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  • 1
    Electronic Resource
    Electronic Resource
    Springer
    Microchimica acta 86 (1985), S. 85-100 
    ISSN: 1436-5073
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Different combined procedures involving element preconcentration and ICP-OES or polarography are described for the determination of the alpha emitters uranium and thorium in aluminium. The results are compared with those of instrumental neutron activation analysis. After extraction with ethyl acetate, uranium and thorium can be determined by ICP-OES (uranium detection limit, given as 3so, 12 ng/g, standard deviation 0.95 ng/g at 12.5 ng/g; thorium detection limit 8 ng/g, standard deviation 0.9 ng/g at 12.5 ng/g). After a second extraction with tri-n-octyl phosphine oxide, uranium can be determined by polarography (detection limit 10 ng/g, standard deviation 4.4 ng/g at 200 ng/g). Thorium also can be coprecipitated with Fe(OH)3 and determined with ICP-OES (detection limit 5 ng/g, standard deviation 0.6 ng/g at 10 ng/g). The results obtained by wet chemical analyses lie within the spread of accuracy of the INAA results obtained by several laboratories. In general, the comparative results indicate that super pure aluminium containing less than 1 ng/g uranium and thorium can be produced.
    Type of Medium: Electronic Resource
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  • 2
    Electronic Resource
    Electronic Resource
    Springer
    Fresenius' Zeitschrift für analytische Chemie 343 (1992), S. 734-740 
    ISSN: 1618-2650
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary At VAW today, high-purity aluminium is analysed using three analytical procedures as a matter of routine. When the set purity requirements are lower, spark emission spectrometry (OES) is used; for higher purity requirements, mass spectrometry (GDMS) and instrumental neutron activation analysis (INAA) are employed. The efficiency of these routine methods is described briefly. Reliable VAW reference samples, as well as regular comparison tests, serve as a basis for analytical quality assurance. The quality of these reference materials and of high-purity aluminium analysis has been attested by round-robin analysis, using different analytical procedures, and by experienced analytical laboratories. Several multi-step procedures are described to illustrate the methods of operation. Today ICP-MS also belongs to these, a useful addition to the special multi-step procedures for the determination of individual elements and to multistep procedures with atom spectrometrical end determination. ICP-MS is an efficient alternative method for routine trace analysis work.
    Type of Medium: Electronic Resource
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  • 3
    Electronic Resource
    Electronic Resource
    Springer
    Fresenius' Zeitschrift für analytische Chemie 354 (1996), S. 811-817 
    ISSN: 1618-2650
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The existence of isobaric and polyatomic ion interferences has been considered to be a significant shortcoming of inductively coupled plasma – mass spectrometry (ICP-MS). In the special case of Mo-Zr-alloys problems caused by polyatomic ions are substantial. The determination of trace elements by using classical univariate linear regression of single signals or any correction equations presented by the instrumental software is impossible. There are various possibilities to overcome spectral interferences, in principle. The application of high-resolution ICP-MS, separation methods or alternative sample introduction systems is limited by the high cost and the apparative expenditure. In this report methods of multisignal calibration, like partial least squares (PLS) regression and canonical correlation analysis (CCA), are used to overcome isobaric or chemical interferences in ICP-MS. It is shown, that PLS and CCA are able to handle or tolerate, respectively, spectral interferences existing in a Mo-Zr-O-H-F system. The results of quantitative analysis provided by PLS and CCA were comparable.
    Type of Medium: Electronic Resource
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  • 4
    Electronic Resource
    Electronic Resource
    Springer
    Fresenius' Zeitschrift für analytische Chemie 314 (1983), S. 466-468 
    ISSN: 1618-2650
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Zusammenfassung Für die Bestimmung hoher Siliciumgehalte wurde eine wirtschaftliche und leistungsfähige naßchemische Methode entwickelt. Sie wurde an AlSi-Legierungen, Zeolithen, Natriummetasilikat und Wasserglas erprobt und eignet sich auch für Ferrosilicium. Grundlage des Verfahrens ist die Umsetzung von Fluorid mit Kieselsäure zu Hexafluorosilicat unter Freisetzung von Hydroxidionen. Die Hydroxidionen werden acidimetrisch mit Salzsäure titriert. Freies Alkali wird vor der Fluoridzugabe neutralisiert. Störende Aluminium-, Eisen- und einige andere Metallionen werden durch Extraktion mit Acetylaceton in Chloroform abgetrennt. Borat wird miterfaßt und muß durch gesonderte Bestimmung berücksichtigt werden. Die Methode ist für Siliciumgehalte über 2% (w/w) geeignet und kann innerhalb von 30 min durchgeführt werden. Die Varianz beträgt 〈1% bei Gehalten bis 20% und 〈0,5% bei Gehalten bis 40%.
    Notes: Summary A wet-chemical method, which is both efficient and economic, has been developed for the determination of high silicon contents. It was tested with AlSi alloys, zeolites, sodium metasilicate and waterglass, and can also be applied to ferrosilicon alloys. The method is based on the reaction of fluoride ions with silicic acid to form hexafluorosilicate and hydroxide ions. Caustic soda is neutralized before adding fluoride and the hydroxide ions are titrated acidimetrically. Interfering metal ions, as aluminium, iron and others, are removed by extraction with acetylacetone in chloroform. Borate also interferes and must be taken into account by separate determination. The method, which takes about 30 min, can be used for silicon contents above 2% (w/w). The variation is 〈1% for contents up to 20% and 〈0.5% for those up to 40%.
    Type of Medium: Electronic Resource
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