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  • 1980-1984  (634)
  • 1970-1974
  • 1980  (634)
  • Physics  (558)
  • Gas chromatography
  • Nuclear reactions
  • 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.
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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.
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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.
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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.
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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.
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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.
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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.
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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.
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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.
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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.
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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.
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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.
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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.
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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.
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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.
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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.
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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.
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  • 35
    Electronic Resource
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    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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    Weinheim : Wiley-Blackwell
    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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    Weinheim : Wiley-Blackwell
    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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    Weinheim : Wiley-Blackwell
    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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    Weinheim : Wiley-Blackwell
    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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    Chromatographia 13 (1980), S. 203-206 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Carrier gas purity ; Sample stability
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The amount of oxygen which may be present in the gas volume corresponding to a peak is investigated and compared to the sample amounts. It is shown that even with high purity carrier gases one may have a significant excess of oxygen present at low sample amounts. Attention is drawn to the possibility of impurity build-up by diffusion e.g. through the septum.
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  • 76
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    Chromatographia 13 (1980), S. 263-270 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Metal complexes ; Enantiomers ; Isotopic composition
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The high selectivity of complexation gas chromatography has been employed for enantiomer resolution and isotope separation. Thus, a chiral olefin, 3-methylcyclopentene, has been resolved analytically on optically active dicarbonyl-rhodium(I)-3-trifluoroacetyl-1R-camphorate in squalane. The deuterated ethylenes C2H4−nDn have been separated on the same rhodium(I)-containing stationary phase. The chiral aliphatic oxiranes epoxypropane andtrans-2,3-epoxybutane have been resolved on optically active nickel(II)-bis-3-trifluoroacetyl-1R-camphorate in squalane.
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  • 77
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    Journal of Polymer Science: Polymer Physics Edition 18 (1980), S. 1237-1242 
    ISSN: 0098-1273
    Keywords: Physics ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Electron microscopy reveals a high-temperature morphological transition in a styrene-butadiene-styrene block copolymer of 7000 polystyrene block molecular weight and 43,000 polybutadiene block molecular weight (7S-43B-7S). Samples quenched in liquid nitrogen from temperatures above 150°C show no structure, whereas those quenched from temperatures below 140°C clearly show a multiphase structure. We previously reported that the 7S-43B-7S polymer exhibits a relatively sharp melt rheological transition in the temperature region between 140 and 150°C from highly viscoelastic and nonlinear viscous behavior to linear viscous behavior with insignificant elasticity. The dynamic viscoelastic properties are measured at different strain amplitudes in this study, and the results show that the melt rheological transition behavior is not influenced by the strain amplitude. This study clearly shows that the melt rheological transition in the 7S-43B-7S results from a morphological transition from a multiphase structure below about 140°C to a single-phase structure above about 150°C.
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  • 78
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    Journal of Polymer Science: Polymer Physics Edition 18 (1980), S. 1257-1270 
    ISSN: 0098-1273
    Keywords: Physics ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The intensity of the glass transition in semicrystalline polycarbonate was measured by differential scanning calorimetry and by thermally stimulated discharge of electrets. Solution-cast and bulk-crystallized samples possessing widely varying crystallinities and morphologies were investigated. It is shown that the intensity of the glass transition is governed by the extent of primary crystallization and is a linear combination of intensities from the bulk amorphous regions and from noncrystalline polymer within semicrystalline aggregates such as spherulites. The intensity of the glass transition within spherulites is about 0.1-0.3 as great as that in bulk amorphous regions. A three-phase model incorporating two distinct types of noncrystalline polycarbonate is proposed to account for the properties of this polymer.
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  • 79
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    Journal of Polymer Science: Polymer Physics Edition 18 (1980), S. 1311-1324 
    ISSN: 0098-1273
    Keywords: Physics ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: A detailed description of the morphology and the complex melting behavior of poly(ethylene terephthalate) crystallized isothermally in the range 100-245°C is presented. Double or single melting endotherms can deliberately be obtained by varying the heating rate in the differential scanning calorimeter (DSC). In the case of double melting peaks, the first endotherm (I) corresponds to the melting of the crystalline material formed at the crystallization temperature Tc. The second melting endotherm (II) originates from the melting of a fraction of the original crystalline material reorganized during the DSC scan. The appearance of one melting endotherm (I or II) relates to the melting of the original structure or the melting of a completely transformed structure. Taking the end of the melting endotherm I as the final melting temperature TM of the material, an equilibrium melting temperature of 290°C is obtained from a plot of TM vs. Tc. A detailed morphological study of the isothermally crystallized samples by electron microscopy and both small-angle and wide-angle x-ray scattering raises questions about the use of the two-phase concept in relating morphological parameters and melting behavior at low crystallization temperatures.
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  • 80
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    Journal of Polymer Science: Polymer Physics Edition 18 (1980), S. 1361-1381 
    ISSN: 0098-1273
    Keywords: Physics ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: A temperature-dependent small-angle x-ray scattering and electron microscopic study on a sample of low-density polyethylene affords a determination of the structure changes in a heating and cooling cycle and suggests a new model of partial crystallization and melting. The analysis of SAXS data is based upon some general properties of the electron-density correlation function. Electron micrographs are obtained from stained sections γ irradiated at elevated temperatures and are analyzed quantitatively by statistical means. According to the model proposed here the thickness distribution in the amorphous layers, rather than that of the crystalline regions, is the essential factor governing the crystallization and melting behavior. The temperature-dependent changes in this thickness distribution provide a natural explanation for the large reversible changes in long-spacing.
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  • 81
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    Journal of Polymer Science: Polymer Physics Edition 18 (1980), S. 1421-1431 
    ISSN: 0098-1273
    Keywords: Physics ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Solid solutions of two low-molecular-weight polyethylene fractions, formed by rapid quenching from the melt, were studied by differential scanning calorimetry, low-frequency Raman spectroscopy, and Fourier-transform infrared spectroscopy. Two kinds of defects exist in these solid solutions; namely, a disruption of chain extension and the presence of monoclinic packing. The distribution of fully extended chain-segment lengths and the intensity of the 717 cm-1 infrared band, characteristic of the monoclinic phase, are found to be composition dependent. Our spectroscopic studies of the solid solutions support the model first proposed by Ott and Slagle.
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  • 82
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    Journal of Polymer Science: Polymer Physics Edition 18 (1980), S. 1413-1419 
    ISSN: 0098-1273
    Keywords: Physics ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The thermal behavior of α nylon-12 film cast from a phenol-ethanol mixture has been studied by differential scanning calorimetry. Polymorphism has been analyzed by x-ray diffraction. The γ form exhibits a single endothermic melting peak in the thermogram, whereas the α form exhibits double peaks. Samples with mixed α and γ forms show double peaks at the same positions and the area ratio changes in accordance with the amounts of the two forms. The appearance of the γ peak, even for the α sample, is explained by recrystallization to the γ form after melting of the α form. The melting point of α nylon-12 is ca. 173°C, which is lower by 6-7° than that of the γ form. Once the α or γ sample has been melted and then cooled, its heating thermogram shows a small peak before the appearance of the main peak. The small peak seems to be due to incomplete and/or smaller crystallites formed during cooling. Heat treatment below the melting point of α nylon-12 is effective in transforming the α form to the γ form, probably via a melt-recrystallization process.
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  • 83
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    Journal of Polymer Science: Polymer Physics Edition 18 (1980), S. 1433-1438 
    ISSN: 0098-1273
    Keywords: Physics ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: A 40:60 mole ratio poly(ethylene terephthalate-co-p-oxybenzoate) was studied by dynamic scanning calorimetry. Vitrification occurred in two steps, which could be linked by optical microscopy to a two-phase structure. For the lower glass transition, hysteresis was absent on heating and cooling through the transition temperature. Since all prior studied glasses show such hysteresis, this may be linked to the mesophase structure and raises the question whether mesophases always display such glass-transition behavior.
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  • 84
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    Journal of Polymer Science: Polymer Physics Edition 18 (1980), S. 1469-1480 
    ISSN: 0098-1273
    Keywords: Physics ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: A small-angle x-ray scattering (SAXS) investigation of two linear segmented polyurethanes was carried out to learn about the respective domain structure (morphology). Both urethanes had a hard segment of methylene-bis(4)phenyl isocyanate (MDI) and butanediol. These two components comprised 28% by weight of each system. The soft segments differed in that one was a polyether (tetramethylene oxide, molecular weight 1000), while the other was a polyester (polytetramethylene adipate, molecular weight 1000). Both of these segmented urethanes were stored at room temperature for over 6 months prior to investigation. Using an automated Kratky camera, SAXS scans were made. By detailed analysis (using the computer program of Vonk) the average interfacial thickness E of the domains was determined by two approaches. The value of E for the polyester was 10-12 Å, while it was 5-7 Å for the polyether. Within the limits of the assumptions used for analysis, these data directly support the conjecture that polyether urethanes generally lead to better phase separation. Other aspects of the analysis provided further information on the morphological structure. Some cautionary comments are provided on the use of quantitative SAXS data obtained from these or similar systems.
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  • 85
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    Journal of Polymer Science: Polymer Physics Edition 18 (1980), S. 1481-1482 
    ISSN: 0098-1273
    Keywords: Physics ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Additional Material: 1 Ill.
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  • 86
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    Journal of Polymer Science: Polymer Physics Edition 18 (1980), S. 1513-1522 
    ISSN: 0098-1273
    Keywords: Physics ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The melting behavior of low-density polyethylene was studied by electron microscopy. The experimental techniques and method of evaluation chosen were such as to deliver quantitative numerical data. The values which could be derived from suitably prepared histograms were the minimum, maximum, average, and most probable values of the crystal thickness d and long-spacing L. All these values were in good agreement with small-angle x-ray scattering results. The histograms also show the distribution functions for d and L, so that effects leading to changes in the average values can be observed in detail. The results provide further support for a model of melting and crystallization proposed in a previous paper.
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  • 87
    ISSN: 0098-1273
    Keywords: Physics ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The kinetics of crystallization and structure formation of polycaproamide (PCA) during anionic adiabatic polymerization of ε-caprolactam was studied. The adiabatic crystallization was shown to comprise three successive stages. In the first stage PCA forms dendritelike structures, the space between which is filled with the monomer. In the second stage rather rapid crystallization proceeds to give large loose spherulites. The dendritic structures serve as nuclei for development of spherulites. In the third stage slow secondary crystallization occurs. It is accomplished by crystallization of the residual amorphous substance located both in the dendritic nucleus and throughout the volume of the spherulites. This process is followed by the partial disappearance of the dendritic nuclei and by thickening of lamellae, which results in a substantial densification of initial structures and appearance of fine spherulites. As a result, a fine spherulitic structure with 50% crystallinity is formed.
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  • 88
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    Journal of Polymer Science: Polymer Physics Edition 18 (1980), S. 1533-1559 
    ISSN: 0098-1273
    Keywords: Physics ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: An enquiry is presented into the nature and origin of thermoreversible gelation of poly(vinyl chloride) (PVC). In line with a previous paper it is demonstrated by direct x-ray diffraction evidence that the origin of the gelation is crystallization, and that this crystallinity can be conspicuously apparent even for the usual technological polymer. In addition some unusual diffraction effects become apparent such as do not obviously follow from existing notions of the PVC structure. Combined infrared dichroism and x-ray studies revealed that these new effects are attributable to a two-component nature of the crystallinity where the components are distinguished by their orientation behavior, lateral extension, and possibly morphology of the crystallites. Some of the crystals orient with their a axes (type A crystals) and some with their c axes (type B crystals) along the stretch direction. Other more complex orientability differences are also manifest during film formation. Crystals B are smaller, and are believed to correspond to the network forming junctions, hence to fringed micellar crystals. Crystals A have a less evident connection with the network and are hypothesized to be of lamellar character, the behavior of which is closely simulated by lamellar crystal additives (stabilizer crystals). High-temperature x-ray work revealed no melting of crystals even in the temperature range where endotherms appear in the thermograms.
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  • 89
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    Journal of Polymer Science: Polymer Physics Edition 18 (1980), S. 1587-1597 
    ISSN: 0098-1273
    Keywords: Physics ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Monad, dyad, and triad populations have been derived from the 13C NMR spectra of eight ethylene-propylene copolymers. Using these values, Kinetic parameters of the polymerization have been calculated, including conditional probabilities, and reactivity ratios. The fraction of propylene entering in an inverted order has been found to be about 20%. The copolymerization is dominated by the relatively large reactivity of ethylene. There is an alternating tendency for the two monomers which is evident both in the normal addition of propylene and the inverted addition. Penultimate effects do not play a significant role.
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  • 90
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    Journal of Polymer Science: Polymer Physics Edition 18 (1980), S. 1621-1632 
    ISSN: 0098-1273
    Keywords: Physics ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The permeability and time lag at pressures below 1 atm were measured for carbon dioxide in five polystyrene samples with different molecular weights at 25 to 40°C. The apparent permeability coefficient decreases with increasing carbon dioxide pressure and also decreases with increasing molecular weight of polystyrene, whereas the apparent diffusion coefficient calculated from time lag increases with pressure and is independent of molecular weight. Parameters for the partial-immobilization model were determined from the apparent diffusion and permeation coefficients by using a nonlinear least-squares optimization program without using sorption data. The results suggest that the void-saturation constant C′H decreases as the molecular weight of the polymer increases or as the chain-end free volume decreases. The significance of these observation and their interpretation is discussed in terms of free-volume theory for glassy polymers.
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  • 91
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    Journal of Polymer Science: Polymer Physics Edition 18 (1980), S. 1643-1650 
    ISSN: 0098-1273
    Keywords: Physics ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Changes in density and in the corresponding degree of crystallinity with radiation dose are studied experimentally for γ-irradiated polytetrafluoroethylene (PTFE) in the dose range from 1 X 103 to 1 X 109 R. The relation between the amorphous fraction and the radiation dose is derived from a quantitative analysis of cold crystallization by scission of polymer backbone chains. The characteristic radiation dose, at which one break occurs on the average per initial molecule, is estimated as about 3 X 104 R on the basis of a derived kinetic equation. The theoretical relation is modified by considering microvoids produced in the irradiated samples. The radii of microvoids in the form of spheres are evaluated as about 0.2 nm, and are also related to cage spheres relevant to the chain scission process. Good agreement between the modified theoretical relation and experimental data is attained over the entire range of radiation dose.
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  • 92
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    Journal of Polymer Science: Polymer Physics Edition 18 (1980), S. 1663-1664 
    ISSN: 0098-1273
    Keywords: Physics ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Additional Material: 1 Ill.
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  • 93
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    Journal of Polymer Science: Polymer Physics Edition 18 (1980), S. 1673-1683 
    ISSN: 0098-1273
    Keywords: Physics ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Light scattering and viscometric studies have been carried out on dilute solutions of a polybenzimidazole in N,N-dimethylacetamide. The data, which span the molecular weight range 2.9 ≦ 10-4Mw ≦ 23.3, and the temperature range 290 ≦ T/K ≦343, yield the dependence of the mean-square radius of gyration 〈s2〉LS, the second virial coefficient A2, and the intrinsic viscosity [η] on molecular weight Mw and temperature. The unperturbed mean-square radius 〈s20〉LS was calculated using experimental values of 〈s2〉LS and A2. It was found that excluded volume effects on 〈s2〉LS are very small. The unperturbed hydrodynamic chain dimension 〈s20〉η was estimated by considering draining effects. A small value of the draining parameter was obtained. Analysis of the temperature dependence of A2 and [eta;] leads to the conclusion that this system approaches a lower theta temperature with increasing temperature. The steric factor σ = 〈s20〉/〈s20〉f, based on the value of 〈s20〉f calculated for the polymer chain with free rotation, is nearly unity. Most of these properties can be interpreted in terms of long rotational units within the main chain.
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  • 94
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    Journal of Polymer Science: Polymer Physics Edition 18 (1980), S. 1707-1716 
    ISSN: 0098-1273
    Keywords: Physics ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: An anisotropic dispersive continuum model for the collective modes of polyethylene of any degree of crystallinity is suggested. The model successfully explains the experimental results for specific heat of polyethylene of 100%, 84.1%, 74.5%, 45.9%, and 0% crystallinity in the temperature range 2.5-60 K, where the specific heat of amorphous polyethylene is markedly different from that of crystalline polyethylene. The variation of specific heat with degree of crystallinity can be obtained by varying only one parameter θ1 (characterizing the low energy cubic modes), keeping the other two parameters (characterizing the transverse and longitudinal chain modes) constant. Thus, in going from the crystalline to the amorphous state, it is essentially the interchain binding which is affected, the chain modes being left undisturbed. Using the calculated values of specific heat for varying degrees of crystallinity, the variation of θ1 with the crystallinity is reported. Observed high-temperature specific heats for crystalline and amorphous polyethylene up to 300 K are also explained using additional optical modes. The anisotropic Mössbauer elastic scattering fraction (MESF) for polyethylene of different degrees of crystallinity in the temperature range 0-425 K is obtained. For a given degree of crystallinity there is marked anisotropy in MESF which increases with increase in temperature. For a given direction, longitudinal or transverse, there is a large difference between the MESF of 0% and 100% crystalline polyethylene, which also increases with the increase in temperature. It is quite possible that the MESF experiment may prove to be more sensitive than the usual method for the determination of degree of crystallinity.
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  • 95
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    Journal of Polymer Science: Polymer Physics Edition 18 (1980), S. 1747-1752 
    ISSN: 0098-1273
    Keywords: Physics ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Previous work has shown that in the environmental stress cracking (ESC) of polyethylene, there are three major zones of behavior depending on the applied stress and the nature of the liquid environment. These three zones correspond to “pure” ESC (zone 1), ESC controlled by the speed of penetration of the liquid within a growing crack (zone 2), and behavior as in the absence of liquid (zone 3). Analysis of the transitions between zones has shown that, in the present case, a given liquid will either be capable of giving rise to all three types of behavior depending on the stress applied, or will be totally inactive. A related analysis has enabled the order of magnitude of the dimensions of the crack tip to be estimated and this has been found to be in the range of a micron.
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  • 96
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    Journal of Polymer Science: Polymer Physics Edition 18 (1980), S. 1771-1780 
    ISSN: 0098-1273
    Keywords: Physics ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Smith-Ewart Case-2 kinetics are applied to a continuous stirred tank reactor operating at steady state in the high and middle range of conversion. Above the conversion CD at which the monomer droplets disappear in a batch reaction, the predictions are surprising. The particle size is predicted to be inversely proportional to the effective soap concentration S and independent of mean residence time θ below CD it is predicted to be proportional to the one-third power of θ and independent of S. Above CD the particle concentration should be proportional to the cube of S and independent of θ; below this it should be as predicted by previous workers. The expressions for conversion are also different above CD. A new, more instructive, derivation is used. Simple analytic expressions are given for commonly used breadth parameters of the particle size distribution. It is shown that when conversion is low, an approximation made by previous workers is invalid, in that the growth rate can no longer be considered continuous.
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  • 97
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    Journal of Polymer Science: Polymer Physics Edition 18 (1980), S. 1847-1851 
    ISSN: 0098-1273
    Keywords: Physics ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Additional Material: 4 Ill.
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  • 98
    Electronic Resource
    Electronic Resource
    New York : Wiley-Blackwell
    Journal of Polymer Science: Polymer Physics Edition 18 (1980), S. 1879-1890 
    ISSN: 0098-1273
    Keywords: Physics ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Fluorescence polarization was used to measure segmental orientation in stretched polyisoprene networks. Stress and orientation of chemically bonded fluorescent labels were simultaneously recorded during stretching. Two deviations from the classical theory of rubber elasticity were observed: (i) an extra orientation of dry networks, which was interpreted by assuming the existence of weak nematiclike interactions between segments, and (ii) a saturation of orientation at high elongation which could be due to local conformational changes.
    Additional Material: 10 Ill.
    Type of Medium: Electronic Resource
    Library Location Call Number Volume/Issue/Year Availability
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  • 99
    Electronic Resource
    Electronic Resource
    New York : Wiley-Blackwell
    Journal of Polymer Science: Polymer Physics Edition 18 (1980), S. 1907-1917 
    ISSN: 0098-1273
    Keywords: Physics ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The measurement of the sedimentation velocity coefficient of narrow distribution linear, four-arm and six-arm star and comb polystyrenes in a theta solvent permits the experimental determination of h, i.e., the ratio of the translational friction coefficients of the branched polymer to that of its linear homolog. A comparison of experimental h/g1/2 values with theoretical predictions can then be made. It was observed that the equivalent hydrodynamic radii derived from sedimentation and intrinsic viscosity measurements are identical within experimental error.
    Additional Material: 6 Ill.
    Type of Medium: Electronic Resource
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  • 100
    Electronic Resource
    Electronic Resource
    New York : Wiley-Blackwell
    Journal of Polymer Science: Polymer Physics Edition 18 (1980), S. 1945-1954 
    ISSN: 0098-1273
    Keywords: Physics ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: X-ray diffraction, thermally stimulated depolarization, and piezoelectric and pyroelectric current measurements have been carried out on biaxially oriented polyvinylidene fluoride film, corona-poled both negatively and positively, at elevated temperature. Larger piezoelectric and pyroelectric coefficients are obtained at lower values of the poling field, when corona charging takes place at elevated temperature rather than room temperature. Negative charging is more effective than positive. The polarization mechanism is dipole alignment, and a conversion of Form-II crystallites to Form I. The large space-charge injected by the corona, and trapped in the material, acts through creation of high internal fields, and shows little, if any, piezoelectric and pyroelectric effects of its own.
    Additional Material: 6 Ill.
    Type of Medium: Electronic Resource
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