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Vol 48, No 1 (2017)

Original Paper

Molecular Mobility in Amorphous Polylactic Acid Studied Using 1H–13C Cross Polarization NMR

Kovaľaková M., Fričová O., Hutníková M., Olčák D., Chodák I.

Abstract

The 1H–13C cross polarization nuclear magnetic resonance technique was used for the study of molecular mobility in amorphous polylactic acid. The cross polarization buildup curves for methine and methyl functional groups measured at magic angle spinning rates of 4 and 10 kHz, under Hartmann–Hahn conditions determined from corresponding Hartmann–Hahn matching profiles, confirmed the presence of 1H–13C spin pairs isolated from lattice since transient oscillations were observed in the initial stages of buildup curves. The values of dipolar coupling constants derived from Fourier transforms of cross polarization buildup curves indicate the presence of rigid methine groups and two kinds of methyl functional groups which differ in mobility. This could be due to the presence of amorphous phase with chain aggregations and phase with less spatial restrictions in this material. Fitting of theoretical expressions to experimental data provided additional information on the cross polarization process in this material.

Applied Magnetic Resonance. 2017;48(1):23-33
pages 23-33 views

NMR Diffusion and Relaxation for Monitoring of Degradation in Motor Oils

Förster E., Nirschl H., Guthausen G.

Abstract

Different nuclear magnetic resonance (NMR) methods such as spectroscopy, diffusometry and relaxometry are applied with the aim to monitor motor oil degradation. Chemical degradation is detected by 1H NMR spectroscopy. With respect to quality control, low-field NMR is the established technique, which mostly uses relaxation and diffusion. Conventional methods such as mono-exponential data modeling lead to inadequate description of relaxation and diffusion data of complex fluids like motor oils. Inverse Laplace transform has difficulties in quantification, comparability and interpretation. Therefore, various data processing approaches are investigated to obtain the physico-chemically and numerically most correct description of the data. The gamma distribution model for diffusion and also for T1 and T2 relaxation data numerically describes the data with high accuracy. Three differently degraded motor oils were exemplarily investigated with regard to spectroscopic, relaxation and diffusion parameters.

Applied Magnetic Resonance. 2017;48(1):51-65
pages 51-65 views

Variable Temperature Single Crystal EPR Studies of Cu(II) in Dipotassium Diaquabis(Malonato-κ2O,O′) Nickelate Dihydrate: An Example of Contaminated Ground State

Natarajan B.

Abstract

Single crystal X-band electron paramagnetic resonance (EPR) studies on divalent copper ions embedded in dipotassium diaquabis(malonato-κ2O,O′) nickelate dihydrate have been performed at 300, 123 and 77 K to understand the nature of Jahn–Teller distortion in the paramagnetic host lattice. The angular variation of the EPR spectra reveals the presence of two sites, with one site not showing hyperfine resolution even at 77 K. The spin-Hamiltonian parameters of this six-coordinated Cu(II) ion, evaluated from EPR spectra at various temperatures, are:

  • 300 K: g11 = 2.125, g22 = 2.118, g33 = 2.290, no copper hyperfine resolution

  • 123 K: g11 = 2.229, g22 = 2.113, g33 = 2.319 and A11 = 5.02, A22 = 3.82, A33 = 6.87 mT

  • 77 K: g11 = 2.224, g22 = 2.114, g33 = 2.324 and A11 = 5.32, A22 = 3.90, A33 = 7.06 mT

respectively. The low value observed for A33 at 123 and 77 K has been explained by assuming a ground state \({\text{d}}_{{x^{2} - y^{2} }}\) wave function for Cu(II) ions, contaminated with the excited state \({\text{d}}_{{z^{2} }}\). From the temperature dependence of the EPR spectra, the Cu(II) ions can be considered as a static Jahn–Teller system, with contaminated ground state. The admixture coefficients and bonding parameters have also been calculated by combining EPR and optical data. The EPR spectrum of powder sample confirms single crystal data.

Applied Magnetic Resonance. 2017;48(1):35-50
pages 35-50 views

Brain Imaging with Slotted Hybridized Magnetic Metamaterial Hat at 7-T MRI

Ali H., Forsberg E., Jun H.

Abstract

Study of human pathologies and acquisition of anatomical images without any surgical intervention inside human body is possible because of magnetic resonance imaging (MRI), which is the keystone technique to characterize the psychology and neurochemistry of human body. However, for clinical trials, the study and cure of human diseases are followed by medical investigations of different animal anatomies. By employing different imaging techniques to animal anatomical models during their clinical trials yielded in exceptional image acquisition without any surgical invasion in the model, which resulted in noninvasive technique as compared to surgical invasion and opened the possibility to study human pathologies more precisely. This work exploits the notable properties of unique combination of multi-circular hybridized surface coils which can be used as hybridized magnetic metamaterial hat (HMMH). HMMH not only strengthens the uniformity of radio frequency (RF) rotational symmetry around its axis but also improves the signal-to-noise ratio (SNR) for rat’s brain imaging at 7-T MRI. We analyzed a periodic array of strongly coupled circular copper coils attached on circular coil shaped printed circuit board (PCB) substrate. In the design, some copper coils were inspired by the slot cavity loaded with parametric elements (capacitor and inductor). In addition, coils in the form of HMMH exploited the advantages of the hybrid modes which exhibited better and deeper RF sensitivity into the region of interest (ROI) as compared to single loop RF coil by exciting two Eigen modes simultaneously which resulted in homogenized magnetic field (B-field) and enhanced SNR at ROI. At resonance, the value of relative negative permeability, μr = −7 + j11 was achieved at 300 MHz for 7-T MRI. Furthermore, image quality at ROI was optimized by varying rat’s head position under magnetic resonance (MR) coil of MRI apparatus and in the presence or absence of HMMH. Design configuration and circuit model analysis were also done.

Applied Magnetic Resonance. 2017;48(1):67-83
pages 67-83 views

Magnetic Properties of Fe/Ni and Fe/Co Multilayer Thin Films

Ay F., Rameev B.Z., Basaran A.C., Kupriyanova G.S., Goikhman A.Y., Aktaş B.

Abstract

In this work, the magnetic and transport properties of Fe/SiO2/Ni and Fe/SiO2/Co multilayers grown on Si/SiO2 substrates have been studied. The samples have been prepared by two-stage deposition process. In the first stage, Fe layer and SiO2 interlayer of both samples are grown by ion beam deposition technique at room temperature. Then the samples are taken out to ambient atmosphere and loaded into a pulse laser deposition (PLD) chamber. Prior to the deposition of top layer, the samples are cleaned by annealing at 150 °C. In the second stage, Ni (or Co) layer is prepared by PLD technique at room temperature. The thickness of deposited layers has been measured by Rutherford back scattering (RBS). Magnetic properties of ferromagnetic bilayers have been investigated by room-temperature ferromagnetic resonance (FMR) and vibrating sample magnetometer (VSM) techniques. Standard four-point magneto-transport measurements at various temperatures have been performed. Two-step switching in the in-plane hysteresis loops of Fe/SiO2/Ni and Fe/SiO2/Co samples is observed. A crossing in the middle of hysteresis loops of both samples points to a weak antiferromagnetic interaction between the magnetic layers of the stacks. Saturation magnetization values have been obtained from the VSM measurements of samples with DC magnetic field perpendicular to the films surface. Magneto-transport measurements have shown the predominant contribution of anisotropic magnetic resistance both at room and low temperatures. FMR studies of Fe/SiO2/Ni and Fe/SiO2/Co samples have revealed additional non-uniform (surface and bulk SWR) modes, which behavior has been explained in the framework of the surface inhomogeneity model. An origin of the antiferromagnetic interaction has been discussed.

Applied Magnetic Resonance. 2017;48(1):85-99
pages 85-99 views

How Far can the Anisotropy Deviate from Uniaxiality in a Dy-Based Single-Molecule Magnet? Dinuclear Dy(III) Complex Study

Baniodeh A., Mondal A., Galeev R., Sukhanov A., Eremina R., Voronkova V., Anson C.E., Powell A.K.

Abstract

The DyIII ions in the dimer [Dy2(H2tea)2(O2CPh)4]·2H2O (1) (H3tea = triethanolamine) have the 9-coordinate monocapped square-antiprismatic ligand field environment. Compound 1 shows slow relaxation of magnetization which is observable only with applied magnetic fields. This is consistent with the idea that low-symmetry ligand fields allow for the quantum tunneling of magnetization. This is reflected by the fact that there are no observable maxima in the out-of-phase ac susceptibility above 1.8 K. The {g}-tensor of the DyIII ions {gx = 11, gy = 8.2, gz = 1} further underlying the reduced uniaxiality in this system was determined in electron paramagnetic resonance (X- and Q-band) studies of 1 at temperatures down to 4 K.

Applied Magnetic Resonance. 2017;48(1):101-113
pages 101-113 views

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