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  • 1
    ISSN: 1618-2650
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Summary The formation of stable diatomic molecules in graphite tube furnaces is described. It is also shown that the new isothermal evaporation techniques in AAS do not lead to complete dissociation of molecules with dissociation energies 〉 3–4 eV. Systematic errors of AA results follow. Systematic studies of the application of diatomic molecules (MX-type) for trace analysis of non-metals (X) were carried out. Many results are given for molecular absorption with electrothermal evaporation (MAS-ETE). Trace determinations in ng level (μl samples) for F, Cl, Br, S and I and their anions are possible. Examples for real analysis are given. Principles of “over-excitation” for improvement of detection limits of non-metals are applied to diatomic molecules. The application of the non-thermal FANES excitation leads to the development of the new method MONES-ETE (molecular non-thermal emission spectrometry with electrothermal evaporation) with detection limits below 1 ng for F, Cl, Br using InX molecules. The application of the principle of laser excited fluorescence leads to the new method LAMOFS-ETE (laser excited molecular fluorescence with electrothermal evaporation) with the upto now best detection limits for F, Cl, Br at pg level using AlBr, InCl, MgF molecules.
    Notes: Zusammenfassung Es wird die Bildung von stabilen, vorwiegend 2-atomigen Molekülen in Graphitrohrküvetten beschrieben. Es wird festgestellt, daß auch die modernen isothermen Verdampfungstechniken bei Molekülen mit Dissoziationsenergien 〉 3–4 eV nicht zur vollständigen Dissoziation führen. Systematische Fehler von AA-Resultaten sind die Folge. Systematische Untersuchungen zur Anwendung 2-atomiger Moleküle vom MX-Typ (z. B. AlF) für die Spurenanalyse von Nichtmetallen (X) werden beschrieben. Umfangreiche Ergebnisse werden zur Molekülabsorption mit elektrothermischer Verdampfung (MAS-ETV) angeführt. Spurenbestimmungen im Nanogramm-Bereich (Mikroliter-Proben) sind möglich für F, Cl, Br, S und I bzw. deren Anionen. Prinzipien der Überanregung werden zur Verbesserung der Nachweisgrenzen von Nichtmetallen auf 2-atomige Moleküle angewendet. Die Anwendung der nichtthermischen FANES-Anregung führt zur Entwicklung der neuen Methode MONES-ETV (Molekül-nichtthermische Emissionsspektroskopie mit elektrothermischer Verdampfung) mit Nachweisgrenzen unterhalb des Nanogramm-Bereichs für F, Cl und Br durch InX-Moleküle. Die Anwendung des Prinzips der laserangeregten Atomfluorescenz führt zur neuen Methode LAMOFS-ETV (laserangeregte Molekülfluorescenzspektrometrie mit elektrothermischer Verdampfung) mit den bisher besten Nachweisgrenzen von einigen Picogramm für F, Cl, Br durch Anwendung der AlBr, InCl und MgF-Moleküle.
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  • 2
    ISSN: 1618-2650
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Heavy metal levels in tooth compartments would appear to be a suitable indicator of long-term exposure. A method has been developed to assess the heavy metal levels (Mn, Cu, Zn, Cd and Pb) in tooth compartments like dentin and enamel. For the simultaneous determination of these elements in small dentin sample amounts (in some cases less than 1 mg) inductively coupled plasma mass spectrometry with electrothermal vaporization was the method of choice. Sample preparation, method development and first results of the application of the method for the analysis of tooth compartments have been described. Variation in the elemental concentrations depending on the kind of tooth and the sampling position have been observed. The method is useful for epidemiological studies of the heavy metal exposure of children.
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  • 3
    ISSN: 1432-1130
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The suitability of eleven modifiers (Pd-, Mg-, K-, Ca- and NH4-salts) for electrothermal vaporization coupled to inductively coupled plasma mass spectrometry (ETV-ICP-MS) for the determination of Mn, Cu, Zn, Cd and Pb has been studied. Solutions containing varying quantities (10–2000 ng absolute) of these salts have been added to four different amounts of analyte to study their suitability as modifier and their mass dependent influence. The best sensitivity enhancement for all elements tested was achieved with IrCl3 and PdCl2. From a comparison of the effect of PdCl2 vs. Pd(NO3)2 it could be concluded that the mechanism of matrix modification also depends on the chemical form of the modifier. Particularly, for the volatile elements Cd and Zn differences in the behavior of the different chemical compounds of one metal (e.g. Pd) is evident, which shows that the enhancement effect is a result of the stabilization of the analytes in the graphite tube prior to vaporization and the improvement of the transport efficiency after vaporization.
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  • 4
    ISSN: 1432-1130
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The determination of iodine in aqueous solutions suffers from several serious problems, caused by the formation of iodine species, derived from the oxidative pretreatment of biological materials. For the determination of these iodine species an ion chromatograph was coupled with an ICP-mass spectrometer. Because of the possible interconversion of the iodine species depending on the pH-value, different eluent-column combinations were used for acidic or alkaline sample solutions, respectively. Iodide, iodate, and several not identified, presumably organo-iodine species could be separated and detected. Unfortunately, the iodine (I2) itself could not be determined with the method proposed. The reaction products of pretreatment are influenced strongly by the matrix. Mixtures of different iodine containing components are received, dependent on the matrix composition and particularly on the pH-value.
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