Origin and age of the Eisenkappel gabbro to granite suite (Carinthia, SE Austrian Alps).

The northern part of the Karawanken plutonic belt is a gabbro-granite complex located just north of the Periadriatic lineament near the Slovenian-Austrian border. Petrographic and geochemical studies of the Eisenkappel intrusive complex indicate that this multiphase plutonic suite developed by a combination of crystal accumulation, fractional crystallization and assimilation processes, magma mixing and mingling. The mafic rocks are alkaline and have within-plate geochemical characteristics, indicating anorogenic magmatism in an extensional setting and derivation from an enriched mantle source. The mafic melts triggered partial melting of the crust and the formation of granite. The granitic rocks are alkalic, metaluminous and have the high Fe/Fe + Mg characteristics of within-plate plutons. Temperature and pressure conditions, derived from amphibole-plagioclase and different amphibole thermobarometers, suggest that the analysed Eisenkappel gabbros crystallized at around 1000 ± 20 °C and 380-470 MPa, whereas the granitic rock crystallized at T ≤ 800 ± 20 °C and ≤ 350 MPa. Mineral-whole rock Sm-Nd analyses of two cumulate gabbros yielded 249 ± 8.4 Ma and 250 ± 26 Ma (εNd: + 3.6), garnet-whole rock Sm-Nd analyses of two silicic samples yielded well-constrained ages of 238.4 ± 1.9 Ma and 242.1 ± 2.1 Ma (εNd: - 2.6).

Quantification of lanthanides in rocks using succinic acid-derivatized sorbents for on-line SPE-RP-ion-pair HPLC

The use of new poly(norbornene-block-7-oxanorborn-2ene-5,6-dicarboxylic acid)-coated silica-based sorbents as well as of beaded polymers based on poly(norborn-2-ene-5,6-dicarboxylic acid-co-1,4,4a,5,8,8a-hexahydro-1,4,5,8-exo-endo-dimethanonaphthalene) for the on-line preconcentration of lanthanides from rock digests and their subsequent RP-ion-pair HPLC separation is described. Block co-polymers of norborn-2-ene and 7-oxanorborn-2-ene-5,6-dicarboxylate used for coating were prepared by ring-opening metathesis polymerization (ROMP) and poly(norborn-2-ene-5,6-dicarboxylic acid-co-1,4,4a,5,8,-8a-hexahydro-1,4,5,8-exo-endo-dimethanonaphthalene)-based polymer beads were prepared by ring-opening metathesis precipitation polymerization. Both types of sorbents exhibit an extraordinarily good pH stability, are hydrophilic and therefore easily wetable by water alone, and show high extraction efficiencies for lanthanides within a pH of 3.5-5.5. The rare earth element (REE) content in the investigated rocks varied over 3 orders of magnitude (0.19-108 microg/g). REE concentrations prior to enrichment were typically in the range of 1-25 ng/mL; the total amount of each REE sorbed onto the precolumn was in the range of 8-270 ng. Extraction selectivities of the sorbent may be enhanced by adding 5-sulfosalicylic acid as a masking agent for iron and aluminum as well as methanol as an inhibitor for the precipitation of o-silicic acid. Gradient elution of the lanthanides from the precolumn and their subsequent separation on a RP-C18 column was achieved using hydroxyisobutyric acid (HIBA) and sodium octanesulfonate. Depending on the actual concentration of the lanthanides in the digests and in order to suppress interfering cations, UV detection was carried out with two different postderivatization reagents, 4-(2-pyridylazo)resorcinol (PAR) and arsenazo III. The high selectivity in enrichment as well as the complementary use of post-derivatization reagents allows the fast, quantitative, and highly reproducible quantification of REEs present in rocks by complete removal or suppression of all other interfering components. Thus, recoveries were found to be within a range of 97-103% for most REEs with relative standard deviations of 2-5%.

Semi-quantitative chemical analysis of hard coatings by Raman micro-spectroscopy: the aluminium chromium nitride system as an example.

A new method for chemical analyses of nitride-based hard coatings is presented. Raman band shifts in the spectra of Al(x)Cr(1-x)N coatings, deposited by physical vapour deposition from Al(x)Cr(1-x) targets with x (T,Al) = 0, 0.25, 0.50, 0.70 and 0.85, are calibrated using compositional data of the coatings derived by elastic recoil detection analysis (ERDA) and electron probe micro-analysis (EPMA). Inserting the composition-dependent Raman shift of a combinatorial acoustic-optic lattice mode into an empirically derived equation allows the determination of Al/Cr ratios of the coating with an accuracy of about +/-2%. Spot, line and area analyses of coated cemented carbide and cold work steel samples by using a computer-controlled, motorized x,y-stage are demonstrated and the most important errors influencing precision and accuracy are discussed. Figure Raman map of a coated cold-work steel sample.

Combined analysis of kidney stones by X-ray diffraction and electron microprobe.

Oxalate, apatite, struvite, uric acid and cystine stones were routinely analysed by X-ray diffraction. A second analysis was performed by electron microprobe. The substances not detected by X-ray diffraction were apatite and struvite in oxalate and cystine stones. Oxalate was not found in uric acid stones because of insufficient routine sample preparation, but could be detected in a second X-ray analysis. Conclusions concerning the exact stone composition can only be reached after X-ray diffraction has been completed in conjunction with a second procedure, such as electron microprobe analysis. For clinical routine use X-ray diffraction is sufficient if adequate sample preparation is performed. The electron microprobe analysis provides further information about mixed phase formations (single or multiple layers, diffuse distributions etc.) and about inclusions in a phase, which have some clinical consequences.

Trace element investigations in kidney stone patients.

31 different trace elements were analyzed in 24 kidney stones using the atomic absorption method. Where a significant trace element content in the concrements was detected, blood, urine and hair from the stone patients were investigated with respect to their trace element concentrations. In calcium stones mainly Fe, Pb, Sr and Zn and in organic stones As, Fe and Zn were found. No correlation could be found between the trace element content in stones, blood and urine. The hair of a woman with high As content in her stone contained a normal As concentration.

[Analysis of a dacrolith ]. / Analyse eines Dakryolithen.

Dacryoliths are uncommon and there are only a few reports in the literature. In a patient with recurrent stenosis of the lacrimal drainage system a lacrimal stone (dacryolith) was removed from the lacrimal sac during dacryocystorhinostomy. A histological and immunohistochemical examination was performed and keratin antibodies could be detected. In a chemical analysis calcium, sulfur and some phosphorus were determined as major constituents.

Intraperitoneal cholelithiasis after laparoscopic cholecystectomy--behavior of 'lost' concrements and their role in abscess formation.

UNLABELLED: In two experimental studies we sought preliminary information about the behavior of concrements lost in the peritoneal cavity during laparoscopic cholecystectomy. MATERIALS AND METHODS: In study 1, human gallstones were analyzed using X-ray diffraction, classified in three groups and examined with an ultramicroscope; then they were implanted in the peritoneal cavity of rats. After 8 weeks or 6 months, the animals were sacrificed and the concrements analyzed again as before. The tissues surrounding the calculi were also examined histologically. In study 2, human gallstones were examined with regard to bacterial contamination on the surface or in the middle of the calculi. The cholesterol content was analyzed, and the stones were divided into three groups and implantated in the rats as in the first study. After 8 weeks, the animals were sacrificed and areas with identifiable tissue reactions were examined histologically and microbiologically. RESULTS: The concrements lost their crystalline formation without any relation to their former cholesterol content, as shown by X-ray diffraction as well as ultramicroscopy. Mineralogically, these changes are a certain sign of structural dissolution. Cholesterol stones only caused abscess formations in association with gram-negative bowel germs. Sterile pigment concrements often led to a mesenchymal reaction such as granulomas. Contaminated pigment stones also resulted in extensive abscess formations.