Application of pressurized sample preparation methods for the analysis of steels and copper alloys

Pressurized sample preparation devices (High Pressure Asher, Pressurized Microwave Digestion system, compared with a PTFE decomposition vessel) were used to dissolve certified metal alloy samples (steel, copper) for ICP analysis. Based on the results of the analysis it was established that both up-to-date devices can be advantageously applied to quickly and quantitatively dissolve metal alloy samples. To dissolve the samples, two different kinds of acid mixtures (A: nitric and hydrochloric acid; B: nitric and hydrochloric and sulphuric and phosphoric acid) were used. The sample preparation is simpler and less time-consuming than the earlier commonly used methods, sample loss and degree of contamination are also reduced. Steel samples containing tungsten, titanium and niobium (less than 0.5%) can only be analyzed using a mixture of the four acids. By dissolving steel samples in the nitric and hydrochloric acid mixture, the concentration of their most common elements (Cr, Ni, Mn, V, Cu) as well as their S and P content can be determined. Copper alloy samples can be dissolved quickly by the pressurized microwave decomposition device using hydrochloric acid and diluted (1:1) nitric acid.     

Oxorhenium(V) dithiolates catalyze the oxidation by tert-butyl hydroperoxide of sulfoxides and sulfides, including 4,6-dimethyldibenzothiophene

tert-Butyl hydroperoxide (TBHP) efficiently converts a wide variety of sulfides to sulfoxides and sulfones. The method offers the advantage that one product or the other can be obtained in high purity by a modest variation of conditions. The reactions occur smoothly at 25minus sign50 C in chloroform and, to the extent studied, in toluene and methylene chloride. A catalyst is required; the most extensively studied was MeReO(mtp)PPh(3), 1, where mtpH(2) is 2-(mercaptomethyl)thiophenol. Other chelating dithiolate ligands can be used with comparable results. These oxidations were tested for dialkyl, alkylminus signaryl, and diaryl sulfides; thiophenes; and thianthrene. Even the "hard" sulfide, 4,6-dimethyldibenzothiophene (DMDBT) was quantitatively oxidized to the dioxide with TBHP:DMDBT 3.0-3.5 and 0.05-3.8 mol % 1. The mechanism was explored in kinetics studies carried out only for methyl tolyl sulfide. The product buildup curve was complex, with an induction period followed by a rapid growth phase. The kinetic data could be modeled adequately but not perfectly by allowing five rate constants to refine. Their values are consistent with the chemical sense of the mechanism.     

Synthesis of N,N'-Diacyl-1,2-di-(4-pyridyl)ethylenedianiines

Reaction of N-(4-pyridylmethyl)benzamide N-oxides with acetic anhydride yielded dimerization compounds. This dimerization occurs at the atom attached to the pyridine ring. These compounds so obtained were evaluated for analgesic and antiinflammatory activity.     

Determination of total iron in standard rocks by spectrophotometric titration with EDTA

A method for the determination of total iron in silicate rocks is described. It is based on spectrophotometric titration of iron(III) with EDTA after decomposition in a PTFE bomb. No prior separation of interfering elements is needed. The method was tested by analysis of the U.S. Geological Survey reference rocks G-2, AGV-1, GSP-1, BCR-1 and PCC-1. The same sample solutions were also analysed by atomic-absorption spectrophotometry. The agreement with published and recommended values was good.     

Stoichiometric hydrogenations using tetracarbonylcobaltate(—I)

Methanolic solutions of tracarbonylcobaltate(—I) in the presence of an acid are simple and useful reducing agents for the selective hydrogenation of conjugated carbon-carbon double bonds. The reaction has the following stoichiometry:

     

Protein surface area and retention in hydrophobic interaction chromatography

Summary Molecular surface areas accessible to a 4 ? diameter spherical probe were calculated from crystallographic data for five proteins: α-chymotrypsinogen A, lysozyme, trypsinogen, ribonuclease A and ribonuclease S. The retention factors of various proteins were measured on stationary phases having polyether- and phenylligates and with aqueous eluents containing (NH₄)₂SO₄, Na₂SO₄ or NaCl at pH 7.0. The logarithmic retention factors were plotted against the salt molality and the hydrophobic interaction parameters evaluated from the limiting slopes of the plots at high salt concentrations for the proteins in the chromatographic systems investigated. The hydrophobic interaction parameters thus obtained were linear in both the molecular surface areas of the proteins and the molal surface tension increments of the salts. The experimental results obtained with these relatively simple proteins of known molecular structure, which were available in high purity, support earlier theoretical predictions for the dependence of the hydrophobic interaction parameter on the surface area of the protein and the surface tension raising effect of the salt.     

Coloring linear hypergraphs: the Erdős–Faber–Lovász conjecture and the Combinatorial Nullstellensatz

Designs, Codes and Cryptography - The long-standing Erdős–Faber–Lovász conjecture states that every n-uniform linear hypergaph with n edges has a proper vertex-coloring using...     

Certain graphs with exactly one irreducible T-module with endpoint 1, which is thin

Journal of Algebraic Combinatorics - Let $$\Gamma $$ denote a finite, simple and connected graph. Fix a vertex x of $$\Gamma $$ and let $$T=T(x)$$ denote the Terwilliger algebra of $$\Gamma $$ with...     

Polarographische Bestimmung des Pyridoxols in pharmazeutischen Präparaten

Zusammenfassung Es wird eine neue polarographische Methode zur direkten Bestimmung des Pyridoxols in Injektionspräparaten und Tabletten beschrieben. Die ausgearbeitete Methode beruht auf der polarographischen Reduktion des Pyridoxolmoleküls im Milieu von Ammoniak-Ammoniumchlorid-Puffern und weiter auf der Bildung einer katalytischen Stufe des Pyridoxols in Veronalpuffern. Die polarographische Methode ist rascher und in manchen Fällen genauer und empfindlicher als die bisher in Gebrauch stehenden Methoden. Die Anwesenheit der in den Präparaten laufend vorkommenden Begleitstoffe des Pyridoxols stört nicht die polarographische Bestimmung. Die Methode kann auch zur Bestimmung des 3-Hydroxy-4-methoxymethyl-5-oxymethyl-2-methylpyridins benutzt werden, das ein Zwischenprodukt bei der Pyridoxolerzeugung ist.

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Summary A new polarographic method is described for the direct determination of pyridoxol in injection preparations and tablets. This method is based on the polarographic reduction of the pyridoxol in ammonia-ammonium chloride buffer medium and also on the formation of a catalytic stage of the pyridoxol in veronal buffers. The polarographic method is faster and in many cases more accurate and more sensitive than the methods now in use. The presence of the materials which always accompany the pyridoxol in the preparations does not interfere with the polarographic determination. The method can likewise be used for determining 3-hydroxy-4-methoxymethyl-5-oxymethyl-2-methylpyridine, which is an intermediate product in the manufacture of pyridoxol.

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Résumé On décrit une nouvelle méthode polarographique pour le dosage direct du pyridoxol dans les préparations pour injections et dans les comprimés. La méthode élaborée repose sur la réduction polarographique de la molécule de pyridoxol dans le milieu tampon ammoniaque-chlorure d'ammonium, et, en outre, sur la formation d'une phase catalytique du pyridoxol dans les tampons au véronal. La méthode polarographique est plus rapide et dans de nombreux cas plus exacte et plus sensible que les méthodes utilisées jusqu'ici. La présence d'impuretés existant couramment dans les préparations à côté du pyridoxol ne gêne pas le dosage polarographique. On peut aussi utiliser la méthode pour le dosage de l'hydroxy-3 méthoxyméthyl-4 oxyméthyl-5 méthyl-2 pyridine, substance intermédiaire dans la préparation du pyridoxol.

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Herrn Dr.P. Zuman danken wit für Ratsehläge bei der Abfassung dieser Arbeit.     

Generalized Sidon sets of perfect powers

The Ramanujan Journal - For $$h \ge 2$$ and an infinite set of positive integers A, let $$R_{A,h}(n)$$ denote the number of representations of the positive integer n as the sum of h distinct terms...