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  • 1
    Electronic Resource
    Electronic Resource
    Springer
    Biology and fertility of soils 26 (1997), S. 1-15 
    ISSN: 1432-0789
    Keywords: Key words Analytical pyrolysis ; Humic substances ; Heterocyclic nitrogen ; 15N NMR ; Mass spectrometry ; Soil organic matter ; Model structure ; Unidentified nitrogen
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Geosciences , Agriculture, Forestry, Horticulture, Fishery, Domestic Science, Nutrition
    Notes: Abstract 1. From the data presented herein it is possible to deduce the following distribution of total N in humic substances and soils: proteinaceous materials (proteins, peptides, and amino acids) – ca. 40%; amino sugars – 5–6%; heterocyclic N compounds (including purines and pyrimidines) – ca. 35%; NH3–19%; approximately 1/4 of the NH3 is fixed NH4 +. Thus, proteinaceous materials and heterocyclics appear to be major soil N components. 2. Natural 15N abundance levels in soils and humic materials are so low that direct analysis by 15N NMR is very difficult or impossible. To overcome this difficulty, the soil or humic material is incubated with 15N-enriched fertilizer. Even incubation in the laboratory for up to 630 days does not produce the same types of 15N compounds that are formed in soils and humic materials over hundreds or thousands of years. For example, very few 15N-labelled heterocyclics are detected by 15N NMR. Does this mean that heterocyclics are not present? Or are the heterocyclics that are present not labelled under these experimental conditions and therefore not detected by the 15N NMR spectrometer ? Another possibility is that a large number of N heterocyclics occur in soils, but each type occurs in very low concentrations. Until the sensitivity is improved, 15N NMR will not provide results that can be compared with data obtained from the same soil and humic material samples by chemical methods and mass spectroscopy. 3. What is most important with respect to agricultural is that all major N forms in soils are available to organisms and are sources of NH3 or NH4 + for plant roots and microbes. Naturally, some of the NH3 will enter the N cycle. 4. From chemical and pyrolysis-mass spectrometric analyses it appears that N heterocylics are significant components of the SOM, rather than degradation products of other molecules due to pyrolysis. The arguments in favor of N heterocyclics as genuine SOM components are the following: a) Some N-heterocyclics originate from biological precursors of SOM, such as proteinaceous materials, carbohydrates, chlorophyll, nucleic acids, and alkaloids, which enter the soil system as plant residues or remains of animals. b) In aquatic humic substances and dissolved organic matter (DOM) at considerably lower pyrolysis temperatures (200 to 300°C), free and substituted N-heterocyclics such as pyrroles, pyrrolidines, pyridines, pyranes, and pyrazoles, have been identified by analytical pyrolysis (Schulten et al 1997b). c) Their presence in humic substances and soils was also detected without pyrolysis by gel chromatography – GC/MS after reductive acetylation (Schnitzer and Spiteller 1986), by X-ray photoelectron spectroscopy (Patience et al. 1992), and also by spectroscopic, chromatographic, chemical, and isotopic methods (Ikan et al. 1992). 5. While we can see light at the end of the tunnel as far as soil-N is concerned, further research is needed to identify additional N-containing compounds such as N- heterocyclics, to determine whether these are present in the soil or humic materials in the form in which they were identified or whether they originate from more complex structures. If the latter is correct, then we need to isolate these complex N-molecules and attempt to identify them.
    Type of Medium: Electronic Resource
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  • 2
    ISSN: 0165-2370
    Keywords: Agave americana ; biopolymers, insoluble, non-hydrolyzable ; cuticle ; gas chromatography ; mass spectrometry ; pyrolysis.
    Source: Elsevier Journal Backfiles on ScienceDirect 1907 - 2002
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
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  • 3
    Electronic Resource
    Electronic Resource
    Amsterdam : Elsevier
    Journal of Analytical and Applied Pyrolysis 17 (1990), S. 275-281 
    ISSN: 0165-2370
    Keywords: Agricultural soils ; compaction ; humus ; mass spectrometry ; mechanical soil strength ; pyrolysis.
    Source: Elsevier Journal Backfiles on ScienceDirect 1907 - 2002
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
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  • 4
    Electronic Resource
    Electronic Resource
    Amsterdam : Elsevier
    Journal of Analytical and Applied Pyrolysis 15 (1989), S. 197-207 
    ISSN: 0165-2370
    Keywords: Field ionization ; intermolecular reactions ; mass spectrometry ; mixtures ; polyesters ; pyrolysis.
    Source: Elsevier Journal Backfiles on ScienceDirect 1907 - 2002
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
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  • 5
    Electronic Resource
    Electronic Resource
    Amsterdam : Elsevier
    Journal of Analytical and Applied Pyrolysis 25 (1993), S. 97-122 
    ISSN: 0165-2370
    Keywords: Agriculture ; ecology ; field ionization ; geochemistry ; mass spectrometry ; pyrolysis ; soil organic matter ; soil science.
    Source: Elsevier Journal Backfiles on ScienceDirect 1907 - 2002
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
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  • 6
    Electronic Resource
    Electronic Resource
    Amsterdam : Elsevier
    Journal of Analytical and Applied Pyrolysis 12 (1987), S. 149-186 
    ISSN: 0165-2370
    Keywords: Fulvic acids ; humic acids ; mass spectrometry ; pyrolysis ; soil profiles ; whole soils.
    Source: Elsevier Journal Backfiles on ScienceDirect 1907 - 2002
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
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  • 7
    ISSN: 0165-2370
    Keywords: Fulvic acids ; gas chromatography ; humic acids ; humins ; humus ; mass spectrometry ; pyrolysis.
    Source: Elsevier Journal Backfiles on ScienceDirect 1907 - 2002
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
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  • 8
    Electronic Resource
    Electronic Resource
    Amsterdam : Elsevier
    Journal of Analytical and Applied Pyrolysis 11 (1987), S. 465-498 
    ISSN: 0165-2370
    Keywords: Cellulose ammonium phosphate ; fire-resistant materials ; mass spectrometry ; polymers ; pyrolysis ; transition metal complexes.
    Source: Elsevier Journal Backfiles on ScienceDirect 1907 - 2002
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
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  • 9
    Electronic Resource
    Electronic Resource
    Springer
    Fresenius' Zeitschrift für analytische Chemie 302 (1980), S. 387-392 
    ISSN: 1618-2650
    Keywords: Best. von Tritium in Steroiden ; Massenspektrometrie ; Felddesorption ; Isotopenverteilg. in Biochemikalien
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Summary The first application of field desorption mass spectrometry (FD-MS) to the determination of the label content and the statistical isotopic distribution in radiolabelled substances is reported. The total amount of tritium in steroids such as [6,7-3H]estradiol and [2,4,6,7-3H]estradiol was estimated. Data are easily derived from the field desorption mass spectra which allow the calculation of the distribution of the radioisotope in the investigated biochemicals with an accuracy below 1%. The two main advantages of the technique reported here are the small sample consumption in the nanogram range (which is particularly important for radiolabelled chemicals of high specific activity) and the highmolecular ion abundance of polar substances (the thermal and mass spectrometric fragmentation is almost completely missing) which give optimal information about the isotopic composition of the intact molecule. In addition, the short analysis time by FD-MS of approximately 30 min for the complete isotopic determination and the good precision of a few tenths of a percent underline the utility of this new method for the assay of radioisotopes in compounds of biochemical, medical and environmental interest.
    Notes: Zusammenfassung Die erste Anwendung der Felddesorptions-Massenspektrometrie (FD-MS) für die Bestimmung des Markierungsgrades und der statistischen Isotopenverteilung in radioaktiv markierten Verbindungen wird beschrieben. Der Gesamtgehalt von Tritium in Steroidhormonen, wie [6,7-3H]Östradiol und [2,4,6,7-3H]Östradiol, wurde mit einem Fehler unter 1% quantitativ bestimmt. Aus den Felddesorptions-Massenspektren lassen sich leicht Daten ableiten, die die Berechnung der Verteilung des Radioisotops in den untersuchten Biochemikalien ermöglichen. Zwei Hauptvorteile der beschriebenen Methode sind: 1) der geringe Probenverbrauch im Nanogrammbereich — dies ist gerade im Hinblick auf die geltenden Vorschriften für den Strahlenschutz von besonderer Bedeutung für radioaktiv markierte Verbindungen mit hoher spezifischer Aktivität — und 2) da die thermischen und massenspektrometrischen Fragmentierungen fast völlig fehlen, liefern die hohen relativen Intensitäten der Molekülionen von polaren Substanzen die optimale Information über die isotopische Zusammensetzung des intakten Moleküls. Darüber hinaus ergibt sich aus den kurzen Analysenzeiten von etwa 30min für eine komplette Isotopenbestimmung und aus der hohen Präzision von einigen Zehntel Prozent die Brauchbarkeit des beschriebenen neuen Verfahrens zur Bestimmung von Radioisotopen in Verbindungen, die für Biochemie, Medizin und Umweltforschung von Interesse sind.
    Type of Medium: Electronic Resource
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  • 10
    Electronic Resource
    Electronic Resource
    Springer
    Fresenius' Zeitschrift für analytische Chemie 284 (1977), S. 193-195 
    ISSN: 1618-2650
    Keywords: Gemischanalyse von polycyclischen Kohlenwasserstoffen ; Quantitative Massenspektrometrie ; Felddesorption
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Zusammenfassung Die Molekülionen von Gemischen polycyclischer Kohlenwasserstoffe wurden auf der Photoplatte eines hochauflösenden Felddesorptions-Massenspektrometers registriert. Die erhaltenen Schwärzungsintensitäten wurden mit der relativen Konzentration der eingesetzten Mischungskomponenten verglichen. Proben im Mikrogrammbereich ergaben Abweichungen von etwa ± 5%.
    Notes: Abstract The molecular ions of mixtures of polycyclic hydrocarbons were recorded on the photographic plate of a high resolution field desorption mass spectrometer. The blackening intensities obtained were compared with the relative concentration of the employed components of the mixture. Samples in the μg range yielded deviations of about ± 5%.
    Type of Medium: Electronic Resource
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