Eine neue papierchromatographische Methode zum Nachweis von Blei

Zusammenfassung Es wird über eine papierchromatographische Methode zum Nachweis von Bleiverunreinigungen in Schwermetallsalzen berichtet, die auf dem Unterschied zwischen der Löslichkeit des Bleisulfats und der übrigen Schwermetallsulfate beruht. Als Lösungsmittel wird das durch Rex u. Diller vorgeschlagene Gemisch Methanol-Schwefelsäure-Wasser verwendet. Nach der Chromatographie bleibt das Blei auf der Startlinie, während die übrigen Metalle mit R_f-Werten von 0,7–0,9 wandern. In den untersuchten Co²⁺-, Ni²⁺-, Cd-, Zn- und Cu-Salzen konnten im allgemeinen Bleiverunreinigungen von 30 g/g (=0,003%) nachgewiesen werden. Ni-, Cd- und Cu-Sulfate bleiben gleichfalls auf der Startlinie zurück, weshalb in diesen Salzen das Blei nach der beschriebenen Methode nicht nachgewiesen werden kann.Herrn Prof. Dr. A. Végh sind wir für die Unterstützung unserer Arbeit zu Dank verpflichtet.     

Ready-made matrix-assisted laser desorption/ionization target plates coated with thin matrix layer for automated sample deposition in high-density array format.

The methodology for ready-made matrix-assisted laser desorption/ionization (MALDI) target plates covered with an optimized thin layer consisting of matrix and nitrocellulose has been developed. Piezoelectric microdispensing enabled sample depositions in a high-density array format of 2000 sample depositions on a conventionally sized target plate (45 x 47 mm). The sample depositions were made reproducibly in a fully automated mode by using an in-house developed computer-controlled piezoelectric flow-through microdispenser. Additionally, the piezoelectric technique facilitated significant analyte enrichment that increased the detection sensitivity. The MS signal was obtained rapidly, generally within ten laser pulses. An airbrush device was used to generate a fine spray of matrix and nitrocellulose dissolved in acetone. The acetone evaporated instantly when reaching the target plate leaving the entire surface with a thin and uniform matrix/nitrocellulose coating consisting of very small crystals of matrix embedded in the nitrocellulose. These crystals acted as a seed-layer on subsequent analyte depositions, rendering homogeneous sample spots when using alpha-cyano-4-hydroxycinnamic acid (CHCA) as matrix. The relative standard deviation of the signal intensity between spots was (20-30)% (n = 30). The detection sensitivity was improved by restricting the sample spot diameter to 300 microm. The spot size was affected by the deposition rate and the evaporation rate of the dispensed sample volume. Mass spectra of a 25-amol peptide mixture deposition were successfully recorded.     

Polynomials dertermined by a few of their coefficients

We prove some results which indicate that a monic polynomial over a field of characteristic zero with exactly κ distinct zeros may be determined up to finitely many possibilities by any κ of its nonzero proper coefficients.     

Calorimetric test of purity II

Dynamic and stepwise purity test techniques were compared, and it was established that in dynamic measurement the sample in many cases can not be considered to be in a state of equilibrium from the thermodynamic aspect. The problems of the measuring time and the accuracy of the results are discussed for the two-peak method, applicable for the processing of data obtained by the stepwise technique. It was established that the two-peak method can be improved. By using several peaks, the accuracy of the results and measuring time can be optimized.     

Identification of the IR frequencies of the interstitial carbon atom in some M6C (M = Fe,Ru) carbonyl clusters by13 C-enrichment

¹³C-enriched carbido carbonyl clusters of the type [M₆C(CO) _n ] ^z? (M=Fe,n=16,z=2; M=Ru,n=16 ifz=2 andn=17 ifz=0) have been prepared and their IR spectra observed in the 900?600 cm^?1 region; the band shifts occurring upon¹³ C substitution enable the assignment to the stretching modes of the interstitial C atom. Band patterns reflect the symmetry of the M₆C core, but the frequencies seem dependent on other molecular features.     

Preparation dependent superconductivity in TlCaBa2Cu3O7.5±d above 100 K

Different heat treatment procedures were applied during sample preparation, which resulted in different superconducting properties in samples of the same nominal composition, TlCaBa₂Cu₃O_7.5±d . This manifests itself in different critical temperatures: 104 K, 107 K and 93 K. The highestT _c belongs to the best-crystallized samples in which the tetragonal Tl₂Ca₁Ba₂Cu₂O_8±d phase is responsible for the superconductivity. The effect of heat treatments is reflected in the structural and magnetic properties as well.