Structural role of fluoride in the ion-conducting glass system B(2)O(3)-PbO-LiF studied by single- and double-resonance NMR

The local structure of an ion-conducting glass with nominal composition 50B(2)O(3)-10PbO-40LiF has been investigated by complementary (7)Li, (11)B, (19)F, and (207)Pb single- and double-resonance experiments. The results give insight into the structural role of the lithium fluoride additive in borate glasses: (1) LiF is seen to actively participate in the network transformation process contributing to the conversion of three- into four-coordinate boron units, as shown by (11)B single-resonance as well as by (11)B{(19)F} and (19)F{(11)B} double-resonance experiments. (2) (19)F signal quantification experiments suggest substantial fluoride loss, presumably caused by formation of volatile BF(3). A part of the fluoride remains in the dopant role, possibly in the form of small LiF-like cluster domains, which serve as a mobile ion supply. (3) The extent of lithium-fluorine and lead-fluorine interactions has been characterized by (7)Li{(19)F} and (207)Pb{(19)F} REDOR and SEDOR experiments. On the basis of these results, a quantitative structural description of this system has been developed.

Evidence for magnetic phase separation in La(0.86)Sr(0.14)Mn(1-x)Cu(x)O(3+delta) manganites from NMR and magnetic measurements

Polycrystalline La(0.86)Sr(0.14)Mn(1-x)Cu(x)O(3+delta) (x = 0, 0.05, 0.10, 0.15, 0.20) manganites were investigated by means of magnetic measurements and zero-field (139)La and (55)Mn nuclear magnetic resonance (NMR) spectroscopy. Magnetization versus temperature measurements revealed a paramagnetic to ferromagnetic transition in most samples, with lower Curie temperatures and broader transitions for samples with higher Cu contents. The details of the magnetization measurements suggested a phase-separated scenario, with ferromagnetic clusters embedded in an antiferromagnetic matrix, especially for the samples with large Cu contents (x = 0.15 and 0.20). Zero-field (139)La NMR measurements confirmed this finding, since the spectral features remained almost unchanged for all Cu-doped samples, whereas the bulk magnetization was drastically reduced with increasing Cu content. (55)Mn NMR spectra were again typical of ferromagnetic regions, with a broadening of the resonance line caused by the disorder introduced by the Cu doping. The results indicate a coexistence of different magnetic phases in the manganites studied, with the addition of Cu contributing to the weakening of the double-exchange interaction in most parts of the material.

Cardiovascular assessment of patients with Ullrich-Turner's Syndrome on Doppler echocardiography and magnetic resonance imaging

OBJECTIVE: To assess the cardiovascular features of Ullrich-Turner's syndrome using echocardiography and magnetic resonance imaging, and to correlate them with the phenotype and karyotype of the patients. The diagnostic concordance between the 2 methods was also assessed. METHODS: Fifteen patients with the syndrome were assessed by echocardiography and magnetic resonance imaging (cardiac chambers, valves, and aorta). Their ages ranged from 10 to 28 (mean of 16.7) years. The karyotype was analyzed in 11 or 25 metaphases of peripheral blood lymphocytes, or both. RESULTS: The most common phenotypic changes were short stature and spontaneous absence of puberal development (100%); 1 patient had a cardiac murmur. The karyotypes detected were as follows: 45,X (n=7), mosaics (n=5), and deletions (n=3). No echocardiographic changes were observed. In regard to magnetic resonance imaging, coarctation and dilation of the aorta were found in 1 patient, and isolated dilation of the aorta was found in 4 patients. CONCLUSION: The frequencies of coarctation and dilation of the aorta detected on magnetic resonance imaging were similar to those reported in the literature (5.5% to 20%, and 6.3% to 29%, respectively). This confirmed the adjuvant role of magnetic resonance imaging to Doppler echocardiography for diagnosing cardiovascular alterations in patients with Ullrich-Turner's syndrome.

Magnetic resonance imaging in the diagnosis of type 1 dermoid sinus in two Rhodesian ridgeback dogs

Two cases of type 1 dermoid sinus in Rhodesian ridgebacks are described, with emphasis on the use of magnetic resonance imaging (MRI) in the diagnosis and delineation of the lesions. Magnetic resonance imaging was useful in identifying fluid-filled structures, fibrous capsules, and sinus tracts, but was not able to identify the termination of the tracts.

Radiography, computed tomography and magnetic resonance imaging at 0.5 Tesla of mechanically inducedosteoarthritis in rabbit knees

In the present experimental study we assessed induced osteoarthritis data in rabbits, compared three diagnostic methods, i.e., radiography (XR), computed tomography (CT) and magnetic resonance imaging (MRI), and correlated the imaging findings with those obtained by macroscopic evaluation. Ten young female rabbits of the Norfolk breed were used. Seven rabbits had the right knee immobilized in extension for a period of 12 weeks (immobilized group), and three others did not have a limb immobilized and were maintained under the same conditions (control group). Alterations observed by XR, CT and MRI after the period of immobilization were osteophytes, osteochondral lesions, increase and decrease of joint space, all of them present both in the immobilized and non-immobilized contralateral limbs. However, a significantly higher score was obtained for the immobilized limbs (XT: P = 0.016, CT: P = 0.031, MRI: P = 0.0156). All imaging methods were able to detect osteoarthritis changes after the 12 weeks of immobilization. Macroscopic evaluation identified increased thickening of joint capsule, proliferative and connective tissue in the femoropatellar joint, and irregularities of articular cartilage, especially in immobilized knees. The differences among XR, CT and MRI were not statistically significant for the immobilized knees. However, MRI using a 0.5 Tesla scanner was statistically different from CT and XR for the non-immobilized contralateral knees. We conclude that the three methods detected osteoarthritis lesions in rabbit knees, but MRI was less sensitive than XR and CT in detecting lesions compatible with initial osteoarthritis. Since none of the techniques revealed all the lesions, it is important to use all methods to establish an accurate diagnosis.

Phosphorus magnetic resonance spectroscopy in malformations of cortical development

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

The Anatomy of the Thoracic Spinal Canal Investigated with Magnetic Resonance Imaging

BACKGROUND: We investigated, with magnetic resonance imaging, the distance of the dura mater to the spinal cord in patients without spinal or medullar disease at the 2nd, 5th, and 10th thoracic segments.METHODS: Fifty patients in the supine position underwent magnetic resonance imaging. Medial sagittal slices of the 2nd, 5th, and 10th thoracic segments were measured for the relative distances using the 1.5-T superconducting system (Gyroscan Intera, Philips Medical Systems, Best, the Netherlands). In 10 patients, the angles relative to the tangent at the insertion point on the skin were measured.RESULTS: The posterior dural-spinal cord distance is significantly greater at the midthoracic region (5th thoracic = 5.8 +/- 0.8 mm) than at the upper (2nd thoracic = 3.9 +/- 0.8 mm) and lower thoracic levels (10th thoracic = 4.1 +/- 1.0 mm) (P < 0.015). There were no differences between interspaces T2 and 110. There was no correlation between age and the measured distance between the dura mater and the spinal cord. The entry angle of the needle at T2 was 9.0 degrees +/- 2.5 degrees; at T5, 45.0 degrees +/- 7.4 degrees; and at T10, 9.50 degrees +/- 4.2 degrees.CONCLUSIONS: This study demonstrated that there is greater depth of the posterior subarachnoid space at the T2, T5, and T10 levels. The greater distance was found at T5. (Anesth Analg 2010;110:1494-5)

Three-dimensional magnetic resonance reconstruction images before and after surgical therapy of spontaneous canine brain tumors

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Electrically detected and conventional magnetic resonance investigation of surface and bulk states in polyaniline thin films

Electrically detected magnetic resonance (EDMR) and electron paramagnetic resonance (EPR) were used to investigate emeraldine base polyaniline films. The magnetic susceptibility presented a Curie (localized spins)-Pauli (delocalized spins) transition at 240 K, when we also observed a transition in the dependence of the g factor with temperature (T). Peak-to-peak linewidth decreases with increasing temperature, reflecting that motional narrowing limits the hyperfine and dipolar broadening in this polymer. EDMR spectra could only be observed above 250 K in accordance to EPR results. Surface and bulk transport could be separated and their analysis reflected the effect of magnetic interaction with oxygen. (c) 2007 American Institute of Physics.

Nuclear magnetic relaxation of F-19 in fluoride glasses

Temperature and frequency dependence of the F-19 nuclear spin relaxation of the fluoroindate glass, 40InF(3)-20ZnF(2)- 20SrF(2)-2GaF(3)-2NaF-16BaF(2) and the fluorozirconate glass, 50ZrF(4)-20BaF(2)-21LiF-5LaF(3)-4AlF(3); are reported. Measurements were undertaken on pure and Gd3+ doped samples, in the temperature range of 185-1000 K, covering the region below and above the glass transition temperature, T-g. The temperature and frequency dependence of the spin-lattice relaxation rate, T-1(-1), measured in the glassy state at temperature <300 K, is less than the observed dependence at higher temperatures. At temperatures >T-g, the fluorine mobility increases, leading to a more efficient spins lattice relaxation process. Activation energies, for F- motion, are 0.8 eV for the fluoroindate glass and 1 eV for the fluorozirconate glass. The addition of Gd3+ paramagnetic impurities;at 0.1-wt%, does not alter the temperature and frequency dependence of T-1(-1), but increases its magnitude more than one order of magnitude. At temperatures <400 K, the spin-spin relaxation time, T-2(-1), measured for all samples, is determined by the rigid-lattice nuclear dipole-dipole coupling, and it is temperature independent within the accuracy of the measurements. Results obtained for the pure glass, at temperatures >400 K, show that T-2(-1) decreases monotonically as the temperature increases. This decrease is explained as a consequence of the motional narrowing effect caused by the onset of the diffusive motion of the F- ions, with an activation energy around 0.8 eV. For the doped samples, the hyperfine interaction with the paramagnetic impurities is most effective in the relaxation of the nuclear spin, causing an increase in the T(2)(-1)s observed at temperatures >600 K. (C) 1999 Elsevier B.V. B.V. All rights reserved.

Exciton formation in dye doped OLEDs using electrically detected magnetic resonance

Electrically Detected Magnetic Resonance (EDMR) was used to investigate the influence of dye doping molecules on spin-dependent exciton formation in Aluminum (III) 8-hydroxyquinoline (Alq(3)) based OLEDs with different device structures and temperature ranges. 4-(dicyanomethylene)-2-methyl-6-{2-[(4-diphenylamino-phenyl]ethyl}-4H-pyran (DCM-TPA) and 5,6,11,12-tetraphenylnaphthacene (Rubrene) were used as dopants. A strong temperature dependence have been observed for doped OLEDs, with a decrease of two orders of magnitude in EDMR signal for temperatures above similar to 200 K. The signal temperature dependence were fitted supposing different spin-lattice relaxation processes. The results suggest that thermally activated vibrations of dopants molecules induce spin pair dissociation, reducing the signal.

Electric and magnetic properties of polymer electrolyte/carbon black composites

Measurements of 1H Nuclear Magnetic Resonance (NMR) relaxation times, Electron Paramagnetic Resonance (EPR) and AC Impedance Spectroscopy (IS) are reported for composites based on PEO8:LiClO4 and carbon black (CB), prepared by two methods: solvent and fusion processing. Three nuclear relaxation processes were identified for 1H nuclei: (i) belonging to the polymer chains in the amorphous phase, loosely bound to the CB particles, whose dynamics is almost the same as for unfilled polymer, (ii) belonging to the polymer chains which are tightly attached to the CB particles, and (iii) belonging to the crystalline phase in the loose polymer chain. The paramagnetic electronic susceptibility of the composite samples, measured by EPR, was interpreted by assuming a contribution of localized spin states that follow a Curie law, and a Pauli-like contribution of delocalized spins. A significant change of the EPR linewidth was observed at 40 K, which is the temperature where the Curie and Pauli susceptibilities equally contribute to the paramagnetic electronic susceptibility. The electrical properties are very sensitive to the preparation methods of the composites, which conditions the interaction between carbon particle-carbon particle and carbon particle-polymer chain. Classical statistic models to describe the conductivity in these media were not satisfactory. © 1998 Published by Elsevier Science B.V. All rights reserved.

Pesquisa e desenvovimento de novos materiais microporosos e mesoporosos para uso em ressonância magnética nuclear por imagem como agentes de contraste

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Desenvolvimento de um magnetometro a precessão nuclear

O objetivo desta tese foi desenvolver um magnetômetro à precessão nuclear para prospecção geofísica e estações-base magnéticas. O magnetômetro à precessão nuclear mede a intensidade total do campo magnético. Seu funcionamento é baseado na ressonância magnética nuclear. A medida de campo é feita pela de terminação da freqüência de precessão de núcleos de hidrogênio – prótons - de líquidos não viscosos no campo magnético terrestre. O magnetômetro é constituído de duas partes: o sensor e o instrumento de medida. O sensor é uma bobina solenoidal, cujo núcleo é preenchido com o líquido. Três líquidos diferentes foram testados; água, propanol e um querosene sintético. Optou-se pelo uso do querosene porque oferece maior amplitude no sinal de precessão, dando, conseqüentemente, maior relação sinal/ ruído. O sistema de medida contém os circuitos de sintonia e amplificação do sinal e, os circuitos lógicos para a programação da operação e contagem da freqüência de precessão. Cada ciclo de medida tem duração de 3 segundos, sendo 2,3s para a polarização e 0,7s para a recepção do sinal. São possíveis dois modos de operação: manual, reciclando automaticamente e por controle remoto. O sinal de precessão é amplificado seletivamente em uma das 14 faixas de sintonia, que cobrem medidas entre 22000 e 95000 gammas. A freqüência de precessão é multiplicada por um fator de 64 e contada durante um tempo igual a 0,36699s, determinado com base na razão giromagnética do próton. O número de pulsos contados é numericamente igual ao valor do campo magnético em gammas. A resposta pode ser lida em mostradores digitais ou na saída BCD paralela quando operando por controle remoto. A precisão da medida é de 1 gamma. O instrumento foi testado no campo para avaliar a relação sinal/ruído, gradiente suportável e consumo de potência. Nos testes de aplicação do protótipo, foram obtidos dados de variação diurna e realizaram-se levantamentos magnético de reconhecimento e detalhe em um sítio arqueológico na Ilha de Marajó, Pará. As respostas dos testes foram comparados com dois magnetômetros comerciais - o GP-70, McPhar e o G-816, Geometrics e, ainda, com dados do Observatório Magnético de Tatuoca-Pa. Em todos os casos, a comparação dos dados mostrou bom desempenho do magnetômetro em teste.