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    Detecting Microbially Induced Calcite Precipitation in a Model Well-Bore Using Downhole Low-Field NMR
    (2017-02) Kirkland, Catherine M.; Zanetti, Sam; Grunewald, Elliot; Walsh, David O.; Codd, Sarah L.; Phillips, Adrienne J.
    Microbially induced calcite precipitation (MICP) has been widely researched recently due to its relevance for subsurface engineering applications including sealing leakage pathways and permeability modification. These applications of MICP are inherently difficult to monitor nondestructively in time and space. Nuclear magnetic resonance (NMR) can characterize the pore size distributions, porosity, and permeability of subsurface formations. This investigation used a low-field NMR well-logging probe to monitor MICP in a sand-filled bioreactor, measuring NMR signal amplitude and T2 relaxation over an 8 day experimental period. Following inoculation with the ureolytic bacteria, Sporosarcina pasteurii, and pulsed injections of urea and calcium substrate, the NMR measured water content in the reactor decreased to 76% of its initial value. T2 relaxation distributions bifurcated from a single mode centered about approximately 650 ms into a fast decaying population (T2 less than 10 ms) and a larger population with T2 greater than 1000 ms. The combination of changes in pore volume and surface minerology accounts for the changes in the T2 distributions. Destructive sampling confirmed final porosity was approximately 88% of the original value. These results indicate the low-field NMR well-logging probe is sensitive to the physical and chemical changes caused by MICP in a laboratory bioreactor.
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    NMR relaxation measurements of biofouling in model and geological porous media
    (2011-09) Codd, Sarah L.; Vogt, Sarah J.; Hornemann, Jennifer A.; Phillips, Adrienne J.; Maneval, James E.; Romanenko, K. R.; Hansen, L.; Cunningham, Alfred B.; Seymour, Joseph D.
    Recently 2D nuclear magnetic resonance (NMR) relaxation techniques have been able to access changes in pore structures through surface and diffusion based relaxation measurements. This research investigates the applicability of these methods for measuring pore and surface changes due to biofilm growth in various model porous systems and natural geological media. Model bead packs of various construction containing 100 lm borosilicate and soda lime glass beads were used to demonstrate how changes in the measured relaxation rates can be used to non-invasively verify and quantify biofilm growth in porous media. However significant challenges are shown to arise when trying to implement the same techniques to verify biofilm growth in a natural geological media.
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    Microbial and algal alginate gelation characterized by magnetic resonance
    (2012-10) Fabich, H. T.; Vogt, Sarah J.; Sherick, Matthew L.; Seymour, Joseph D.; Brown, Jennifer R.; Franklin, Michael J.; Codd, Sarah L.
    Advanced magnetic resonance (MR) relaxation and diffusion correlation measurements and imaging provide a means to non-invasively monitor gelation for biotechnology applications. In this study, MR is used to characterize physical gelation of three alginates with distinct chemical structures; an algal alginate, which is not O-acetylated but contains poly guluronate (G) blocks, bacterial alginate from Pseudomonas aeruginosa, which does not have poly-G blocks, but is O-acetylated at the C2 and/or C3 of the mannuronate residues, and alginate from a P. aeruginosa mutant that lacks O-acetyl groups. The MR data indicate that diffusion-reaction front gelation with Ca2+ ions generates gels of different bulk homogeneities dependent on the alginate structure. Shorter spin–spin T2 magnetic relaxation times in the alginate gels that lack O-acetyl groups indicate stronger molecular interaction between the water and biopolymer. The data characterize gel differences over a hierarchy of scales from molecular to system size.
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    NMR study comparing capillary trapping in Berea sandstone of air, carbon dioxide, and supercritical carbon dioxide after imbibition of water
    (2016-02) Prather, Cody A.; Bray, J. M.; Seymour, Joseph D.; Codd, Sarah L.
    Nuclear magnetic resonance (NMR) techniques were used to study the capillary trapping mechanisms relevant to carbon sequestration. Capillary trapping is an important mechanism in the initial trapping of supercritical CO2 in the pore structures of deep underground rock formations during the sequestration process. Capillary trapping is considered the most promising trapping option for carbon sequestration. NMR techniques noninvasively monitor the drainage and imbibition of air, CO2, and supercritical CO2 with DI H2O at low capillary numbers in a Berea sandstone rock core under conditions representative of a deep underground saline aquifer. Supercritical CO2 was found to have a lower residual nonwetting (NW) phase saturation than that of air and CO2. Supercritical CO2 behaves differently than gas phase air or CO2 and leads to a reduction in capillary trapping. NMR relaxometry data suggest that the NW phase, i.e., air, CO2, or supercritical CO2, is preferentially trapped in larger pores. This is consistent with snap-off conditions being more favorable in macroscale pores, as NW fluids minimize their contact area with the solid and hence prefer larger pores.
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    Recrystallization inhibition in ice due to ice binding protein activity detected by nuclear magnetic resonance
    (2014-09) Brown, Jennifer R.; Seymour, Joseph D.; Brox, T. I.; Skidmore, Mark L.; Wang, Chen; Christner, Brent C.; Luo, B. H.; Codd, Sarah L.
    Liquid water present in polycrystalline ice at the interstices between ice crystals results in a network of liquid-filled veins and nodes within a solid ice matrix, making ice a low porosity porous media. Here we used nuclear magnetic resonance (NMR) relaxation and time dependent self-diffusion measurements developed for porous media applications to monitor three dimensional changes to the vein network in ices with and without a bacterial ice binding protein (IBP). Shorter effective diffusion distances were detected as a function of increased irreversible ice binding activity, indicating inhibition of ice recrystallization and persistent small crystal structure. The modification of ice structure by the IBP demonstrates a potential mechanism for the microorganism to enhance survivability in ice. These results highlight the potential of NMR techniques in evaluation of the impact of IBPs on vein network structure and recrystallization processes; information useful for continued development of ice-interacting proteins for biotechnology applications.
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    In situ detection of subsurface biofilm using low-field NMR: A field study
    (2015-09) Kirkland, Catherine M.; Herrling, M. P.; Hiebert, Dwight Randall; Bender, A. T.; Grunewald, Elliot; Walsh, David O.; Codd, Sarah L.
    Subsurface biofilms are central to bioremediation of chemical contaminants in soil and groundwater whereby micro-organisms degrade or sequester environmental pollutants like nitrate, hydrocarbons, chlorinated solvents and heavy metals. Current methods to monitor subsurface biofilm growth in situ are indirect. Previous laboratory research conducted at MSU has indicated that low-field nuclear magnetic resonance (NMR) is sensitive to biofilm growth in porous media, where biofilm contributes a polymer gel-like phase and enhances T2 relaxation. Here we show that a small diameter NMR well logging tool can detect biofilm accumulation in the subsurface using the change in T2 relaxation behavior over time. T2 relaxation distributions were measured over an 18 day experimental period by two NMR probes, operating at approximately 275 kHz and 400 kHz, installed in 10.2 cm wells in an engineered field testing site. The mean log T2 relaxation times were reduced by 62% and 43%, respectively, while biofilm was cultivated in the soil surrounding each well. Biofilm growth was confirmed by bleaching and flushing the wells and observing the NMR signal’s return to baseline. This result provides a direct and noninvasive method to spatiotemporally monitor biofilm accumulation in the subsurface.
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    Biofilm detection in a model well-bore environment using low-field magnetic resonance
    (2015-09) Kirkland, Catherine M.; Hiebert, Dwight Randall; Phillips, Adrienne J.; Grunewald, Elliot; Walsh, David O.; Seymour, Joseph D.; Codd, Sarah L.
    This research addresses the challenges of the lack of non-invasive methods and poor spatiotemporal resolution associated with monitoring biogeochemical activity central to bioremediation of subsurface contaminants. Remediation efforts often include growth of biofilm to contain or degrade chemical contaminants, such as nitrates, hydrocarbons, heavy metals, and some chlorinated solvents. Previous research indicates that nuclear magnetic resonance (NMR) is sensitive to the biogeochemical processes of biofilm accumulation. The current research focuses on developing methods to use low-cost NMR technology to support in situ monitoring of biofilm growth and geochemical remediation processes in the subsurface. Biofilm was grown in a lab-scale radial flow bioreactor designed to model the near wellbore subsurface environment. The Vista Clara Javelin NMR logging device, a slim down-the-borehole probe, collected NMR measurements over the course of eight days while biofilm was cultivated in the sand-packed reactor. Measured NMR mean log T2 relaxation times decreased from approximately 710 to 389 ms, indicating that the pore environment and bulk fluid properties were changing due to biofilm growth. Destructive sampling employing drop plate microbial population analysis and scanning electron and stereoscopic microscopy confirmed biofilm formation. Our findings demonstrate that the NMR logging tool can detect small to moderate changes in T2 distribution associated with environmentally relevant quantities of biofilm in quartz sand.
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    Application of PFG-NMR to study the impact of colloidal deposition on hydrodynamic dispersion in a porous medium
    (2014-05) Fridjonsson, E. O.; Codd, Sarah L.; Seymour, Joseph D.
    Colloidal particulate deposition affects the performance of industrial equipment, reverse osmosis membranes and sub-surface contaminant transport. Nuclear magnetic resonance (NMR) techniques, i.e. diffusion, diffraction and velocity imaging, are used to study the effect deposited colloidal particulate have on the fluid dynamics of water inside a model porous medium. Specially prepared oil-filled hard-sphere particles allow monitoring of particulate accumulation via NMR spectroscopy. Evidence of preferential spatial deposition is observed after the initial colloidal particulate deposition. Loss of spatial homogeneity is observed through NMR diffraction, while observations of the probability distributions of displacement (propagators) indicate the formation of back-bone type flow. This paper presents unique dynamic NMR data for the non-invasive non-destructive investigation of fluid transport in opaque porous media experiencing colloidal deposition.
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