Towards validating a method for two-dimensional electrophoresis/silver staining

Two-dimensional electrophoresis (2-DE) is a technique involving numerous steps, many of them to be performed manually. Hence, some operator dependency must be taken into account. An attempt to elucidate the reliability of 2-DE combined with silver staining is presented, employing the general practice to validate a method in pharmaceutical analysis. Most proteomic studies employing 2-DE aim at qualitative or quantitative differences in protein expression. One of the most sensitive and broadly applied staining techniques is silver staining. In order to gain information on accuracy, precision, linearity, and ruggedness of this technique, gels were run in replicates with different amounts of protein from a complex standard sample. In addition, sets of gels were repeated by two different operators in a second independent laboratory equipped with identical hardware and software. Our results show that reliable qualitative data on differential protein expression can be obtained by 2-DE, nevertheless replicate gels should be run and experimental conditions have to be kept stringently to a standardized protocol. Quantitative data are just achievable with spots, which are well-resolved, of high quality, with an optical density (OD) above a certain threshold (OD > 10), and which show a linear response. Quantitative differences occurring due to method-derived deviations may easily be misinterpreted as true changes in protein expression. After normalization, relative standard deviation (RSD) values of approximately 30% (n = 4) could be obtained, therefore minor changes (< 50%) should be critically reviewed.     

Analytical electron microscopy studies of lithium aluminum hydrides with Ti- and V-based additives

The microstructure of LiAlD(4) with TiCl(3).1/3(AlCl(3)) and VCl(3) additives has been studied during different steps of the decomposition process using electron energy loss spectroscopy and energy-dispersive X-ray spectroscopy in a scanning transmission electron microscope. Energy filtered transmission electron microscopy was used to show elemental distributions in the samples. The spatial distribution of the additives and the main elements within the alanate particles was examined with a resolution of a few nanometers. The analysis of the electron energy loss spectra reveals the chemical state of Al, O, and the additives. Ti and V do not appear to mix chemically with Al to a significant degree. V was found in high concentration in just a few particles, while Ti is more uniformly distributed. All the samples showed evidence of oxidation despite procedures being adopted to avoid exposing the material to air. The additives are oxidized in all the samples, and Al(2)O(3) forms a thin layer at the surface of the particles. This paper gives a comparison between samples at different stages of the decomposition process using different additives.     

A domino ring-closing metathesis as a key-step in the synthesis of chiral lactones from d-mannitol

Chiral lactones were synthesized in six steps from d-mannitol. The key-step was a domino ring-closing metathesis reaction leading to the symmetric cleavage of a d-mannitol triene derivative and to the formation of two molecules of the desired lactone.     

Relaxationserscheinungen in Elektronenstrahlen

In electron beams with high charge density there are observed anomalous shiftings and broadenings as well as symmetrizations of the energy distribution (Boersch 1954). Continuing former work, where these phenomena were ascribed to a relaxation process changing the energy distribution to a new equilibrium distribution, quantitative expressions are derived for the energy spread and the shape of this new energy distribution. Furthermore a relaxation degree is defined which measures the progress of relaxation. Measurements are described with the highest relaxation degrees reached up to now. In addition to the verification of former results up to these new limits the shape of the measured energy-distributions can be fitted to the derived one with suitable choice of a single parameter. Peculiarities of measurements with superposed axial magnetic fields are discussed.     

Cosmological black holes are coloured too

A new solution of the Einstein-Yang-Mills system with axial symmetry and cosmological constant is given here. This new metric, which in the absence of matter becomes the de Sitter universe, is the natural generalization of both a recent result of Perry for stellar (asymptotically flat) black holes and a well-knwn family of solutions of the Einstein-Maxwell system with nonvanishing cosmological constant given some time ago by Carter. Calculations have been carried out making extensive use of the coordinates found by Plebanski.     

Untersuchung komplexer und kovalenter Eisenverbindungen mit Hilfe des Mößbauer-Effekts von Fe57

A number of complex and covalent iron compounds in the oxydation states 0, +2, +3, +6 and with coordination numbers 4, 5, 6 has been investigated at different temperatures. A source of Co⁵⁷ in Pd has been made, which was shown to be well suited for such measurements. The influence of the cristalline environment has been studied by putting iron complexes in different lattices. Ligands of iron complexes have been exchanged to look for influences of different bonds. It has been shown that measurements are also possible in frozen solutions and applications of this method are discussed. It has been found that in Prussian blue and Turnbulls blue there is no socalled electron exchange between the different Fe. The Curie point of KFeS₂ has been determined to be ?28° C and it was possible to study the fields and lineshifts in its neighbourhood. For some compounds indications for their structure and the sign of the electric field gradient could be derived from the data. The data are compiled in tables to allow further discussions from different points of view.     

Zur Mahlerschen Vermutung im Komplexen

Ohne ZusammenfassungVorgetragen am 20. 10. 1959 auf der Tagung der DMV in Münster.