Application of microimaging to diffusion studies in nanoporous materials

Adsorption - Microimaging on the basis of, respectively, interference microscopy and IR microscopy permit the observation of the distribution of guest molecules in nanoporous solids and their...     

The role of NAA in studies of organic diagenesis of rocks

The Delaware Mountain Group in west Texas and southeast New Mexico provides a unique opportunity to evaluate the impact of organic matter alteration in sediment diagenesis. Trace elements have been measured using neutron activation analysis in organic bitumen as well as authigenic and detrital material separates. Correlations between siltstone organic matter and authigenic minerals in adjacent permeable sandstones establish the close relationship between the organic matter and pore water from which the authigenic minerals precipitated.     

中子活化分析在鄂尔多斯地区元素分析中的应用

利用中子活化对鄂尔多斯盆地油气田上方的地质样品进行了某些元素的检测,通过实验分析,得到了该地区岩石中某些元素的含量,并对该地区的放射性元素作出了评价,绘制了样品的稀土配分模式图和评价了当地的金属矿产资源情况.结果表明,在油气田的上方,放射性元素铀呈现出负异常;钍和钾无明显异常;岩石中的其它元素和中国大陆地壳元素丰度基本...     

Application of NAA standardization methods using a low power research reactor

Two widely used neutron activation analysis (NAA) standardization methods (relative and k ₀) have been validated at the Ghana Research Reactor-1 (GHARR-1) Centre using environmental and biological standard reference materials (SRMs). The samples were IAEA Soil-7 as an environmental sample, and NIST Orchard Leaves 1571 as a biological sample. The qualitative and quantitative analyses were done using a high resolution Canberra N-type high purity germanium (HPGe) detector. The accuracy and precision were evaluated for the elements analysed. The concentrations of most of the elements were found to be within 10% of the certified values. Precision was calculated from six replicate measurements and was found to be within 15%.     

Rutherford backscattering spectrometry studies of iodine diffusion in polyimide

Rutherford backscattering spectrometry with a 2.1-meV He²⁺ion beam is used to measure the diffusion of iodine into polyamic acid and polyimide films. The iodine diffusion coefficient D decreases from its initial value of about 2X10^?13cm²/s in polyamic acid to approximately 1.4 × 10^?15cm²/s in partially cured polyimide, but then increases to a value of nearly 1.5 × 10^?14 cm²/s in fully cured polyimide. This dramatic increase in D cannot be attributed to the “in-plane” biaxial orientation of the polyimide molecules since indential D's were found with isotropic specimens. Microvoids less than 2 nm in size caused by water and carbon dioxide formation during imidization may, however, give rise to the observed behavior. The results demonstrate that Rutherford backscattering spectrometry with its excellent depth resolution (better than 30 nm) and good sensitivity (50 ppm iodine can be detected) is very useful for measuring the diffusion of slowly diffusing species in glassy polymers.     

Application of k 0-based NAA for multielement determination in serpentines and associated minerals

The k ₀-based neutron activation analysis method was applied for multielement determination in black and yellow serpentines along with two associated minerals namely altered and unaltered dolomites and intrusive rock dolerite, obtained from the asbestos mines of Cuddapah basin, Andhra Pradesh, India. Concentrations of 20 elements were determined and they were used to predict the process of formation of fibrous chrysotile asbestos. Majority of elements as well as REEs reveal the contribution of elements from both dolerite and dolomite during the process of contact metamorphism in forming the mineral serpentine.     

Tracing pore-space heterogeneities in X-type zeolites by diffusion studies

Pore-space homogeneity of zeolite NaX was probed by pulsed field gradient (PFG) NMR diffusion studies with n-butane as a guest molecule. At a loading of 0.75 molecules per supercage, a wide spectrum of diffusivities was observed. Guest molecules in the (well-shaped) zeolite crystallites were thus found to experience pore spaces of quite different properties. After loading enhancement to 3 molecules per supercage, however, molecular propagation ideally followed the laws of normal diffusion in homogeneous media. At sufficiently high guest concentrations, sample heterogeneity was thus found to be of no perceptible influence on the guest mobilities anymore.     

Holographic grating relaxation studies of probe diffusion in amorphous polymers

Probe diffusion of camphorquinone, thymoquinone, and diacetyl in polymers was studied by the laser-induced holographic grating relaxation (HGR) technique in polymers. The effects of changing the probe size and various parameters of the polymer, such as the molecular weight, chain conformation, and the glass transition temperature, on the probe diffusion coefficient have been investigated. Furthermore, effects of cross-linking and plasticizing the chains of the polymer host on the probe diffusion coefficient were also studied. Temperature-dependent studies show that except for the very low molecular weight poly(methyl methacrylate), all probe diffusion coefficient data above the glass transition temperature fit well to the WLF equation. ©1995 John Wiley & Sons, Inc.     

Non-uniformity and representative sampling in NAA

An instrumental procedure of activation analysis has been developed to study the distribution of some minor components in synthetic granates, ferrites and glass charges in some environmental materials. The determination of the degree of non-uniformity by NAA has been used for the preparation of uniform mixtures and for representative sample estimation in the analysis of nonhomogeneous materials.     

Isothermal diffusion studies of water-choline chloride-hydrogen chloride system

Sets of four diffusion coefficients were obtained for the water-choline chloridehydrogen chloride system at 25°C. The cross-term diffusion coefficients were found to be very large, and the electrostatic force is the dominant factor for these cross-term diffusion coefficients.     

Automation and Computerization of NAA

A PC controlled automatic INAA system is briefly introduced. The unique features of the system in software, hardware, and quality control procedures are described. Major performances are given to show the analytical quality and productivity of the system.     

The standardization of standardless NAA

This review describes how the original `standardless' (absolute and single-comparator) NAA-calibration methods, introduced in the mid-1960s, were stepwise upgraded with respect to their accuracy and manageability, leading to the launching of the k ₀-method in the mid 1970s. Next, an account is given of the achievements in the continuous development of the k ₀-standardization of NAA up to the present. Topics highlighted are:the k 0 -data library, the development of dedicated calibration procedures, extensions and limitations, computerization and quality control/assurance. Finally, a short outline is given of the international dissemination of the k ₀-methodology.     

Selenium determination in biological materials by NAA

Results for Se in several biological standard reference materials obtained by INAA and selective RNAA procedures developed in our laboratory, are presented and discussed. The comparison of selenium levels in selected blood plasma samples determined by non-destructive NAA and HG-AAS is also presented. The reproducibility and accuracy of the analytical procedure was tested and the results of these investigations were compared with the certified values.     

The role of NAA in nuclear chemistry education

One of the missions of our Institute is the promotion of basic nuclear teaching for students as well as professional teaching for workers in nuclear industry and research. For nuclear chemistry education, we present here a one day teaching course on radioactive decay and nuclear reactions, and a two or three days course based on reactor irradiation of uranium oxide, instrumental and radiochemical analysis of fission products. In the first experiment, the neutron capture is presented as an example of nuclear reaction; the neutron activation of a silver coin with a Am-Be neutron source, followed by γ-ray spectrometry, is used to identify three radionuclides of silver and to calculate their half-lives. In the second experiment, our teaching reactor is used as a neutron source with a flux about 10¹⁰ n·cm⁻²·s⁻¹ at a low thermal power (10 kW). This low flux allows us to irradiate a small uranium sample which is usable for spectrometry after a short cooling time of about two hours. The first day is reserved for instrumental analysis of the fission products and a second day for the radiochemical separation of a fission radionuclides. With these experimental results, the students have to calculate the number of fissions in the irradiated sample. On optional third day for postgraduate students is devoted to the presentation of NAA and some applications as uranium determination by the fission product spectrometry.     

Water sorption and diffusion studies in an epoxy resin system

The kinetics of water absorption in epoxide materials was studied by the aid of a diglycidyl ether of bisphenol‐A–triethylenetetramine (DGEBA–TETA) epoxy–resin system containing various amounts of the plasticizer THIOCOL (0–40 phr). The presence of plasticizer permits the formation of products with different crosslinking densities and hydrophilic characters. Dynamic water absorption experiments were carried out at 15, 40, and 70°C. For the fitting of the experimental results, a new model was used, based on a model proposed earlier by Jacobs and Jones. This model considers epoxide product as a two‐phase system consisting of a master phase (where the major part of the water is absorbed), which is homogeneous and nonpolar (phase 1), and of a second phase with different density and/or hydrophilic character (phase 2). By making the assumption that water diffusion can take place independently in the different phases of the material in accordance with Fick's second law, we can calculate the diffusion coefficient D and the water content at saturation M_∞ for each phase separately. Equilibrium water sorption measurements were performed at 40°C, and the data were analyzed and discussed based on the Guggenheim–Anderson–de Boer (GAB) equation, the results being in support of the two‐phase model used in the analysis of absorption kinetics. The linear expansion coefficient and the glass transition temperature of the materials, employed in the discussion of the results, were measured by thermomechanical analysis. © 1999 John Wiley & Sons, Inc. J Polym Sci B: Polym Phys 37: 1165–1182, 1999     

Single molecule spectroscopy studies of diffusion in mesoporous silica thin films

Single molecule spectroscopy is applied in studies of diffusion and surface adsorption in sol-gel-derived mesoporous silica thin films. Mesoporous films are obtained by spin casting surfactant-templated sols onto glass substrates. Small-angle X-ray diffraction results are consistent with hexagonally ordered mesophases in as-synthesized (i.e., surfactant-containing) films. Upon calcination, a 30% contraction and disordering of these structures occurs. Nile Red is used as a fluorescent probe of both the as-synthesized and calcined films. It is loaded into the samples at subnanomolar levels either prior to spin casting or after calcination. Fluorescence imaging and single-point fluorescence time transients show the dye molecules to be relatively mobile in the as-synthesized samples. In contrast, the molecules appear entrapped at fixed locations in dry calcined films. In calcined films rehydrated under high humidity conditions, the Nile Red molecules again become mobile. Time transients obtained from the as-synthesized and rehydrated samples provide clear evidence for frequent reversible adsorption of the dye to the silica surfaces. Autocorrelations of the time transients provide quantitative data on the mean diffusion coefficients (D = 2.4 x 10(-10) and 2.6 x 10(-10) cm2/s) and mean desorption times (1/k = 25 and 40 s) for the as-synthesized and rehydrated films, respectively. The results prove both water and surfactant play important roles in governing matrix interactions and mass transport.     

Determination of Impurities in Gallium Oxide by NAA

Neutron activation analysis has been applied to determine 12 elements, viz. Na, Mn, As, Fe, Co, Zn, Se, Sc, Cr, Sb, Hf and Ta in high-purity Ga₂O₃. The first 7 elements could be determined by anion exchange separation and isopropyl ether extraction, and the last 8 elements by instrumental method. It is recommended that the first 3 elements are determine by one of the radiochemical modes and the others by the instrumental method.     

A new FTIR-ATR cell for drug diffusion studies

The drug diffusion of most compounds, particularly hydrophilic molecules through the skin is limited by the permeation of the outermost cell layers of the epidermis, the stratum corneum(SC). For this reason it is of interest to characterize drug diffusion processes through this skin layer. A new FTIR-ATR cell was developed for non-invasive real time measurements of drug diffusion. The diffusion of water through an artificial polyethyleneglycol-polydimethylsiloxane membrane was studied. Additionally the diffusion of urea in human SC was analyzed. Based on a mathematical model the diffusion coefficients were derived. We could reveal that this cell associates the advantages of the Franz diffusion cell and the FTIR-ATR spectroscopy as a new powerful method for determining drug diffusion through biological membranes.