1H, 23Na and 35Cl Imaging in Cementitious Materials with NMR.

A set-up especially designed for semi-simultaneous measurements of 1H, 23Na and 35Cl in ordinary cementitious materials using nuclear magnetic resonance was built. This setup makes use of the main field of a whole body magnetic resonance imaging system (Philips Intera), which has allowed us to combine two measurement setups into one, i.e., a 23Na/35Cl and a 1H insert. This 1.5 T field was chosen as a compromise between the signal-to-noise ratio of the spin-echo signal, which increases at higher frequencies, and the line broadening due to the presence of magnetic impurities of these materials, which leads to a decrease of the resolution at higher magnetic fields. The preliminary experiments show that this setup can be used to the study the interaction of different types of ions with cementitious materials. One-dimensional profiles of the moisture and dissolved ions can be measured with a spatial resolution of about 2 mm for 1H, 6 mm for 23Na and 9 mm for 35Cl.

[Monitoring steam sterilisation processes in the dental office]. / Het monitoren van stoomsterilisatieprocessen in de mondzorgpraktijk.

In dental offices, steam sterilisation is used to sterilise instruments and in that way to prevent the cross-contamination of patients and the dental team. In order to ensure that the sterilisation process has been executed successfully, every sterilisation process has to be monitored. The monitoring of every load in the steam steriliser is necessary and often even required, either directly (by legislation) or indirectly (by harmonised standards). The complete monitoring protocol consists of controls of the installation, the exposure, the loading, the packaging and, finally, the 'track and trace' of the instruments. For examining the installation, a steam penetration test, such as the Bowie and Dick test, can be carried out.

Measuring non-condensable gases in steam.

In surgery, medical devices that are used should be sterilized. To obtain surface steam sterilization conditions, not only in the sterilizer chamber itself but also in the loads to be sterilized, the amount of non-condensable gases (NCGs), for instance air, should be very low. Even rather small fractions of NCGs (below 1%) seriously hamper steam penetration in porous materials or devices with hollow channels (e.g., endoscopes). A recently developed instrument which might detect the presence of residual NCGs in a reliable and reproducible way is the 3M(TM) Electronic Test System (ETS). In this paper, a physical model is presented that describes the behavior of this instrument. This model has been validated by experiments in which known fractions of NCGs were introduced in a sterilizer chamber in which an ETS was placed. Despite several approximations made in the model, a good agreement is found between the model predictions and the experimental results. The basic principle of the ETS, measuring the heat transfer by condensation on a cooled surface, permits a very sensitive detection of NCGs in harsh environments like water vapor at high temperatures and pressures. Our model may serve to develop adapted and optimized versions of this instrument for use outside the field of sterilization, e.g., in heat exchangers based on steam condensation.

One-dimensional scanning of moisture in heated porous building materials with NMR.

In this paper we present a new dedicated NMR setup which is capable of measuring one-dimensional moisture profiles in heated porous materials. The setup, which is placed in the bore of a 1.5 T whole-body scanner, is capable of reaching temperatures up to 500 °C. Moisture and temperature profiles can be measured quasi simultaneously with a typical time resolution of 2-5 min. A methodology is introduced for correcting temperature effects on NMR measurements at these elevated temperatures. The corrections are based on the Curie law for paramagnetism and the observed temperature dependence of the relaxation mechanisms occurring in porous materials. Both these corrections are used to obtain a moisture content profile from the raw NMR signal profile. To illustrate the methodology, a one-sided heating experiment of concrete with a moisture content in equilibrium with 97% RH is presented. This kind of heating experiment is of particular interest in the research on fire spalling of concrete, since it directly reveals the moisture and heat transport occurring inside the concrete. The obtained moisture profiles reveal a moisture peak building up behind the boiling front, resulting in a saturated layer. To our knowledge the direct proof of the formation of a moisture peak and subsequent moisture clogging has not been reported before.

Temperature dependence of F-, D- and z-values used in steam sterilization processes.

AIMS: To develop a model, based on microbiological principles, to safely optimize steam sterilization processes. METHODS AND RESULTS: The minimum exposure time F for a decontamination process at a certain temperature is usually calculated from an empirical model with the decimal reduction time D and the temperature resistance coefficient z as parameters. These are implicitly assumed to be independent of temperature. Using a microbiological approach, it is shown that also D and z depend on temperature, indicating that the usual models provide only reliable results in a limited temperature region. The temperature dependence of F resulting from this approach describes the available experimental data very well. Safety margins to assure sterility can be included in a straightforward way. CONCLUSIONS: The results from the present approach can be used to safely optimize decontamination processes. The corresponding mathematical model can be implemented rather directly in process control systems. SIGNIFICANCE AND IMPACT OF THE STUDY: Our results show that for steam sterilization and disinfection processes the values of F predicted by the usual models largely underestimate the required minimum exposure times at temperatures below 120 degrees C. This has important consequences for the optimization of such processes.

Curing processes in solvent-borne alkyd coatings with different drier combinations.

The concern regarding the effect of chemicals on the environment has increased considerably in recent years. Nowadays, technological developments in the coating industry are largely influenced by environmental issues and subsequent legislation. One of these issues is the tendency to replace cobalt as a catalyst with more environmentally friendly alternatives, because studies have indicated possible carcinogenicity. Not much knowledge is available on the effects of catalysts (driers) on the in-depth drying of alkyd coatings. Therefore we have studied the effect of cobalt as a primary drier combined with Ca and Zr as secondary driers on the in-depth curing of high solid solvent-borne alkyds. The profiling of the curing of alkyd coatings is performed with a new high-spatial-resolution NMR setup. In this study, two effects observed in the solvent-borne alkyd coatings are investigated. One is that when Ca and Zr are added as secondary driers the speed of the observed cross-linking front increases. Second, in the deeper un-cross-linked region below the front, the signal of the NMR profiles was found to decrease proportional to . This could be explained by the presence of slowly reacting species that diffuse into the deeper uncured region of the coating, after which they cross-link. The model describing the effect of these reactive species also indicates that the signal decrease is inversely proportional to coating thickness L, which was confirmed by additional measurements.

Experimental evidence of crystallization pressure inside porous media.

Crystallization pressure of salt in porous materials is one of the mechanisms that may induce serious damage, for example, weathering of buildings and monuments of cultural heritage. Since this pressure also causes the solubility of the salt inside a porous material to differ from the bulk solubility, it can be assessed experimentally by measuring the solubility inside the pores. We show that this is possible by NMR, and study Na(2)CO(3) and Na(2)SO(4) in a series of model porous materials. Using the solubility data the crystal-liquid surface energies are estimated as gamma = 0.09 N/m for Na(2)CO(3) . 10H(2)O and gamma = 0.06 N/m for Na(2)SO(4) . 10H(2)O. For pore sizes below about 30 nm, the resulting pressure exceeds the tensile strength of typical building materials (3 MPa). No pressure is induced by the metastable Na(2)SO(4) . 7H(2)O, which suggests for this crystal a value of gamma close to zero.

Ischemia-induced ADC changes are larger than osmotically-induced ADC changes in a neonatal rat hippocampus model.

Diffusion-weighted imaging (DWI) is frequently used to diagnose stroke. However, the origin of the observed reduction in the apparent diffusion coefficient (ADC) in the acute phase following ischemia is not well understood. Although cell swelling is considered to play an important role, it is unclear whether this can completely explain the large ADC decrease. We developed a method to induce in neonatal rat hippocampal slices both osmotic perturbations, which lead to cell swelling, and oxygen/glucose deprivation (OGD), which simulates ischemia. A perfusion system was used to provide the hippocampal slices with nutrients and oxygen to maintain slice viability, which was verified with the use of fluorescent dyes (live/dead staining). Upon induction of OGD, the ADC decreased to approximately 57% of the initial value within 2 hr. The ADC reduction cannot fully be explained by changes due to cell swelling, since these led only to a maximum decrease of approximately 83%. Therefore, in addition to cell swelling, other changes must contribute significantly to the ADC reduction.

Sodium NMR relaxation in porous materials.

The NMR relaxation of hydrogen nuclei of a fluid in a porous material is generally interpreted in terms of the Brownstein-Tarr model, in which the relaxation rate of the signal is inversely proportional to the pore size. We have investigated whether this model can be applied to the relaxation of Na nuclei in a NaCl solution in a porous material. The results indicate that the ion distribution over the pores can be obtained from an analysis of the Na NMR signal decay, if the pore sizes are roughly below 1 microm. This information is very useful for studies of combined moisture and ion transport in porous building materials.

Diffusion in porous building materials with high internal magnetic field gradients.

Measuring the water diffusivity in porous building materials with NMR is hindered by the presence of large internal magnetic field gradients originating from magnetic impurities (Fe). To investigate the diffusion of water in these materials, a stimulated echo NMR technique is applied. A new analytical equation for the long-time signal decay in the presence of spatially varying internal field gradients is derived. This equation is experimentally confirmed by measurements on representative materials with large internal gradients (fired-clay brick and sintered crushed glass) and a material with very small internal gradients (glass filter). The diffusivity is determined in the long time limit, where it is constant and limited by the tortuosity of the pore structure. Tortuosities of different samples derived from the NMR data show an excellent agreement with the macroscopic tortuosities measured by electrochemical impedance spectroscopy. The developed technique can also be applied in unsaturated media, during e.g., drying, water absorption, and concentration changes. The characteristic length scales of the internal field fluctuations estimated from the model are compared with the structural length scales, whereas the magnitude of these fluctuations is compared with results of macroscopic magnetization measurements.

Salt transport and crystallization in porous building materials.

Salt weathering is a major cause of deterioration of porous building materials. To obtain information about the mechanisms underlying these damage processes we have studied the moisture and ion transport. We measured the time evolution of NaCl saturated samples of fired-clay brick during one-sided drying using Nuclear Magnetic Resonance. The moisture content and amount of dissolved Na ions could be measured quantitatively as a function of position. The NaCl concentration profiles obtained from these data reflect the competition between advection to the surface and redistribution by diffusion. By representing the measured moisture and NaCl profiles in an efflorescence pathway diagram (EPD) also the crystallization can be taken into account.

Random-walk simulations of NMR dephasing effects due to uniform magnetic-field gradients in a pore.

A random-walk simulation program was developed to study the effect of dephasing spins in a uniform magnetic-field gradient in a porous material. It is shown that this simulation program correctly reproduces basic nuclear magnetic resonance behavior, such as the formation of a spin echo. The spin-echo decay due to dephasing in a nonrestricted medium gives the well-known exponential relation containing the cube of time, whereas the spin-echo decay due to dephasing in a porous material gives a monoexponential decay. By varying the pore size and magnetic-field gradient, the motional averaging regime and the localization regime can be simulated. Moreover, the unknown intermediate regime is investigated. By choosing the right scaling parameters, the spin-echo decay due to dephasing in a pore can be described by one master curve for all pore sizes and gradient strengths. This master curve reveals a small intermediate regime, perfectly symmetrical around the gradient for which the dephasing length is exactly equal to the structural length of the pore.

Cryoporometry and relaxometry of water in silica-gels.

Both cryoporometry and relaxometry are tools to determine the pore size distribution (PSD) of a porous material with NMR. The melting point depression is described by the Gibbs-Thomson equation, yielding the PSD from cryoporometry. The enhanced relaxivity is caused by the surface of the porous material, yielding the PSD from relaxometry. The description in the classical paper of Brownstein and Tarr is only valid for one pore (size). The extended theory of McCall et al. is needed to describe a heterogeneous coupled porous system. As testing material a series of silica-gels called Nucleosil is chosen with typical pore sizes of 5, 10, 12 and 30 nm. Transverse relaxation time distributions are measured using a CPMG-sequence for every temperature of the cryoporometry measurement. These show a mono exponential behaviour, indicating a strongly coupled porous structure. Using the cryoporometry data, an attempt is made to reproduce the averaged relaxivity. Agreement is found for pores with typical pore sizes between 10 nm and 1 microm. The model is not valid for pores smaller than 10 nm.

Ion transport in porous media studied by NMR.

Moisture and salt transport in masonry can give rise to damages. Therefore a detailed knowledge of the moisture and salt transport is essential for understanding the durability of masonry. A special NMR apparatus has been made allowing quasi-simultaneous measurements of both moisture and Na profiles in porous building materials. Using this apparatus both the absorption of a 4 M NaCl solution in a calcium silicate brick and the drying of a 3 M NaCl capillary saturated fired-clay brick have been studied. It was found that during the absorption process the Na ions clearly stay behind, which this is caused by adsorption of these ions to the pore surface. For the drying it was found that at the beginning of the drying process the ions accumulate near the surface. As the drying rate decreases, diffusion becomes dominant and the ion profile levels off again.

Dealing with the subvoxel vessel position relative to the reconstruction voxel grid in 2D MR quantitative flow measurements.

A method is introduced that quantifies the error in 2D MR Quantitative Flow measurements induced by the position of the vessel relative to the reconstruction voxel grid, called the subvoxel vessel position. In this method, the vessel area and the volume flow rate are determined for all possible subvoxel vessel positions resulting in a mean value with standard deviation. Since the subvoxel vessel position in standard MR image reconstruction is completely arbitrary, the standard deviation can be considered as a measure of its random error contribution. Simulation studies and in vivo measurements show that our method can be used to quantify and subsequently eliminate this random error. It is further quantitatively shown that, for low noise levels, Fourier interpolation to a higher reconstruction matrix also decreases the random error. We conclude that the precision of a 2D MR Quantitative Flow measurement is improved either by using our method or by reconstruction to a higher matrix.

Venous signal suppression in 3D dynamic Gd-enhanced carotid artery imaging using the eigenimage filter.

A three-dimensional dynamic gadolinium-enhanced carotid artery imaging protocol with 10 sec per phase was evaluated with respect to the acquisition of an arterial-only phase after contrast bolus injection. Subsequently, the eigenimage filter was used to suppress any venous signal based on a difference in arterial and venous temporal enhancement patterns. From 63 consecutive scans of the carotid bifurcation, venous enhancement in the maximal arterial phase was found to be absent in 43%, weak in 19%, and strong in 38% of cases. Our eigenimage filter successfully suppressed the low signal veins in 100% and the high signal veins in 67% of cases. The number of acquired high-quality arterial-only images increased from 43% without to 87% with the use of the filter. In conclusion, even when a dynamic scan cannot resolve the short physiological delay between arterial and venous enhancement, the eigenimage filter can effectively be used to suppress the veins. Magn Reson Med 42:307-313, 1999.

Separation of haemodynamic flow waves measured by MR into forward and backward propagating components.

Physiological information on the action of the heart and on the reflection sites in the arterial system can be derived respectively from the forward and the backward propagating pressure or flow wave components. Earlier work on the separation of these components was exclusively based on invasive measurements of pressure or flow. In this study magnetic resonance (MR), which is a non-invasive imaging technique, was used to measure the blood flow waveform simultaneously at multiple positions along a vessel. Linear one dimensional transmission-line theory was used to separate the flow waves into forward and backward propagating components. First results, obtained from the thoracic aorta of five healthy male volunteers, consistently showed a negative reflection with a delay of about 100 ms between the foot of the forward and the foot of the backward propagating flow wave. Our model, consisting of a single vessel segment with constant diameter and wall properties, was validated by the excellent agreement between the vessel area as calculated from the flow data using the law of mass conservation and as directly measured with a different independent MR technique.

Water absorption in mortar determined by NMR.

Nuclear magnetic resonance (NMR) offers the possibility to determine moisture profiles in porous building materials. Moreover, the relaxation of the nuclear magnetic resonance signal can provide additional information on the water distribution in the microstructure. For mortar, it is shown that the transverse relaxation yields information on the distribution of water in the gel pores and capillary pores. Moisture profiles and relaxation were measured during water absorption. The effect of the drying treatment on the microstructure and the water absorption was investigated.

Determination of moisture profiles in porous building materials by NMR.

Because moisture in porous building materials can give rise to several kinds of damage, a detailed knowledge of the moisture transport is essential. for such studies it is important to measure dynamic moisture profiles quantitatively. Nuclear Magnetic Resonance (NMR) offers a powerful technique to measure such profiles in a nondestructive way. Because of the large amount of paramagnetic ions present in many of these materials (0.1-5% Fe) standard NMR imaging equipment cannot be used. A NMR apparatus will be described that was especially developed to study the moisture transport in porous building materials. At the moment, one-dimensional moisture profiles in samples with a diameter of 20 mm can be measured with an accuracy of 1% and a resolution of 1 mm. It takes about 40 s to determine the moisture content at a specific position.