Multiple Electron Beam Analyses Applied to Eclogite from the Western Alps

 The occurrence of compositional and microtextural relics within metamorphic rocks can provide useful information on the pressure-temperature history of the host rock. The grain-size of these microstructures, such as coronitic reaction microtextures, is mostly too fine to be detected by optical microscopy. Therefore, a more detailed analytical approach is needed. In this paper multiple electron beam techniques including the acquisition of X-ray multi-element maps, micro and nano-analysis performed by SEM/EDS and TEM/STEM-EDX systems were applied to a specific petrological problem related to metamorphism. Fine-grained decompressional reaction microtextures of an eclogitic sample (Mt. Rosa Nappe, Western Alps) are described and discussed.     

Comparative Analysis of a Solar Control Coating on Glass by AES, EPMA, SNMS and SIMS

 A solar control coating was analysed by different methods of surface analysis with respect to the layer sequence and the composition and thickness of each sublayer. The methods used for depth profiling were Auger electron spectroscopy, electron probe microanalysis, secondary neutral mass spectroscopy and secondary ion mass spectroscopy based on MCs⁺. The structure of the coating was unknown at first. All methods found a system of two metallic Ag layers, embedded between dielectric SnO_X layers. Additionally, thin Ni-Cr layers of 1–2 nm were detected on top of the Ag layers. Thus the detected layer sequence is SnO_X/Ni-Cr/Ag/SnO_X/Ni-Cr/Ag/SnO_X/glass. The Ni:Cr ratio in the nm-thin layers could be quantified by every method, the Cr fraction corresponding to less than one monolayer. We compare the capabilities and limitations of each method in routinely investigating this solar control coating. Importance was attached to an effective investigation. Nevertheless, by combining all methods, measuring artefacts could be uncovered and a comprehensive characterisation of the system was obtained.     

Voltammetric study of the interaction of the ofloxacin–copper complex with DNA, and its analytical application

The electrochemical behavior of the ofloxacin–copper complex, Cu(II)L₂, at a mercury electrode, and the interaction of DNA with the complex have been investigated. The experiments indicate that the electrode reaction of Cu(II)L₂ is an irreversible surface electrochemical reaction and that the reactant is of adsorbed character. In the presence of DNA, the formation of the electrochemically non-active complexes Cu(II)L₂-DNA, results in the decrease of the peak current of Cu(II)L₂. Based on the electrochemical behavior of the Cu(II)L₂ with DNA, binding by electrostatic interaction is suggested and a new method for determining nucleic acid is proposed. Under the optimum conditions, the decrease of the peak current is in proportional to the concentration of nucleic acids in the range from 3 × 10⁻⁸ to 3 × 10⁻⁶ g · mL⁻¹ for calf thymus DNA, from 1.6 × 10⁻⁸ to 9.0 × 10⁻⁷ g · mL⁻¹ for fish sperm DNA, and from 3.3 × 10⁻⁸ to 5.5 × 10⁻⁷ g · mL⁻¹ for yeast RNA. The detection limits are 3.3 × 10⁻⁹, 6.7 × 10⁻⁹ and 8.0 × 10⁻⁹ g · mL⁻¹, respectively. The method exhibits good recovery and high sensitivity in synthetic samples and in real samples.     

Basics, Possibilities and Limitations of the Microscopic X-Ray Fluorescence Analysis

 Microscopic X-ray fluorescence (MXRF) analysis was used to investigate different samples: meteorites, Jasper, coated glas and, reference materials. The element distribution within sections of two different meteorites have been determined – one metal rich and one oxide rich. The metal rich showed a matrix of Fe with Ni-, Ti-, and Si-enriched regions. The oxide rich also showed a Fe rich matrix and regions with different concentrations of other elements. A reference sample with a flat and polished but systematically tilted surface was used to assure, that roughness of the sections of the meteorites has only negligible influence. Nondestructive investigations in Jasper with included Stromatolithes, which were fossilized more than 2 billion years ago, showed the Stromatolithes to have Fe as main element instead of Si in the Jasper matrix. The thickness of Yb-layers on glas was determined from the intensity of the Yb fluorescence peak. Calibration was done by using a sample without coating and a reference sample whose thickness of the layer was determined by XRD reflectometry. Futhermore it has been shown that materials can be analysed even if mounted in glas capillaries or covered by plastic foils. By using Mark capillaries the elements from S to U may be detected instead of Na to U while working in vacuum mode.     

XRF Analysis of Microsamples of Semiconductor Type Multielement Materials by the Thin Layer Method. Determination of Cr, Co, Ni, Cu, Zn, Ga, Se, Sb, Yb

 A simple and quick method of durable samples preparation by the thin layer method through direct digesting of the analysed material on the substrate has been presented. Four- and three-component mono- and polycrystals have been analysed. Standards have been used in calibration containing: Cr, Co, Ni, Cu, Zn, Ga, Se, Sb, Yb. To improve the correlation between the concentration and the fluorescent radiation models of mathematical corrections have additionally been used: multiple linear regression, Lucas-Tooth-Pyne model (L. T. P.) and de Jongh model (d. J.). Statistical parameters: detection limits for 0.5 mg samples: Cr–0.041%, Co–0.034%, Ni–0.042%, Cu–0.053%, Zn–0.054%, Ga–0.057%, Se–0.057%, Sb–0.113%, Yb–0.077%. Correlation coefficients: simple regression 0.9946–0.9997, multiple regression 0.9974–1.0000, L. T. P. 0.9993–1.0000, d. J. 0.9995–1.0000. Received August, 1, 1998. Revision March 25, 1999.     

Chelating Sorbents Prepared by the Modification of Silica Gel, Lichroprep RP-8 and Lichroprep RP-18 with Calcon and Their Application in the Analysis of Some Metal Ions

 Two new chelating sorbents for metal ions were prepared by the impregnation of chemically modified silicas LiChroprep RP-8 and RP-18 with ion pairs composed of the cation of Aliquat 336 and the anion of Calcon. The sorbents were compared with an analogous sorbent with a plain silica carrier containing the same ion pairs. A hypothesis for binding this ion pair by the surfaces of the applied carriers was presented. A higher stability of the two sorbents in comparison with that of the plain silica chelating sorbent was demonstrated. The sorbents obtained were applied for chromatographic separations of some chosen mixtures of some metal ions and for additional purification of aqueous solutions of alkali metals from trace amounts of heavy metals. The multiple use of the sorbents based on RP-8 and RP-18 in sorption–desorption processes of metal ions without deterioration of their sorption capacities was demonstrated. Received March 8, 2000. Revision March 5, 2001.