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  • 1985-1989  (7,239)
  • 1850-1859
  • 1985  (7,239)
  • Chemistry  (7,239)
  • 101
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 8 (1985), S. 156-157 
    ISSN: 0935-6304
    Keywords: 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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  • 102
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 8 (1985), S. 169-169 
    ISSN: 0935-6304
    Keywords: 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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  • 103
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 8 (1985), S. 193-195 
    ISSN: 0935-6304
    Keywords: Atmospheric residue ; Capilary columns ; Gas chromatography ; Pyrex ; Simulated distillation (SIMDIS) ; 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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  • 104
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 8 (1985), S. 200-208 
    ISSN: 0935-6304
    Keywords: 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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  • 105
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 8 (1985), S. 306-307 
    ISSN: 0935-6304
    Keywords: Liquid chromatography, LC ; Hydrophobic interaction chromatography, HIC ; Separation of proteins ; Type of salt ; TSKgel phenyl-5PW ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
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  • 106
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 8 (1985), S. 37-38 
    ISSN: 0935-6304
    Keywords: Liquid chromatography, HPLC ; Racemate separation ; Crosslinked acetylcellulose as chiral matrix ; Polarimetry ; UV-detection ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
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  • 107
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 8 (1985), S. 256-258 
    ISSN: 0935-6304
    Keywords: Liquid chromatography, HPLC ; Non-aqueous ion exchange ; Abietanoic diterpenoids ; Coleons, royleanones ; Quinone methides, hydroxyquinones ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A method is described for the HPLC separation of moderately acidic, dehydrated, and multi-oxygenated diterpenoids, compounds which hitherto could not be handled by HPLC. It is based on chemically bonded silica strong cation exchangers in the protonated form, using organic solvents of the full polarity range as eluents. Thus a stable and easy-to-regenerate substitute for buffered silica gel is obtained.
    Additional Material: 4 Ill.
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  • 108
    ISSN: 0935-6304
    Keywords: Liquid chromatography, HPLC ; Electron paramagnetic resonance, EPR ; Metalloporphyrins ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 2 Ill.
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  • 109
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 8 (1985), S. 290-292 
    ISSN: 0935-6304
    Keywords: Liquid chromatography, HPLC ; Post column, colorimetric detection ; Sugars ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
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  • 110
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 8 (1985), S. 301-302 
    ISSN: 0935-6304
    Keywords: Gas chromatography, GC ; Glass capillary columns ; Kovats retention indices ; Monocyclic terpene alcohols ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 1 Tab.
    Type of Medium: Electronic Resource
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  • 111
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 8 (1985), S. 94-97 
    ISSN: 0935-6304
    Keywords: 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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  • 112
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 8 (1985), S. 318-319 
    ISSN: 0935-6304
    Keywords: 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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  • 113
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 8 (1985), S. 326-331 
    ISSN: 0935-6304
    Keywords: Gas chromatography, GC ; Fused silica capillary columns ; Deactivation ; Hydrothermal treatment ; Wettability of fused silica ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The activity of fused silica capillary tubing has been shown to vary considerably, which severely influences the reproducibility of column deactivation and inertness. Methods for producing a reproducible, high activity surface with maximum hydroxylation by various hydrothermal treatments were evaluated. Columns pretreated with 20% nitric acid at 200°C for 10 hours, deactivated with D4, coated with OV-73, and crosslinked with azo-tert-butane were found to possess excellent inertness for sensitive analytes such as alcohols, amines, and alkaloid drugs.
    Additional Material: 7 Ill.
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  • 114
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 8 (1985), S. 357-359 
    ISSN: 0935-6304
    Keywords: Gas chromatography, GC ; Fused silica capillary columns ; Effluent splitter ; Heart cutting ; Multiple detection ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
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  • 115
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 8 (1985), S. 364-365 
    ISSN: 0935-6304
    Keywords: Monte Carlo model of adsorption ; Multi-site adsorption ; Chemically bound stationary phases ; 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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  • 116
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 8 (1985), S. 371-372 
    ISSN: 0935-6304
    Keywords: 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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  • 117
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 8 (1985), S. 378-384 
    ISSN: 0935-6304
    Keywords: Gas chromatography, GC ; Fused silica capillary columns ; Deactivation ; Phenylhydrosiloxanes ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: In this work, an investigation of new organosilicon hydride reagents with phenyl functional groups for deactivation and surface modification of fused silica capillary columns is described. Different reagents were tested for their ability to deactivate the fused silica surface, and actual critical surface tension measurements were made using the capillary rise method. The deactivation procedure required lower optimum temperatures than conventional methods. Deactivated capillaries and coated capillary columns were prepared and tested for reproducibility, efficiency, and surface inertness towards basic and acidic compounds at the low nanogram level.
    Additional Material: 7 Ill.
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  • 118
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 8 (1985), S. 283-289 
    ISSN: 0935-6304
    Keywords: Gas chromatography, GC ; Fused silica capillary columns ; Microbial mutagenicity ; Solvent refined coal ; Creosote oils ; Polyaromatic hydrocarbons ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The chemical composition of a commercially available creosote was compared to a direct coal liquefaction product, i.e., solvent refined coal-II fuel oil blend (SRC-II FOB) using high resolution gas chromatography (HRGC). In addition, hydrogenated products of these materials were studied. Samples were fractionated by chemical class on neutral alumina. Those fractions previously shown to be the most mutagenic and tumorigenic in laboratory bioassays of coal-derived materials were analyzed and compared by HRGC and gas chromatography/mass spectrometry (GC/MS). Individual components were tentatively identified and quantitated. Although similar chemical components were present in the creosote and SRC-II FOB fractions studied, the creosotes had higher concentrations of heavy molecular weight materials and a lower ratio of alkylated to parent polycyclic aromatic compounds than the coal liquefaction products. The creosote samples also had a significantly higher concentration of components which eluted in the polycyclic aromatic hydrocarbon (PAH) chemical class fraction. Amino-substituted PAH were present in both nonhydrogenated coal liquid and creosote materials. The creosote and SRC-II FOB crudes and nitrogen-containing polycyclic aromatic compound (NPAC) chemical class fractions expressed similar microbial mutagenicity. Based on chemical analysis data, the predicted tumorigenic potency of the creosote in laboratory bioassay systems would be equivalent to or greater than the SRC-II FOB.
    Additional Material: 2 Ill.
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  • 119
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    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 8 (1985), S. 308-308 
    ISSN: 0935-6304
    Keywords: 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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  • 120
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 8 (1985), S. 313-316 
    ISSN: 0935-6304
    Keywords: 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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  • 121
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 8 (1985), S. 521-524 
    ISSN: 0935-6304
    Keywords: Gas chromatography, GC ; Fused silica capillary columns ; Mixture and trace analysis ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: About three years ago, fused silica capillary columns were introduced in the Quality Control Laboratory of the Shell refinery/chemical complex at Pernis. In general, long, thick-film, wide-bore capillary columns are used together with low split ratios and hydrogen as carrier gas. These conditions enable the analysis of relatively large sample amounts, resulting in low detection limits for the minor components without overloading by the major components, while still maintaining a satisfactory resolution. A number of applications are shown, such as the analysis of complex mixtures, the determination of trace impurities and the analysis of residual volatiles in polymers.
    Additional Material: 5 Ill.
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  • 122
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 8 (1985), S. 535-538 
    ISSN: 0935-6304
    Keywords: Gas chromatography, GC ; Glass capillary columns ; Polyethylene glycol immobilization ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Polyethylene glycols can be immobilized in glass capillary columns by a new procedure involving covering the glass walls with a layer of graphitized carbon black and by flowing a mixture of the stationary phase and dicumyl peroxide. After curing and conditioning the column is ready for use. Excellent performance is reported for Carbowax 20 M and high molecular weight glycols. For other glycols the immobilized layer is less stable and can be washed out.
    Additional Material: 4 Ill.
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  • 123
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 8 (1985), S. 572-575 
    ISSN: 0935-6304
    Keywords: Gas chromatography, GC ; Capillary columns ; Cooled needle sampling ; Split injection ; Splitless injection ; Simulated distillation ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Cooled needle sampling using syringes was applied to splitless injection and to simulated distillation analyses. Slight changes of the construction of the previous device are also described. The changes concern the temperature profile within the injector and especially the vaporization insert. Even with the low carrier gas flow through the injector during splitless injection, discrimination by component volatility can be avoided. Precision and accuracy of simulated distillation data obtained with split sampling also can be improved by the cooled needle technique.
    Additional Material: 3 Ill.
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  • 124
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    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 8 (1985), S. 585-590 
    ISSN: 0935-6304
    Keywords: Gas chromatography, GC ; Fused silica capillary columns ; Glass packed columns ; Polychlorinated biphenyls ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: This article describes and critically evaluates a complete method for the quantitation of PCB in sediment samples. The extraction and clean-up procedure is described. Packed column and capillary column results are compared. Capillary column quantitation yields lower values for total PCB loading. Preferences for capillary column quantitation are discussed and explained. Capillary quantitation is based on the combination of an external Aroclor standard and an internal decachlorobiphenyl standard for normalizing data. In light of the recent report of synthesis of all 209 PCB congeners a suggestion is made to use these as absolute standards to establish a bank of primary standard Aroclors.
    Additional Material: 1 Ill.
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  • 125
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    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 8 (1985), S. 611-617 
    ISSN: 0935-6304
    Keywords: Gas chromatography, GC ; Temperature programmed retention indices ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The procedure for calculating linear temperature programmed indices as described in part 1 has been evaluated using five different nonpolar columns, with OV-1 as the stationary phase. For fourty-three different solutes covering five different classes of components, including n-alkanes and alkyl-aromatic compounds, both isothermal and temperature programmed indices were determined. The isothermal information was used to calculate temperature programmed indices. For several linear programmed conditions accuracies better than 0.51T-units were usually obtained. The results are compared with published procedures.It is demonstrated that isothermal retention information obtained on one column can be transferred to another column with the same stationary phase but different column dimensions and/or phase ratio. The temperature programmed indices calculated in this way also have an accuracy better than 0.51T-u.The temperature accuracy and precision of the GC-instrumentation used was of the order of 0.1°C. All calculations can be run with a Basic-programmed microcomputer.
    Additional Material: 12 Tab.
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  • 126
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    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 8 (1985), S. 664-672 
    ISSN: 0935-6304
    Keywords: Gas chromatography, GC ; Fused silica capillary columns ; CP-MAS NMR ; Deactivation methods ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The effect of deactivating a fused silica surface by silylation with 1,1,3,3-tetraphenyl-1,3-dimethylilazane (TPDMDS), triphenylsilylamine (TPSA), and octamethylcyclotetrasiloxane (D4) and by polydimethylsiloxane degradation (PSD) is studied. Rehydrated, dried, and deactivated Cab-O-Sil M5 samples are used as model materials for 29Si CP-MAS NMR analysis.At about 350 °C, TPDMDS yelds mainly diphenylmethylsiloxysilane, dimethyldisiloxysilane, and triphenylsiloxysilane groups. TPSA yields phenyltrisiloxysilane, diphenyldisiloxysilane, and triphenylsiloxysilane groups. At 400°C, the products formed initially are eventually replaced by methyltrisiloxysilane or phenyltrisiloxysilane groups, while a substantial number of silanol groups still remains. The possible consequences for wettability are discussed.D4 reacts with Cab-O-Sil even at 200°C, but a large number of silanol groups remains. This number decreases gradually at higher temperatures and becomes negligible above 400°C. The formation of methyltrisiloxysilane groups, which starts at 425°C, is predominant at 490°C.
    Additional Material: 9 Ill.
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  • 127
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    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 8 (1985), S. 726-733 
    ISSN: 0935-6304
    Keywords: Coupled HPLC-capillary GC ; Retention gap ; Concurrent solvent evaporation ; Extraction techniques ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: HPLC fractions involving eluents of low to intermediate polarity can be introduced into capillary GC using the retention gap technique. Partial or complete solvent evaporation during sample introduction reduces the length of, or almost eliminates, the zone in the column inlet (retention gap) flooded by the introduced liquid, allowing introduction of larger HPLC fractions and/or use of shorter retention gaps. The corresponding techniques are reviewed. The retention gap technique is poorly suited for water-containing HPLC eluents (reversed phase HPLC) and fails completely if HPLC eluents contain, e.g., buffer salts. Various techniques for extracting such HPLC eluents are considered, preference being given to extraction into GC stationary phases from where solutes are thermally desorbed into the GC separation column. Limiting factors are diffusion of solutes within the liquid phase to be extracted and retention power of the extraction tubes.
    Additional Material: 6 Ill.
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  • 128
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary columns ; Automatic analysis of volatiles ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A system for automatic analysis of volatile compounds by purge-and-cold-trapping/capillary gas chromatography is described. It is suitable for analysis of volatile compounds in a wide variety of samples, such as water, food products and environmental samples. Possibilities and limitations of the system are evaluated in relation to several parameters. The efficiency of different types of cryogenic trap (open tubular, coated, packed) is also investigated; it depends on purge-flow rate, temperature of trapping, and total purge volume. Examples of the analysis of volatile compounds in foods and water are given.
    Additional Material: 11 Ill.
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  • 129
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 8 (1985), S. 824-828 
    ISSN: 0935-6304
    Keywords: Supercritical fluid chromatography, SFC ; Aromatic hydrocarbons ; Multidimensional chromatography ; Normal and reversed phase ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A two-dimensional chromatographic separation is described which makes use of the unusual properties of supercritical carbon dioxide mobile phase. This solvent has the property of giving a separation of polycyclic aromatic hydrocarbons (PAH) on amine-bonded columns similar to that given by usual normal-phase solvents, and on octadecylsilane-bonded columns similar to that given by usual reversed-phase solvents.Packed columns were used, arranged so that they could be switched in or out of the solvent flow. Polycyclic aromatic hydrocarbon mixtures isolated from coal tar were fractionated according to number of aromatic carbon atoms on an amine-bonded column, and these fractions were trapped on an octadecysilane-bonded column. They were subsequently eluted according to the polarity of the individual compounds. Separations from fractions containing 16 and 18 aromatic carbon atoms are shown.
    Additional Material: 7 Ill.
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  • 130
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 8 (1985), S. 838-842 
    ISSN: 0935-6304
    Keywords: Thin-layer chromatography, HPTLC ; Elution characteristics ; Temperature effect ; Solvent polarity effect ; Polar lipids ; Boric acid ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 5 Ill.
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  • 131
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 8 (1985), S. 852-853 
    ISSN: 0935-6304
    Keywords: Gas chromatography, GC ; Gas sampling ; Gas 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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  • 132
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 8 (1985), S. 860-862 
    ISSN: 0935-6304
    Keywords: Liquid chromatography, LC ; Solvent peaks ; Mixed eluents ; UV-visualization ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 3 Ill.
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  • 133
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary columns ; Simulated distillation ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The characterization of heavy petroleum fractions is essential for the design and improvement of cracking plants converting heavy feedstock into valuable “white” products. Conventional simulated distillation methods using packed columns are unsuitable for this purposes, being limited to boiling points up to about 600°C. The method presented is able to cover a boiling points interval ranging from about 150°C up to around 800°C. It employs a short, nonpolar, highly thermostable capillary column routinely operated at temperatures around 430°C. The analytical system is based on a high temperature versions of a fully automatic, capillary dedicated gas chromatograph. The experimental data demonstrate that cold on-column injection is the sole sampling system suitable for such heavy compounds. The conversion of the retention times into boiling points, based on the use of low molecular weight polyethylenes, is extremely reliable, as demonstrated by the excellent retention time reproducibilities. The lower part (up to 550-600°C TBP) of the boiling point distribution curves of heavy petroleum fractions obtained on capillary columns fits well with the corresponding distribution curves based on packed column data. For the petroleum fractions fully eluted from the column the quantitative results obtained either using internal standards or by direct processing of the elution curves are in excellent agreement (less than 0.3 weight% differences). The method has been applied to the determination of the true boiling points corresponding to short path vacuum distillation (DISTACT) cut points over 300°C.
    Additional Material: 18 Ill.
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  • 134
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 8 (1985), S. 807-810 
    ISSN: 0935-6304
    Keywords: Capillary gas chromatography (CGC) ; High resolution ; High efficiency ; Optimal elution temperature ; Ketosteroids ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 3 Ill.
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  • 135
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 8 (1985), S. 816-823 
    ISSN: 0935-6304
    Keywords: Gas chromatography, GC ; Fused silica capillary columns ; Stationary phase synthesis ; Cyclic siloxanes ; Supercritical fluid chromatography, SFC ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A comparison is made between dichlorosilanes and cyclic siloxanes as starting materials in the synthesis of stationary phases for capillary gas chromatography (CGC) and supercritical fluid chromatography (SFC). Siloxanes containing one or more of the side groups methyl, vinyl, phenyl, and cyanoethyl in various ratios were synthesized and compared. These phases were characterized by chromatographic (gel permeation, GPC), spectroscopic (IR, 1H NMR, 29Si NMR), and thermal (DSC) methods. Coated fused silica columns were evaluated with respect to polarity, crosslinkability with several free-radical initiators, and thermal stability. A new liquid phase, 7% cyanoethyl, 7% phenyl, 1% vinyl methyl polysiloxane is shown to be more polar than OV-1701, more temperature stable, easily crosslinked and suitable for use in supercritical fluid chromatography.
    Additional Material: 5 Ill.
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  • 136
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 8 (1985), S. 847-848 
    ISSN: 0935-6304
    Keywords: 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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  • 137
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 8 (1985), S. 693-694 
    ISSN: 0935-6304
    Keywords: Gas-liquid chromatography, GLC ; Capillary columns ; Static coating ; Monitoring device ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 3 Ill.
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  • 138
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    Journal of High Resolution Chromatography 8 (1985), S. 863-866 
    ISSN: 0935-6304
    Keywords: Capillary GC ; Retentention hole ; Wine analysis ; Diethylene glycol determination ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 3 Ill.
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  • 139
    ISSN: 0935-6304
    Keywords: Gas chromatography-mass spectrometry ; Capillary columns ; Stationary phases ; Silicones ; Thermal degradation ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The applicability of capillary columns for gas chromatography is often limited by stationary phase degradation at elevated temperatures. In order to achieve a better understanding of column thermostability, column bleed products have been analyzed qualitatively by gas chromatography-mass spectrometry (GC-MS). Three silicone stationary phases were studied: SE-52, SE-54, and OV-1701. Each of these was immobilized in the columns. The proportion of cyclics containing diphenyl in column bleed from SE-52 reflected to a large extent the composition of the polymer, while for SE-54 the proportion of such cyclics was unexpectedly high. The polar moiety of OV-1701, the cyanopropyl(phenyl)siloxy unit, was found to exert a highly destabilizing effect on the polymer, and the thermal degradation products consisted mainly of cyclosiloxanes containing this unit.
    Additional Material: 6 Ill.
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  • 140
    ISSN: 0935-6304
    Keywords: Capillary gas chromatography ; Selectivity ; Selectivity tuning ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The selection of stationary phases in capillary gas chromatography is discussed. Methyl silicone, phenyl methyl silicone, trifluoropropylmethyl silicone, biscyanopropyl silicone, and high molecular weight (HMW) polyethylene glycol are considered to be the basic phases. Selectivities and polarities between these phases are obtained by selectivity tuning. Selectivity tuning can be performed in three different ways, namely by synthesizing a tuned stationary phase, by mixing the basic phases, or by coupling capillary columns of different selectivities. In coupling capillary columns the variables are column length, β-value, temperature, and/or pressure.
    Additional Material: 27 Ill.
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  • 141
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    Materialwissenschaft und Werkstofftechnik 16 (1985), S. 55-60 
    ISSN: 0933-5137
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics
    Description / Table of Contents: Preparation of Wear Resistant WC-Co Coatings by Hypersonic Flame SprayingThe basic principle of hypersonic flame spraying is shortly described. With this process WC-Co coatings are produced, using two powders of the same chemical composition and same range of grain size, but different in their morphology. The investigation of the coatings leads to the result that sound coatings of high density, high hardness and high bond strength can be produced within a wide range of process parameters. Significant differences in the microstructure of such coatings can be achieved through the difference in powder morphology rather than through a variation of process parameters.
    Notes: Das Hypersonic Flammspritzen, ein neuartiges Verfahren zur thermischen Beschichtung von Oberflächen, wird kurz beschrieben. Es werden Spritzversuche mit zwei WC-Co Pulvern durchgeführt, die die gleiche chemische Zusammensetzung und Korngrößenverteilung, aber eine unterschiedliche Morphologie aufweisen. Die Untersuchung der Schichten zeigt, daß sich bei beiden Pulvern in einem relativ breiten Bereich von Spritzparametern Schichten mit hoher Dichte, hoher Härte und hoher Haftfestigkeit herstellen lassen. Deutliche Unterschiede hinsichtlich der Mikrostruktur dieser Schichten lassen sich weniger über eine Variation der Spritzparameter als über die Morphologie der verwendeten Pulver erzielen.
    Additional Material: 7 Ill.
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  • 142
    ISSN: 0933-5137
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics
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  • 143
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    Materialwissenschaft und Werkstofftechnik 16 (1985), S. 74-74 
    ISSN: 0933-5137
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics
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  • 144
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    Materialwissenschaft und Werkstofftechnik 16 (1985), S. A22 
    ISSN: 0933-5137
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics
    Additional Material: 2 Ill.
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  • 145
    ISSN: 0933-5137
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics
    Description / Table of Contents: Fracture Mechanics Characterization of Fatigue in SiSiCThe behaviour of microscopic “natural” cracks and of artificial sharp cracks was investigated on a fracture mechanics base for extruded and slip casted SiSiC. The resulting strength and crack propagation data were used to calculate relations between loading time and probability of fracture and thus provide a base for the practical application of the investigated materials in structures. Examples of calculated life times and probabilities of failure as well as results of experiments performed to check the calculations are discussed.
    Notes: An SiSiC-Keramik wurde sowohl das Verhalten künstlich eingebrachter, makroskopischer Risse als auch das Verhalten der auf die Herstellung und die Bearbeitung zurückzuführenden, „natürlichen“, mikroskopischen Rissen auf bruchmechanischer Grundlage untersucht. Die vorliegenden Ergebnisse zum Festigkeits- und Bruchverhalten und die daraus rechnerisch abgeleiteten und z. T. experimentell überprüften Zusammenhänge zwischen Belastungsdauer und Versagenswahrscheinlichkeit bilden praktisch anwendbare Grundlagen für den Einsatz der untersuchten keramischen Werkstoffe.
    Additional Material: 8 Ill.
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  • 146
    ISSN: 0933-5137
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics
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  • 147
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    Materialwissenschaft und Werkstofftechnik 16 (1985), S. A34 
    ISSN: 0933-5137
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics
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  • 148
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    Materialwissenschaft und Werkstofftechnik 16 (1985), S. 113-115 
    ISSN: 0933-5137
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics
    Description / Table of Contents: The Meaning of the Safety Factor for the Design with CeramicsFor glass and ceramics a safety factor analogous to that for ductile materials is being discussed. Defining this safety factor the subcritical crack growth was neglected. Therefore the discussed safety factor cannot be used without restrictions. The factor can be used for all glasses and ceramics when a short-time load is applied, and for a few important engineering ceramics even when a long-time load is applied.
    Notes: Es wird in Analogie zum Sicherheitsbeiwert für metallische Werkstoffe ein Sicherheitsbeiwert für Glas und Keramik diskutiert. Bei der Ableitung dieses Faktors wurde das unterkritische Rißwachstum nicht berücksichtigt.Hieraus resultieren Beschränkungen. Der Sicherheitsfaktor ist bei Glas und Keramik universell anwendbar für kurzzeitige Belastung, für Langzeitbelastung nur bei einigen wichtigen Ingenieurkeramiken.
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  • 149
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    Materialwissenschaft und Werkstofftechnik 16 (1985), S. A44 
    ISSN: 0933-5137
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics
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  • 150
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    Materialwissenschaft und Werkstofftechnik 16 (1985), S. 194-203 
    ISSN: 0933-5137
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics
    Notes: Passivity of tin has been investigated in phosphate buffer (pH 6.7) using potentiodynamic and cyclic voltammetric techniques. The formation of thin transparent electronically conducting passive film on which O2 is evolved in the transpassive range is indicated. The solution remains clear. Potentiodynamic measurements performed from -1.2 to 2.5 V (SCE) and backward at scan rates between 1 and 100 mV/sec give one anodic peak. In the reverse scanning, two cathodic peaks appear at low scan rates and disappear completely at higher rates. Values of the open dircuit potential, the corrosion potentials Ecor (forward and reverse), the anodic peak potential Ep and the anodic peak cd Ip are recorded. The results are compared with our previous work in neutral chloride, bromide, iodide, and sulphate solutions. Thermodynamic data are used to predict the possible oxidized species constituting the anode film.Cyclic voltammetric measurements have been carried out in the potential range between H2 and O2 evolution, and in limited potential ranges at scan rates between 1 and 200 mV/sec. One anodic peak is detected in all cases. While a short arrest and a cathodic peak appear in the results between H2 and O2 evolution, two distinct cathodic peaks appear up to 100 mV/sec in the results taken between -1.2 and -0.224 V. Plots of Ip vs the square root of scan rate are linear, and indicate diffusion-controlled kinetics for the reactions initiating passivity. Linear relations are observed for Ep vs log scan rate indicating the irreversible nature of the anodic processes. While the formation of SnO and SnO2 is predicted from thermodynamics at potentials more negative than Ep, the formation of Sn(OH)4 is predicted at potentials more positive than Ep. The conclusions drawn from the results obtained with the two different techniques are generally the same. The results are compared with and discussed on the light of previous work using cyclic voltammetry.
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  • 151
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    Materialwissenschaft und Werkstofftechnik 16 (1985), S. 204-209 
    ISSN: 0933-5137
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics
    Description / Table of Contents: Relaxation Behaviour of the Austenitic Stainless Steel X6 CrNi 18 11 (DIN 1.4948) in the Temperature Range 450 °C to 650 °CBased upon a set of actual data from relaxation tests after tensile loading in the temperature range 450-650 °C and with test times up to 100 h, an average stress vs. time relation for relaxation behaviour is derived. The actual dataset at the temperature of 550 °C is compared with the average relation.Relaxation behaviour is numerically computed from creep data of X6 CrNi 18 11 using different hardening theories and compared with the average relation derived from actual data.
    Notes: Anhand eines umfangreichen Meßdatenfeldes von Relaxationsversuchen nach einsinniger Belastung, das den Temperaturbereich 450-650 °C und Versuchszeiten bis 1000 h abdeckt, wird für den Werkstoff X6 CrNi 1811 eine mittlere Spannungs-Zeit-Beziehung für das Relaxationsverhalten abgeleitet. Für die ausgewählte Temperatur von 550 °C werden die Meßdaten einer repräsentativen Halbzeuglieferung und die abgeleiteten mittleren Beziehungen vergleichend gegenübergestellt.Aus der schon veröffentlichten Charakterisierung des mittleren Kriechverhaltens des Werkstoffs X6 CrNi 18 11 wird unter Verwendung gängiger Verfestigungstheorien numerisch das Relaxationsverhalten berechnet und mit der aus den Daten abgeleiteten mittleren Beziehung verglichen.
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  • 152
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    Materialwissenschaft und Werkstofftechnik 16 (1985), S. 215-222 
    ISSN: 0933-5137
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics
    Description / Table of Contents: Surface Treatment of Carbon Fibres and Resulting Composite PropertiesIn composites carbon fibres are used as reinforcing fibres with thermosetting and thermoplastic resins as martices. These carbon fibres differ strong in their micro-structure and therefrom in fibre properties. To achieve sufficiant composite properties special carbon fibre surface treatment methods are necessary. This paper describes a systematic study on oxidative surface treatment of carbon fibres by wet-, dry- and anodic oxidation. Further investigations by matrix variation show us the influence of matrix strength on the mechanical composite properties. Finally it is shown that in case of impact load composite fracture behaviour is controlled only by the fibre itself.
    Notes: In neuester Zeit finden Kohlenstoffasern zunehmend Verwendung als Verstärkungsfasern in Verbundkörpern mit thermoduren und thermoplastischen Matrixsystemen. Aufgrund des strukturellen Feinaufbaus unterscheiden sich deren mechanischen Eigenschaften. Um die Fasereigenschaften jedoch im Verbund gezielt ausnutzen zu können, müssen spezielle Methoden der Oberflächenaktivierung angewandt werden. Im vorliegenden Fall werden naßchemische, thermische und elektrochemische Oxidation von Kohlenstoffasern vorgestellt, die Auswirkungen auf Faser- und Verbundeigenschaften untersucht und vergleichend diskutiert. Weiterführende Studien durch Matrixvariation verdeutlichen deren Bedeutung bei der Verbundkörperherstellung. Endlich wird gezeigt, daß bei schneller Lastaufgabe die Eigenschaft der Verstärkungsfaser völlig die Verbundeigenschaft kontrolliert.
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  • 153
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    Particle and Particle Systems Characterization 2 (1985), S. 31-37 
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
    Notes: Practical procedures are described for a stereological method which determines the spatial distribution of particle orientation from the distribution observed on cross sections. First, the two dimensional distribution of needle-like particles is determined by counting the number of intersections with parallel probe lines. Next, the three dimensional distribution of needle-like particles is determined by counting the number of intersections with a cutting plane. Then, the three dimensional distribution of disklike particles is determined by counting the number of intersections with a probe line. Finally, the distribution of disklike particles is determined by measuring the total length of the cross sections on a cutting plane.
    Additional Material: 11 Ill.
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  • 154
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    Particle and Particle Systems Characterization 2 (1985), S. 62-66 
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
    Notes: The need for particle shape characterization has been internationally recognised and has resulted in a number of publications proposing a variety of methods for particle shape analysis and shape description. Though very important in chemical engineering, correlations between shape parameters and bulk properties are still rare.This paper describes theoretical and experimental investigations of dynamic shape factors for use when calculating the settling velocity of a particle. For this purpose a study of the settling velocities of particles of various shapes has been made. A correlation is developed from the data with which to quantify the effect of shape on settling velocity for particles falling freely in a fluid in the laminar flow range.
    Additional Material: 8 Ill.
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  • 155
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    Particle and Particle Systems Characterization 2 (1985), S. 39-48 
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
    Notes: Product quality is influenced by the properties of feedstocks and by production parameters. In contrast to gases and liquids, the quality of solids is also affected by the particle properties, such as size, specific surface area, structure and shape. These are the properties which are primarily changed in solids process engineering.The accuracy and cost of possible methods for the measurement of the particle properties of feedstocks, intermediates and end products are discussed. Examples of the methods discussed are laser diffraction spectrometry, quantitative image analysis and photon correlation spectroscopy.The measuring techniques required for monitoring production processes in solids process engineering are illustrated by simple examples. In the field of process control in particular, there is still room for improvement, since there is a lack of suitable sensors and models. Process monitoring is necessary in order to ensure that product quality meets requirements which are constantly increasing.
    Additional Material: 25 Ill.
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  • 156
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    Particle and Particle Systems Characterization 2 (1985), S. 56-61 
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
    Notes: Fractal dimensions are numbers between the classical whole number dimensions which can be used to describe the ruggedness of a fineparticle boundary. This communication explores the utility of fractal dimensions between 1 and 2 for characterizing the ruggedness of fineparticle profiles. This type of fractal boundary is evaluated by estimating the perimeter of a profile of a fineparticle at various levels of scrutiny and then plotting a graph of the logarithm of the perimeter estimates against the logarithm of a unit representing the scale of scrutiny. Such a graph is known as a Richardson plot. Boundaries describable by fractal dimensions exhibit characteristic datalines on this type of graph.Aluminum shot fineparticles produced by the break up of turbulent jet of molten metal have irregular shapes because of the fluid turbulence in the regions where they solidify, but a smooth texture because of the effect of surface tension forces as the fineparticle solidifies. It is shown in this communication that the dataline on a Richardson plot of the estimated perimeter of an aluminum shot fineparticle consists of two regions. The first portion, at coarse levels of scrutiny, permits the calculation of a fractal dimension descriptor of the ruggedness of the profile. A second dataline at high resolution is parallel to the scrutiny axis indicating that at such levels of inspection the profile is effectively smooth and euclidean. Studies are reported of the changes in the ruggedness of an eroding aluminum shot fineparticle suspended in acid. It is shown that fractals can be used to describe the progress of corrosion and that, as corrosion proceeds, the euclidean portion of the Richardson plot of perimeter estimate recedes and disappears within the levels of scrutiny employed in these experiments.
    Additional Material: 11 Ill.
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  • 157
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    Particle and Particle Systems Characterization 2 (1985), S. 71-76 
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
    Notes: In this paper a reciprocating shear cell, which has been developed to measure dynamic wall friction, is described. The cell has also been used to study the attrition behaviour of sand samples at the bounding wall. This attrition causes a considerable change in the angle of wall friction.
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  • 158
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
    Notes: The rheological behaviour of a fluidised bed of alumina powder was determined using a specially designed form of rotating viscometer. Several different geometries of the inner and outer cylinder were tested. In the machine the two cylinders can be rotated independently, in either direction, which enables both their relative velocity and absolute velocity to be varied. Thus, the torque on the inner cylinder, strain-rate and the absolute velocity have been chosen as the consistency variables. Some examples of the derived consistency surface are given. The characteristics of these surfaces could be explained by assuming different states of structure, to which a certain mobility can be ascribed. It is proposed that any state of structure which can exist in the bed is an intermediate of two extremes the first being the immobile state which is elastic and has a yield value and the second being the dynamic state which behaves like a Newtonian fluid.
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  • 159
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    Journal of High Resolution Chromatography 8 (1985) 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 160
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    Journal of High Resolution Chromatography 8 (1985), S. 34-36 
    ISSN: 0935-6304
    Keywords: Gas chromatography, GC ; Injecting liquid samples ; Septumless sample injection ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 4 Ill.
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  • 161
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    Journal of High Resolution Chromatography 8 (1985), S. 39-41 
    ISSN: 0935-6304
    Keywords: Liquid chromatography, HPLC ; Mass detector ; Carbohydrates ; Heavy petroleum distillates ; Hormonal steroids ; Nonionic surfactants ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 4 Ill.
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  • 162
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    Journal of High Resolution Chromatography 8 (1985), S. 98-100 
    ISSN: 0935-6304
    Keywords: Gas chromatography, GC ; Capillary columns ; On-column injection ; Injector temperature control ; Polychlorinated dibenzo-p-dioxins ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 2 Ill.
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  • 163
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    Journal of High Resolution Chromatography 8 (1985), S. 4-7 
    ISSN: 0935-6304
    Keywords: Gas chromatography/mass spectrometry, GC/MS ; Fused silica capillary columns ; Drilling muds ; Diesel fuel ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A GC/MS technique that provides quantitative and qualitative information on diesel fuel components in drilling muds is described. Several low molecular mass aromatic components of diesel fuel are identified as indicators of diesel fuel. The presence and relative concentration of these indicators is used to identify diesel fuel contamination. This information can be used to approximate the amount of diesel fuel contamination in off-shore drilling discharges.
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  • 164
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    Journal of High Resolution Chromatography 8 (1985), S. 23-27 
    ISSN: 0935-6304
    Keywords: Preparative liquid chromatography, HPLC ; Aminopropyl silica bonded phases ; β-Lactams ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The capabilities of a preparative chromatograph assembled at moderate cost from commercially available components are examined in relation to the purification of β-lactam derivatives. It is shown that high efficiency separations can be achieved rapidly, economically, and on a scale sufficient to provide adequate quantities of material for spectroscopic identification and biological testing. In the synthesis of a large batch of aminopropyl silica for preparative HPLC purification of an impure sample of cephacetrile, three different grades of silica were investigated. The material giving the best performance was prepared on a 100 g scale and baseline separations for 0.5 g loadings of the impure cephacetrile were obtained on a 30 cm × 2.2 cm i.d. column. The pure cephalosporin was recovered in high yield by freeze drying of the eluate.
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  • 165
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    Journal of High Resolution Chromatography 8 (1985), S. 320-320 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 166
    ISSN: 0935-6304
    Keywords: Preparative planar chromatography, PPC ; Sequential centrifugal layer chromatography, SCLC ; Centrifugal layer chromatography, CLC ; Circular development ; Anticircular development ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Sequential centrifugal layer chromatography (SCLC), a new preparative planar separation technique, combines the advantages of preparative centrifugal layer chromatography (CLC) and analytical, horizontal, anticircular, and sequential thin-layer chromatography (TLC). In this on-line preparative method, solvent delivery is locally and temporally variable, which means that the mobile phase can be brought onto the plate at any desired place.The SCLC apparatus operates in two modes: circular, with the help of centrifugal force in an inclined position, and anticircular, by means of capillary action in a horizontal position. These two operation modes can be combined and repeated as often as required, hence the separation space becomes practically unlimited. In this way the capacity and separation performance is significantly increased.In the present paper the apparatus and the method are described and some practical aspects are mentioned.
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  • 167
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 8 (1985), S. 369-369 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 168
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    Journal of High Resolution Chromatography 8 (1985), S. 366-367 
    ISSN: 0935-6304
    Keywords: Thin-layer chromatography, HPTLC ; Quantitative analysis ; Metallic complexes ; Diethyldithiocarbomates ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 2 Ill.
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  • 169
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    Journal of High Resolution Chromatography 8 (1985), S. 385-387 
    ISSN: 0935-6304
    Keywords: Gas chromatography, GC ; Fused silica capillary columns ; Column switching ; Fourier transform infrared spectroscopy ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A dual oven gas chromatograph incorporating a micro, mechanical switching valve has been interfaced to an FTIR spectrometer. With this system, each oven can be operated with independent temperature control. Complete choice of the columns' type and capacity gives flexibility in the separation prior to spectroscopic evaluation. An application which demonstrates some of the advantages of column switching in GC/FTIR is presented. Minor sample components have been successfully analyzed by heart-cutting the appropriate section of the separation from a high to a low capacity column. In this way, the dynamic range of the technique is effectively increased while an efficient chromatographic inlet to the FTIR is maintained.
    Additional Material: 4 Ill.
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  • 170
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    Journal of High Resolution Chromatography 8 (1985), S. 400-403 
    ISSN: 0935-6304
    Keywords: Gas chromatography, GC ; Capillary columns, FSOT ; Steroid profiling ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The accuracy and reproducibility of steroid and steroid conjugate determinations using capillary GC are evaluated. It is possible to analyze many unconjugated steroids, steroid sulfates, and some steroid glucuronides simultaneously, simply by using group fractionation based on successive hydrolysis and solvent extraction steps. However, a reliable determination of corticosteroid glucuronides can only be obtained after previous isolation of the glucuronides as a group, with ion exchange chromatography. In complex chromatograms, the combined use of nitrogen specific detection and flame ionization detection facilitates peak identification.
    Additional Material: 1 Ill.
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  • 171
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    Journal of High Resolution Chromatography 8 (1985), S. 395-400 
    ISSN: 0935-6304
    Keywords: Multidimensional gas chromatography, GC ; Capillary columns ; Electron capture detection ; Flame ionization detection ; Double oven instrument ; Kovats indices ; Halogenated aromatic hydrocarbons ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A multidimensional GC-system containing two capillary columns of different polarities, operated within a double oven instrument, was used for the optimized separation of complex isomeric mixtures of various types of chlorinated aromatic compounds such as PCB, PCDD, or PCDF. Electron capture was applied parallel to flame ionization detection to obtain sensitive signals of the PCB or PCDD and the n-alkane standards required for identification by Kovats indices, respectively. Electron capture detection within a valvelessly operated MDGC system forced changes in the usual instrumental set-up, the live-switching coupling piece being located within the second oven of the double oven instrument. This oven is operated isothermally to ensure optimal and interference-free detection, for stable flow conditions within the coupling piece and for the determination of the isothermal retention indices (Kovats), which are much more suitable for identification by retention than the so-called “linear” indices.
    Additional Material: 6 Ill.
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  • 172
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    Journal of High Resolution Chromatography 8 (1985), S. 411-414 
    ISSN: 0935-6304
    Keywords: Gas chromatography, GC ; Capillary columns ; Automated derivatization ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: In the gas chromatographic analysis of complex biological samples, the most time-consuming and error-prone steps are the pretreatment required for isolation and purification of the compounds of interest and, for most analytes, the derivatization to chemically and thermally stable compounds with high volatility. These wet-chemical steps are usually carried out manually, and for routine analysis of large numbers of samples they are often rate-limiting. A dedicated automated derivatizer has been constructed, the employment of which significantly reduces the time required for manual labor and increases the reproducibility of derivatization and hence the accuracy of analysis.
    Additional Material: 2 Ill.
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  • 173
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    Journal of High Resolution Chromatography 8 (1985), S. 469-474 
    ISSN: 0935-6304
    Keywords: Liquid chromatography, LC ; Packed capillary columns ; On-Line multidimensional chromatography ; Gas chromatography, GC ; Capillary columns ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The introduction of selected fractions from a liquid chromatograph into a gas chromatograph has been described; however, analyses were performed by off-line experiments requiring collection and reinjection of the separate fractions or by on-line procedures where disadvantageously, only a fraction of the separated peak or a well resolved component in a mixture could be introduced into a gas chromatograph. This disadvantage is overcome by the apparatus and method described in this paper, which utilizes a multidimensional chromatography system employing a high efficiency, packed capillary LC column coupled on-line to a capillary gas chromatograph.The liquid chromatograph (so designed) can act as a highly efficient clean-up or chemical class fractionation step prior to introduction into the gas chromatograph, significantly reducing sample preparation times in many applications. Thus minor components in a complex matrix can be determined without prior sample clean-up, an example of which is the determination of polychlorinated biphenyls in a complex hydrocarbon matrix.
    Additional Material: 12 Ill.
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  • 174
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    Journal of High Resolution Chromatography 8 (1985), S. 480-484 
    ISSN: 0935-6304
    Keywords: Gas chromatography, GC ; Supercritical fluid chromatography, SFC ; Packed columns ; Fused silica and glass capillary columns ; Liquid crystal stationary phases ; Polyaromatic hydrocarbons ; Insect sex pheromones ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Novel monomeric and polymeric liquid crystalline compounds were synthesized as stationary phases for gas chromatography (GC) and supercritical fluid chromatography (SFC). Monomeric liquid crystalline compounds were used in packed column gas chromatography for the separation of isomeric aromatic compounds and insect sex pheromones. Liquid crystalline polymers possess long nematic ranges and a uniform coating was easily achieved in glass and fused silica capillaries, which could stand temperatures up to 250°C in GC and pressures of 200 MPa at 160°C in SFC. The columns provide excellent selectivity and resolution for fused ring aromatic compounds such as the isomers anthracene and phenanthrene or triphenylene and chrysene.
    Additional Material: 7 Ill.
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  • 175
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    Journal of High Resolution Chromatography 8 (1985), S. 491-492 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 176
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    Journal of High Resolution Chromatography 8 (1985), S. 497-503 
    ISSN: 0935-6304
    Keywords: Gas chromatography, GC ; Capillary columns ; Film thickness ; Tube diameter ; Phase ratio ; “Efficiency” ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: This paper briefly surveys three important considerations related to the tube diameter and film thickness. These are the interrelationship of these two parameters through the phase ratio, the different meanings of the term “efficiency”, and the influence of film thickness and tube diameter on sample capacity. Comparative examples are given for columns having different diameters and film thicknesses.
    Additional Material: 1 Ill.
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  • 177
    ISSN: 0935-6304
    Keywords: Capillary columns ; Gas chromatography, GC ; Stationary phases ; Liquid crystal ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Mesomorphic biphenylcarboxylate esters were coupled via flexible aliphatic hydrocarbon spacers to a polysiloxane backbone. The influence of spacer length, percent mesomorphic substitution, and crosslinking of the stationary phase on liquid-crystalline transition temperatures and on chromatographic performance was investigated. Unique selectivity and good efficiency over a wide temperature range for gum and cross-linked liquid-crystalline phases were demonstrated by the separation of various isomeric polycyclic aromatic compounds.
    Additional Material: 4 Ill.
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  • 178
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 179
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    Journal of High Resolution Chromatography 8 (1985), S. 391-394 
    ISSN: 0935-6304
    Keywords: Gas chromatography, GC ; Capillary columns ; Crosslinking ; Enantiomeric separation ; Polymeric chiral phases ; Polysiloxane skeleton ; Polyethylene glycol skeleton ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Crosslinking experiments for immobilization of the well-known chiral stationary phases XE 60-L-valine-(S)- and XE 60-L-valine-(R)-α-phenylethylamide within capillary columns have been successfully carried out. Crosslinking was also obtained with mixtures of the chiral compound acrylyl-L-valine-(S)-α-phenylethylamide and the polyethylene glycol Carbowax 20M. Immobilization of 75% to 90% was achieved by crosslinking the polymeric chiral phases, but sometimes up to 100% of these phases remained within the columns after the usual subsequent solvent treatment. The crosslinking of Carbowax 20M with acrylyl-L-valine-(S)-α-phenylethylamide led to a chiral polymer of a polarity different from that of the common siloxane type chiral phases.
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  • 180
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    Journal of High Resolution Chromatography 8 (1985), S. 407-411 
    ISSN: 0935-6304
    Keywords: Electrophoresis ; Electroosmosis ; Borosilicate, fused silica, and teflon capillary columns ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Separation efficiency in capillary zone electrophoresis was examined as a function of capillary length and diameter as well as solute concentration for a borosilicate glass capillary/phosphate buffer system. Electroosmotic flow coefficients in borosilicate, fused silica, and teflon capillaries were measured over the useful operating pH range of 3-8 at constant applied power (0.333 W). Sample introduction by a simple, low-dispersion electromigration method was found to be a reliable procedure for solute quantitation.
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  • 181
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    Journal of High Resolution Chromatography 8 (1985), S. 426-431 
    ISSN: 0935-6304
    Keywords: Gas chromatography, GC ; Capillary columns, fused silica ; Ultra-narrow bore columns ; Increased residence time ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The resolution of the diastereoisomers of norpristane, pristane, and phytane was studied as a function of the column internal diameter and/or the residence time of the compounds in the column. Increasing the residence time in the column by operating the column at a lower temperature program rate enhances the resolution more than reducing the internal diameter of the column. Practical experience with ultra narrow bore columns is also presented.
    Additional Material: 10 Ill.
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  • 182
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    Journal of High Resolution Chromatography 8 (1985), S. 440-443 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; GC/MS ; Capillary column, fused silica ; EI-MS/CI-MS ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: In order to facilitate the gas chromatographic determination of butyric as well as other short chain fatty acids, triglycerides containing these fatty acids were transbutylated and transpentylated to give FABES (fatty acid butyl esters) and FAPES (fatty acid pentyl esters), respectively. This method allows the molecular weight of the compounds to be increased while their polarity is decreased. Short chain esters elute sufficiently separated from the solvent; due to the decreased polarity, elution of long chain fatty acids is only slightly retarded compared to the corresponding methyl esters. Quantitative evaluation over a large series of injections proved the linearity of correction factors in both cases, FABES and FAPES, with a slight deviation for 16:0 and 18:0, respectively. Structural characterization was performed by GC/MS. It was shown that there are characterstic fragmentations for FABES as well as for FAPES. The El-mass spectra give structural information about the alcohol and acid moieties, the ester molecule and the Cl-spectra indicate the molecular weight. The absence of abundant highly characteristic peaks in the spectra of these esters makes the detection of FABES or FAPES in complex mixtures more difficult than the detection of FAMES with their very characteristic ions at m/z 74 and 87.
    Additional Material: 4 Ill.
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  • 183
    ISSN: 0935-6304
    Keywords: Gas chromatography, GC ; Fused silica and glass capillary columns ; Selective complexation ; Isomer separation ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The use of glass and fused silica open tubular columns for selective separation of structural, configurational, and optical isomers (enantiomers) of underivatized aliphatic alcohols and ketones by complexation gas chromatography on optically active metal chelates is described. The method represents a powerful analytical tool for the precise determination of diastereomeric (d.e.) and enantiomeric (e.e.) excesses in asymmetric syntheses and in natural product characterization. The direct screening of the enantiomeric composition and absolute configuration of terpinene-4-ol, the aggregation phermone of Polygraphus poligraphus (L), is described.
    Additional Material: 7 Ill.
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  • 184
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    Journal of High Resolution Chromatography 8 (1985), S. 718-726 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary columns, glass ; Inert, stable stationary phases ; Leaching ; Immobilization by condensation ; OH terminal groups ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Coating intensively leached silica surfaces with OH-terminated phases provides a new way of producing, by simple means, columns with substantially increased inertness and thermostability. In addition, their separation efficiency is found to be typically higher than that of columns with traditional coatings. The underlying basic effect is a condensation process between terminal silanol groups of the phase and residual silanols, of the glass surface, thus producing the mentioned inertness. Moreover, the surface-bonded molecules are immobilized without addition of a radical generator. If required, crosslinking can also be effected using a volatile azo compound. No vinyl groups are required for this additional immobilization process. The paper discusses all processes involved, and gives detailed working directions for the following medium polar phases. OV-1701-OH, OV-31-OH (new, 17% cyanopropyl), OV-61-OH, and OV-17-OH, and the apolar phases PS-347.5 and PS-086. There is no doubt so far that the principle of terminal silanol groups is applicable to all silicone phases, and may replace the traditional endcapped stationary phases in the future.
    Additional Material: 4 Ill.
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  • 185
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    Journal of High Resolution Chromatography 8 (1985), S. 747-754 
    ISSN: 0935-6304
    Keywords: Gas chromatography, high resolution ; Chemometrics ; Principal component analysis ; K-nearest neighbor ; PCB-homolog specific analysis ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A principal components multivariable statistical method based on SIMCA 3B (Soft Independent Method of Class Analogy) algorithms was evaluated and applied to interpretation of homolog-specific analysis of polychlorinated biphenyls by high resolution gas chromatography. High resolution gas chromatograms can be evaluated in high resolution separations of individual PCB isomers and grouped into the homologous series. The chromatograms show distinct differences between PCB compositions with different contents of chlorine atoms in technical mixtures (Aroclors). The objective of utilizing SIMCA 3B was its evaluation for a possible identification, classification, and categorization of Aroclors in environmental samples.
    Additional Material: 6 Ill.
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  • 186
    ISSN: 0935-6304
    Keywords: Open tubular gas chromatography ; Theory ; Vacuum outlet ; BASIC program for calculation of optimum conditions ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The Golay-Giddings and Poiseuille equations are used to derive equations for the calculation of the maximum plate number and minimum time conditions for given columns at fixed, but selectable, outlet pressures. In addition, expressions are presented for the determination of minimum analysis times for separation problems requiring given plate numbers. In this instance, the optimum column length can be calculated as a function of outlet pressure. A Basic computer program, incorporating the equations for the various optima, together with the H-ū curves, is described. Input variables are either column length or desired plate number, column diameter, film thickness, capacity ratio of the solute, column outlet pressure, seperation temperature, and carrier gas. The carrier gas viscosity is automatically calculated in the case of hydrogen, helium, or nitrogen. For these gases, and if the solute is a n-alkane, the diffusivity of the solute in the mobile phase is calculated. In this case, the carbon number of the solute is needed in the computation.For high molecular weight polydimethylsilicone phases (e.g. SE-30), the program can approximate the diffusivity of n-alkanes in the stationary phase at the given temperature as a function of the carbon number. Of course, manually entered values of viscosity and diffusion coefficients can be included in the calculations.
    Additional Material: 4 Tab.
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  • 187
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    Journal of High Resolution Chromatography 8 (1985), S. 698-699 
    ISSN: 0935-6304
    Keywords: Gas chromatography, GC ; Fused silica capillary columns ; Back fat of pigs ; 5α-Androst-16-en-3-one ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 2 Ill.
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  • 188
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    Journal of High Resolution Chromatography 8 (1985), S. 700-700 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 189
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    Journal of High Resolution Chromatography 8 (1985), S. 709-714 
    ISSN: 0935-6304
    Keywords: Deactivation ; Capillary columns ; Silylation ; HPLC-silica ; Surface group concentration ; Pore alterations ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: High-temperature silylation (HTS) used for the deactivation of capillary columns was studied on the silica commonly used in HPLC to gain a better insight into this process. LiChrosorb Si 100 was silylated with disilazanes at different temperatures and the materials obtained were compared in terms of organic and silanol group surface concentration, IR reflection spectra, HPLC behavior, and pore distribution parameters. Applying diphenyltetramethyldisilazane, the volatile reaction products were monitored during the HTS process. With increasing silylation temperature up to 400°C the silanol surface concentration is reduced to a very small level independent of the organic group concentration which exhibits a broad maximum depending upon substituents and temperature. Up to 350°C triorganosiloxy groups prevail as bonded organic groups. It could be proved that HTS is accompanied by pore alterations of the silica matrix. Arguments proposed by different authors in explaining HTS effects are discussed.
    Additional Material: 4 Ill.
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  • 190
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    Journal of High Resolution Chromatography 8 (1985), S. 741-747 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Fused silica capillary columns ; Deactivation ; Cyanopropylhydrosiloxanes ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A method is described for surface deactivation and modification of fused silica capillary columns with a cyanopropyl-containing reagent. The deactivation procedure involved a dehydrocondensation reaction between a bis(cyanopropyl)methylhydropolysiloxane reagent and surface silanol groups at an optimum temperature of only 250°C. Actual critical surface tension measurements were made using the capillary rise method. Excellent deactivation for acidic and basic compounds at the low ng level, and wettability for nonpolar and polar polysiloxane stationary phases were obtained. A procedure was developed to remove acidic impurities that are present in polar stationary phases.
    Additional Material: 5 Ill.
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  • 191
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    Materialwissenschaft und Werkstofftechnik 16 (1985), S. A4 
    ISSN: 0933-5137
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics
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  • 192
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    Materialwissenschaft und Werkstofftechnik 16 (1985), S. A7 
    ISSN: 0933-5137
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics
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  • 193
    ISSN: 0933-5137
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics
    Description / Table of Contents: Temperaturwechselverhalten hochfester ingenieurkeramischer Werkstoffe - Kenndaten, Gefügeeinfluß, VerbesserungTeil I: Kenndaten des Temperaturwechselverhaltens hochfester ingenieurkeramischer Werkstoffe.Aufbauend auf den Kriterien zur Verbesserung des Thermoschockverhaltens werden zwei Gefügeaspekte diskutiert: Der Einfluß des Gefüges auf das Thermoschockverhalten und die Verbesserung des Thermoschockverhaltens auf der Basis mikrostruktureller Überlegungen. In diesem Rahmen weden zunächst einmal Kenndaten des Temperaturwechselverhaltens (für Thermoschockbeanspruchung und für zyklische thermische Langzeitbeanspruchung) verschiedener hochfester ingenieurkeramischer Werkstoffe präsentiert.Anhand der zwei Werkstoffe, dichtes und poröses reaktionsgesintertes Si3N4, wird der Einfluß verschiedener Gefügeparameter auf die mechanischen und thermischen Eigenschaften, die das Thermoschockverhalten bestimmen, diskutiert und de Zusammenhang mit dem Thermoschockverhalten dargestellt. Weiterhin wird gezeigt, wie das Thermoschockverhalten durch Gefügeoptimierung verbessert werden kann. Einige Beispiele für die Verbesserung des Thermoschockverhaltens durch die Entwicklung von Verbundwerkstoffen werden gegeben.Die Arbeit ist in 3 Teile gegliedert: Teil I Kenndaten des Temperaturwechselverhaltens hochfester ingenieurkeramischer Werkstoffe. Teil II: Einfluß des Gefüges auf das Thermoschockverhalten hochfester ingenieurkeramischer Werkstoffe. Teil III: Verbesserung des Temperaturwechselverhaltens hochfester ingenieurkeramischer Werkstoffe.
    Notes: Based on the criteria for the improvement of thermal shock resistance mainly two microstructural aspects of thermal stress resistance are discussed: First, the influence of microstructure on thermal shock resistance to fracture initiation, and second, the improvement of thermal shock resistance on the basis of microstructural considerations. In this connection, data of thermal stress resistance (thermal shock and thermal cycling) of various engineering ceramic materials are presented. Using laboratory grades with well-defined microstructures the interdependence between various microstructural variables and the mechanical and thermal properties, which control the thermal shock resistance, is discussed and the relation to thermal shock resistance is outlined by the example of the two materials, dense and porous reaction-bonded Si3N4. Moreover, the improvement of thermal shock resistance by microstructural optimization is demonstrated. Some examples of the improvement of thermal stress resistance by developing advanced composite materials are given.The paper is divided into three parts: Part I: Data of Thermal Stress Resistance of High-Strength Engineering Ceramics Part II: Influence of Microstructure on Thermal Shock Resistance of High-Strength Engineering Ceramics Part III: Improvement of Thermal Stress Resistance of High-Strength Engineering Ceramics.
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  • 194
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    Materialwissenschaft und Werkstofftechnik 16 (1985), S. A15 
    ISSN: 0933-5137
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics
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  • 195
    ISSN: 0933-5137
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics
    Description / Table of Contents: Temperaturwechselverhalten hochfester ingenieurkeramischer Werkstoffe - Kenndaten, Gefügeeinfluß, Verbesserung Teil II: Einfluß des Gefüges auf das Thermoschockverhalten hochfester ingenieurkeramischer WerkstoffeIm Teil I dieser Arbeit wurden zunächst grundlegende Kriterien zur Verbesserung des Thermoschockverhaltens ingenieurkeramischer Werkstoffe zusammengefaßt. Weiterhin wurden Kenndaten des Thermoschockverhaltens und der zyklischen thermischen Langzeitbeanspruchung aufgeführt. Im Teil II dieser Arbeit wird der Einfluß des Gefüges auf das Thermoschockverhalten diskutiert. Dieser Punkt beinhaltet auch die Diskussion des Einflusses verschiedener Gefügeparameter auf die mechanischen und thermischen Eigenschaften, die im wesentlichen das Thermoschockverhalten bestimmen. Diese Zusammenhänge werden für Al2O3, insbesondere aber am Beispiel des dichten und porösen reaktionsgesinterten Si3N4 aufgezeigt. Zusätzlich werden einige andere Faktoren, die das Thermoschockverhalten beeinflussen, erläutert: Der Einfluß der Temperaturabhängigkeit der Eigenschaften auf die Gefügeabhängigkeit des Thermoschockverhaltens, sowie der Einfluß der Streuung der Ausgangsfestigkeit auf das Festigkeitsverhalten nach dem Thermoschock.
    Notes: In part I of this paper basic criteria for the improvement of thermal shock resistance of engineering ceramics were summarized. Moreover, data were presented about thermal shock resistance to fracture initiation and about thermal cycling behaviour of high-strength engineering ceramics. In this part the influence of microstructure on thermal shock resistance to fracture initiation is discussed. This subject also includes the discussion of the influence of various microstructural variables on the mechanical and thermal properties which mainly control the thermal shock resistance to fracture initiation. These relations are demonstrated with Al2O3, but in particular by the example of dense and porous reactionbonded Si3N4. Furthermore, some other factors affecting thermal shock resistance are outlined: the influence of temperature dependence of properties on the microstructural effects on thermal shock resistance, and the influence of data scatter of the initial strength on the strength behaviour after thermal shock.
    Additional Material: 16 Ill.
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  • 196
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    Weinheim : Wiley-Blackwell
    Materialwissenschaft und Werkstofftechnik 16 (1985), S. 73-73 
    ISSN: 0933-5137
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics
    Type of Medium: Electronic Resource
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  • 197
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    Weinheim : Wiley-Blackwell
    Materialwissenschaft und Werkstofftechnik 16 (1985) 
    ISSN: 0933-5137
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics
    Type of Medium: Electronic Resource
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  • 198
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    Weinheim : Wiley-Blackwell
    Materialwissenschaft und Werkstofftechnik 16 (1985), S. A26 
    ISSN: 0933-5137
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics
    Type of Medium: Electronic Resource
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  • 199
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    Weinheim : Wiley-Blackwell
    Materialwissenschaft und Werkstofftechnik 16 (1985), S. 88-94 
    ISSN: 0933-5137
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics
    Description / Table of Contents: Influence of Heat Treatment on the Fatigue Behaviour of 6005A Aluminium AlloyThe influence of industrial heat treatment on the fatigue behaviour of 6005A Aluminium alloy has been investigated.By variation of the cooling rate from solution temperature and holding time at room temperature the size of precipitates improving strength and the width of precipitation free zones at grain boundaries may be altered independently from each other. Increasing the size of precipitates and the width of the precipitation free zones will decrease the tensile properties. In the high cycle fatigue region minor fatigue properties result from a significant broadening of the precipitation free zones, which enhance deformation and crack initiation at the grain boundaries. Coarsening the precipitates has no influence on fatigue behaviour, before crack initiation has taken place, but reduces fatigue crack propagation rate and by this improves the total lifetime.
    Notes: An der aushärtbaren Aluminiumlegierung AlMgSi 0,7 wird der Einfluß betriebsüblicher Wärmebehandlungsbedingungen auf das Ermüdungsverhalten gezeigt.Durch Variation der Abkühlgeschwindigkeit vom Lösungsglühen und der Zwischenlagerungsdauer bei Raumtemperatur lassen sich die Größe der festigkeitssteigernden Ausscheidungen und der ausscheidungsfreien Säume an den Korngrenzen nahezu unabhängig voneinander beeinflussen. Eine Vergrößerung der Ausscheidungen und der ausscheidungsfreien Säume wirkt auf alle Kenngrößen des Zugversuchs negativ. Auf das Dauerschwingverhalten im unteren Zeitfestigkeitsgebiet wirkt sich eine signifikante Verbreiterung der ausscheidungsfreien Säume aufgrund einer erleichterten Verformbarkeit und Rißbildung an den Korngrenzen negativ aus. Eine Vergröberung der Ausscheidungen läßt das Verhalten bis zur Bildung von Ermüdungsanrissen unbeeinflußt, wirkt jedoch in der Rißausbreitungsphase mindernd auf die Ausbreitungsgeschwindigkeit der Ermüdungsrisse und führt deshalb zu einer Erhöhung der Lebensdauer.
    Additional Material: 19 Ill.
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  • 200
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    Weinheim : Wiley-Blackwell
    Materialwissenschaft und Werkstofftechnik 16 (1985), S. 101-112 
    ISSN: 0933-5137
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics
    Description / Table of Contents: Fatigue Strength under Nonsynchronous Multiaxial StressesIn [1] various multiaxial criteria for synchronous stresses as well as for combined and alternating stresses have been reviewed. This paper discusses various criteria for nonsynchronous stresses, e. g. out-of-phase stresses, nonsinusoidal stress time functions and different frequencies between stress components. The criteria aim at the predictions of high cycle fatigue only.Two groups of multiaxial criteria are considered:  - critical plane criteria that means fatigue failure is governed by stresses on certain critical planes and - criteria of integral straining (Anstrengung) that means the stresses in all interference planes of a volume element effect the fatigue behaviour.Only the last groups, i. e. Effective Shear Stress Criteria [8, 32], Shear Stress Intensity Hypothesis (SIH) [10] allow a reliable fatigue evaluation both for constant and changing direction of principal stresses. An extensive comparison between test results (phase difference, different frequencies, complex stress time functions) and prediction, according to the SIH, shows good agreement.
    Notes: Behandelt werden Festigkeitshypothesen für die Dauerschwingfestigkeit duktiler Werkstoffe für den ebenen Spannungszustand, wobei beliebige periodische Beanspruchungs-Zeitabläufe (Phasenverschiebung, unterschiedliche Frequenzen der Komponenten, nichtsinusförmige Abläufe usw.) betrachtet werden. Die „Methoden der kritischen Schnittebene“ sind nur anwendbar bei Beanspruchungsfällen mit konstanter Hauptspannungsrichtung während eines Schwingspiels. Dagegen erfüllen die „Methoden der integralen Anstrengung“ die Invarianzforderungen für eine Festigkeitshypothese bei veränderlichen Hauptspannungsrichtungen: Unabhängigkeit der Vergleichsspannung vom ortsfesten und vom Hauptspannungskoordinatensystem.Experimentell ermittelte und nach der Schubspannungsintensitätshypothese SIH berechnete Dauerfestigkeitswerte zeigen gute Übereinstimmung. Die Treffsicherheit ist somit bei Phasenverschiebung, unterschiedlichen Frequenzen der Komponenten, nichtsinusförmigen Abläufen und komplexen Beanspruchungsfällen ähnlich wie bei synchronen Beanspruchungen, vergl. [1].Nicht behandelt wird der Einfluß der mehrachsigen Beanspruchung bei endlicher Lebensdauer, d. h. auf Betriebsfestigkeit, LCF und Rißfortschritt.
    Additional Material: 12 Ill.
    Type of Medium: Electronic Resource
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