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  • 1
    ISSN: 1432-0789
    Keywords: Agriculture ; Flash pyrolysis ; Gas chromatography/mass spectrometry ; Heterocyclics ; Mineral soils ; Organic nitrogen ; Unknown N
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Geosciences , Agriculture, Forestry, Horticulture, Fishery, Domestic Science, Nutrition
    Notes: Abstract Curie-point pyrolysis-gas chromatography mass spectrometry with N-selective detection was used to characterize the structure of organic N compounds in four mineral soils. The technique was found suitable for the fast, sensitive, and highly specific identification of N-containing pyrolysis products from whole soils with total N contents between 0.08 and 0.46%. In order to optimize the methodology, one agricultural soil was pyrolyzed at final temperatures of 573, 773, and 973 K. Almost no chemical alterations to identifiable pyrolysis products were observed when the final pyrolysis temperature was increased from 573 to 973 K. More than 50 N-containing pyrolysis products were identified, and were divided into compound classes chracterized by specific molecular-chemical structures. These included pyrroles, imidazoles, pyrazoles, pyridines, pyrimidines, pyrazines, indoles, quinolines, N derivatives of benzene, alkyl nitriles, and aliphatic amines. Three additional soil samples different in origin and N content were analyzed at 773 K and each showed a specific thermosensitive N-selective chromatogram. Many N-containing pyrolysis products were identified in all samples, which indicated general qualitative regularities in the thermal release of N-containing pyrolysis products from the four soils. In the pyrolyzates of the investigated soils a number of compounds were identified, which is usually not detectable in pyrolysis-gas chromatography spectrometry analyses with N-selective detection of plants and microorganisms. Among these were N derivatives of benzene and long-chain alkyl nitriles, which appear to be soil-specific and suggest significant transformations of organic N in soils. Thus, our results contribute to a better understanding of the molecular-chemical structure of unknown N.
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  • 2
    Electronic Resource
    Electronic Resource
    Springer
    Biology and fertility of soils 24 (1997), S. 249-254 
    ISSN: 1432-0789
    Keywords: Key words Acid hydrolysis ; Agriculture ; Analytical pyrolysis ; Field ionization mass spectrometry ; Gas chromatography/mass spectrometry ; Heterocyclics ; Mineral soils ; Unknown nitrogen
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Geosciences , Agriculture, Forestry, Horticulture, Fishery, Domestic Science, Nutrition
    Notes: Abstract Curie-point pyrolysis-gas chromatography/mass spectrometry (Py-GC/MS) and in-source pyrolysis-field ionization mass spectrometry (Py-FIMS) were applied for the first time to the structural characterization of organic nitrogen in hydrolyzates and hydrolysis residues resulting from the classical 6M HCl hydrolysis of mineral soils. Two well-described soils of widely different origin (i.e., a Gleysol Ah and a Podzol Bh) were investigated. Py-GC/MS was performed using a nitrogen-selective detector to detect and identify N-containing pyrolysis in the hydrolyzate (e.g., pyrazole and/or imidazole, N,N-dimethylmethanamine, benzenacetonitrile, propane- and propenenitriles) and the hydrolysis residue (e.g., pyrroles, pyridines, indoles, N-derivatives of benzene, benzothiazol, and long-chain aliphatic nitriles). Moreover, temperature-resolved Py-FIMS allowed us to record the thermal evolution of the N-containing compounds during pyrolysis. These were characterized by a particularly high thermostability compared to their thermal release from whole soils. The combination of pyrolysis with mass spectrometric methods permitted analyses of the identities and thermal stabilities of complex nitrogen compounds in hydrolysis residues of whole soils, which cannot be done by wet-chemical methods. Pyrolysis-methylation GC/MS with tetramethyl-ammonium hydroxide (TMAH) as methylating agent enabled the identification of N,N-dimethylbenzenamine and so confirmed the identification of benzeneamine by Py-GC/MS in nonmethylated hydrolysis residues. The described N-derivatives of benzene and long-chain nitriles are usually not detectable by pyrolysis-mass spectrometry of plants and microorganisms. These compounds are characteristic of soils, terrestrial humic substances and hydrolysis residues and seem to be specific, stable transformation products of soil nitrogen.
    Type of Medium: Electronic Resource
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