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  • 1980-1984  (1,166)
  • 1915-1919
  • 1980  (1,166)
  • Inorganic Chemistry  (757)
  • Computational Chemistry and Molecular Modeling  (333)
  • Gas chromatography
  • Nuclear reactions
Material
Years
  • 1980-1984  (1,166)
  • 1915-1919
Year
  • 1
    ISSN: 1432-2048
    Keywords: Boron ; Foliar nutrition ; Nuclear reactions ; Transport (boron) ; Trifolium
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Notes: Abstract The growth of white clover (Trifolium repens L.) is severely inhibited by boron starvation, but a foliar treatment with boric acid can transitorily alleviate the deficiency symptoms. The 10B(n ,α)7 Li nuclear reaction has been used to study boron transport in the plant after foliar application. More than 98% of the boron supplied remained at the point where it was applied to the leaves, and less than 2% was useful to the growth of the treated plant. This small “efficient” portion of boron was quite mobile. It was distributed to the different parts of the plant, then was transferred from the oldest parts to the newly formed leaves. Physiological and agronomical implications of these data are discussed.
    Type of Medium: Electronic Resource
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  • 2
    ISSN: 1432-1076
    Keywords: Phenylketonuria ; Phenylpyruvic acid ; Phenylacetates ; Gas chromatography
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Notes: Abstract There is a steady and nonlinear relationship between the levels of both phenylpyruvic acid (PPA) and o-hydroxyphenylacetic acid (oOPAA) in urine and the plasma levels of phenylalanine (phe) in children more than two years of age with phenylketonuria (PKU). If phe levels in blood rise above 0.35 mM (5.8 mg/100 ml) both aromatic acids are found regularly in urine. Typically, urinary concentrations of PPA are about 5 times higher than those of oOPAA. This report is based on the analysis of 94 samples from 51 children, on or off diet.
    Type of Medium: Electronic Resource
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  • 3
    Electronic Resource
    Electronic Resource
    Springer
    Archives of toxicology 44 (1980), S. 291-297 
    ISSN: 1432-0738
    Keywords: Tetrodotoxin ; 2-Amino-6-hydroxymethyl-8-hydroxyquinazoline ; (C9-base) ; Gas chromatography ; Mass spectrometry ; Autopsy material
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Description / Table of Contents: Zusammenfassung Eine gaschromatographische Methode zum Nachweis von Tetrodotoxin im Obduktionsmaterial wird beschrieben. Das Derivat (2-Amino-6-hydroxymethyl-8-hydroxychinazolin, C9-Base), das sich durch die Einwirkung der Alkalilauge auf Tetrodotoxin gewinnen ließ, wurde schließlich durch Gaschromatographic nachgewiesen. Die Massenspektren der trimethylsilyerten C9-Base werden neben den Ergebnissen der gaschromatographischen Untersuchung von acht tödlichen Intoxikationsfällen angegeben.
    Notes: Abstract A gas Chromatographic method for the detection of tetrodotoxin in autopsy material is described. The derivative (2-amino-6-hydroxymethyl-8-hydroxyquinazoline, C9-base), which was obtained from tetrodotoxin by alkali treatment, was finally detected by gas chromatography. The mass spectra of the trimethylsilylated (TMS) C9-base are presented together with the result of a gas Chromatographic investigation of 8 cases of fatal intoxication.
    Type of Medium: Electronic Resource
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  • 4
    Electronic Resource
    Electronic Resource
    Springer
    International archives of occupational and environmental health 45 (1980), S. 153-161 
    ISSN: 1432-1246
    Keywords: Pentachlorophenol ; High-performance liquid chromatography ; Gas chromatography ; Biological monitoring ; Pentachlorphenol ; Hochdruck-Flüssigkeits-Chromatographie ; Gaschromatographie ; Biological monitoring
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Description / Table of Contents: Zusammenfassung Für die Bestimmung von freiem Pentachlorphenol in der Luft und im Blut wurden leistungsfähige chromatographische Routineverfahren ausgearbeitet. Für die Raumluftbestimmung wird Pentachlorphenol durch Einleiten von Luft in einer Vorlage angereichert und nach Aufarbeitung in freier Form durch Hochdruck-Flüssigkeits-Chromatographie quantitativ erfaßt. Alternativ kann die Analyse nach Derivatisierung durch Kapillar-Gaschromatographie erfolgen. Freies Pentachlorphenol im Vollblut wird nach Aufarbeitung und Derivatisierung durch Kapillar-Gaschromatographie in Verbindung mit dem Elektroneneinfang-Detektor quantitativ bestimmt. Bei den beschriebenen chromatographischen Methoden sind die Eichkurven über den angegebenen Konzentrationsbereich linear. Die gaschromatographische Trennung blieb über den gesamten Untersuchungszeitraum völlig reproduzierbar. Die problemlose Derivatisierung läßt die beschriebene gaschromatographische Methode in Verbindung mit einem automatischen Probengeber für das biological monitoring auch größerer Kollektive geeignet erscheinen.
    Notes: Summary Efficient chromatographic procedures for the determination of free pentachlorophenol in air and in blood have been developed. Free pentachlorophenol from the indoor environment is preconcentrated in an impinger. Following a simple extraction, it is detected by high performance liquid chromatography without derivatisation. An alternate method is capillary gas chromatography of a suitable derivative. Unchanged pentachlorophenol in whole blood is similarly derivatised and determined quantitatively by capillary gas chromatography using an electron capture detector. The calibration curves of the described chromatographic methods were linear within the specified concentration range. Reproducibility of gas chromatographic separation remained unchanged during the whole research period. Owing to its relative simplicity, the described gas chromatographic method is advantageous for the biological monitoring of large collectives.
    Type of Medium: Electronic Resource
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  • 5
    Electronic Resource
    Electronic Resource
    Springer
    Chromatographia 13 (1980), S. 651-660 
    ISSN: 1612-1112
    Keywords: Capillary columns, glass ; Gas chromatography ; Column preparation
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Glass capillary column chromatography is the most rapidly growing part of gas chromatography. There are many complex new analytical tasks and they require special capillary columns. Fortunately there is a wide range of column preparation methods available, and they make the preparation of glass capillary columns a more varied job than that of packed columns. In this paper these methods are reviewed and suggestions are given for making task-oriented columns.
    Type of Medium: Electronic Resource
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  • 6
    ISSN: 1612-1112
    Keywords: Configuration ; Chiral phases ; Gas chromatography ; Isovaline
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The D-(resp. R) configuration of isovaline (=2-ethylalanine) was proved for the peptide antibiotics antiamoebin, Tü 165 (CBS 382.62), stilbellin, samarosporin (=emerimicin IV), suzukacillin B (A), trichotoxin A-40 and A-50. This contradicts the previously reported L-configuration for isovaline in antiamoebin and emerimicin IV. The configuration was determined by GC of the N-trifluoroacetyl-isovaline n-propyl ester on glass capillary columns coated with the chiral stationary phase N-propionyl-L-valine tert.-butylamide polysiloxane (Chirasil Val). The D-configuration of the isovaline from trichotoxin A-40 was also established independently using GC of N-pentafluoro-propionyl-isovaline (+)-3-methyl-2-butyl esters on glass capillary columns coated with OV 17.
    Type of Medium: Electronic Resource
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  • 7
    Electronic Resource
    Electronic Resource
    Springer
    Chromatographia 13 (1980), S. 567-571 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Helium detector
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Four main factors which determine the shape and the polarity of the helium detector signal are discussed. All possible responses of this detector, both in elution and in vacancy chromatography, are presented and special attention is drawn to the intermediate region. The idea of ionization vacancy is introduced for the specific case of two components which are unresolved by the column and to which the detector responds with different sensitivity.
    Type of Medium: Electronic Resource
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  • 8
    Electronic Resource
    Electronic Resource
    Springer
    Chromatographia 13 (1980), S. 574-575 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Xylenol isomers ; Sugar derivatives as liquid phases
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Adenosine, guanosine and inosine used as liquid phases in gas chromatography permits the separation of all six xylenol isomers.
    Type of Medium: Electronic Resource
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  • 9
    Electronic Resource
    Electronic Resource
    Springer
    Chromatographia 13 (1980), S. 61-67 
    ISSN: 1612-1112
    Keywords: Optimization ; Carrier gas velocity ; Gas chromatography ; Influence of temperature on optimum velocity
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Zusammenfassung Die Wahl der mittleren, linearen Trägergasgeschwindigkeit bei der Analyse von Mehrkomponentengemischen unter isothermen und temperaturprogrammierten Bedingungen wird diskutiert. Es wird gezeigt, daß stets eine Trägergasgeschwindigkeit gewählt werden sollte, die mindestens gleich, besser jedoch höher ist, als die optimale Gasgeschwindigkeit für den ersten Peak, gemessen bei der Starttemperatur (Temperaturprogramm) oder bei der eingestellten Ofentemperatur (isotherme Fahrweise).
    Type of Medium: Electronic Resource
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  • 10
    Electronic Resource
    Electronic Resource
    Springer
    Chromatographia 13 (1980), S. 686-692 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Micropacked columns in GC ; Microparticles
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Porous silica microparticles designed for modern liquid chromatography have proven effective in gas chromatography. Columns of 35–50 cm gave plate heights as low as 3.3 particle diameters and speeds of 2400 theoretical plates per second or 500 effective theoretical plates per second. Inlet pressures up to 70 atmospheres were required using hydrogen as carrier gas. The particles as received were too retentive for fast chromatography and gave asymmetric peaks. A coating of fluorosilicone oil overcame both problems. Other coatings were less effective. Bonded phases proved less satisfactory on both counts and also gave substantially less efficient columns and greater flow resistance. Column efficiency and flow resistance were sharply dependent on physical properties of the particles. The most efficient packing was clearly spherical particles of 5–10 μm diameter with narrow size distribution, pore diamters about 50 nm, BET surface areas of 25–50 m2/g and surfaces modified with trifluoropropyl silicone. A six-component hydrocarbon sample was separated in 33 s with a resolution of 4 for the most difficult pair and in 2.6 s with a minimal resolution. Performance was limited by end effects and by available pressure so that much better performance can be expected from longer columns and higher pressures.
    Type of Medium: Electronic Resource
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  • 11
    Electronic Resource
    Electronic Resource
    Springer
    Chromatographia 13 (1980), S. 752-754 
    ISSN: 1612-1112
    Keywords: Xylenol isomers ; Gas chromatography ; Polyols and polyethers as stationary phase ; Hydrogen bonding
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Xylenol isomers can be resolved on most polyols (sugars or sugar alcohols) and polyethers (polyethylene glycol or polypropylene glycol) with hydrogen-bonding interaction. They are separated on vinical polyols which have more hydroxy hydrogen than tetrol, and even on vicinal triol when its hydroxy hydrogen is acidic (stronger proton donor). The stronger is the hydrogen bonding interaction between xylenols and the liquid phase, the better is the separation of 2,4- and 2,5-xylenol, and the poorer the separation of 2,4-and 2,3-xylenol.
    Type of Medium: Electronic Resource
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  • 12
    ISSN: 1432-0878
    Keywords: Preputial glands ; Nude mice ; Ultrastructure ; Gas chromatography
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Medicine
    Notes: Summary The preputial glands of male nude (nu/nu) mice were analyzed by a combination of electron microscopy and gas chromatography to determine whether or not they are affected, like developing hairs and nails, by the nu/nu genotype. Results of the analyses revealed no differences between the glands of nude and normal male mice in either their ultrastructural characteristics or lipid secretory products.
    Type of Medium: Electronic Resource
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  • 13
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 3 (1980), S. 89-90 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary, glass ; Histamine TMS derivatives, complete separation, 2 minutes ; NPD used for quantitation down to 20 pg ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Complete separation of the TMS derivatives of histamine, 1-methyl histamine and 3-methyl histamine was achieved in two minutes in a 7 m × 0.25 mm column coated with SP 2250. Using NPD, histamine was detectable at levels as low as 20 pg. This offers a rapid, sensitive procedure with potential for clinical diagnosis and food analysis.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
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  • 14
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 3 (1980), S. 301-302 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Polychlorinated biphenyls ; Liquid crystal phase ; Choice of stationary phases for analysis ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 2 Tab.
    Type of Medium: Electronic Resource
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  • 15
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 3 (1980), S. 351-352 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Injector ; Concentrator ; Electrically heated inlet ; Capillary columns ; Vapor sampler ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
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  • 16
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 3 (1980), S. 86-86 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Recycle chromatography ; Multiple-pass chromatography ; Thermal focussing ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
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  • 17
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 3 (1980), S. 146-146 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Cold trap heating ; Thermal focussing ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
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  • 18
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 3 (1980), S. 25-27 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Instrumental modification to multidimensional separation ; Application with packed columns on complex sample composition ; Indene to pyrene range in coal tar ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
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  • 19
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 3 (1980), S. 91-91 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary, glass ; Static coating technique details ; End-sealing without failure, under ethanol ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
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  • 20
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 3 (1980), S. 195-195 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Columns, packed ; High resolution ; Packing apparatus ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
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  • 21
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 3 (1980), S. 298-298 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary, glass ; Closing technique for static coating ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
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  • 22
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 3 (1980), S. 302-302 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary ; Fitting silica capillary columns ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
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  • 23
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 3 (1980), S. 303-305 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary columns ; Surface modification ; Sulfur dioxide treatment ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
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  • 24
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 3 (1980), S. 473-474 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary, glass ; Complex wax ester mixtures ; Resolution of components by total carbon number and by degree of unsaturation ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A glass capillary GC method providing high resolution analysis of complex wax ester mixtures is described. The two key parameters needed for evaluating a wax ester mixture for industrial utility - the total carbon chain length and the number of carbon-carbon double bonds present in each component - are simply and rapidly obtained by this method.
    Additional Material: 3 Ill.
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  • 25
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 3 (1980), S. 405-410 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Determination of adsorption ; Irreversible adsorption on glass columns made visible ; Fluorescent compound PMBF2 ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: PMBF2, a pyrromethene pigment, can be used in gas chromatography. Because of its fluorescence, adsorption sites on glass columns and connections can be traced in situ. The compound can be employed to check the inertness of glass surfaces after deactivation procedures. Some applications are described.
    Additional Material: 7 Ill.
    Type of Medium: Electronic Resource
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  • 26
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 3 (1980), S. 525-526 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary, glass ; Static coating ; Filling the column by pressure, not by vacuum ; Device for filling by pressure ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
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  • 27
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 3 (1980), S. 521-522 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Computerized gas chromatography/mass spectrometry ; Capillary, OV-73 fused silica ; On-column injection ; Alkyl porphyrins ; Bis(trimethylsiloxy)silicon(IV) derivatives ; Fused silica as a GC/MS interface ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
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  • 28
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary, glass ; Electron capture detection ; Analysis of carboxylic acids and phenols in water ; Extractive alkylation ; Pentafluorobenzyl derivatives ; Steam condensate and domestic sewage effluent ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A method is presented for the simultaneous determination of a wide range of carboxylic acids and phenols in water. Extractive alkylation is used with the tetrabutylammonium ion as counter ion and pentafluorobenzylbromide as alkylating agent. Extracts are analyzed by glass capillary gas chromatography and electron capture detection. Using one ml of water sample, the detection limit lies in the range of 1-10 μg/l. Application has been made to the analysis of steam condensate and domestic sewage effluent.
    Additional Material: 7 Ill.
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  • 29
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 3 (1980), S. 627-633 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Vaporizing injectors ; Dicrimination of high-boiling components ; Elution out of the syringe needle ; “Hot needle”, “solvent flush” techniques ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Unequal elution of sample components of different volatility out of the syringe needle is one of the major causes for discrimination occuring during the injection, i.e. the phenomena which results in peak areas for the high boiling compounds which are too small compared with the volatiles. This problem, associated with all vaporizing injectors that are used with syringes, can be minimized by careful choice of the needle handling technique. Various methods are compared experimentally. The “solvent flush” method is discussed in detail and demonstrated to be ineffective for reducing losses in the syringe needle. The “hot needle” technique, where the empty needle is preheated in the injector before pushing the plunger, was found to be superior or equal to an improved “solvent flush” method (which included preheating the needle and omitting the air plug between sample and flushing solvent. Generally it was found that the discrimination due to the syringe needle was reduced for larger sample volumes, although no further changes were noticed when these exceeded 2.5 to 3μl.
    Additional Material: 6 Ill.
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  • 30
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 3 (1980), S. 641-642 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary, glass ; Polar open-tubular columns ; Silar 10CP, 0.2% ; Recoating of capillary columns to restore efficiency ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
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  • 31
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 3 (1980), S. 107-114 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary, glass ; Two-dimensional GC ; Odour evaluation ; Fraction collection, heart-cutting and enrichment ; Applications, essential oil analysis ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A simple but effective GC approach to odour evaluation and fraction collection with capillary columns is described. An allglass device splits the column effluent, with one splitter arm going to an FID. For odour evaluation, the other splitter arm is led via teflon tubing to the nose. Off-line heart-cutting is carried out by collecting the split effluent on a glass capillary microtrap, the inner walls of which are coated with OV-101. This allows recovery of nanogram amounts of material. Multipass operation or repeated collection leads to preparative capillary GC for further spectroscopic investigation. These techniques do not involve sophisticated equipment or valves. Applications of this type of smell analysis, heart-cutting and enrichment in the analysis of Rhododendron fragrantissimum essential oil, black pepper essential oil and hop essential oil, illustrating the versatility of the systems, are presented.
    Additional Material: 7 Ill.
    Type of Medium: Electronic Resource
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  • 32
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 3 (1980), S. 169-171 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Glass capillary columns ; Trimethylsilyl derivatives ; Pregnant mares' urine estrogens ; Estrone-equilin separation ; OV-225, Silar 10C stationary phases ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Glass capillary columns coated with OV-225 and Silar 10C were used to analyze estrogens (as their trimethylsilyl derivatives) present in pregnant mares' urine. Such columns provide better resolution in a shorter time than the corresponding packed columns, as exemplified by the separation of estrone from equilin.
    Additional Material: 2 Ill.
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  • 33
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 3 (1980), S. 196-196 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary, glass ; Persilylation ; Barbiturates ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
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  • 34
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 3 (1980), S. 493-496 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary, glass ; Persilylation procedure ; Discussion of experimental parameters ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Persilylated glass capillary columns are the most universal GC columns available. They are relatively easy to prepare, but there is nevertheless a great need for helpful practical instructions. In the recent literature, methods and conditions for the preparation of persilylated columns have been recommended, but these might confuse the individual column maker, since they seem to originate from limited observations rather than from comprehensive investigation. They will hardly help to make column preparation safer. This paper attempts a summarized view of the present experience with persilylation and provides basic information for column makers.
    Type of Medium: Electronic Resource
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  • 35
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 3 (1980), S. 523-524 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Precoating capillary columns ; Aromatic amines ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 3 Ill.
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  • 36
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 3 (1980), S. 527-528 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary, glass ; Surface deactivation ; High temperature silylation ; Cyclic trifluoropropylsiloxanes ; Improved surface wettability ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 1 Ill.
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  • 37
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 3 (1980), S. 124-128 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Series-coupled chemically differing columns ; Fundamental studies on the properties for basic theory started ; Retention time and separation efficiency ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Basic expressions are derived for both the retention time and the effective separation factor in serially coupled GC columns. The retention time is determined by two main parameters. The first is the fractional time spent by an unretarded solute in each column which, in turn, is determined by the relative column lengths and flow velocities through each column. The second parameter is the relative mass distribution coefficient of a particular solute in each column; a variable that can be adjusted by changing the relative temperatures of the columns. The expression for the effective separation factor relates the measured separation factor for the series combination to the separation factors on the individual columns, the fractional time spent by an unretarded peak in each column, as well as the relative values of the mass distribution coefficients of a particular solute on the different columns.
    Additional Material: 5 Ill.
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  • 38
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 3 (1980), S. 129-132 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Quantitative determination of the drug derivative in 1 ml biological fluid ; 10 ng/ml level ; Standard curve ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: 1-(o-methoxyphenoxy)-3-isopropylamino-2-propanol hydrochloride (moprolol, OmeralR), is a new β-adrenergic blocking agent. A gas chromatographic method for determining unchanged moprolol in human biological fluids has been developed. After solvent extraction, a bis-trifluoroacetyl derivative was formed and measured by an electron capture detector. The quantification was checked by using an internal standard (pronethalol), which was added to all samples. The electron capture response was linear between 10 and 500 ng/ml. To avoid contamination of the peaks, careful extraction was imperative. The main advantages offered by the described method are: specificity, high sensitivity (10 ng.ml-1) and the small amount of biological fluids (1 ml plasma a. e.) required.
    Additional Material: 4 Ill.
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  • 39
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 3 (1980), S. 648-650 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; N-P detector ; Sequential simplex optimization ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 2 Ill.
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  • 40
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 3 (1980), S. 309-310 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Amino-carboxylic acid ; Silylation ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 2 Ill.
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  • 41
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 3 (1980), S. 326-332 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Column chromatography ; Run comparison with corrections for variations in injected sample sizes ; Chromatogram reconstruction on a graphics terminal ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The application of a Hewlett-Packard 3354 B Laboratory Automation System has been studied in order to compare a series of gas chromatographic analyses. A computer program has been designed for the chromatogram reconstruction of all valid sample runs from a system subsequence on an HP-2648 A graphics CRT terminal. The detector signals of the runs are compensated for variations in injected sample sizes when a number of conditions are met.
    Additional Material: 5 Ill.
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  • 42
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 3 (1980), S. 359-360 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Mass spectrometry ; All-glass interface ; Fused silica ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 2 Ill.
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  • 43
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 3 (1980), S. 23-24 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary, glass or metal ; Connecting cement ; Silver chloride ; Heat-stable to 400°C ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 4 Ill.
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  • 44
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 3 (1980), S. 248-252 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Column loadability - overload phenomenon ; Non-classical approach to theory of loadability ; Effect on retention times, peak shape ; Effect of column length ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The usual concepts of the dynamics of an overloaded solute band fail to explain several phenomena such as the typical “leading-tail” shape and retention deviations exhibited by overloaded peaks, and why these defects are more commonly observed in short columns. These and other related deviations from theory can be rationalized by a non-classical approach to the overloading phenomenon.
    Additional Material: 4 Ill.
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  • 45
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 3 (1980), S. 286-290 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary ; Discrimination due to FID ; Effect of carrier gas flow changes on detector sensitivity ; Hydrogen as carrier gas ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The sensitivity of an FID may change when the carrier gas flow rate changes during a chromatographic run. Sample parts which are eluted at reduced FID sensitivity produce a reduced peak area, hence are discriminated as compared to other components. Sensitivity changes were studied for hydrogen as carrier gas. For the detector tested, differences in the carrier gas flow rates of 1 ml/min shifted the FID sensitivity by 1 to 5% (depending on the fuel gas supply). Thus the stability of the sensitivity is no longer ensured as soon as the carrier gas flow rate is changed manually or by an automatic programmer during an analysis. Sensitivity drifts may also occur during temperature programmed runs with a pressure regulated carrier gas supply since the gas flow through the capillary drops with increasing temperature. Such shifts in the response became noticeable as soon as relatively high carrier gas flow rates combined with long range temperature programmes were used. The typical patterns of such discriminations are shown, closing with a discussion on the possibilities for minimizing such undesired effects.
    Additional Material: 5 Ill.
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  • 46
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 3 (1980), S. 583-584 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; (Fused silica) capillary columns ; Intermediate test ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 2 Ill.
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  • 47
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 3 (1980), S. 87-88 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary, wide-bore glass WCOT ; Fourier Transform Infrared/glass capillary GC on-the-fly ; Coupling successful ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: By the use of a wide-bore WCOT capillary column, it was possible to obtain the first on-the-fly GC/FT-IR spectra with a WCOT column. This wide-bore WCOT column gave improved separation, as compared to a SCOT column, and yielded identifiable infrared spectra for a real sample.
    Additional Material: 2 Ill.
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  • 48
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    Journal of High Resolution Chromatography 3 (1980), S. 299-300 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary, WCOT glass ; Urea herbicides ; s-Triazines herbicides and metabolites ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The authors have shown that capillary columns are perfectly adequate for the separation of s-triazine herbicides and urea herbicides. The method presented remains adequate when the initial molecules are accompanied by some of their metabolites.
    Additional Material: 4 Ill.
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  • 49
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    Journal of High Resolution Chromatography 3 (1980), S. 307-308 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Volatile polymers ; Polyethylene glycols ; Comparison between CPG and ofter methods ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 3 Tab.
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  • 50
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 3 (1980), S. 352-354 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Short capillary columns ; Rapid analysis ; Polycyclic aromatic hydrocarbons ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 4 Ill.
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  • 51
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    Journal of High Resolution Chromatography 3 (1980), S. 166-168 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Packed columns ; Single compounds of special interest accurately analysed in multicompound mixtures ; Separation efficiency in MDSS separation multiplied, therefore often comparable to capillary GC separation ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Methanol, 2-Me-propanol-2, propanol-2, benzene, toluene and xylenes in gasoline blends were determined using a valveless multi-dimensional switching system (MDSS) with two packed columns and temperature programming.Compounds of interest, interfering with paraffins and naphthenes, were in a sequence of four heart cuts transferred onto the second column. The resulting baseline separation enabled precise quantitative measurement within a short analysis time. Instrument settings, times of switching and integration parameters were stored in an instrument memory file (user table) and thus high precision in the measurements was achieved.
    Additional Material: 3 Ill.
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  • 52
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    Journal of High Resolution Chromatography 3 (1980), S. 333-336 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Liquid crystal ; N,Ń, Bis (p-phenylbenzylidene)-α, α′-bi-p-toluidine (BPhBT) ; Steroids ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A gas-chromatographic separation of underivatized steroids is described, in which the liquid crystal N,Ń-bis(p-phenylbenzylidene)α,α′-bi-p-toluidine (BPhBT) was used isothermally at 265°C for the stationary phase. The nematic range of this crystal is 247 to 403°C. Use of the BPhBT crystal allowed operations in a temperature range where steroids are volatile and unlikely to display broad elution peaks and long retention times.With columns precoated with 2.5 weight percent of BPhBT, steroids containing minor structural differences in the ring system were readily differentiated. For example, 5-androsten-17α-ethinyl-3β, 17β-diol was found to elute more rapidly than its 3-keto analog, ethisterone. Ethisterone was distinguished readily also from its 19-nor analog, norethisterone. Additionally, differences in side-chain functionality and resultant molecular dimensions facilitated the separation of steroids of identical ring structure, as in the comparison of cholesterol with methyl 3β-hydroxy-5-cholenate and 25-hydroxycholesterol.An enhancement of separation according to the molecular length-to-breadth ratio was observed; in general, the larger this length-to-breadth ratio, the greater the retention period on the column.
    Additional Material: 4 Ill.
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  • 53
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 3 (1980), S. 357-358 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary column, glass ; Interface, home-made ; Headspace analysis ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 3 Ill.
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  • 54
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 3 (1980), S. 411-412 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary, glass ; All-glass T-joints and manifolds with small dead volume, production of ; Up to five-channel outlet splitter ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 2 Ill.
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  • 55
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    Journal of High Resolution Chromatography 3 (1980), S. 419-420 
    ISSN: 0935-6304
    Keywords: Meprobamate ; Overdose toxicology ; Plasma monitoring ; Gas chromatography ; High-pressure liquid chromatography ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 2 Ill.
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  • 56
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    Journal of High Resolution Chromatography 3 (1980), S. 447-451 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary, glass ; Organic gas phase cigarette smoke ; Volatile phase cigarette smoke ; Heated injection ; Nitrogen-phosphorous detector (NPD) ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A heated injection system for a microprocessor-controlled GC has been developed for the (GC)2 analysis of the volatile phase of whole smoke of a cigarette. Effects of injection port temperature and the presence of a Cambridge filter pad are demonstrated. Chromatograms are shown for smoke samples with and without a Cambridge Filter with the sample valve oven at 25°, 165° and 205°C. The use of a flame ionization and a nitrogen-phosphorous detector is illustrated.
    Additional Material: 7 Ill.
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  • 57
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    Journal of High Resolution Chromatography 3 (1980), S. 461-470 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Series-coupled columns equipped with different stationary phases ; Independent temperature control of columns ; Retention time expressions ; Theory ; Selectivity control ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The promising technique of controlling chromatographic selectivity by the adjustment of individual column temperatures in systems of series-coupled columns is investigated by means of a general model incorporating the effects of temperature and mobile phase compressibility. Expressions are derived for the linear flow velocity, the effective partition coefficient and the retention time for a system of n columns assuming an ideal mobile phase gas, under conditions of constant overall pressure drop and neglect of the temperature dependence of the mobile phase viscosity. The results indicate the importance of thermodynamic parameters, relative to parameters influencing the linear flow velocity, in determining the effect of temperature on the chromatographic retention time. Numerical results are illustrated graphically for two-column systems which are discussed in greater detail. Switching of columns is also discussed and it is shown that even if thermodynamic contributions remain unchanged, non-thermodynamic contributions have a notice-able effect.
    Additional Material: 11 Ill.
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  • 58
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    Journal of High Resolution Chromatography 3 (1980), S. 537-544 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Chromatographic properties of glass surfaces ; Fluorad FC 431 ; Glass capillary GC of basic compounds ; Modification of glass surfaces ; Deactivation of glass surfaces ; Acid-base behaviour of GC columns ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: “Leaching” or “etching” by strong mineral acids seems to be a necessary pretreatment step for the most commonly used deactivation procedures of glass capillaries by reaction with either polyethylene glycol or silylation reagents. The acidic sites which are formed on the surface during this acid treatment cannot be completely removed by the subsequent deactivation process. This drawback can be overcome by performing the leaching with water vapour, resulting in an accumulation of cations at the surface and a decrease in the number of silanol groups. Capillaries of this type show excellent properties for the chromatography of strongly basic compounds. After the wash-out of the alkaline surface layer, the acidity of the support is suited for the chromatography of strongly basic as well as strongly acidic compounds. Due to a lack of reactive acidic sites, special deactivation procedures have to be applied to capillaries produced in this way.
    Additional Material: 5 Ill.
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  • 59
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    Journal of High Resolution Chromatography 3 (1980), S. 21-22 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary, glass ; Deactivation ; Dynamic vapour-phase silylation ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 1 Ill.
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  • 60
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary, glass ; Preparation of deactivated capillaries for routine analysis ; Easy deactivation and pretreatment steps described in detail ; Comparison of different modes given ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A new surface pretreatment for the preparation of wall-coated open tubular (WCOT) glass capillary columns has been evaluated. This technique involves the application of a non-extractable layer of Superox™-4, a 4,000,000 MW polyethylene glycol, to the glass surface as a pretreatment and deactivation agent. Unlike other polyethylene glycols, Superox-4 is stable at high temperatures (〉 300°C) in the absence of oxygen, coats smoothly onto a bare glass surface and resists droplet formation. WCOT columns (SE-54, Carbowax 20M, and SP-2250) prepared using this technique are compared to columns prepared using a modified Grob [2,3] BaCO3 procedure. The Superox-4 pretreated columns were equal or superior in quality to the BaCO3 pretreated columns, based on the appearance of an activity standard and the effective theoretical plates (Neff) per meter. Chromatograms showing practical application of the WCOT columns prepared using both methods is given.
    Additional Material: 12 Ill.
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  • 61
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    Journal of High Resolution Chromatography 3 (1980), S. 35-36 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary, glass ; Enantiomer separation ; Chiral stationary phase ; D.L. proline and D. L. secondary amines ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 2 Ill.
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  • 62
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    Journal of High Resolution Chromatography 3 (1980), S. 197-198 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary, glass ; Introducing phenyl groups by persilylation ; Dependence of wettability on density of phenyl groups ; Practical instructions ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 1 Tab.
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  • 63
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    Journal of High Resolution Chromatography 3 (1980), S. 241-247 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary, glass ; Quantitative analysis at 10-10g level ; Steroids in urine ; Amino acid fluorobutyrates (19 in 35 min) ; Installation of glass capillaries ; Connection to FM-ECD ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Glass capillary columns are ideal for analysis of urinary steroid profiles (i.e. the total steroid neutral fraction without prior separation into sub-groups).In this paper performance of both SCOT and wide-bore WCOT columns has been compared, resulting in no significant quantitative difference on urine extracts run as trimethylsilyl ether derivatives. However, because of increased efficiency the WB-WCOT column exhibited more sensitivity in measurement of small amounts of 11-ox-aetiocholanolone. Sensitivity of other steroids was greatly enhanced by use of either SCOT or WB-WCOT, leading to an almost tenfold increase over conventional packed columns (e.g. androsterone and aetiocholanolone 〈 40 μg per 24 h urine sample). A simple splitless injection system (based on a design of Dr. W. Greenaway, Oxford University) is presented.Experiments were also carried out using a SCOT column in conjunction with an FM-electron capture detector. Whilst efficiency was impaired due to the design of the detector, use of He (carrier) and N2 (make up gas) showed that several steroid derivatives could be easily measured at well below the 10-10 g level with much more rapid retention times than with a 1½m packed column. Highly successful separation of 19 amino acids (as fluoro-acyl derivatives) was achieved in 35 minutes using a SCOT (30 m) SP2100 column.
    Additional Material: 12 Ill.
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  • 64
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    Journal of High Resolution Chromatography 3 (1980), S. 311-312 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Fused silica capillaries ; Free amines ; Humidity of carrier gas ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 1 Ill.
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  • 65
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    Journal of High Resolution Chromatography 3 (1980), S. 471-472 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary, fused silica ; Element-selective MED ; Organometallics ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 3 Ill.
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  • 66
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    Journal of High Resolution Chromatography 3 (1980), S. 528-530 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Two-phase derivatization technique ; Yeast ; Splitless injection ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 2 Ill.
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  • 67
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    Journal of High Resolution Chromatography 3 (1980), S. 545-550 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary, fused silica columns ; Selective detectors: TSD, ECD, FPD ; POTW sludge extracts ; Effluent splitter ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Combination of various GC detectors by using a Varian effluent splitter with glass capillary columns has been found to be a rapid procedure for profiling organics extracted from sludges and river sediments. The selectivity and the increased sensitivity of the thermionic nitrogen-phosphorus detector (TSD), the electron capture detector (ECD), and the flame photometric detector (FPD) over the flame ionization detectors (FID) or mass spectrometers allow the detection of compounds present at trace levels without need for extensive sample cleanup. Furthermore, the combination of two selective detectors may supplement the information with regard to the chemical functionalities required for structure elucidation.
    Additional Material: 3 Ill.
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  • 68
    ISSN: 0935-6304
    Keywords: Gas chromatography ; High performance liquid chromatography ; Theoretical basis of column chromatography in multicomponent separations ; Required value of peak resolution and accuracy of obtained, quantitative method ; Plate height of solute with capacity ratio equal to one or approaching to infinity ; Linearity between peak width and retention value ; High efficient GC columns ; HPLC small-bore column ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The point of our published papers since 1957 is reviewed. The relations between the required value of peak resolution, K1 (or R), and peak separation, K3 (eqn 9); K1 and relative accuracy of a peak height quantitative method, Ph (eqn. 10); K1 and relative accuracy of a peak area method, Pa, (eqn. 12) at different concentration ratios, φ, are derived. The final result in Table 2 shows a large influence of φ on the required value of K1.The approximately linear relation between peak width and retention value (eqn. 18) exists not only in GC. but also in HPLC. Plate height values H1 and H∞ for a solute with capacity ratio, k′, equal to unity or approaching infinity, respectively, are used to evaluate the column efficiency (eqn. 20). The measuring methods (eqn. 21,22,23) and parameters effecting on H1 and H∞ are given for GC packed column (eqn. 24), GC open tubular column (eqn. 25) and HPLC (eqn. 26). In the light of this, columns of high efficiency were developed. Some typical chromatograms for high speed analysis and separation of complex mixtures are given.
    Additional Material: 16 Ill.
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  • 69
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    Journal of High Resolution Chromatography 3 (1980), S. 585-586 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary, glass or fused silica ; Adsorptive and catalytic activity ; Distinction of effects ; Discussion of active sites ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 1 Ill.
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  • 70
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    Springer
    Chromatographia 13 (1980), S. 73-84 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Gas hold-up time ; Dead time
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The two approaches used for the calculation of the gas hold-up time and thus, the adjusted retention time are outlined, first for the restricted case when the carbon numbers of the three homologues used for the calculation are evenly spaced (c3−c2=c2−c1) and then, for the general case when (c3−c2) differs from (c2−c1). The basic difference in the philosophy of the two approaches is shown.
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  • 71
    ISSN: 1612-1112
    Keywords: Gas chromatography ; On-column abstraction ; Aliphatic aldehydes ; Amine antioxidants
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The selective on-column abstraction of aliphatic aldehydes by gas chromatographic stationary phases containing N-iso-propyl N′-phenyl-p-phenylenediamine is described.
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  • 72
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    Chromatographia 13 (1980), S. 35-39 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Nitromethane ; Nitroalkanes
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Impurities in commercially available nitromethane have been determined by gas-liquid chromatography using six different column packings. Besides nitromethane, 1-nitropropane, 2-nitropropane, acetonitrile, methanol, small amounts of ethanol and acetaldehyde have been detected. The presence of formaldehyde, ethyl acetate and acetone is probable. Mixtures containing comparable amounts of the four nitroalkanes could be separated on all columns, but plots of logarithms of the retention times vs. carbon number or boiling points of the nitroalkanes or column temperatures were linear only in case of columns packed with Porapak R and Q.
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  • 73
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Column characterization ; Oxidation ; Stationary phases
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The on-column oxidation of hydrocarbons commonly used as stationary phases in column characterization is investigated. In each case significant shifts of retention are observed, which may be negative or positive depending upon the polarity of the test solutes and the adsorptivity of the support material. In order to reduce the consequent uncertainties in the Rohrschneider [1] and McReynolds [2] polarity values, a new method of column characterization is proposed. The applicability of the new method is illustrated by a consideration of a range of silicone liquid phases.
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  • 74
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    Chromatographia 13 (1980), S. 207-208 
    ISSN: 1612-1112
    Keywords: Trace determination ; Hydrogen chloride ; Ethylene oxide ; Gas chromatography ; Chlorinated solvents
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A method is described for the determination of small quantities of hydrochloric acid in two chlorinated organic solvents (CHCl3 and CCl4). An excess of gaseous ethylene oxide is added to a liquid sample; the 2-chloroethanol formed is then analyzed by gas chromatography. The procedure is simpler and more sensitive in comparison with other conventional methods. It can be modified for other organic solvents.
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  • 75
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    Berichte der deutschen chemischen Gesellschaft 113 (1980) 
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 76
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    Berichte der deutschen chemischen Gesellschaft 113 (1980), S. 1-8 
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Preparation of 3-Alkoxy-4-alkyl-3-cyclobutene-1,2-dionesSeveral squaric acid esters (2a-g) are prepared. They react with Grignard compounds to give the title compounds (11a-n). 1,2- vs. 1,4-Grignard addition and the benzyl-tolyl rearrangement coincidental with the Grignard reaction are discussed. Hydrolysis of compounds 11 leads to 4-alkyl-3-hydroxy-3-cyclobutene-1,2-diones (12).
    Notes: Verschiedene Quadratsäureester (2a-g) werden dargestellt und mit Grignard-Reagentien in die Titelverbindungen (11a-n) verwandelt. 1,2- gegen 1,4-Grignard-Additionen und die Benzyl-Tolyl-Umlagerung bei der Grignard-Reaktion werden diskutiert. Hydrolyse der Verbindungen 11 liefert 4-Alkyl-3-hydroxy-3-cyclobuten-1,2-dione (12).
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  • 77
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    Berichte der deutschen chemischen Gesellschaft 113 (1980), S. 19-23 
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Hydrogen Transfer Reactions, Part 3. Stereochemistry of Palladium-Catalysed Disproportionation of 1,2-DihydronaphthaleneIn the presence of metallic palladium two hydrogens are stepwise and stereoselectively cis-eliminated from 1,2-dihydronaphthalene (1). Before addition to a second molecule 1 occurs the eliminated hydrogens scramble.
    Notes: Der erste Schritt der durch Palladium katalysierten Disproportionierung von 1,2-Dihydronaphthalin (1) ist eine stufenweise cis-Eliminierung von zwei Wasserstoffen, die hoch stereoselektiv abläuft. Die abgespaltenen Wasserstoffe äquilibrieren, bevor sie an ein zweites Molekül 1 addiert werden.
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  • 78
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Novel μ-Hydroxo-Transition Metal Complexes, III. Preparation of Binuclear Complexes of Rhodium(III) Containing a μ-Acetato- and μ-Carbonato-Bridge. The Structure of the trans-Diaqua-di-μ-hydroxo-bis[(1,4,7-triazacyclononane)-rhodium(III)] CationThe binuclear tri-μ-hydroxo-bis[(1,4,7-triazacyclononane)rhodium(III)] cation 4 has been prepared. In acidic solutions 4 forms the trans-diaqua-di-μ-hydroxo-bis[(1,4,7-triazacyclononane)-rhodium(III)] cation 3, the structure of which has been established by single crystal X-ray diffraction. 3 reacts with acetic acid to yield the μ-acetato complex 5; whereas in alkaline solutions 6 reacts with carbonate ions forming a μ-carbonato complex 7.
    Notes: Das zweikernige Tri-μ-hydroxo-bis[(1,4,7-triazacyclononan)rhodium(III)]-Kation 4 wird dargestellt. In saurer Lösung entsteht daraus das trans-Diaqua-di-μ-hydroxo-bis[(1,4,7-triazacyclononan)rhodium(III)]-Kation 3, dessen Struktur röntgenographisch bestimmt wurde. Mit Essigsäure reagiert 3 zum μ-Acetato-Komplex 5; wohingegen in alkalischer Lösung aus 6 mit Carbonat-Ionen der μ-Carbonato-Komplex 7 entsteht.
    Additional Material: 1 Ill.
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  • 79
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    Berichte der deutschen chemischen Gesellschaft 113 (1980), S. 70-78 
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The Reaction of Dinitrogen with Benzyne in the Coordination Sphere of TitaniumThe formation of aniline from dinitrogen during the thermolysis of diphenyltitanocene (1) and in the system (C5H5)2TiCl2 (3) + Mg + o-bromofluorobenzene (4) + N2 has been found to proceed via N2 reaction with intermediate Ti-benzyne complex (2). This is indicated by the isomeric composition of toluidines obtained from N2 and ditolyltitanocenes, the formation of [2-D1]aniline in the system 3 + Mg + 4 + N2 on hydrolysis with D2O and by nitrogen isotope fractionations at natural 15N-abundance in the reaction products.
    Notes: Die Bildung von Anilin aus Stickstoff bei der Thermolyse von Diphenyltitanocen (1) und im Reaktionssystem (C5H5)2TiCl2 (3) + Mg + o-Bromfluorbenzol (4) + N2 verläuft über die Reaktion von N2 mit einem intermediären Titan-Dehydrobenzol-Komplex (2). Das ergibt sich aus der Isomerenverteilung von Toluidinen, die aus N2 und Ditolyltitanocenen erhalten wurden, aus der Bildung von [2-D1]Anilin bei Hydrolyse des Systems 3 + Mg + 4 + N2 mit D2O sowie aus Stickstoffisotopen-Fraktionierungen in den Reaktionsprodukten mit natürlicher 15N-Häufigkeit.
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  • 80
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    Berichte der deutschen chemischen Gesellschaft 113 (1980), S. 79-89 
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Acylcarbodiimides, III. Preparation and Reactions of (Thiocarbamoyl)carbodiimidesStarting from 1,1,5-trisubstituted dithiobiuretes (1) and with the aid of cyanuric trichloride/triethylamine several (thiocarbamoyl)carbodiimides (2) were prepared and partly isolated. This procedure can be used only in special cases for the preparation of 1,1-dialkyl-5-aryl-dithiobiuretes. Carbodiimides without a bulky substituent (R′) are prone to dimerization. Several dimers 4 were isolated, the structure of them was elucidated. Addition of water, alcohols, and amines afforded the thiocarbamoylureas 5, isoureas 7 and guanidines 6, cycloaddition of different acyl isothiocyanates and of benzoyl isocyanate gave the 1,3,5-thiadiazines 8 and 9.
    Notes: Aus 1,1,5-trisubstituierten Dithiobiureten (1) wurden mit Cyanurchlorid/Triethylamin eine Reihe von (Thiocarbamoyl)carbodiimiden (2) hergestellt und z. T. isoliert. Das Verfahren ist auf 1,1-Dialkyl-5-aryl-dithiobiurete nur begrenzt anwendungsfähig. Carbodiimide 2 ohne sperrigen Rest R′ neigen zur Dimerisierung; mehrere Dimere 4 wurden isoliert und in der Konstitution geklärt. Addition von Wasser, Alkoholen und Aminen lieferte die entsprechenden (Thiocarbamoyl)harnstoffe (5), -isoharnstoffe (7) und -guanidine (6). Cycloaddition von verschiedenartigen Acylisothiocyanaten und von Benzoylisocyanat führten zu den 1,3,5-Thiadiazinen 8 und 9.
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  • 81
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    Berichte der deutschen chemischen Gesellschaft 113 (1980), S. 129-141 
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Stereochemistry of Aliphatic Carbocations, 13. Protonated Cyclopropanes as Intermediates in 1,2-Alkyl ShiftsThe nitrous acid deamination of 2-ethyl-1-methylbutylamine (10), 1,2-diethylbutylamine (35), and 2-ethyl-1-methylpentylamine (43) has been studied with respect to 1,2-alkyl shifts. Optically active and deuterated amines were employed whenever possible. The structure, configuration, and deuterium distribution of various products (e.g. 16 from 10, 40 and 48 from 35, 56 from 43) are most reasonably explained in terms of alkyl-bridged intermediates (corner-protonated cyclopropanes) which isomerize via proton shifts from corner to corner. The alternative interconversion of open ions via 1,3-H shifts is incompatible with our experimental results.
    Notes: Die Desaminierung von 2-Ethyl-1-methylbutylamin (10), 1,2-Diethylbutylamin (35) und 2-Ethyl-1-methylpentylamin (43) mit salpetriger Säure wurde im Hinblick auf 1,2-Alkylverschiebungen untersucht. Soweit möglich wurden optisch aktive und deuterium-markierte Amine eingesetzt. Die Struktur, Konfiguration und Deuterium-Verteilung verschiedener Produkte (z.B. 16 aus 10, 40 und 48 aus 35, 56 aus 43) wird am besten erklärt mit Hilfe alkylverbrückter Zwischenstufen (eckenprotonierter Cyclopropane), die durch Protonenverschiebung von Ecke zu Ecke isomerisieren. Die alternative Umwandlung offener Kationen durch 1,3-H-Verschiebung ist mit unseren experimentellen Ergebnissen unvereinbar.
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  • 82
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    Berichte der deutschen chemischen Gesellschaft 113 (1980), S. 142-151 
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Reactions of (Dichlorophosphinyl)methanesulfonyl ChlorideSubstitution of chlorine by fluorine in (dichlorophosphinyl)methanesulfonyl chloride (2) Cl2P(O)CH2SO2Cl leads to the fluorides F2P(O)CH2SO2X (X = Cl, F); their reactions leading to the fluorophosphorane F4PCH2SO2F and fluorophosphate anions of the type [F5PCH2SO2X]- and [O(F)P(O)CH2SO2X]- (X = Cl, F) were investigated. Hydrolysis of 2 yields the acid (HO)2P(O)CH2SO2OH, from which esters and amides have been derived. The conversion of the esters to α,β-unsaturated sulfonic acid derivatives via the Horner-Wittig reaction is also described.
    Notes: Substitution von Chlor durch Fluor in (Dichlorphosphinyl)methansulfonylchlorid (2), Cl2P(O)CH2SO2Cl liefert die Fluoride F2P(O)CH2SO2X (X = Cl, F), deren Umwandlung zum Fluorphosphoran F4PCH2SO2F und zu Fluorophosphat-Anionen des Typs [F5PCH2SO2X]- bzw. [O(F)P(O)CH2SO2X]- (X = Cl, F) untersucht wird. Die Hydrolyse von 2 führt zur Säure (HO)2P(O)CH2SO2OH, von der Ester und Amide dargestellt werden. Die Ester werden in einer Horner-Wittig-Reaktion in α,β-ungesättigte Sulfonsäureverbindungen umgewandelt.
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  • 83
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    Berichte der deutschen chemischen Gesellschaft 113 (1980), S. 165-170 
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Preparation of Methoxythiocarbonyl Substituted UreasThe alkali metal salts 4 of phenylthiocarbamic O-methyl ester (1) yields with phosgene a carbonyl chloride (5), which is a suitable starting material for the preparation of the hitherto unknown group of methoxythiocarbonyl substituted ureas. In its reactions with carbonyl chlorides or sulfonyl chlorides, 4 shows the typical behaviour of an ambident anion.
    Notes: Die Alkalisalze 4 des Phenylthiocarbamidsäure-O-methylesters (1) liefern mit Phosgen ein Säurechlorid (5), welches einen bequemen Zugang zur bisher unbekannten Gruppe der methoxythio-carbonyl-substituierten Harnstoffe 6 eröffnet. Die Umsetzung von 4 mit Carbonylchloriden bzw. mit Sulfonylchloriden zeigt, daß 4 das typische Verhalten einer ambifunktionellen Verbindung aufweist.
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  • 84
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    Berichte der deutschen chemischen Gesellschaft 113 (1980), S. 183-192 
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Reaction of Substituted Hydrazones with Thionyl Chloride and Sulfuryl ChlorideTreatment of acetylhydrazones 2, ethoxycarbonylhydrazones 3, p-tolylsulfonylhydrazones 4 or semicarbazones 5 with thionyl chloride leads to the 1,2,3-thiadiazoles 6a-o. Sulfuryl chloride on the other hand accomplishes the transfer of chlorine without incorporating a sulfur atom. The new synthesized 1,2,3-thiadiazoles 6g-o are characterized in detail by spectroscopic methods.
    Notes: Die Einwirkung von Thionylchlorid auf Acetylhydrazone 2, Ethoxycarbonylhydrazone 3, p-Tolylsulfonylhydrazone 4 oder Semicarbazone 5 führt zu den 1,2,3-Thiadiazolen 6a-o. Sulfurylchlorid dient dagegen lediglich als Chlorüberträger; Schwefel wird nicht eingebaut. Für die neu auf diesen Wegen synthetisierten 1,2,3-Thiadiazole 6g-o wird eine eingehende spektroskopische Charakterisierung durchgeführt.
    Additional Material: 2 Tab.
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  • 85
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Microbial Transformations of Steroids, XVII. Preparation of Several Mono- and Diketo-structures of D-Homo-4-pregnene-3,20-dione and D-Homo-1,4-pregnadiene-3,20-dione11α- (2) and 15α-monohydroxy- (3), 6β,11α-(4), 11α,15α- (5), 12β,15α- (6), 15α,16α- (7), 7β,11α- (8), 11β,17α- (9), 7β,17α-dihydroxy- (11), and 17α-hydroxy-11-oxo-D-homoprogesterone (10) were prepared by microbiological transformations of D-homoprogesterone (1) with various fungi. The compounds were oxidized by the method of Jones before and after microbiological 1,2-dehydrogenation with Bacillus lentus to the corresponding keto-structures 12 to 17 and 20 respectively 26 to 30. The 14α-hydroxy-11-ketone 18 and 7α,14α-dihydroxy-11-ketone 19 were obtained by microbiological hydroxylation of the 11-ketone 12 with Curvularia lunata. Penicillium lilacinum degraded D-homoprogesterone (1) to D-homotestosterone.
    Notes: Durch mikrobiologische Umwandlung von D-Homoprogesteron (1) mit verschiedenen Pilzstämmen wurden 11α- (2) und 15α-Monohydroxy- (3), 6β,11α- (4), 11α,15α- (5), 12β,15α- (6), 15α,16α- (7), 7β,11α- (8), 11β,17α- (9), 7β,17α-Dihydroxy- (11) und 17α-Hydroxy-11-oxo-D-homo-progesteron (10) hergestellt. Die Verbindungen wurden vor und nach mikrobiologischer 1,2-Dehydrierung mit Bacillus lentus zu den entsprechenden Ketostrukturen 12 - 17 und 20 bzw. 26 - 30 nach Jones oxidiert. Ein 14α-Hydroxy-11-keton 18 und 7α,14α-Dihydroxy-11-keton 19 wurden durch mikrobiologische Zweithydroxylierung des 11-Ketons 12 mit Curvularia lunata erhalten. Penicillium lilacinum baute D-Homoprogesteron (1) zu D-Homotestosteron ab.
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  • 86
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    Berichte der deutschen chemischen Gesellschaft 113 (1980), S. 226-232 
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Crystal and Molecular Structures of the S3N2+ Radical Cation in S3N2+SO3CF3- · 1/2 CH3CN and of S3N2(NSO2F)The molecular and crystal structures of S3N2+SO3CF3- · 1/2 CH3CN (1) and S3N2NSO2F (2) were determined from single crystal X-ray diffraction data. The S3N2+ radical cation in 1 is planar, two cations being connected through weak S—S bonding interactions to form dimers with a chair configuration. The S3N2 ring of 2, in which the NSO2F group is covalently bonded to one of the S atoms of the S — S group, is not planar; the S — S bond is weaker than in 1.
    Notes: Die Röntgenstrukturanalysen von S3N2+SO3CF3- - 1/2 CH3CN (1) und S3N2NSO2F (2) zeigen in 1 ein planares S3N2+-Radikalkation, wobei zwei Kationen über schwache S-S-Wechselwirkungen zu sesselförmigen Dimeren assoziiert sind. Der an einem S-Atom der S — S-Gruppe substituierte S3N2-Ring in 2 ist nicht planar; die S — S-Bindung ist schwächer als in 1.
    Additional Material: 3 Ill.
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  • 87
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Kinetic and Mechanistic Investigations of Transition Metal Complex Reactions, IV. Reactions of Complex Ligands, XVIII. Kinetic and Mechanism of the Insertion of 1-(Diethylamino)-1-propyne into the Metal-Carbene Bond of Pentacarbonyl(arylmethoxycarbene)chromium(0) and -tungsten(0)Pentacarbonyl(arylmethoxycarbene) complexes (CO)5M[C(p-C6H4R)OCH3] (M = Cr, W; R = CF3, Br, H, CH3, OCH3) (1a - g) add 1-(diethylamino)-1-propyne (2) via insertion of the alkyne into the metal-carbene bond. The formation of pentacarbonyl[(diethylamino)(2-aryl-2-methoxy-1-methylethenyl)carbene]chromium(0) and -tungsten(0) (3a - g) in octane follows a second-order rate law: d[3]/dt = k[1][2]. The tungsten complexes react faster than the analogous chromium compounds. Replacement of R = H by electron withdrawing substituents (CF3, Br) results in an increase, by electron donating groups (CH3, OCH3) in a decrease of the reaction rate. The activation enthalpies ΔH≠ are low (25.1 - 39.4 kJ · mol-1), the activation entropies ΔS≠ strongly negative (-129 to -145 J · mol- K-1). The results are discussed on the basis of an associative stepwise mechanism with an attack of the ynamine at the carbene carbon in the first reaction step.
    Notes: Pentacarbonyl(arylmethoxycarben)-Komplexe (CO)5M[C(p-C6H4R)OCH3] (M = Cr, W; R = CF3, Br, H, CH3, OCH3) (1a - g) addieren 1-(Diethylamino)-1-propin (2) unter Einschiebung des Alkins in die Metall-Carbenkohlenstoff-Bindung. Die Bildung von Pentacarbonyl[(diethylamino)(2-aryl-2-methoxy-1-methylethenyl)carben]chrom(0) und -wolfram(0) (3a - g) in Octan erfolgt nach einem Geschwindigkeitsgesetz zweiter Ordnung: d[3]/dt = k[1][2]. Die Wolframkomplexe reagieren schneller als die entsprechenden Chromverbindungen. Ersatz von R = H durch elektronenziehende Substituenten (Br, CF3) führt zu einer Erhöhung, durch elektronenspendende Gruppen (CH3, OCH3) zu einer Verringerung der Reaktionsgeschwindigkeit. Die Aktivierungsenthalpien ΔH≠ sind niedrig (25.1 - 39.4 kJ · mol-1), die Aktivierungsentropien ΔS≠ stark negativ (-129 bis -145 Jmol-1 K-1). Die Ergebnisse werden auf der Grundlage eines mehrstufigen Mechanismus mit einem Angriff des Inamins am Carbenkohlenstoff im ersten Reaktionsschritt diskutiert.
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  • 88
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Electron Donor-Acceptor Compounds, XIX. Intramolecular Quinhydrones of the [3.3]Metacyclophane Series: syn- and anti-6,9,15,18-Tetramethoxy[3.3]metacyclophanes as PrecursorsIn the context of the synthesis of [3.3]metacyclophane quinhydrones (e. g, 1 and 2) the stereoisomeric 7,10,17,20-tetramethoxy-2,13-dithia[4.4]metacyclophanes (5/6) were synthesized via 8 - 12. From the disulfones, prepared by oxidation of 5/6, by vacuum gas-phase pyrolysis (570°C/10-4 Torr) two stereoisomeric 6,9,15,18-tetramethoxy[3.3]metacyclophanes were obtained the assignment of which to the syn-constitution 3 and the anti-constitution 4 has been made on the basis of 1H NMR spectra. As experiments on thermal isomerisation show the conformational stability of 3/4 as well as 5/6 is remarkably high. - As side-products of the cyclisation of 11 and 12, and of the sulfone pyrolysis, resp., the compounds 13 - 16 were isolated.
    Notes: Mit dem Ziel der Synthese von Chinhydronen der [3.3]Metacyclophan-Reihe (z. B. 1 und 2) wurden die stereoisomeren 7,10,17,20-Tetramethoxy-2,13-dithia[4.4]metacyclophane (5/6) über die Vorstufen 8 - 12 synthetisiert. Aus den durch Oxidation von 5/6 erhaltenen Disulfonen entstanden durch Gasphasen-Vakuum-Pyrolyse (570°C/10-4 Torr) zwei stereoisomere 6,9,15,18-Tetramethoxy[3.3]metacyclophane, deren Zuordnung zur syn-Konstitution 3 und anti-Konstitution 4 aufgrund der 1H-NMR-Spektren getroffen wurde. Wie Versuche zur thermischen Isomerisierung zeigen, ist die konformative Stabilität von 3/4 wie auch von 5/6 bemerkenswert groß. - Als Nebenprodukte der Cyclisierung von 11 und 12 bzw. der Sulfon-Pyrolyse wurden die Verbindungen 13 - 16 isoliert.
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  • 89
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Electron Donor-Acceptor Compounds, XX. Intramolecular Quinhydrones of the [3.3]Metacyclophane Series: Synthesis, Stability, and Charge Transfer Absorptions of Stereoisomeric [3.3]Metacyclophane QuinhydronesOn the attempt to synthesize the syn- and anti-[3.3]metacyclophane quinhydrones 1 and 2 by demethylation of 3 and 4, resp., and subsequent oxidation the same [3.3](2,6)-p-benzoquinonophane (5) was obtained which on catalytic hydrogenation yielded syn-[3.3]metacyclophane quinhydrone 1. Partial demethylation, however, and following oxidation led from 3 to the dimethyl ether 7 of the syn-quinhydrone 1, and analogously from 4 to the dimethyl ether 8 of anti-[3.3]-metacyclophane quinhydrone 2. The structural assignment of the stereoisomers was confirmed by an X-ray structure analysis of 7. In addition to 7 and 8, the corresponding monomethyl ethers 10 and 12 were obtained. - The anti-[3.3]metacyclophanes 8 and 12 undergo a complete thermal rearrangement to the syn-isomers 7 and 11, resp., from which a stronger ground state stabilisation by charge transfer interaction is concluded for the donor-acceptor systems of the syn-series. - The quinhydrones 7, 8, 10, 11, and 12 show broad, intensive charge transfer absorptions in the range from 300 to 550 nm which for the pairs of stereoisomers 7/8 and 11/12, in spite of the very different donor-acceptor orientation, are surprisingly similar: the absorption intensity of the CT band, however, is considerably stronger for the anti-quinhydrones than for their syn-isomers.
    Notes: Bei Versuchen zur Darstellung der syn- und anti-[3.3]Metacyclophan-Chinhydrone 1 und 2 wurde durch Demethylierung von 3 bzw. 4 und anschließende Oxidation dasselbe [3.3](2,6)-p-Benzochinonophan (5) erhalten, das durch katalytische Hydrierung syn-[3.3]Metacyclophan-Chinhydron 1 ergab. Partielle Demethylierung und anschließende Oxidation führten jedoch ausgehend von 3 zum Dimethylether 7 des syn-Chinhydrons 1 und entsprechend aus 4 zum Dimethylether 8 des anti-[3.3]Metacyclophan-Chinhydrons 2. Die Strukturzuordnung der Stereoisomeren wurde durch Röntgen-Strukturanalyse von 7 bestätigt. Neben 7 und 8 wurden die entsprechenden Monomethylether 10 und 12 erhalten. - Die anti-Verbindungen 8 und 12 lagern sich thermisch quantitativ in die syn-Isomeren 7 bzw. 11 um, woraus auf eine stärkere Grundzustands-Stabilisierung durch Charge-Transfer-Wechselwirkung bei den Donor-Acceptor-Systemen der syn-Reihe geschlossen wird. - Die Chinhydrone 7, 8, 10, 11 und 12 zeigen breite, intensive Charge-Transfer-Absorptionen im Bereich von 300 - 550 nm, die bei den Stereoisomeren-Paaren 7/8 und 11/12 trotz der sehr unterschiedlichen Donor-Acceptor-Orientierung überraschend ähnlich sind; die Absorptionsintensität der CT-Bande ist jedoch bei den anti-Chinhydronen beträchtlich größer als bei den syn-Isomeren.
    Additional Material: 4 Ill.
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  • 90
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 113 (1980), S. 278-288 
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Fluorenylsilanes, I. Preparation and Structural Investigations of Fluorenylsilanes with Functional Groups at SiliconChloro-9-fluorenyldiphenylsilane (3a) and 9-fluorenyltris(trimethylsilyl)silane (3b) have been prepared by the reaction of the corresponding halosilanes with 9-fluorenyl lithium. The chloro substituent in 3a can be exchanged for other functional groups. With alkaline conditions cleavage of the fluorenyl-silicon bond may happen. The molecular structures of 3b and 9-fluorenyldiphenylsilanole (6a) have been determined by X-ray diffraction. In both compounds the substituents at the Cfluorenyl—Si bond are exactly staggered. The fluorenyl group in 3b is slightly folded, the Cfluorenyl—Si bond is lengthened to 194.7 (4) pm.
    Notes: Chlor-9-fluorenyldiphenylsilan (3a) und 9-Fluorenyltris(trimethylsilyl)silan (3b) wurden durch Umsetzung der entsprechenden Halogensilane mit 9-Fluorenyllithium dargestellt. Der Chlorsubstituent in 3a läßt sich gegen andere funktionelle Gruppen austauschen; im alkalischen Medium kann daneben die Fluoren-Silicium-Bindung gespalten werden. Von 3b und 9-Fluorenyldiphenylsilanol (6a) wurden Röntgenstrukturanalysen durchgeführt. In beiden Verbindungen stehen die Substituenten bezüglich der CFluorenyl— Si-Bindung streng gestaffelt. Der Fluorenyl-Rest in 3b ist leicht gefaltet, die CFluorenyl—Si-Bindung auf 194.7 (4) pm aufgeweitet.
    Additional Material: 2 Ill.
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  • 91
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 113 (1980), S. 289-301 
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The Oxidation of Hexathioethanes to Tetrathioethene Radical CationsThe oxidation of hexakis(alkylthio)ethanes (RS)3C — C(SR)3 by AlCl3/H2CCl2, NOBF4, or I2 yields tetrakis(alkylthio)ethene radical cations (RS)2Ċ=⊕C(SR)2. The dark violet tetrahydrotetrathiafulvalenium triiodide 1 · I3 (n = 2) has been obtained as a crystalline solid. Other derivatives such as the dibenzotetrathiafulvalene (2) and the quinodimethane (4) radical cations have been characterized by ESR spectroscopy in solution: The coupling constants and the g values reveal that the spin density accumulates preferentially at the S centers. The alkyl proton coupling is rationalized advantageously by angle-independent spin polarization. For tetrathiafulvalene, geometry-optimized MNDO calculations predict a lengthening of the central C = C bond on oxidation and the positive charge centered predominantly at sulfur.
    Notes: Die Oxidation von Hexakis(alkylthio)ethanen (RS)3C — C(SR)3 mit AlCl3/H2CCl2, NOBF4 oder I2 führt zu Tetrakis(alkylthio)ethen-Radikalionen (RS)2Ċ=⊕C(SR)2. Das schwarzviolette Tetrahydrotetrathiafulvalenium-triiodid 1 · I3 (n = 2) konnte in Substanz isoliert werden. Weitere Derivate wie das Dibenzotetrathiafulvalen- (2) und das Chinodimethan-(4)-Radikalion werden in Lösung ESR-spektroskopisch charakterisiert: Aus den Kopplungskonstanten und g-Faktoren folgt, daß sich die Spindichte überwiegend an den S-Zentren befindet. Die Alkylprotonen-Kopplungen lassen sich vorteilhaft mit winkelunabhängiger Spinpolarisation beschreiben. Für Tetrathiafulvalen ergeben geometrieoptimierte open-shell-MNDO-Berechnungen, daß sich die zentrale C = C-Bindung bei Oxidation verlängern, und daß die positive Ladung überwiegend am Schwefel zentriert sein sollte.
    Additional Material: 5 Ill.
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  • 92
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 113 (1980), S. 324-332 
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Trimethylsilyl Cyanide - A Reagent for Umpolung, IV. Substituent Effects in the Acylating Nucleophile for Directing 1,2-/1,4-Addition to α,β-Unsaturated KetonesMesityl oxide (6) is attacked by nucleophilic anions 5a - f in DME at the C-1 and/or C-3 position. Depending on the p-substituent in 5 the whole scale from 100% 1,2-adduct 7 (with 5a, X = N(CH3)2) to 100% 1,4-adduct 9 (with 5f, X = CN) is covered. In ether the amount of 9 is strongly enhanced. The control of regiospecificity has to be ascribed to differing “hardness” of 5a - f, since possible ion pairing produces opposite effects. The oxidation potentials of 5 and the reduction potential of 6 in DME exclude electron transfer before 1,4-addition. The easily reducible dienone 14, however, reacts with 5c via radicals.
    Notes: Die nucleophilen Anionen 5a - f greifen Mesityloxid (6) in DME in C-1- und/oder C-3-Position an, wobei in Abhängigkeit vom p-Substituenten in 5 die gesamte Skala von 100% 1,2-Addukt 7 (mit 5a, X = N(CH3)2) zu 100% 1,4-Addukt 9 (mit 5f, X = CN) durchlaufen wird. In Ether erhöht sich der Anteil an 9 erheblich. Die Steuerung muß der unterschiedlichen „Härte“ von 5a - f zugeschrieben werden, da eine mögliche Ionenpaarbildung gegenläufig wirkt. Die Oxidationspotentiale von 5 und das Reduktionspotential von 6 schließen in DME eine vorgelagerte Elektronenübertragung bei 1,4-Addition aus, während das leicht reduzierbare Dienon 14 mit 5c radikalisch reagiert.
    Additional Material: 1 Ill.
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  • 93
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: NMR Studies of Boron Compounds, XVII. 17O NMR Studies on Organyloxyboranes, Organyloxydiboranes(4), Dioxaborolanes, and Boroxins17O chemical shifts of 30 boron-oxygen compounds containing tricoordinate boron atoms can be interpreted in terms of B - O(pp)π interaction. In consonance with other physical data a decrease in the π bond order is indicated by the δ17O data along the series (R2B)2O 〉 (RBO)3 〉 R2BOR 〉 RB(OR)2 〉 B(OR)3 (R either CH3 or C2H5). Natural abundance 17O NMR spectra are recorded by PFT NMR spectroscopy in relatively short time as “routine” measurements.
    Notes: Die 17O-chemischen Verschiebungen von 30 Bor-Sauerstoff-Verbindungen, die dreifach koordiniertes Bor enthalten, sind mit B - O(pp)π-Wechselwirkung zu interpretieren. In Übereinstimmung mit anderen physikalischen Daten legen die δ17O-Werte eine Abnahme der π-Bindungsordnung in der Reihe (R2B)2O 〉 (RBO)3 〉 R2BOR 〉 RB(OR)2 〉 B(OR)3 (R = CH3 oder C2H5) nahe. 17O-NMR-Spektren von Verbindungen mit natürlicher Isotopenhäufigkeit werden mittels PFT-NMR-Spektroskopie relativ rasch in „Routinemessungen“ erhalten.
    Additional Material: 3 Ill.
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  • 94
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 113 (1980), S. 391-394 
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: An Improved Method for the Synthesis of 1,3,3-Triethyl-2-methyleneindoline1,3,3-Triethyl-2-methyleneindoline (8) has been synthesized in 40% yield by alkylation of 2-methylindole with iodoethane in ethanol at 100 - 110°C/50 bar using an improved separation procedure. The 1H- and 13C-NMR spectra of 8 and its tetrafluoroborate salt are examined.
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  • 95
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Contributions to the Chemistry of Boron, CIV. New Ring Systems Containing Diboron Units: Dithiadisilaboracyclopentanes, Dithiatriborolanes, and DithiatetraborinanesThe pyridine-catalysed comproportionation between the cyclothiasilanes 1 or 4 and the dithiatetrasilacyclohexane 2 yields the dithiatrisilacyclopentane 3. 3 reacts with R2N(Cl)B - B(Cl)NR2 (5), and the R2Si - SiR2 group is specifically eliminated from 3 yielding the dithiasiladiboracyclopentane 6, which is also obtained from 5 and 1 or 4, respectively. Further action of 5 on 6 results in the dimethylamino derivative of a dithiatetraborinane (7). Moreover, a dithiadisilaboracyclopentane (8) results from the S2Si4 system 2 and phenylborane dichloride, and finally, a dithiatriborolane (10) is obtained from 6 and CH3B(SCH3)2. The new heterocyclic compounds were fully characterized chemically and spectroscopically. The X-ray structure analysis of 6 and 7 reveals nonplanar rings with short B — N bonds.
    Notes: Die mit Pyridin katalysierte Komproportionierung der Cyclothiasilane 1 und 4 mit dem Dithiatetrasilacyclohexan 2 liefert das Dithiatrisilacyclopentan 3. Dieses reagiert spezifisch mit R2N(Cl)B - B(Cl)NR2 (5) zu einem Dithiasiladiboracyclopentan (6), ebenfalls erhältlich aus 5 und 1 bzw. 4. Mit weiterem 5 setzt sich 6 zum Dimethylamino-Derivat eines Dithiatetraborinans (7) um. Ein Dithiadisilaboracyclopentan (8) entsteht aus dem S2Si4-System 2 und Phenylbordichlorid, ein Dithiatriborolan-Derivat (10) aus 6 und CH3B(SCH3)2. Die neuen Heterocyclen werden chemisch und spektroskopisch charakterisiert. Die Röntgenstrukturanalyse sicherte für 6 und 7 nichtplanare Ringsysteme mit kurzen B — N-Bindungen.
    Additional Material: 2 Ill.
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  • 96
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 113 (1980), S. 395-397 
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Simple Synthesis of Novel 1,3,9-TriazaanthracenesWittig reaction of the bromoacetate 1 with aryl isocyanates gives rise to the 10-hydroxy- 9 and 10-amino-2,4-dioxo-1,3,9-triazaanthracenes 10. These have not yet been described.
    Additional Material: 1 Tab.
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  • 97
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 113 (1980) 
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 98
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 113 (1980), S. 401-407 
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: 1,4-Addition of Grignard Compounds to α,β-Unsaturated Ethyl Cyanoacetates1,4-Addition of several Grignard compounds and hydrogen cyanide to the α,β-unsaturated ethyl cyanoacetates 1 and 4 leading to 2a - n and 5a - d.
    Notes: Die 1,4-Addition von verschiedenen Grignard-Verbindungen und Blausäure an die α,β-ungesättigten Cyanessigsäure-ethylester 1 und 4 unter Bildung von 2a - n und 5a - d wurde untersucht.
    Additional Material: 3 Tab.
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  • 99
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 113 (1980), S. 451-456 
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Kolbe Synthesis of 3,11-Dimethyl-2-nonacosanone, a Pheromone of the German Cockroach Blattella germanica3,11-Dimethyl-2-nonacosanone (5) is synthesized by coelectrolysis of 6-methyltetracosanoic acid (3b) with 5-methyl-6-oxoheptanoic acid (4). 3b is obtained by hydrolysis of the corresponding methyl ester 3a, which is prepared from 3-methylheneicosanoic acid (2) by coelectrolysis with methyl glutarate. The sec-butyl ester of 2 is obtained by 1,4-addition of octadecylmagnesium bromide to sec-butyl crotonate (1). 4 can be prepared by alkylation of potassium ethyl 2-methyl-acetoacetate with ethyl 4-bromobutyrate via 6.
    Notes: 3,11-Dimethyl-2-nonacosanon (5) wird durch Coelektrolyse von 6-Methyltetracosansäure (3b) mit 5-Methyl-6-oxoheptansäure (4) synthetisiert. 3b wird durch Verseifung des entsprechenden Methylesters 3a gewonnen, der aus 3-Methylheneicosansäure (2) durch Coelektrolyse mit Glutarsäure-monomethylester erhältlich ist. Den sek-Butylester von 2 liefert die 1,4-Addition von Octadecylmagnesiumbromid an Crotonsäure-sek-butylester (1). 4 läßt sich durch Alkylierung von Kalium-2-methylacetessigsäure-ethylester mit 4-Brombuttersäure-ethylester über 6 darstellen.
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  • 100
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 113 (1980), S. 511-519 
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: A Contribution to the Mechanism of Light-induced Isomerizations of the 4-Methylenebicyclo[3.1.0]hex-2-eneDeuterium-labelling of 1,2,3,5,6-exo-pentamethyl-4-methylenebicyclo[3.1.0]hex-2-ene (exo-1) and 1,2,3,5,6-endo-pentamethyl-4-methylenebicyclo[3.1.0]hex-2-ene (endo-1) was used to get insight into the mechanisms of the reversible photo-isomerization exo-1 ⇌ endo-1 and of their light-induced rearrangements to 1,2,3,4,6-pentamethyl-5-methylene-1,3-cyclohexadiene (2).
    Notes: Durch Verfolgung des Verbleibs von Deuterium im markierten 1,2,3,5,6-exo-Pentamethyl-4-methylenbicyclo[3.1.0]hex-2-en (exo-1) und 1,2,3,5,6-endo-Pentamethyl-4-methylenbicyclo[3.1.0]-hex-2-en (endo-1) wurden Hinweise über die Mechanismen der reversiblen Photo-Isomerisierung exo-1 ⇌ endo-1 und der gleichfalls licht-induzierten Umlagerung dieser Verbindungen zum 1,2,3,4,6-Pentamethyl-5-methylen-1,3-cyclohexadien (2) erhalten.
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