Application of a custom-built, 400 MHz NMR probe on Eagle Ford Shale core plug samples, Gonzales and La Salle counties, Texas

Abstract

Nuclear magnetic resonance (NMR) has become an increasingly important tool for estimating porosity, permeability, and fluid characteristics in oil and gas reservoirs since its introduction in the 1950s. While NMR has become common practice in conventional reservoirs, its application is relatively new to unconventional reservoirs such as the Eagle Ford Shale. Porosity and permeability estimates prove difficult in these exceptionally tight rocks and are routinely below the detection limit and/or resolution of low frequency (2 MHz or less) NMR. High frequency (400 MHz) NMR has been applied to address these issues; however, previous studies have been limited to crushed rock samples or millimeter-sized core plugs. In response, a custom-built NMR probe has been constructed, capable of measuring 0.75-inch diameter, 0.45-inch length core plugs at 400 MHz, to determine if larger core plug sizes yield higher resolution T2 distributions in the Eagle Ford Shale. The tool is composed of two primary elements, the structural framework and the radio frequency circuit. Each element was designed and constructed iteratively to test various layouts while maintaining functionality. The probe's structural design was initially based on retired, commercial probes then modified to operate within a Bruker Ascend 400WB NMR spectrometer. Designs were drafted and 3D-printed multiple times to determine proper physical dimensions and clearances. Once designs were deemed satisfactory, structural components were manufactured and assembled to create the structural framework. A radio frequency circuit was then built to measure T2 distributions at the desired frequency and sample size. Multiple inductor designs and capacitor combinations were tested until a stable circuit, capable of matching impedance and tuning to the proper frequency, was achieved. The probe's stability and data quality were then confirmed by measuring the NMR spectra of deuterated water in a Teflon container. The NMR probe was validated by comparing high frequency (400 MHz) data acquired in-house to low frequency (2 MHz) data measured at a commercial laboratory. Twelve core plugs (0.75-inch diameter, 1-inch length) were cut from two Eagle Ford Shale subsurface cores located in Gonzales and La Salle counties, Texas. Low frequency T2 distributions were measured twice: first after drying core plug samples in a vacuum oven and again after spontaneous imbibition with various brine solutions (deionized water, 8 wt.% KCl, or 17.9 wt.% KCl) for one week. These contrasting saturation states were applied to highlight immovable water in the core plugs. For high frequency data measurements, samples were trimmed to 0.45-inch lengths to fit inside the newly-built NMR probe, leaving two sub-samples for each of the original core plugs. T2 distributions were first acquired "as-is" (e.g., without drying or imbibition). After as-is data acquisition, samples were dried in a vacuum oven then allowed to spontaneously imbibe the same brine solutions used in the low frequency study. T2 distributions were measured again after imbibition and compared to the low frequency data acquired by the commercial laboratory. Qualitatively, high frequency T2 distributions resemble low frequency data; however, the absolute T2 values are routinely higher by one order of magnitude. The difference may be caused by data acquisition, data processing, fluid-rock interactions, magnetic field inhomogeneities, or some combination thereof. In spite of not attaining the higher-resolution T2 distributions desired, the project still provides a proof-of-concept that T2 relaxation times can be measured in conventional-sized core plugs using 400 MHz NMR. Although limited in its outcomes, the study delivers promising results and elicits future research into utilizing high frequency NMR spectroscopy as a petrophysical tool for unconventional reservoirs.