huminite/vitrinite reflectance and spectral fluorescence], all of which showed no detectable systematic (statistically insignificant) changes between the original sample and its heat-treated products. We also compared huminite/vitrinite reflectance of six low thermal maturity samples (those most likely to react to transient heating) mounted via both cold-setting epoxy-resin and heat-setting thermoplastic. Results indicate measured VR o of a sample prepared by one mounting process was within the standard deviation of reflectance for the same sample prepared via the other process. Moreover, VR o results were not systematically higher in thermoplastic mounts. Contrary to previous work, these results suggest thermoplastic mounting or other transient exposure to elevated temperatures does not impact thermal maturity estimates from reflectance measurement for low thermal maturity organic samples. Furthermore, the average interlaboratory difference in measured VR o (between OGS and USGS) for the same sample prepared by either epoxy-resin or thermoplastic mounting was 0.038%, about double the average difference between VR o for the same sample prepared via epoxy-resin versus thermoplastic in a single laboratory (0.024%). This result indicates interlaboratory variability impacts VR o measurement reproducibility to the extent that systematic differences could not be observed between thermoplastic and cold-setting sample preparation approaches, even if such differences were present.

International Journal of Coal Geology↗

USGS1999

A possible link between Balkan endemic nephropathy and the leaching of toxic organic compounds from Pliocene lignite by groundwater: Preliminary investigation

Balkan endemic nephropathy (BEN) is a fatal kidney disease that is known to occur only in clusters of villages in alluvial valleys of tributaries of the Danube River in Bulgaria, Romania, Yugoslavia, Bosnia, and Croatia. The confinement of this disease to a specific geographic area has led to speculation that an environmental factor may be involved in the etiology of BEN. Numerous environmental factors have been suggested as causative agents for producing BEN, including toxic metals in drinking water, metal deficiency in soils of BEN areas, and environmental mycotoxins to name a few. These hypotheses have either been disproved or have failed to conclusively demonstrate a connection to the etiology of BEN, or the clustering of BEN villages. In previous work, we observed a distinct geographic relationship between the distribution of Pliocene lignites in the Balkans and BEN villages. We hypothesized that the long-term consumption of well water containing toxic organic compounds derived from the leaching of nearby Pliocene lignites by groundwater was a primary factor in the etiology of BEN. In our current work, chemical analysis using 13C nuclear magnetic resonance (13CNMR) spectroscopy indicated a high degree of organic functionality in Pliocene lignite from the Balkans, and suggested that groundwater can readily leach organic matter from these coal beds. Semi-quantitative gas chromatography/mass spectroscopy analysis of solvent extracts of groundwater from shallow wells in BEN villages indicated the presence of potentially toxic aromatic compounds, such as napthalene, fluorene, phenanthrene, and pyrene at concentrations in the ppb range. Laboratory leaching of Balkan Pliocene lignites with distilled water yielded soluble organic matter (> 500 MW) containing large amounts of aromatic structures similar to the simple/discrete aromatic compounds detected in well water from BEN villages. These preliminary results are permissive of our hypothesis and suggest that further work on the possible relationship between the etiology of BEN and toxic aromatic substances leached from Pliocene lignites in well water is warranted.A distinct geographic relationship between the distribution of Pliocene lignites in the Balkans and villages where Balkan endemic nephropathy (BEN) occurs has been observed, indicating a possible link between BEN and the long-term consumption of well water containing toxic organic compounds derived from the leaching of nearby Pliocene lignites. Preliminary investigations by NMR spectroscopy, gas chromatography/mass spectroscopy and leaching experiments show a high degree of organic functionality in the Pliocene lignites, high-leachability by groundwater of organic matter from these beds, and the presence of toxic aromatic compounds.

International Journal of Coal Geology↗

USGS2011

Physical properties of sediment from the Mount Elbert Gas Hydrate Stratigraphic Test Well, Alaska North Slope

This study characterizes cored and logged sedimentary strata from the February 2007 BP Exploration Alaska, Department of Energy, U.S. Geological Survey (BPXA-DOE-USGS) Mount Elbert Gas Hydrate Stratigraphic Test Well on the Alaska North Slope (ANS). The physical-properties program analyzed core samples recovered from the well, and in conjunction with downhole geophysical logs, produced an extensive dataset including grain size, water content, porosity, grain density, bulk density, permeability, X-ray diffraction (XRD) mineralogy, nuclear magnetic resonance (NMR), and petrography. This study documents the physical property interrelationships in the well and demonstrates their correlation with the occurrence of gas hydrate. Gas hydrate (GH) occurs in three unconsolidated, coarse silt to fine sand intervals within the Paleocene and Eocene beds of the Sagavanirktok Formation: Unit D-GH (614.4 m-627.9 m); unit C-GH1 (649.8 m-660.8 m); and unit C-GH2 (663.2 m-666.3 m). These intervals are overlain by fine to coarse silt intervals with greater clay content. A deeper interval (unit B) is similar lithologically to the gas-hydrate-bearing strata; however, it is water-saturated and contains no hydrate. In this system it appears that high sediment permeability (k) is critical to the formation of concentrated hydrate deposits. Intervals D-GH and C-GH1 have average "plug" intrinsic permeability to nitrogen values of 1700 mD and 675 mD, respectively. These values are in strong contrast with those of the overlying, gas-hydrate-free sediments, which have k values of 5.7 mD and 49 mD, respectively, and thus would have provided effective seals to trap free gas. The relation between permeability and porosity critically influences the occurrence of GH. For example, an average increase of 4% in porosity increases permeability by an order of magnitude, but the presence of a second fluid (e.g., methane from dissociating gas hydrate) in the reservoir reduces permeability by more than an order of magnitude.

Alaska↗

USGS2011

Chemical structures of coal lithotypes before and after CO2 adsorption as investigated by advanced solid-state 13C nuclear magnetic resonance spectroscopy

Four lithotypes (vitrain, bright clarain, clarain, and fusain) of a high volatile bituminous Springfield Coal from the Illinois Basin were characterized using advanced solid-state 13 C nuclear magnetic resonance (NMR) spectroscopy. The NMR techniques included quantitative direct polarization/magic angle spinning (DP/MAS), cross polarization/total sideband suppression (CP/TOSS), dipolar dephasing, CH n selection, and recoupled C–H long-range dipolar dephasing techniques. The lithotypes that experienced high-pressure CO 2 adsorption isotherm analysis were also analyzed to determine possible changes in coal structure as a result of CO 2 saturation at high pressure and subsequent evacuation. The main carbon functionalities present in original vitrain, bright clarain, clarain and fusain were aromatic carbons (65.9%–86.1%), nonpolar alkyl groups (9.0%–28.9%), and aromatic C–O carbons (4.1%–9.5%). Among these lithotypes, aromaticity increased in the order of clarain, bright clarain, vitrain, and fusain, whereas the fraction of alkyl carbons decreased in the same order. Fusain was distinct from other three lithotypes in respect to its highest aromatic composition (86.1%) and remarkably small fraction of alkyl carbons (11.0%). The aromatic cluster size in fusain was larger than that in bright clarain. The lithotypes studied responded differently to high pressure CO 2 saturation. After exposure to high pressure CO 2 , vitrain and fusain showed a decrease in aromaticity but an increase in the fraction of alkyl carbons, whereas bright clarain and clarain displayed an increase in aromaticity but a decrease in the fraction of alkyl carbons. Aromatic fused-rings were larger for bright clarain but smaller for fusain in the post-CO 2 adsorption samples compared to the original lithotypes. These observations suggested chemical CO 2 –coal interactions at high pressure and the selectivity of lithotypes in response to CO 2 adsorption.

International Journal of Coal Geology↗

USGS2022

Gas hydrate saturation estimates, gas hydrate occurrence, and reservoir characteristics based on well log data from the hydrate-01 stratigraphic test well, Alaska North Slope

The Hydrate-01 Stratigraphic Test Well was drilled at the Kuparuk 7-11-12 site on the Alaska North Slope in December 2018. Sonic log data provide compressional (P) and shear (S) slowness from which we determine gas hydrate saturation ( S gh ) estimates using effective medium theory. The sonic S gh estimates compare favorably with S gh estimated from resistivity and nuclear magnetic resonance (NMR) logs, showing that gas hydrate occupies up to approximately 90% of the pore space in the target reservoir sands. The informally named B1 sand (2294 feet below mean sea level) shows lower V P / V S ratios than the D1 sand (2770 feet below mean sea level), with the lower part of the B1 sand showing lower V P / V S ratios than the upper part of the B1 sand. This corresponds to a stiffer, or more “cemented”, behavior for the lower B1 sand and less cemented behavior for the D1 sand. This trend could be due to differences in the reservoirs themselves or in the gas hydrate morphology or to both factors. We observe that the presence of gas hydrate in the upper B1 sand has greater impact on hydraulic permeability (measurements suggest a greater difference between intrinsic and effective permeability) than in the D1 sand, possibly related to gas hydrate morphology but more likely due simply to higher gas hydrate saturations in the upper B1 sand. Analyses of S gh relative to porosity, shale fraction, and intrinsic permeability show that reservoir quality (as represented by these three metrics) exerts control on gas hydrate saturation. Grain size and mineralogy data show somewhat smaller grains and better sorting in the D1 reservoir relative to the upper B1 reservoir and smaller grains and greater clay fraction in the lower B1 reservoir relative to the other two reservoir zones. Together, these data suggest that reservoir characteristics play a role in the observed V P / V S patterns, but gas hydrate morphology (possibly varying with saturation) must also be considered.

Alaska↗

USGS2009

Measurement of soil carbon oxidation state and oxidative ratio by 13 C nuclear magnetic resonance

The oxidative ratio (OR) of the net ecosystem carbon balance is the ratio of net O 2 and CO 2 fluxes resulting from photosynthesis, respiration, decomposition, and other lateral and vertical carbon flows. The OR of the terrestrial biosphere must be well characterized to accurately estimate the terrestrial CO 2 sink using atmospheric measurements of changing O 2 and CO 2 levels. To estimate the OR of the terrestrial biosphere, measurements are needed of changes in the OR of aboveground and belowground carbon pools associated with decadal timescale disturbances (e.g., land use change and fire). The OR of aboveground pools can be measured using conventional approaches including elemental analysis. However, measuring the OR of soil carbon pools is technically challenging, and few soil OR data are available. In this paper we test three solid-state nuclear magnetic resonance (NMR) techniques for measuring soil OR, all based on measurements of the closely related parameter, organic carbon oxidation state (C ox ). Two of the three techniques make use of a molecular mixing model which converts NMR spectra into concentrations of a standard suite of biological molecules of known C ox . The third technique assigns C ox values to each peak in the NMR spectrum. We assess error associated with each technique using pure chemical compounds and plant biomass standards whose C ox and OR values can be directly measured by elemental analyses. The most accurate technique, direct polarization solid-state 13 C NMR with the molecular mixing model, agrees with elemental analyses to ??0.036 C ox units (??0.009 OR units). Using this technique, we show a large natural variability in soil C ox and OR values. Soil C ox values have a mean of -0.26 and a range from -0.45 to 0.30, corresponding to OR values of 1.08 ?? 0.06 and a range from 0.96 to 1.22. We also estimate the OR of the carbon flux from a boreal forest fire. Analysis of soils from nearby intact soil profiles imply that soil carbon losses associated with the fire had an OR of 1.09 1 (??0.00 3 ). Fire appears to be a major factor driving the soil C pool to higher oxidation states and lower OR values. Episodic fluxes caused by disturbances like fire may have substantially different ORs from ecosystem respiration fluxes and therefore should be better quantified to reduce uncertainties associated with our understanding of the global atmospheric carbon budget. Copyright 2009 by the American Geophysical Union.

Journal of Geophysical Research G: Biogeosciences↗

USGS2022

Permeability measurement and prediction with nuclear magnetic resonance analysis of gas hydrate-bearing sediments recovered from Alaska North Slope 2018 Hydrate-01 Stratigraphic Test Well

Permeability of porous media, such as oil and gas reservoirs, is the crucial material parameter for predicting their hydraulic behavior. A nuclear magnetic resonance (NMR) analyzer is widely used as a powerful tool to predict permeability of various media. NMR T 2 (transverse or spin–spin) relaxation time distribution, which is related to pore size distribution, gives the information to allow calculation of effective (initial) permeability. In this study, we investigate effective, intrinsic (absolute), and relative water and gas permeabilities of hydrate-bearing pressure core samples. These samples were recovered from the Alaska North Slope 2018 Hydrate-01 Stratigraphic Test Well by sidewall pressure coring and then analyzed in a laboratory using both fluid flow test and NMR analyzer. The peak of the NMR T 2 distribution was measured at 10–20 ms using a laboratory NMR analyzer, which compares well with in situ measurements obtained via logging while drilling NMR data for two samples with high gas hydrate saturations ( S h = 76% and 74%). Further, comparison of laboratory NMR T 2 distribution after hydrate dissociation revealed that the hydrate existed in large pore spaces. Effective permeabilities predicted by the Timur-Coates (TC) model and the Schlumberger-Doll-Research (SDR) model, with T 2 cutoff 33 ms, were about an order of magnitude less than the laboratory measured values. Alternative TC model-based calculations with the T 2 cutoff reduced to 10 ms and a newly developed hydraulic radius model better matched the laboratory data. For the analysis of the intrinsic permeabilities, the TC model with a T 2 cutoff of 33 ms and SDR model were greater than the laboratory derived values, while the hydraulic radius model more closely matched the laboratory-derived values. In addition, permeability measurements were also made relative to gas and water under constant three-phase flow (water–gas–hydrate) conditions. After hydrate dissociation, a relative permeability curve was developed for each of the analyzed core samples based on the Corey petrophysical model. The results indicate that the gas permeability changed rapidly at high water saturation around 90%. Thus, we infer that the selection of relative reservoir parameters should focus on the higher water saturation conditions.

Alaska↗

USGS1990

Studies of angiospermous woods in Australian brown coal by nuclear magnetic resonance and analytical pyrolysis: new insight into early coalification

Many Tertiary coals contain abundant fossilized remains of angiosperms, which commonly dominated the ancient peat-swamp environments; modern analogs of such swamps can be found in tropical and subtropical regions of the world. Comparisons of angiospermous wood from Australian brown coal with similar wood buried in modern peat swamps of Indonesia have provided some new insights into coalification reactions. These comparisons were made by using solid-state 13 C nuclear magnetic resonance (NMR) techniques and pyrolsis-gas chromatography-mass spectrometry (py-gc-ms). These two modern techniques are especially suited for detailed structural evaluation of the complex macromolecules in coal. The earliest transformation (peatification) of organic matter in angiospermous wood is the degradation and removal of cellulosic components and the concomitant selective preservation of lignin-derived components. The angiospermous lignin that becomes enriched in wood as a result of cellulose degradation also is modified by coalification reactions; this modification, however, does not involve degradation and removal of the lignin. Rather, the early coalification process transforms the lignin phenols (guiacyl and syringyl) to eventually yield the aromatic structures typically found in brown coal. One such transformation, which is determined from NMR data, involves the cleavage of aryl-ether bonds that link guaiacyl and syringyl units in lignin, and this transformation leads to the formation of free lignin phenols. Another transformation, which is also determined from the NMR data, involves the loss of methoxyl groups, probably via demethylation, to produce catechol-like structures. Coincident with ether-cleavage and demethylation, the aromatic rings derived from lignin phenols become more carbon-substituted and cross linked, as determined by dipolar-dephasing NMR studies. This cross linking is probably responsible for preventing the lignin phenols, which are freed from the lignin macromolecule by ether cleavage, from being removed from the coal by dissolution. Pyrolysis data suggest that the syringyl units are altered more readily than are guaiacyl units, and this difference in resistance leads to an enrichment of the guaiacyl units in fossil angiospermous woods. Many of the coalification reactions noted above occur to some degree in all angiospermous fossil wood examined; however, some significant differences are observed in the degree of coalification of the fossil wood samples from the same burial depth in the brown coal. These differences indicate that the depth and duration of burial are probably not entirely responsible for the variations in degree of coalification. Different rates of degradation in peat may have contributed to the variations in the apparent degree of coalification; some woods may have been altered more rapidly at the peat stage than others. Although preliminary, this systematic study of botanically related wood in peat and coal results in a more detailed differentiation of coalification reactions than have previous investigations. The combined use of solid-state 13 C NMR and py-gc-ms has facilitated this detailed insight into the coalification of angiospermous wood.

International Journal of Coal Geology↗