Nuclear Magnetic Resonance Response Research Articles

Depth-wise multiparametric assessment of articular cartilage layers with single-sided NMR.

Articular cartilage (AC) is a specialized connective tissue that covers the ends of long bones and facilitates the load-bearing of joints. It consists of chondrocytes distributed throughout an extracellular matrix and organized into three zones: superficial, middle, and deep. Nuclear magnetic resonance (NMR) techniques can be used to characterize this layered structure. In this study, devoted to a better understanding of the NMR response of this complex tissue, 20 specimens excised from femoral and tibial cartilage of bovine samples were analyzed by the low-field single-sided NMR-MOUSE-PM10. A multiparametric depth-wise analysis was performed to characterize the laminar structure of AC and investigate the origin of the NMR dependence on depth. The depth dependence of the single parameters T1, T2, and D has been described in literature, but their simultaneous measurement has not been fully exploited yet, as well as the extent of their variability. A novel parameter, α, evaluated by applying a double-quantum-like sequence, has been measured. The significant decrease in T1, T2, and D from the middle to the deep zone is consistent with depth-dependent composition and structure changes of the complex matrix of fibers confining and interacting with water. The α parameter appears to be a robust marker of the layered structure with a well-reproducible monotonic trend across the zones. The discrimination of cartilage zones was reinforced by a multivariate principal component analysis statistical analysis. The large number of samples allowed for the identification of the smallest number of parameters or their combination able to classify samples. The first two components clustered the data according to the different zones, highlighting the sensitivity of the NMR parameters to the structural and compositional variations of AC. Using two parameters, the best result was obtained by considering T1 and α. Single-sided NMR devices, portable and low-cost, provide information on NMR parameters related to tissue composition and structure.

Experimental Investigation of Amine Regeneration for Carbon Capture through CO2 Mineralization

Summary The most common method for point-source carbon capture involves the absorption of CO2 from flue gas by amine solutions. The CO2 is then stripped from the amine solution by desorption with steam or heat. While amine solvents exhibit high CO2 absorption efficiency, their desorption process consumes a substantial amount of energy. A more energy-efficient alternative for the regeneration of the amine can be done through a mineralization process. Past studies have shown the feasibility of mineralizing captured CO2 from amine solution using calcium oxide (CaO) or other CaO-containing industrial waste. This study aims to show experimentally the extent of mineralization over time in near-ambient conditions and develop a mechanistic model. Lab-scale experiments are conducted to determine the absorption characteristics of CO2 in monoethanolamine (MEA) solutions and the extent of mineralization. We observe that pH serves as an indicator for CO2 loading in amine solutions. At high concentrations of MEA, CO2 absorption efficiency is about 0.5 mol CO2/mol MEA. Under ambient pressure and a temperature of 40°C, CaO effectively mineralizes CO2 and regenerates MEA. The CaO initially reacts with water to produce calcium hydroxide (Ca(OH)2) and subsequently reacts with dissolved CO2, forming calcium carbonate (CaCO3). Both 13C nuclear magnetic resonance (NMR) and FTIR indicate that MEA can be regenerated with an efficiency close to 69 to 98%, by comparing the carbamate and bicarbonate peaks in the 13C NMR response. A model to describe the absorption and mineralization reaction is proposed using the PHREEQC software; the pH is matched within less than 3% error. This study demonstrates that CO2 desorption from MEA solutions can occur through mineralization, converting CO2 into carbonates at low pressure and temperature with CaO. This method has lower energy consumption and results in the most stable form of CO2, making it a safer sequestration strategy than supercritical CO2 storage in reservoirs.

Water-bearing properties of high rank coal reservoir and the effect on multiphase methane

Coal reservoirs commonly exhibit the coexistence of gas and water, wherein the distribution of water plays a crucial role in influencing methane storage and transportation. The presence of water affects methane adsorption, and models predicting adsorbed methane that do not account for water conditions can introduce errors, posing challenges in meeting practical production needs. In this study, through a series of centrifugation experiments and nuclear magnetic resonance (NMR) adsorption experiments, the distribution characteristics of bound water and movable water in reservoirs and their influence on multiphase methane were assessed. The results indicate that under water-bearing conditions, there exists specific methane in the adsorption space, exhibiting properties similar to free methane. In terms of the relaxation characteristics, the presence of water affects both the peak area and morphology of the T2 spectra of multiphase methane. Based on the NMR response characteristics of adsorbed methane at different water saturations, we proposed and established a theoretical model for predicting the content and density of adsorbed methane under varying water saturations. Additionally, utilizing two-dimensional NMR technology, a simple identification spectrum for multiphase methane was established. The study suggests that the presence of water delays the time of adsorption equilibrium for methane. At low water saturations, water primarily inhibits the adsorption rate of methane. However, with increasing pressure and water saturation, water predominantly suppresses the adsorption capacity of methane. At low water saturations, the bound water has a significant effect on adsorbed methane. Conversely, as water saturations increase, movable water gradually occupies adsorption sites with weaker adsorption potential. It is worth noting that with an increase in water saturation, the content of adsorbed methane decreases, but the adsorption phase density may not necessarily decrease. These research findings provide new insights into the interaction mechanisms between water and methane in water-bearing coal reservoirs.

Gradient-based surface nuclear magnetic resonance for groundwater investigation

In medical magnetic resonance imaging, spatial localization (imaging) is based upon the application of controlled magnetic field gradients on top of the main magnetic field to spatially modulate the frequency and/or phase of the nuclear magnetic resonance (NMR) signal across the volume of investigation. In this work, we have applied similar physical principles to produce controlled magnetic field gradients during surface NMR-based groundwater investigations. In this approach, a gradient pulse of variable amplitude or duration is applied immediately after the excitation pulse to cause predictable phase encoding of the NMR signal as a function of depth. This approach is also applicable to emerging surface NMR detection methods that use a prepolarization field with fast nonadiabatic turn-off to generate detectable NMR signals from the shallow subsurface. In this case, the gradient pulse is applied after terminating the prepolarization field and provides a heretofore unavailable means of localizing the NMR response as a function of depth. The application of gradients can also be combined with tip-angle-based modulation to yield higher imaging resolution than can be achieved through either gradient- or tip-angle-based imaging alone. We implemented this new gradient-based capability into a surface NMR gradient generation accessory that is compatible with the GMR-Flex instrument and developed surface NMR-specific forward modeling and linear inverse models. We validated the accuracy of this novel gradient-based sNMR technology using computer simulations, experiments using a small pool filled with a discrete layer of bulk water, and field experiments at well-characterized groundwater test sites along Ebey Island, WA, and Larned, KS. The gradient-based sNMR imaging observations were compared with high-resolution direct push NMR results observed at these sites. The results of computer simulations and field experiments indicate improvements in both the detection (signal-to-noise ratio) and spatial resolution of shallow subsurface water content using gradient-based surface NMR, compared with traditional surface NMR imaging methods.

Li-Ion Dynamics in Li2S:LiI Composites – on the Effect of Solid-Solution Formation on Overall Li+ Transport

The enormous interest in developing powerful all-solid-state Li-ion batteries led to a boost in electrolyte research. Some Li-ion conductors have Ag-bearing analogs; the fast Ag+ ion conductor, Ag3SI, could be one of such materials. So far, no clear evidence is available that the Li-counterpart, Li3SI, does exist. Here, we treated an equimolar mixture of Li2S and LiI in high-energy ball mills and followed structural changes via X-ray diffraction (XRD) and magic-angle spinning (MAS) 6,7Li nuclear magnetic resonance (NMR) measurements. Differences in local structures as sensed by MAS NMR will be discussed for annealed and non-annealed samples, that is, powder samples directly obtained after finishing the ball-milling procedure. For nanocrystalline, non-annealed Li2S:LiI, the MAS NMR response is characterized by a broad distribution of NMR lines showing chemical shifts between that of pure Li2S and LiI, hence pointing to the formation of solid-solution like regions.Ion dynamics on different length scales was probed with variable-temperature, potentiostatic conductivity spectroscopy as well as solid-state NMR spin-lattice relaxation (SLR) measurements. Defect-rich nanocrystalline Li2S:LiI has to be characterized by an overall conductivity that is 2 orders of magnitude higher as compared to that of the microcrystalline, annealed reference sample. SLR NMR experiments supports this result and reveal lower activation energies for both the fast local hopping ion dynamics and long-range ion diffusivity in the sample directly obtained after ball milling. Finally, mixing-time dependent 6Li 2D exchange NMR spectroscopy reveals even (very) slow Li+ exchange between the Li2S-rich and LiI-rich regions in the nanocrystalline sample. Off-diagonal intensities are especially seen for mixing times longer than 80 ms.

Nuclear magnetic resonance and molecular simulation study of H2 and CH4 adsorption onto shale and sandstone for hydrogen geological storage

Understanding pure H2 and H2/CH4 adsorption and diffusion in earth materials is one vital step toward a successful and safe H2 storage in depleted gas reservoirs. Despite recent research efforts such understanding is far from complete. In this work we first use Nuclear Magnetic Resonance (NMR) experiments to study the NMR response of injected H2 into Duvernay shale and Berea sandstone samples, representing materials in confining and storage zones. Then we use molecular simulations to investigate H2/CH4 competitive adsorption and diffusion in kerogen, a common component of shale. Our results indicate that in shale there are two H2 populations, i.e., free H2 and adsorbed H2, that yield very distinct NMR responses. However, only free gas presents in sandstone that yields a H2 NMR response similar to that of bulk H2. About 10 % of injected H2 can be lost due to adsorption/desorption hysteresis in shale, and no H2 loss (no hysteresis) is observed in sandstone. Our molecular simulation results support our NMR results that there are two H2 populations in nanoporous materials (kerogen). The simulation results also indicate that CH4 outcompetes H2 in adsorption onto kerogen, due to stronger CH4-kerogen interactions than H2-kerogen interactions. Nevertheless, in a depleted gas reservoir with low CH4 gas pressure, about ∼30 % of residual CH4 can be desorbed upon H2 injection. The simulation results also predict that H2 diffusion in porous kerogen is about one order of magnitude higher than that of CH4 and CO2. This work provides an understanding of H2/CH4 behaviors in deleted gas reservoirs upon H2 injection and predictions of H2 loss and CH4 desorption in H2 storage.

Study of nuclear magnetic resonance response mechanism in shale oil and correction of petrophysical parameters

Shale oil reservoirs, characterized by a low porosity, complex mineral composition, and heterogeneity of organic matter distribution, are common unconventional oil and gas reservoirs. Nuclear magnetic resonance (NMR) methods have great potential for the evaluation of petrophysical parameters in porous rocks. However, it is challenging to characterize the petrophysical properties of shale oil due to the complex mineral composition and heterogeneity of organic matter distribution. In this paper, a new NMR relaxation theory for shale was proposed for the first time, and the frequency dependencies of transverse surface relaxivity and internal magnetic field gradient for pore fluids were presented. The accuracy was verified by the extraction experiments, gas chromatography experiments, and multi-frequency NMR experiments for the first time. These experiments were also utilized to determine the transverse surface relaxivity and the transverse bulk relaxation time. Subsequently, the effects of the pyrite and clay minerals on shale oil T2 distributions at different instrument frequencies were analyzed with random walk simulations based on digital core technology for the first time. The results show the echo spacing, instrument frequency, pyrite content, and clay minerals are important parameters affecting the NMR response. Compared with the oil in organic pore, these factors have a greater impact on the NMR response characteristics for water in inorganic pore. When the content of pyrite is 5.3 % and the echo spacing is 0.2 ms, the numerical simulation results show that the NMR porosity of water in inorganic pore is 65.3 %, 12.3 %, and 1.6 % of the real porosity at the instrument frequencies (IF) of 2 MHz, 21.36 MHz, and 200 MHz, respectively. When chlorite with high magnetic susceptibility exists near the formation pores, it can also affect the NMR response of shale oil. The results show the effects of these factors on porosity and T2ML are non-negligible. The cross-plots of petrophysical parameters correction from shale oil T2 distributions were established for the first time. This work provides a theoretical guide for the NMR-based shale oil evaluation, which may be helpful for petrophysical parameter conversion between downhole and laboratory NMR instruments.

Simulation of nuclear magnetic resonance response based on 3D CT images of sandstone core

In recent years, nuclear magnetic resonance (NMR) logging has become increasingly prevalent in the characterization of rock properties such as porosity, permeability, saturation, and pore size distribution. However, interpreting such properties accurately from NMR logging data is challenging for some reservoirs. In particular, the impact of salinity, viscosity, and saturation on NMR measurements is not always clear, which can lead to inaccuracies in the resulting data interpretation. Properly accounting for these factors is essential in order to obtain accurate and reliable measurements for effective characterization of subsurface formations. This study utilized a random walk technique to simulate the NMR response of homogeneous sandstones using 3D CT images and conducted a sensitivity analysis under various salinity, crude oil viscosity, and water saturation conditions. The results indicate that the T2 relaxation time slightly shifts toward the short relaxation direction as the salinity of the formation water increases. In addition, longer echo intervals result in a more significant forward shift in the T2 value than shorter intervals. Whereas, for crude oil, the T2 relaxation time becomes shorter as its viscosity increases. Furthermore, the effect of echo interval on the forward T2 shift is less pronounced for crude oil than it is for formation water. Under water wet conditions, the T2 spectrum of crude oil exhibits a peak at the volume relaxation position. As the water saturation decreases, the left two peaks in the T2 spectrum shift toward shorter relaxation times. Under oil wet conditions, the T2 spectrum exhibits a complex three-peak structure. The method provides a physical basis for interpreting NMR macroscopic responses, and the simulated NMR responses can help identify fluids in reservoirs.

An NMR-assisted laboratory investigation of coal fines migration in fracture proppants during single-phase water production

Proppants are injected with the fracturing fluid to keep the hydraulic fractures open. However, deposition of coal fines in the void spaces between proppants significantly damage flow conductivity of the fractures. In this study, we experimentally model coal fines migration in a proppant pack. Standard quartz sand (16–20 mesh) is used to prepare the proppant pack. The proppant pack is installed within a low-field Nuclear Magnetic Resonance (NMR) facility to record NMR response before and after the experiment of fines suspension injection. The injected suspension consists of water with 500 ppm concentration of coal fines of radius from 2.8 to 142.9 µm. Coal fines are generated by crushing an anthracite coal sample. The permeability is damaged significantly by about 41% after 80 pore volume injection. NMR response suggests that volume of the large-size pores (radius rp > 60 um) decreases while that of the medium-size pores (0.9 um <rp < 60 um) increases. The pore structure change is caused by two possible mechanisms: (a) reducing pore size by fines occupying pore space and (b) developing inter-particulate pore space of fines gathering at the damaged pores. Although the fines size (radius from 2.8 to 142.9 um) is significantly smaller than the pore size (<1005.2 um), the large-size pores can still be damaged by the fines. The results of this study can help to understand mechanisms of fines migration and conductivity evolution in/of the hydraulic fractures during Coal Seam Gas production.

Monitoring fluid migration using in-situ nuclear magnetic resonance core flooding system integrated with fiber optic sensors: A proof of concept

In-situ nuclear magnetic resonance (NMR) core flooding system has enabled researchers to monitor several rock properties such as porosity, pore size distribution, and fluid saturation along the tested samples with high resolutions and under reservoir conditions. However, spatially resolved rock strength/mechanical property alteration coupled to fluid migration/substitution remains poorly characterized. To this end, Fiber Bragg Grating (FBG) multiplex sensors were integrated with NMR core flooding system to monitor rock strength changes, or generally speaking, to observe hydro-mechanical-chemical coupling mechanisms during core flooding tests. In this study, we present a novel approach on how to conduct core flooding experiments, while simultaneously monitoring NMR and FBG strain response of the tested limestone plug. The NMR cell was modified to integrate FBG technology without impeding the NMR signal and core flooding high pressure/temperature capacity. A high spatial resolution optical fiber was attached onto the sample radial surface. The results show the successful association of NMR and FBG sensors to track any change at each stage of brine injection. The FBG is capable of measuring the rock strain variations induced by rock-fluid interactions during brine injection, allowing it to capture the fluid front location along with the sample and at a faster rate than the NMR.

Study on the logging response characteristics and the quantitative identification method of solid bitumen at different thermal evolution stages

Solid bitumen is the intermediate products during the oil and gas generation, and widely exists in petroliferous basins all over the world. Besides damaging the reservoir physical properties, solid bitumen affects the logging parameters and is hard to be identified by the conventional logging method. In this study, two different thermal evolution stages of solid bitumen, separately from the Devonian outcrop profile and the Well ST3 in the northwestern Sichuan Basin, are taken as an example. Through a series of analyses on the porosity, permeability, resistivity, S-wave time difference, P-wave time difference and nuclear magnetic resonance (NMR) before and after bitumen dissolution, the logging response characteristics of solid bitumen at different thermal evolution stages are clarified, and the logging quantitative identification method of solid bitumen is established. The results are as below: (1) The solubility of solid bitumen is linearly correlated with the increment of porosity, permeability, P-wave time difference and S-wave time difference, and exponentially correlated with the decrement of resistivity. (2) Under the equal solid bitumen content and with the increase of thermal evolution, the influence of solid bitumen on porosity and permeability gradually decreases, while the influence on acoustic time difference and resistivity gradually increases. (3) Two kinds of NMR logging interpretation models for bitumen reservoir are established based on the NMR response characteristics of solid bitumen at different thermal evolution stages. The solid bitumen from low thermal evolution stage has a strong response in NMR, while that from high thermal evolution stage is otherwise. The Peak 1 (0.1 ms – 10 ms) of the T2 spectrum can respond to most of the low thermal evolution stage solid bitumen, but just a few of the high thermal evolution stage solid bitumen. (4) The NMR logging quantitative calculation methods on different thermal evolution stage solid bitumen are established respectively to solve the difficult issues of quantitative identification of solid bitumen. All the researches above have important guiding significance for the logging quantitative calculation of solid bitumen and the selection of effective oil/gas test layers.

Pore throat characterization of bioturbated heterogeneous sandstone, Bhuj Formation, Kachchh India: An integrated analysis using NMR and HPMI studies

Nuclear magnetic resonance (NMR) relaxometry and high-pressure mercury intrusion (HPMI) are substantially utilized techniques to characterize the inherent heterogeneity of reservoirs. Bioturbation is one such type of microscale heterogeneity that provides challenges to optimal recovery planning and volumetric estimation of hydrocarbon reserves. A comprehensive approach is determined by acknowledging the applicability and limitation of each method. Due to the wide variation in petrophysical properties resulting from the effect of bioturbation, the sample size ranges from mm to cm; hence, a proper methodology needs to be formulated. The present study extends the available method of generating pseudo Pc curves from NMR studies to analyze the effect of multiscale bioturbation heterogeneity. The samples were chosen from two different classes on a bioturbation scale referred to as the bioturbation index (BI) ranging from 0 to 6, 0 being 0% bioturbation and 6 meaning 100% bioturbation. The results indicate that lower BI samples had unimodal behavior, while the higher BI sample had bimodal characteristics in pore network distribution. Increased anisotropy was evident in the higher BI samples, and the HPMI study revealed a contrasting nature of pore throat connectivity with a lower threshold and displacement pressure and an increased median throat diameter in the bioturbated part compared with the nonbioturbated. The bioturbated volume essentially had better and less tortuous pore throat connectivity. The effects of bioturbation were identifiable in a core-scale study using NMR. The bimodal characteristic behavior with two distinct pore throat classes with the larger throat class as dominant claims the bioturbation-assisted pore throat connectivity established in them. The purpose of the paper is to investigate pore throat distribution in bioturbated or heterogeneous reservoirs by integrating NMR and HPMI methods. This study proposes a method that can correlate NMR responses from logging into pore throat distribution in bioturbated zones of the reservoir.

A laboratory study of the effect of clay, silt, and sand content on low-field nuclear magnetic resonance relaxation time distributions

We have developed a laboratory nuclear magnetic resonance (NMR) study to investigate the effect of clay, silt, and sand content on the NMR relaxation time distribution. Transverse NMR relaxation times ([Formula: see text]) are determined for water-saturated unconsolidated sediment mixtures of 1%–60% kaolinite clay, 5%–85% silt-size glass beads, and 8%–94% quartz sand by mass. Nearly all of the mixtures are characterized by a unimodal [Formula: see text] distribution. When clay is present in quantities greater than 10%, the clay content dominates the response. For these samples, the mean-log relaxation times ([Formula: see text]) range from 0.03 to 0.06 s, regardless of silt or sand content. For mixtures with [Formula: see text] clay, [Formula: see text] decreases with increasing clay content. When the clay content is kept the same, [Formula: see text] decreases with increasing silt content and increases with the increasing sand content. The strong effect of the clay content on the NMR response is due to the high specific surface area of the clay and the distribution of clay throughout the samples. These results will help improve the interpretation of NMR field data in soils and unconsolidated sediments.

19 F NMR Illustrates Novel Aspects of Cytochrome P450 Systems

Understanding conformational dynamics is an integral part of understanding function in cytochrome P450 enzymes (CYPs), a ubiquitous class of heme-coordinated enzymes that are important for xenobiotic and endogenous metabolism. While nuclear magnetic resonance (NMR) is well suited to detect changes in the structures of CYPs and their associated redox partners, use of traditional isotopic labels are difficult to apply to such large enzymes and complexes. In this work, we have employed a thiol-reactive 19F label, 3-bromo-1,1,1-trifluoracetone (BTFA), to probe various aspects of Class-I CYP systems in a targeted approach. 19F is well suited for these studies due in part to its enhanced sensitivity over traditional NMR observable nuclei, as well as the fact that it does not naturally occur in proteins, which reduces the overall complexity of the resulting spectra. Here we deploy this strategy to study different aspects of CYP function, including details of redox partner interaction in a mammalian CYP and dynamics of substrate binding in a bacterial CYP. Our lab has previously used traditional 15N NMR to study the interaction between the vitamin D metabolizing enzyme, CYP24A1, and its redox partner, adrenodoxin (Adx). Using labeled Adx, we were able to titrate unlabeled CYP24A1 and monitor changes in the spectra, but were limited by the extent of signal loss attributed to the size of the complex. Substituting 15N labeling with two selectively placed 19F probes on α-helix 1 and α-helix 3 of Adx, we were able to probe biologically relevant complexes of these enzymes. Upon addition of CYP24A1 to 19F labeled Adx, we observe differential line broadening on α-helix 3, consistent with other studies implicating this region in CYP recognition. We also observe changes in the heterogeneity of the signal at α-helix 3, suggesting that this site undergoes conformational selection upon binding. The same probe was also applied to study the solution structure of CYP121 from Mycobacterium tuberculosis. Crystal structures of CYP121 show ligands clustered to a pocket near the F-G helices, which may play an important role in substrate recognition and control access to the active site. A probe was attached to the loop connecting these two helices (FG-loop) and monitored during titration with the substrate, cyclodityrosine (cYY). The 19F NMR spectrum for the FG-loop is heterogeneous suggesting multiple conformations exist in solution, but converges to a single peak upon cYY addition, representing a bound form. Utilizing an engineered monomer, our data also suggest that the dimer interface confers structural rigidity at this site, and in the dimeric form a population of enzyme exists in the ‘bound’ conformation prior to ligand introduction. Interestingly, the ratios of CYP121:cYY that are required to saturate the observed NMR response do not match with ratios required to detect binding using other techniques, thereby suggesting the 19F probe on the FG-loop is monitoring a ‘pre-catalytic’ binding event. These findings highlight the utility of employing an underutilized NMR label to understand function in an important class of enzymes.

Pore-Structure Characterization of a Complex Carbonate Reservoir in South Iraq Using Advanced Interpretation of NMR Logs

The Rumaila Field is in southeast Iraq and contains multiple reservoir intervals, including the Upper Cretaceous Mishrif carbonate reservoir, one of the major reservoirs in the world, that has been producing for more than 50 years. One of the key challenges in the Mishrif is to characterize the pore-structure distinction between primary and secondary porosity. The secondary porosity in the form of large pores, if present, dominates the petrophysical properties, especially permeability. Advanced logs, e.g., nuclear magnetic resonance (NMR) and image logs, can be used to understand the variations in pore structure, both qualitatively and quantitatively. In this paper, we focused primarily on four new wells with very comprehensive logging and coring programs. NMR logs were acquired using different tools and pulse sequences. This resulted in uncertainty in porosity and T2 distributions and, consequently, complications in the NMR interpretation. We observed two key issues: porosity deficit due to lack of polarization and T2 distribution truncation due to the low number of echoes. We used a single pore model to reproduce the NMR response in different pore sizes and fluid types for different pulse sequences. The results showed that the NMR response, especially in water-filled (water-based-mud filtrate) large pores, is sensitive to polarization time, echo spacing, and tool gradient strength. NMR log data confirmed the modeling results. We recommended an optimum pulse sequence and tool characteristics to fully capture the heterogeneous rock and fluid system in this carbonate reservoir. NMR logs, when available, were the primary tools to identify the large pores. We present a consistent workflow for NMR log analysis that was developed to identify and quantify large pores and extended to all wells in the field. We used advanced NMR interpretation techniques, e.g., factor analysis (NMR FA) (Jain et al., 2013), in a series of oil wells drilled with water-based mud. Using factor analysis, we identified a cutoff value of 847 ms for large pore volumes. In this manuscript, we also present an integration of laboratory measurements, e.g., NMR, mercury intrusion capillary pressure (MICP) data, whole-core CT scanning, and thin-section analysis, in our interpretation workflow. We also compared the large pore volume from image logs with NMR logs and other laboratory data and observed very consistent results. All the available information was integrated to build an “NMR-based” petrophysical model for porosity, rock type, permeability, and saturation determination. The NMR-based model was very comparable with the classic flow zone indicator (FZI) rock typing. The results of this study were used to modify the NMR acquisition program in the field and to build a petrophysical model based on only NMR and image log measurements for carbonate reservoirs. In this paper, we will discuss NMR modeling and corresponding log data from various wells to confirm the results. Furthermore, we will present a novel interpretation workflow integrating laboratory measurements and log data, which led to the modification of the NMR acquisition program in the field and the creation of a data-driven petrophysical model based on only NMR and image log measurements for carbonate reservoirs.

Numerical investigating the low field NMR response of representative pores at different pulse sequence parameters

We developed a numerical simulation algorithm to explore the nuclear magnetic resonance (NMR) response of the porous media based on the Carr-Purcell-Meiboom-Gill (CPMG) pulse sequence and the Bloch equation. The evolution of the magnetization vector of two representative pores at different pulse properties, including the excitation angle, the refocusing angle, the phase angle, as well as the pulse duration are simulate to understand the NMR relaxation signals. The result showed that the normalized magnetization is symmetrical with the excitation angle and positive with the T2 spectrum's amplitude when the excitation angle is less than 90°. In additional, the refocusing angle has no clear influence on the NMR response. The phase angle of the excitation pulse is inversely correlated with the echo amplitude and can be neglected when the value is lower than 15°. The phase angle of the refocusing pulse causes the zig-zag phenomenon, but the response of the even echoes is not disturbed. Moreover, the influence of the pulse duration should not be neglected at higher values, particularly for the mesopore. The simulation results are helpful for the design and optimization of the pulse sequence, and the data manipulation of the measured signals.

NMR-Based Study of the Pore Types’ Contribution to the Elastic Response of the Reservoir Rock

Seismic data and nuclear magnetic resonance (NMR) data are two of the highly trustable kinds of information in hydrocarbon reservoir engineering. Reservoir fluids influence the elastic wave velocity and also determine the NMR response of the reservoir. The current study investigates different pore types, i.e., micro, meso, and macropores’ contribution to the elastic wave velocity using the laboratory NMR and elastic experiments on coal core samples under different fluid saturations. Once a meaningful relationship was observed in the lab, the idea was applied in the field scale and the NMR transverse relaxation time (T2) curves were synthesized artificially. This task was done by dividing the area under the T2 curve into eight porosity bins and estimating each bin’s value from the seismic attributes using neural networks (NN). Moreover, the functionality of two statistical ensembles, i.e., Bag and LSBoost, was investigated as an alternative tool to conventional estimation techniques of the petrophysical characteristics; and the results were compared with those from a deep learning network. Herein, NMR permeability was used as the estimation target and porosity was used as a benchmark to assess the reliability of the models. The final results indicated that by using the incremental porosity under the T2 curve, this curve could be synthesized using the seismic attributes. The results also proved the functionality of the selected statistical ensembles as reliable tools in the petrophysical characterization of the hydrocarbon reservoirs.

A numerical study of field strength and clay morphology impact on NMR transverse relaxation in sandstones

Nuclear magnetic resonance (NMR) relaxometry is a common technique for the petrophysical characterization of sedimentary rocks. The standard interpretation of NMR transverse relaxation responses is based on the assumptions of the fast diffusion limit, dominant surface relaxation, and weak coupling between pores, allowing an interpretation of the NMR response as pore size distribution. In general, three asymptotic relaxation regimes can be defined by comparing dephasing, structural and diffusion length scales. The shortest length scale defines the dominating relaxation regime, which is either the free diffusion, motional averaging, or localization regime. Complex mineralogy and morphology of rocks, especially due to clay minerals, may lead to the co-existence and coupling of multiple relaxation regimes in the presence of surface relaxivity heterogeneity and internal gradient effects.In this work the relationship between morphology of rocks, strength of applied magnetic field, resulting relaxation regimes and observed NMR relaxation responses is studied numerically. Limitations in the discretization of clays typical for micro-CT images are addressed by introducing a fine-scale kaolinite model based on SEM images. The model is utilized to evaluate the field-dependent mean transverse relaxation time and effective diffusion coefficient of clay regions. These effective parameters are incorporated into random-walk simulations on micro-CT images. Relaxation regimes are analysed spatially for three different types of sandstone as function of external magnetic field strength. Increase of paramagnetic clay content, field strength and echo-time increases the fraction of spins relaxing in the localization regime within macro-pores, typically being localised in the regions neighbouring clay pockets and grain surfaces. We demonstrate that a significant contribution of the localization regime to relaxation may lead to incorrect predictions of pore-size distributions and fluid typing. The prefactor of permeability correlations varies significantly due to clay effects. Accounting for these effects should enable more robust petrophysical interpretations.

Surface-to-Underground Nuclear magnetic Resonance Detection of Aquifer

The water hazard is one of the major accidents in coal mines. The existing geophysical exploration methods do not meet the precise requirements for exploration accuracy. Nuclear magnetic resonance (NMR) is currently the only geophysical method that can directly detect groundwater. This paper firstly introduces the basic principles and working methods of surface-to-underground NMR, and then gave the NMR response of the uniform earth excited by a circular loop source, at last, the NMR responses of some aquifers at different depths were simulated by the numerical modeling. The response for the observation underground is higher than that on the surface, which shows that the surface-to-underground NMR can increase the detection depth.

Reconstruction and Analysis of Tight Sandstone Digital Rock Combined with X-Ray CT Scanning and Multiple-Point Geostatistics Algorithm

Unconventional rocks such as tight sandstone and shale usually develop multiscale complex pore structures, with dimensions ranging from nanometers to millimeters, and the full range can be difficult to characterize for natural samples. In this paper, we developed a new hybrid digital rock construction approach to mimic the pore space of tight sandstone by combining X-ray CT scanning and multiple-point geostatistics algorithm (MPGA). First, a three-dimensional macropore digital rock describing the macroscopic pore structure of tight sandstone was constructed by micro-CT scanning. Then, high-resolution scanning electron microscopy (SEM) was performed on the tight sandstone sample, and the three-dimensional micropore digital rock was reconstructed by MPGA. Finally, the macropore digital rock and the micropore digital rock were superimposed into the full-pore digital rock. In addition, the nuclear magnetic resonance (NMR) response of digital rocks is simulated using a random walk method, and seepage simulation was performed by the lattice Boltzmann method (LBM). The results show that the full-pore digital rock has the same anisotropy and good connectivity as the actual rock. The porosity, NMR response, and permeability are in good agreement with the experimental values.