Nanopore structure buildup during endodontic cement hydration studied by time-domain nuclear magnetic resonance of lower and higher mobility 1H.

Time-domain nuclear magnetic resonance (TD-NMR) of (1)H nuclei has been used to monitor and model changes of endodontic cement pastes during hydration, from the initial reaction period up to hours and days. The (1)H in the samples are divided into two major spin groups by fitting each free induction decay, acquired after the second pulse of an inversion recovery (I-R) pulse sequence with variable interpulse delay, by the sum of a quasi-Gaussian (signal from low mobility nuclei) and an exponential (from higher mobility nuclei). The extrapolations to zero time of the signals from the two spin groups give two sets of I-R data that have been analyzed to give quasi-continuous T(1) distributions. After about a day, two clearly solid components appear. From a day to a few days, three liquid populations are identified, one of them mainly in the low-mobility spin group, which later merge, giving a single T(1) or T(2) peak. The rapid onset of the solid components, at the cost of the liquid, and the rapid changes of the relaxation time distributions of all components are clear indicators of the amount and kinetics of reaction products formation (C-S-H gel and Portlandite) and of the C-S-H micronanoporous structure buildup and evolution. At 30 days of hydration, the very short T(1) and T(2) liquid component (T(1) congruent with 200 micros and T(2) congruent with 50 micros) can be assigned to C-S-H intralayer water (thickness of the order of fractions of a nanometer) and the remaining liquid signal to interlayer water (thickness of the order of 1 nm). Comparisons are made among a widely used commercial endodontic cement paste and two more recent commercial pastes, with additive compounds to make the hydration process faster and to increase the workability. Parameters can be extracted from the data to characterize the different kinetics and nanostructure of the pore space formed up to 30 days. The parameters are in agreement with the expected effects of the additives, so the parameters can be used to optimize the formulation of new pastes, in order to improve their therapeutic performance.

Inhomogeneity of rat vertebrae trabecular architecture by high-field 3D mu-magnetic resonance imaging and variable threshold image segmentation.

PURPOSE: To analyze the 3D microarchitecture of rat lumbar vertebrae by micro-magnetic resonance imaging (micro-MRI). MATERIALS AND METHODS: micro-MR images (20 x 20 x 20 microm(3) apparent voxel size) were acquired with a three-dimensional spin-echo pulse sequence on four lumbar vertebrae of two rats. Apparent microarchitectural parameters like trabecular bone fraction (BV/TV), specific bone surface (BS/TV), mean intercept length (MIL), and Euler number per unit volume (Euler density, E(V)) were calculated using a novel semiquantitative variable threshold segmentation technique. The threshold value T was obtained as a point of minimum or maximum of the function E(V) = E(V)(T). RESULTS: Quantitative 3D analysis of micro-MRI images revealed a higher connectivity in the peripheral regions (E(V) = -570 +/- 70 mm(-3)) than in the central regions (E(V) = -130 +/- 50 mm(-3)) of the analyzed rat lumbar vertebrae. Smaller intertrabecular cavities and larger bone volume fractions were observed in peripheral regions as compared to central ones (MIL = 0.18 +/- 0.01 mm and 0.26 +/- 0.01 mm; BV/TV = 34 +/- 3% and 29 +/- 3%, respectively). The quantitative 3D study of MIL showed a structural anisotropy of the trabeculae along the longitudinal axis seen on the images. The inhomogeneity of the bone architecture was validated by micro-computed tomography (micro-CT) images at the same spatial resolution. CONCLUSION: 3D high-field micro-MRI is a suitable technique for the assessment of bone quality in experimental animal models.

Water vapor absorption in porous media polluted by calcium nitrate studied by time domain nuclear magnetic resonance.

Nuclear magnetic resonance relaxation analysis of liquid water (1)H nuclei in real porous media, selected for their similar composition (carbonate rocks) and different pore space architecture, polluted with calcium nitrate, is presented to study the kinetics of water condensation and salt deliquescence inside the pore space. These phenomena are responsible for deterioration of porous materials when exposed to environmental injury by pollution in a humid atmosphere. The theory is well described for simple pore geometries, but it is not yet well understood in real porous media with wide distributions of pore sizes and connections. The experiment is performed by following in time the formation of liquid water inside the pore space by T(1) and T(2) relaxation time distributions. The distributions allow one to see the effects of both the salt concentration and the pore space structure on the amount of water vapor condensed and its kinetics. It is shown that, for a given lithotype, even with different amounts of pollutant, the rate-average relaxation time T(1ra) tends to increase monotonically with NMR signal, proportional to the amount of liquid water. T(1ra) is often inversely associated with surface-to-volume ratio. This suggests a trend toward the filling of larger pores as amounts of liquid water increase, but it does not indicate a strict sequential filling of pores in order of size and starting with the smallest; in fact, relaxation time distributions show clearly that this is not the case. Increased amounts of salt lead to both markedly increased rates and markedly increased amounts of water absorption. NMR measurements of amounts of water, together with relaxation time distributions, give the possibility of information on the effect of pollution in porous materials exposed to humid atmospheres but sheltered from liquid water, even before the absorption of large amounts of moisture and subsequent damage. These phenomena are of importance also in other fields, such as the exploitation of geothermal energy.

Magnetic resonance imaging and relaxation analysis to predict noninvasively and nondestructively salt-to-moisture ratios in dry-cured meat.

The current systems are unable to control and predict the cured meat composition nondestructively and in a reasonable time for production needs. In this work, T1 and T2 maps were obtained, with a monoexponential model, on internal sections of Longissimus dorsi muscle at increasing salting times. The maps allow one to visualize the salting process nondestructively and noninvasively. The method goes beyond the simple qualitative visualization, because, for each section of the sample and in any region of the section, it is possible to obtain quantitative information on the progress of salting and to predict salt-to-moisture ratios. In addition, detailed relaxation measurements were performed on samples cored after imaging in order to define better the relaxation properties of the dry-cured meat.