Open Access Open Access  Restricted Access Access granted  Restricted Access Subscription Access

Vol 49, No 7 (2018)

Original Paper

Effect of NaCl Solution on Swelling Characteristics of Bentonite with Different Diffuse Double Layers

Yu H., Sun D., Gao Y.

Abstract

Soil particles generally possess negative ions, and form an electronic field nearby the particles, which results in generating diffuse double layers on the surface of the particles. There is no diffuse double layer at dry state, and it develops diffuse double layers first when wetted by solution. This paper investigates the effect of NaCl solution on swelling characteristics of bentonite with different initial water contents by performing a series of wetting tests. The wetting test results indicate that when the initial water content is less than 10%, the NaCl solution has no effect on the swelling. When the initial water content is larger than 10%, the swelling strain decreases with increase in the NaCl solution concentration. The nuclear magnetic resonance (NMR) tests on compacted bentonite specimens were performed. The test results indicate that the strongly bound water content is 10%, which is similar to that by other method. The NMR tests on full wetting specimens, whose initial water content is less than 10%, show that the NaCl solution has no effect on NMR tests results. When the initial water content is larger than 10%, the proportion of curves from the NMR tests decreases with increase in the NaCl solution concentration. The NMR tests results indicate that the swelling occurred mainly in the intra-aggregate rather than in the inter-aggregate.

Applied Magnetic Resonance. 2018;49(7):725-737
pages 725-737 views

Exploring the Limits of Overhauser Dynamic Nuclear Polarization (O-DNP) for Portable Magnetic Resonance Detection of Low γ Nuclei

Yoder J.L., Magnelind P.E., Espy M.A., Janicke M.T.

Abstract

Nuclear magnetic resonance (NMR) spectroscopy in portable, permanent magnet-based spectrometers is primarily limited to nuclei with higher gyromagnetic ratio, γ, such as 1H, 19F, and 31P due to the limited field strength achievable in these systems. Overhauser effect dynamic nuclear polarization (O-DNP), which transfers polarization from an unpaired electron to a nucleus by saturating an electron paramagnetic resonance transition with an oscillating radio frequency magnetic field, B1e, can increase the polarization of low γ nuclei by hundreds or even thousands, enabling detection in a portable system. We have investigated the potential for O-DNP to enhance signals using (4-amino-2,2,6,6-tetramethylpiperidin-1-yl)oxyl (TEMPO hereafter) as a source of unpaired electrons in a homebuilt ultra-low field (ULF) O-DNP-NMR spectrometer. We have found, in general, that larger concentrations of TEMPO are required for effective O-DNP with low γ nuclei, which has a number of important effects. Spin exchange effects cause the EPR lines to overlap and ultimately merge at high concentrations of TEMPO, fundamentally increasing the maximum possible enhancement, while the electron–electron dipolar interaction reduces both longitudinal and transverse relaxation times for the electrons, dramatically increasing the required B1e strength. The relationship between TEMPO concentration, B1e magnitude and O-DNP enhancement is quantified, and strategies for achieving these fields are discussed.

Applied Magnetic Resonance. 2018;49(7):707-724
pages 707-724 views

Flowing Liquids in NMR: Numerical CFD Simulation and Experimental Confirmation of Magnetization Buildup

Kespe M., Förster E., Nirschl H., Guthausen G.

Abstract

Process and reaction monitoring by nuclear magnetic resonance (NMR) spectroscopy has attracted considerable attention in the last years not only because of the new generation of low-field NMR spectrometers, but also because of an industrial need of more effectivity and process optimization via real-time monitoring of process and reaction details by diverse analytical tools. Most often, bypass solutions are realized in liquid state monitoring, which leads to questions of residence time distribution, mixing phenomena and accuracy of concentration determination. Exploring chemical engineering knowledge of fluid dynamics and combining it with NMR knowledge of magnetization buildup allow the calculation of magnetization in NMR measurements on flowing substances. This approach reveals the essential parameters to be considered when constructing flow cells and when processing data in NMR process monitoring. 3D computational fluid dynamics combined with Bloch equations allows detailed time and spatially resolved insights into the significant mechanisms of magnetization distribution and opens up new possibilities for experiment design in flow NMR. An experimental confirmation was provided by MRI experiments.

Applied Magnetic Resonance. 2018;49(7):687-705
pages 687-705 views

31P MRS Study of Hyperbaric Oxygenation Effects on Phosphate Metabolism of Normal Human Brain

Manzhurtsev A.V., Vasiukova O.R., Sergeeva V.V., Zaitseva N.L., Menshchikov P.E., Melnikov I.A., Akhadov T.A., Semenova N.A.

Abstract

For the first time, the effects of one hyperbaric oxygenation (HBO) session on cellular phosphate metabolite levels and pH were investigated in vivo. 31P magnetic resonance spectroscopy was used in this study. The optimized protocol of Image-Selected Invivo Spectroscopy pulse sequence for 31P MRS was applied to increase SNR of ATP resonances. An activation of energy metabolism that manifested in the decrease of creatine phosphate and pHint after an HBO session is revealed. The growth of the α-ATP signal is elucidated as well, while other ATP resonances remain unchanged. This might reflect the increase in nicotinamide adenine dinucleotide (NAD) concentration. The rise of its level as well as the detected creatine phosphate expenses immediately after HBO may denote the activation of fast NAD synthesis pathways.

Applied Magnetic Resonance. 2018;49(7):679-686
pages 679-686 views

Rock-Type Definition and Pore Characterization of Tight Carbonate Rocks Based on Thin Sections and MICP and NMR Experiments

Tian F., Wang W., Liu N., Jiang J., Niu C., Zhang Y., Li Y.

Abstract

Thick tight Ordovician carbonate rocks are present at depths exceeding 5300 m in the Tahe oilfield and their matrix is considered to contain no storage space. An integrated petrographical and petrophysical study was conducted on a set of 25 tight carbonate core samples from Ordovician strata, covering a wide range of lithologies and textures. Six carbonate rock types were characterized by integrating both petrographical and petrophysical data, including thin-section observations and porosity, permeability, mercury injection capillary pressure and nuclear magnetic resonance (NMR) measurements. We found that thick grainstone and limestone with half-filled fractures exhibited good reservoir properties. NMR testing is an invaluable tool for characterizing pore structures in tight carbonate rocks. For example, six rock types can be identified from the NMR T2 distributions and the changes in pore volume under different pressures (up to 20 MPa) can be calculated. NMR technology can be used to perform rapid and accurate rock-type identification and pore network evaluation in tight carbonate rocks. The results provide an experimental foundation for NMR logging interpretations and advance the understanding of geological and geophysical characteristics of ultra-deep carbonate reservoirs.

Applied Magnetic Resonance. 2018;49(7):631-652
pages 631-652 views

Peculiarity of the Nuclear Magnetic Resonance Method Application for the Liquid Medium Flow Parameters Control

Davydov V.V., Dudkin V.I., Vysoczkiy M.G., Myazin N.S., Rud’ V.Y.

Abstract

The new peculiarities that arise when using nuclear magnetic resonance (NMR) method for liquid medium stream control are identified and investigated. Signal/noise ratio can be increased fivefold when these peculiarities are taken into account in design of NMR spectrometers. It made it possible first time ever to register NMR absorption spectra from different flowing media and to determine relative concentrations of paramagnetic ions by using these spectra. The increase of signal/noise ratio also allowed measuring longitudinal T1 and transverse T2 relaxation times in flowing media with error rate that does not exceed 0.5%, while in previous NMR spectrometer designs T1 and T2 measurement error rates were greater than 1.0%. The simultaneous use of the absorption spectra and the measured values of the relaxation constants T1 and T2 allows eliminating errors completely when determining flowing medium condition. This is especially important when working with medical suspensions and biological solutions. The results of the experimental investigations of liquid media flows are presented below.

Applied Magnetic Resonance. 2018;49(7):665-678
pages 665-678 views

Enzymatic Activity Prediction Using Time-Domain Nuclear Magnetic Resonance (TD-NMR) and Multivariate Analysis: A Case Study Using Cassava Roots

da Silva Ferreira J., Moraes T.B., Colnago L.A., Pereira F.M.

Abstract

Time-domain nuclear magnetic resonance (NMR) has been widely used in food science. In this work, we demonstrate that the NMR decay obtained with the Carr–Purcell–Meiboom–Gill (CPMG) sequence can be used to estimate the peroxidase activity (PA) in cassava roots. This enzyme has been involved in post-harvest physiological deterioration (PPD), which limits the storage of fresh cassava to a few days. Cassava is a staple food for almost one billion people in tropical areas in Americas, Africa and Asia. A multivariate method using CPMG data and reference values of PA from a standard biochemical assay was built with 216 measurements for non-refrigerated and refrigerated samples of cassava roots. The figures of merit of the global partial least squares model using both types of roots showed a 0.06 μmol min−1 limit of detection (LOD) and a 0.2 μmol min−1 limit of quantification (LOQ) for PA, with 0.4 [intensity (a.u.)/(μmol min−1)] sensitivity and a standard error of cross-validation (SECV) of 0.7 μmol min−1. All of the results demonstrated that TD-NMR has the potential to predict PA in cassava roots that is indicative of the PPD problem.

Applied Magnetic Resonance. 2018;49(7):653-664
pages 653-664 views