Chemical analysis and distribution investigation of trace elements in indium matrix by spark source mass spectrometry

Summary High-purity indium was analysed by spark source mass spectrometry, using electrical and photoplate detection. For the calibration of the differences in elemental sensitivity, a standard sample was prepared in which 10 impurities were determined by graphite furnace atomic absorption spectrometry. In this way accuracies of less than 40% were obtained for relatively homogeneous elements at ppm and sub-ppm level. About 40 elements could be determined with detection limits of 10 to 30 ppb. Two pattern recognition methods, principal component analysis and clustering analysis, were applied to obtain information on trace element distribution, which indicated that a number of elements were strongly spatially correlated in the analysed sample.

---

Chemische Analyse und Verteilungsbestimmung von Spurenelementen in Indium-Matrix durch Funkenquellen-Massenspektrometrie

---

On leave from: Department of Chemistry, Nanjing Normal University, Nanjing, People's Republic of China     

Tube-excited energy-dispersive X-ray fluorescence analysis. II. Energy-dispersive X-ray fluorescence analysis of air particulate material.

The use of monoenergetic exciting radiation of molybdenum obtained with a secondary target set-up, a conventional water-cooled tungsten anode x-ray tube and a Si(Li) semiconductor detector permits many trace and minor constituents from chlorine to strontium to be determined in particulate material collected on cellulose filters. The method is rapid and economical compared to other multielement techniques. The use of one or more single-element thin-film standards to calibrate for the analysis of many elements appears to be possible, but some systematic errors must be prevented. Absorption of the fluorescent radiation is remedied by a simple correction method. The precision and the accuracy of the method were critically examined by independent analysis of a number of samples with instrumental neutron activation analysis and by interlaboratory comparisons on the same samples.     

BRCA1 mutation screening using restriction endonuclease fingerprinting-single-strand conformation polymorphism in an automated capillary electrophoresis system

Efficient mutation scanning techniques are needed for the rapid detection of novel disease-associated mutations and rare-sequence variants of putative importance. The large size of the breast cancer 1 gene (BRCA1) and the many mutations found throughout its entire coding sequence make screening for mutations in this gene particularly challenging. We have developed a method for screening exon 11 of the BRCA1 gene based on restriction enzyme digestion of fluorescence-labeled polymerase chain reaction (PCR) products followed by single-strand conformation polymorphism (SSCP) using an automated capillary electrophoresis system, denoted capillary restriction endonuclease fingerprinting (REF)-SSCP electrophoresis. Using this strategy on a control set of samples, we were able to detect 17 of 18 known sequence alterations. The method was then applied to screen 73 Norwegian females with family histories of breast and/or ovarian cancer. A total of 172 sequence alterations were detected, including substitutions, insertions, and deletions. One novel substitution of unknown function was identified. Sequencing of all samples negative in the capillary REF-SSCP system gave no additional mutations confirming the high sensitivity of the described methodology. Capillary REF-SSCP electrophoresis appeared as a technically convenient technique, requiring amplification of fewer PCR fragments than traditional SSCP. The novel strategy allows high-throughput mutation scanning without radioactive labeling and polyacrylamide gel electrophoresis (PAGE).     

Implementation of an expert system for the qualitative interpretation of X-ray fluorescence spectra

The implementation of an expert system for the automated qualitative interpretation of energy-dispersive x-ray spectra is discussed. The first step in the interpretation process is the extraction of the relevant data from the spectrum, which is done by a preprocessor program, written in FORTRAN. The expert system itself consists of three parts. The knowledge base contains specific information on energy-dispersive x-ray fluorescence spectrometry presented in the form of IF/THEN rules. The data base contains the reduced spectral data and an array of certainty factors associated with each element; the certainty factor for an element represents the probability of its being present in the sample from which the spectrum was taken. Finally, the inference engine performs manipulation of the knowledge. For a particular state of the data base, the certainty factors for all the elements are iteratively modified until convergence is reached by using the rules from the knowledge base. During each cycle, the inference engine selects one rule from the knowledge base and executes it. Rules are selected on the basis of the chemical elements contained in their IF part and according to their previously assigned focus levels. Execution of the THEN part of the selected rule modifies the certainty factors of a number of elements. At the end of the interpretation session, the system lists the elements which have a high probability of being present in the sample. Optionally, the user can be provided with explanations of the reasoning steps taken during the interpretation. Application of the expert system to a particular spectrum shows that it is useful for the reliable interpretation of spectral data obtained from electron microprobe analysis of industrial aerosol particles.     

Classificatin of chinese tea samples according to origin and quality by principal component techniques

Three categories of tea, black, green and oolong tea, with those varieties in each category were analyzed for their contents of cellulose, hemicellulose, lignin, polyphenols, caffeine and amino acids. The data were subjected to multivarige analysis. Principal component analysis and principal component classification provide discrimination between the different categories and varieties. The quality index, assigned to these tea standards by experts, could be predicted form the principal component scores.     

Syntheses of (S)-(+)-trihexyphenidyl hydrochloride and (S)-(+)-procyclidine hydrochloride, two anticholinergics, using (S)-(-)-3-cyclohexyl-3-hydroxy-3-phenylpropanoic acid as chiral synthon

The absolute configuration of the more active (-)-enantiomer of the anticholinergic trihexyphenidyl hydrochloride has been established as (R) by syntheses of (S)-(+)-procyclidine hydrochloride, whose absolute configuration has been established previously, and (S)-(+)-trihexyphenidyl hydrochloride from the same chiral building block, viz. (S)-(-)-cyclohexyl-3-hydroxy-3-phenylpropanoic acid. Both enantiomers of this chiral synthon were prepared by optical resolution of the corresponding racemate, employing (R)- and (S)-1-phenylethylamine, respectively, as resolving agents.     

Energy-dispersive x-ray fluorescence analysis for sulphur,chlorine, potassium and calcium in aerosols

Problems in the use of x-ray spectrometry for the fast multi-element analysis of environmental samples such as aerosols collected on filters arise from absorption of the fluorescence intensity in the filter and in the collected matter. A procedure is described for the determination of the elements sulphur to calcium in aerosols collected on Whatman 41 filters. Two methods are compared for deconvolution of the spectra. These are based on counting in fixed energy channels or on non-linear least-squares analysis. Corrections for absorption effects have been calculated. Calibration is done with thin film standard deposits. The accuracy of the method is better than 15%. Difficulties in ascertaining the chlorine content of the filter are discussed. The evaporation of the chlorine fraction from the filter was studied in detail.     

Pseudochelin A,a siderophore of Pseudoalteromonas piscicida S2040

A new siderophore containing a 4,5-dihydroimidazole moiety was isolated from Pseudoalteromonas piscicida S2040 together with myxochelins A and B, alteramide A and its cycloaddition product, and bromo- and dibromoalterochromides. The structure of pseudochelin A was established by spectroscopic techniques including 2D NMR and MS/MS fragmentation data. In bioassays selected fractions of the crude extract of S2040 inhibited the opportunistic pathogen Pseudomonas aeruginosa. Pseudochelin A displayed siderophore activity in the chrome azurol S assay at concentrations higher than 50 μM, and showed weak activity against the fungus Aspergillus fumigatus, but did not display antibacterial, anti-inflammatory or anticonvulsant activity.     

Pore-Scale Level Set Simulations of Capillary-Controlled Displacement with Adaptive Mesh Refinement

Transport in Porous Media - Multiphase flow simulations on imaged porous rock structures require numerical methods that are accurate and robust when applied on complex geometries. A key element in...     

A non-Gaussian Ornstein–Uhlenbeck model for pricing wind power futures

The recent introduction of wind power futures written on the German wind power production index has brought with it new interesting challenges in terms of modelling and pricing. Some particularities of this product are the strong seasonal component embedded in the underlying, the fact that the wind index is bounded from both above and below and also that the futures are settled against a synthetically generated spot index. Here, we consider the non-Gaussian Ornstein–Uhlenbeck type processes proposed by Barndorff-Nielsen and Shephard in the context of modelling the wind power production index. We discuss the properties of the model and estimation of the model parameters. Further, the model allows for an analytical formula for pricing wind power futures. We provide an empirical study, where the model is calibrated to 37 years of German wind power production index that is synthetically generated assuming a constant level of installed capacity. Also, based on 1 year of observed prices for wind power futures with different delivery periods, we study the market price of risk. Generally, we find a negative risk premium whose magnitude decreases as the length of the delivery period increases. To further demonstrate the benefits of our proposed model, we address the pricing of European options written on wind power futures, which can be achieved through Fourier techniques.