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  • Physics  (1,017)
  • Gas chromatography
  • Wiley-Blackwell  (1,083)
  • 1985-1989  (491)
  • 1980-1984  (592)
  • 1925-1929
  • 1985  (491)
  • 1983  (592)
Collection
Publisher
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  • 1985-1989  (491)
  • 1980-1984  (592)
  • 1925-1929
Year
  • 1
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 6 (1983), S. 36-37 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary column ; Cryogenic focusing ; On-column, pre-column trapping ; Volatile aroma compounds ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 2
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 6 (1983), S. 40-42 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary columns ; Splitless Injection ; Drug analysis ; Concentration dependence of retention values ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 3
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 6 (1983), S. 42-44 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Mg(NO3)2 .6H2O as stationary phase ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 4
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 6 (1983), S. 60-63 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary column ; Cold silanization ; Medium polarity columns ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Silane-coupling agents, commonly used for fiberglass reinforced plastics (FRP), were applied for deactivation of silanol sites in glass capillary columns prior to coating with mediumpolarity phases such as Carbowax and Superox. The columns, prepared in a two-stage process in the case of glass (acidic leaching and drying, dynamic cold silanization followed by static coating with the phase) or a one stage process in the case of fused silica, gave the best results when deactivation and hence wettability were induced by glycidoxypropyltrimethoxy silane.
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  • 5
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Residue analysis ; Fenvalerate ; Fabric protectant ; Woolen cloth ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A method is described for the determination of fenvalerate (cyano(3-phenoxyphenyl)methyl 4-chloro-α-(1-methylethyl)-benzeneacetate) residues on woolen cloth. The fenvalerate was Soxhlet-extracted from the treated fabric with acetone for four hours at a reflux rate of six solvent exchanges per hour. The fenvalerate residue was determined by gas-liquid chromatography with a flame ionization detector. The results were quantitated by comparing integrator counts obtained from extracts of treated samples with those obtained from known standards. The method was sensitive to 0.00054% fenvalerate by weight. Recoveries from fabric treated with 0.00054% to 0.215% averaged 94.8%. The response of the detector was linear over a 400-fold range of fenvalerate concentrations.
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  • 6
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 8 (1985), S. 415-422 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Fused silica capillaries ; High-temperature phases ; Triglyceride analysis ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The analysis of triglycerides on FSOT columns coated with a phenylmethylsilicone gum opens up new perspectives in fat and oil characterization. On phenylmethylsilicone, besides a “carbon number” or CN separation, the triglycerides are also separated according to the different combinations of saturated and unsaturated fatty acids in the triglycerides.
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  • 7
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 6 (1983), S. 273-274 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Solvent effect ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 8
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 6 (1983), S. 269-272 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Retention indices ; Specific retention volumes ; n-Alkanes ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The choice of stationary phase for gas chromatography is dictated by the nature of the analytes. Polarity and selectivity are known to play an important role. This paper suggests equations for calculation of specific retention volumes of any compounds from their retention indices.
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  • 9
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 6 (1983), S. 366-370 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Fused silica capillary column ; Chiral phase ; Amino acid enantiomers ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Heliflex Chirasil-Val, a modified form of the original Chirasil-Val phase coated on fused silica capillary, has been investigated with regard to its resolution efficiency and the separation profile for various enantiomeric derivatives of amino acid. The best results could be obtained with TFA-Et derivatives by reason of the relatively low column temperature required.
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  • 10
    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.
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  • 11
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 6 (1983), S. 386-387 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary columns ; On column injection ; Movable injector ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 12
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 6 (1983), S. 388-389 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Fused silica capillary micro-packed columns ; Separation characteristics ; Application ; Separation of hydrocarbons ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 13
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 6 (1983), S. 392-393 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary columns ; Hydrogen carrier gas ; Pt-Ir tubing ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 14
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 6 (1983), S. 390-391 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Dispersive interactions ; Inductive interactions ; Polycyclic aromatic hydrocarbons ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 15
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 6 (1983), S. 567-568 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Solvent effect ; Headspace analysis ; Trace analysis ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 16
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 6 (1983), S. 4-10 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Ion mobility detector ; Plasma chromatography ; Selective detection ; Quantitative analysis ; Halogenated compounds ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: An ion mobility detector that has been specifically developed for interfacing with capillary gas chromatography is investigated in the negative ion mode. Like the electron capture detector, to which this instrument is closely related, the ion mobility detector shows an enhanced response to low molecular weight halogenated compounds when a small quantity of oxygen is doped into the make-up gas flow. Under O2 doping conditions, the device can operate in a reactant ion monitoring mode responding universally to compounds capable of capturing thermal electrons and in a tunable selective product ion mode providing increased selectivity over that achieved by the ECD. At an oxygen concentration of 0.5%, minimum detectable amounts as low as 600 femtograms have been realized for carbon tetrachloride. Selectivity of chloro- versus bromo- compounds is demonstrated using a mixture of p-dichlorobenzene and p-dibromobenzene.
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  • 17
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    Journal of High Resolution Chromatography 6 (1983), S. 11-15 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary, glass ; ECD ; Halocarbons in water, 0.1-10 ppb ; 0.5-2 μl injected on-column ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Interest in monitoring halogenated organics in drinking water and natural surface and ground water in the low ppb range continues to grow. There is a tendency to include still more volatile halocarbons, the trace determination of which is known to be rather demanding. This prompted us to re-examine the feasibility of large-volume direct aqueous injection onto capillary columns, coupled with ECD. A primary problem was to avoid simultaneous elution of water with halocarbons, since water suppresses the ground current of the ECD. The following measures contributed to the solution of this problem.Apolar, extremely inert, columns are required to elute water completely, and even before very light halocarbons. Their coatings have to be far thicker (≍ 5 mUm) than commonly employed thick films since they must permit isothermal analysis at a column temperature around 100°C in order to ensure rapid and complete elution of water. Finally, it is essential that sampling be carried out on-column for two reasons: diffusion of water vapor in the injector, resulting in delayed elution, is then eliminated, and peak distortion during splitless injection is avoided.Although we now know that persilylated columns with immobilized coatings withstand routine water injections, more longterm experience is needed to provide detailed recommendations for the handling of these columns.
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  • 18
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 6 (1983), S. 34-35 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary, glass ; Samples with varying water content ; Retention times correlated with water content ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 19
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    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
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  • 20
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 6 (1983), S. 213-215 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary column ; HPLC sample work-up ; Valeriana celtica L ; Essential oil ; Nepetalactone, isovaleric acid ; Feline attractant ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 21
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    Journal of High Resolution Chromatography 6 (1983), S. 228-231 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Sample introduction ; Splitless injection ; On-column injection ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 22
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    Journal of High Resolution Chromatography 6 (1983), S. 232-235 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Inlets ; Solvent effect ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 23
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary, glass ; Dynamic versus static leaching ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: It is well known that removal of metal ions from the glass surface greatly improves both the thermal stability and the adsorption characteristics of glass capillary columns. Usually metal ions are removed from a glass surface by acid leaching; in particular, the static leaching procedure with hydrochloric acid is used very often for the preparation of glass capillary columns. This paper discusses the results of an investigation into dynamic leaching. Special attention is paid to those factors which affect the adsorption properties of the leached surface. The importance of the non-specific adsorptivity of the capillary surface due to changes of surface properties induced by the leaching process is pointed out.
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  • 24
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    Journal of High Resolution Chromatography 6 (1983), S. 241-246 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Fused silica capillary columns ; Cobalt-60 gamma radiation ; Immobilized phase ; Crosslinking ; Column activity ; Temperature Stability ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Fused silica capillaries deactivated with D4 and coated with OV-1 were subjected to cobalt-60 gamma radiation in order to elucidate the effect of incident radiation on column performance. The chromatographic performance of these open tubular columns in which OV-1 was polymerized in situ was found to be dependent on the dosage of radiation and was evaluated before and after the irradiated columns were rinsed with solvent. Of the radiation dosages employed, 3 MRad produced superior chromatographic performance coupled with very favorable residual surface activity.
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  • 25
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    Journal of High Resolution Chromatography 6 (1983), S. 247-254 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary, fused silica ; Screening for basic drugs with retention indices differing by only four units ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Capillary columns offer the toxicologist several advantages over packed columns. We have presented a highly reproducible screening procedure based on the retention index system and have shown the use of capillary columns for routine quantitation. We are currently expanding the use of these columns in our laboratory and predict that they will be in routine use by most toxicologists in the near future.
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  • 26
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    Journal of High Resolution Chromatography 6 (1983), S. 255-263 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary, glass, fused silica ; Two-dimensional technique ; Residue analysis in food ; Organophosphorus pesticides ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Two-dimensional gas chromatography with two capillary columns of different polarity (SP 2100 and OV 225) is used for pesticide residue analysis in food samples. By means of “live chromatography” applying pneumatic switching technique according to Deans, unequivocal identification of 57 organophosphorus pesticides in food samples is achieved at trace concentrations. The instrument is equipped with only one injection port and one flame photometric detector. On-line data processing is very helpful, especially in calibration and checking the system's reliability with the multitude of test compounds. The complete pesticide residue analysis including clean-up of about six food samples can be completed by one person in 8 hours.
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  • 27
    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.
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  • 28
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    Journal of High Resolution Chromatography 8 (1985), S. 804-806 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary column ; Stationary-phase focusing ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 29
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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.
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  • 30
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    Journal of High Resolution Chromatography 6 (1983), S. 422-426 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary, glass ; Stationary phase, polar ; DEGA ; Residue analysis of pesticides ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Polydiethylene glycol adipate (DEGA) has been successfully used as stationary phase for residue analysis by glass capillary gas chromatography. A specially stabilized version of the phase yields a good polar column which is stable up to 250°C when used in temperature programmed cycles. The paper lists 90 pesticides that have been successfully chromatographed in ng quantities on a DEGA column.
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  • 31
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    Journal of High Resolution Chromatography 6 (1983), S. 436-440 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary, fused silica ; Superox-4 pretreatment, deactivation ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 32
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    Journal of High Resolution Chromatography 6 (1983), S. 442-443 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Cyclodextrin polymer beads ; Double retention mechanism ; Interaction energy ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 33
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    Journal of High Resolution Chromatography 6 (1983), S. 444-445 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Open-tubular columns ; Reduced diameter ; High pressure ; Coating reservoir ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 34
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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.
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    Journal of High Resolution Chromatography 6 (1983), S. 497-500 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary column, fused silica ; On-column injection ; Solvent polarity ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 36
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    Journal of High Resolution Chromatography 6 (1983), S. 501-504 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary columns ; Van Deemter curves ; Thick film columns ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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    Journal of High Resolution Chromatography 6 (1983), S. 504-507 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary columns ; Effluent splitting ; Polyimide ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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    Journal of High Resolution Chromatography 6 (1983), S. 101-103 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary, fused silica ; GC/MS ; Drugs of abuse ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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    Journal of High Resolution Chromatography 6 (1983), S. 317-319 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary column, fused silica ; Drug screening ; Fused silica capillary column ; Toxicology ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 40
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    Journal of High Resolution Chromatography 6 (1983), S. 319-321 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Supercritical fluid chromatography ; Small diameter capillary columns ; Static coating at elevated temperature ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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    Journal of High Resolution Chromatography 6 (1983), S. 328-332 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Fused silica (capillary) columns ; Bonded (cross-linked ) phases ; Hydrocarbon analysis ; Retention index data ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 42
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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.
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    Journal of High Resolution Chromatography 8 (1985), S. 856-857 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary columns ; Static coating ; Vacuum sources ; Coating solvent ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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    Journal of High Resolution Chromatography 6 (1983), S. 448-450 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary column ; Solute focussing ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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    Journal of High Resolution Chromatography 6 (1983), S. 480-487 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary column ; Residue mixtures ; Inlet characteristics ; Injection procedure ; Repeatability ; Linearity ; Quantification ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Residue mixtures of pesticides in foods which were difficult to separate by packed-column gas chromatography were determined by capillary gas chromatography and electron capture detection. Manual injections of sample and reference standard were made with a 10 μL syringe on a septum-enclosed, split/ splitless inlet system. Optimal peak height repeatability (± 3%( was achieved with three-μL injections which were made within time periods of four hours or less. The average linearity coefficient (slope( obtained for detector response as a function of solution concentration was 1.1.
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    Journal of High Resolution Chromatography 6 (1983), S. 507-509 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary column, glass ; GC/MS ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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    Journal of High Resolution Chromatography 6 (1983), S. 623-624 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary columns ; On-column injection ; Chemistry ; Analytical Chemistry and Spectroscopy
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    Topics: Chemistry and Pharmacology
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    Journal of High Resolution Chromatography 6 (1983), S. 621-622 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Multiplex GC ; Vacancy chromatograms ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 49
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    Journal of High Resolution Chromatography 6 (1983), S. 680-682 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Fused silica capillary column ; Split injector ; Herbicides ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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    Journal of High Resolution Chromatography 8 (1985), S. 715-717 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary column, fused silica ; Immobilization ; Polymethylsiloxane stationary phase ; Priority pollutants ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A new phenyl-cyanopropyl polymethylsiloxane stationary phase, DB-1301, which can be crosslinked and bonded to the fused silica surface, has been synthesized. The phase composition was optimized for the separation of 18 volatile priority pollutants, selected from the so-called “purgables” list because of problems associated with their resolution. The composition of the stationary phase was based on theoretical considerations of binary phase mixtures and window diagram prediction. Columns coated with this stationary phase are compatible with atom selective detectors, such as the electron capture detector. A mixture of 18 volatile priority pollutants and a mixture of chlorinated pesticides were used as test probes on a prototype 30 m × 0.32 mm fused silica column, containing a 1.0 μm film of DB-1301.
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    Journal of High Resolution Chromatography 8 (1985), S. 801-802 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary columns ; Sample introduction ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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    Journal of High Resolution Chromatography 6 (1983), S. 595-604 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; GC/MS ; Pyrolysis GC ; Pyrolysis MS ; Headspace sampling ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Pyrolysis gas chromatography (P/GC) has been successful in differentiating coal tar pitches which are used in the manufacture of high temperature graphite materials [1,2]. In the present study, coal tar and petroleum pitches received from five suppliers were readily differentiated using three distinct methods of polymer analysis: dynamic headspace and pyrolysis gas chromatography mass spectrometry (DH/GC/MS and P/GC/MS, [3]), and pyrolysis mass spectrometry (P/MS, [4,5]). All of these methods are appropriate for the analysis and pattern recognition study of coal and petroleum products; however, methods which incorporate GC usually necessitate long analysis times and are subject to problems associated with gas chromatographic reproducibility (e.g. active sites [6], and nonconstant retention times). As a fingerprint analysis method, P/MS is rapid and ideally suited to computerized pattern recognition study of pitches due to the simple format of P/MS data (computer tabulation of normalized intensities versus masses); whereas, in the present study, the normalized peak area versus retention time date from DH/GC/MS and P/GC/MS analyses were not suitable for direct input to a computerized pattern recognition analysis program, (due to non-constant retention times and improper data format). One limitation is that P/MS does not provide positive identification of thermally evolved products (as can DH/GC/MS and P/GC/MS) due to the complexity of the spectra of a mixture of compounds produced by P/MS. Within the limits of the commercial instrumentation and computer programs used in this study, a combination of all three techniques provided the greatest capability for the differentiation of the five coal tar and petroleum based pitches studied.
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    Journal of High Resolution Chromatography 6 (1983), S. 661-665 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Injector systems ; On-column injection ; Liquid chromatography, HPLC ; Dibenzothiophene oxide and dioxide ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Analytical methods are described for identification and monitoring of the oxygenated metabolites of dibenzothiophene. Since such compounds are thermolabile, GC analysis is seen to be hardly feasible with conventional injectors such as all-glass moving needle or splitless injectors. Only on-column injection gives no degradation products. In addition, reversed-phase HPLC is particularly suitable for the analysis of the sulfone or sulfoxides of dibenzothiophenes.
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    Journal of High Resolution Chromatography 6 (1983), S. 684-685 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Post column trap ; Alumina ; Halocarbons ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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    Journal of High Resolution Chromatography 6 (1983), S. 690-693 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary columns ; Selective on-column injection ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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    Journal of High Resolution Chromatography 6 (1983), S. 133-139 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary, glass ; Advantages of very thick coatings ; Separation efficiency correlated with film thickness ; Preparation of columns with very thick coatings ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: It has become common practice with capillary columns to call film thicknesses of 0.1 - 0.3 μm regular or standard, whereas 0.3 - 1.0 μm is considered to denote thick films. Consequently, films with thickness beyond 1μm (we have explored the range up to 8.0 μm) may be termed very thick. Increasing film thickness, at least to about 5 μm, brings important additionl advantages primarily in terms of loading capacity. Columns with very thick coatings may replace the traditional SCOT columns thanks to at least equivalent loading capacity combined with higher separation efficiency, and better stability characteristics. Additional advantages are increased retention, essential for the analysis of very volatile substances, and increased elution temperature, providing a basis for direct water injection.We observe that TZ (the separation number) drops to roughly 50% when the film thickness is increased by a factor of 300 from 0.025 to 8.0 μm, provided TZ is measured with a standard flow of hydrogen. The reduction is only 30% when the thick-film colums are run with individual optimization with nitrogen as a carrier gas. In contrast to standard columns, very thickly coated columns show slightly increased separation efficiency with nitrogen at drastically reduced flow rate. The HETP increases very slightly in the indicated range of flim thickness. This contradicts widespread theoretical expectations, which probably account for the fact that very thick coatings have so far been neglected. Since the preparation of very thick coatings involves some deviations from the standard procedure, complete and detailed instructions are given.
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    Journal of High Resolution Chromatography 6 (1983), S. 153-155 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary, glass ; Immobilization of moderately polar phases ; Combination of surface bonding and crosslinking ; Vinyl groups in the support surface ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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    Journal of High Resolution Chromatography 6 (1983), S. 185-188 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Injection ; Inlets ; Volume overloading ; Concentration overloading ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 59
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary column ; Automated analysis ; Solvent vapor ; Gas sampling ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Solvent vapors in air may be measured with capillary gas chromatographic columns. By using large diameter columns and sample loops of approximately the same internal diameter, the column may be connected directly to the gas sampling valve. This approach eliminates the use of a splitter or cryogenic trapping and allows low levels to be measured. By operating the column at high velocity, column efficiency is sacrificed for increase in speed.
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    Journal of High Resolution Chromatography 6 (1983), S. 279-281 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary column, glass ; Packed column ; Retention data ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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    Journal of High Resolution Chromatography 6 (1983), S. 281-282 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Si-OR, bonded stationary phase ; Change of physical state ; Retention mechanism ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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    Journal of High Resolution Chromatography 6 (1983), S. 292-299 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Fused silica capillary columns ; GC/MS/DS ; Cryotrapping of organics ; Cryofocusing of organics ; Trace organic analysis ; Priority pollutants ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A 30 m, 0.25 mm ID, fused silica capillary column at temperatures from -60 to -100°C has been shown to be a quantitative trap for organic compounds with volatilities ranging from that of 1, 1 -dichloroethene that of chlorobenzene. This type of “whole column cryotrapping” provided sharp peaks (peak width approximately 4-7 seconds) for all compounds at a trapping temperature of -80°C and with high carrier gas pressures and linear velocities (30 psi and 110 cm/s, respectively). Whole column cryotrapping possesses great simplicity, chromatographic efficiency (no trapping loop connections), and a built-in indicator of quality assurance for trapping efficiency (i.e., peak shape). These advantages are extremely attractive and are indicative of the fact that the potential of this approach has not yet been fully appreciated.
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    Journal of High Resolution Chromatography 8 (1985), S. 580-584 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary columns, in series ; Flow rate changes ; Selectivity ; Retention time ; Residence time ; Multichromatography ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: We describe the polarity of selectivity of a GC separation system in terms of Retention Index data. In a series-coupled capillary system having stationary phases of differing polarity even slight (independent!) carrier gas flow changes in one part of the capillary series result in a dramatic change of selectivity. “Dramatic” is a relative term! Using a simple electronically controlled flow changing device we found retention index changes of several hundred units for polar test compounds such as phenols on a SE30/Carbowax tandem. This means: The classical theoretical model for understanding retention (and selectivity) in chromatography must be corrected. We propose a very simple approach involving addition of the expression RESIDENCE TIME to the chromatographic vocabulary. Instead of using flow resistors, one can just add a pressure regulator to the coupling point. A powerful analytical concept is now in easy reach.
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    Journal of High Resolution Chromatography 6 (1983), S. 510-511 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Optically active compounds ; Determination of trace amounts ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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    Journal of High Resolution Chromatography 6 (1983), S. 561-563 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Fused silica capillary ; On-column injection ; Rotary valve ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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    Journal of High Resolution Chromatography 6 (1983), S. 564-565 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary, fused silica ; Splitless injection ; Trace analysis ; EPA phenols ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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    Journal of Polymer Science: Polymer Chemistry Edition 21 (1983), S. 1-15 
    ISSN: 0360-6376
    Keywords: Physics ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The thermal decomposition of this resin was examined by quantitative pyrolysis - gas chromatography. The decomposition does not follow the Hurd-Blunck mechanism generally obeyed by beta-hydrogen containing esters. Instead, phthalic anhydride is extruded almost quantitatively. It is proposed that the mechanism involves the rearrangement of the phthalate C—O bonds to extrude the anhydride, leaving a maleic acid - dipropylene glycol polyester chain.
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    Journal of Polymer Science: Polymer Chemistry Edition 21 (1983), S. 31-39 
    ISSN: 0360-6376
    Keywords: Physics ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: N-grafted poly(p-phenylene terephthalamide)s (PPTA) were synthesized from PPTA and acrylonitrile or propylene oxide via metalation in a solution of the polymer in a sodium methylsulfinylcarbanion-dimethyl sulfoxide solvent at low temperatures. The introduction of these branches into the amide groups of PPTA increased solubility but decreased thermal stability. The effects of the branches on thermal properties and solubility are discussed. The structure of the graft copolymers is described on the basis of wide-angle x-ray diffraction, infrared spectra, and solubility.
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    Journal of Polymer Science: Polymer Chemistry Edition 21 (1983), S. 73-81 
    ISSN: 0360-6376
    Keywords: Physics ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Polymerization of acrylonitrile initiated by a potassium superoxide (KO2)-nitrobenzene system was carried out in anhydrous dimethylsulfoxide (DMSO) at 25°C. The initial rate of polymerization was rapid and a high-molecular-weight polymer was obtained. The molecular weight was proportional to monomer concentration and inversely to concentration of initiator within 5 min. The overall activation energy was estimated as -2.6kcal/mol deg in the temperature range of 20-50°C. In addition to nitrobenzene anion radical, other anion radicals generated by one-electron transfer from KO2 to charge transfer agents such as m-dinitrobenzene benzoquinone, benzophenone, and naphthalene were effective in the polymerization of acrylonitrile. It is proposed that polymerization proceeds via an anionic mechanism that involves one-electron transfer from anion radicals to monomer.
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    Journal of Polymer Science: Polymer Chemistry Edition 21 (1983), S. 97-109 
    ISSN: 0360-6376
    Keywords: Physics ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Diaryliodonium salts (I) undergo efficient thermal decomposition in the presence of copper (II) compounds. Such systems can be employed as a novel class of latent thermal initiators for cationic polymerization. An investigation of the mechanism of the reaction demonstrated that the copper (II) compound is first reduced to the corresponding copper (I) compound, which subsequently reduces the diaryliodonium salt. The cationic polymerization of some typical monomers using these new initiators was carried out to demonstrate the scope of their utility.
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    Journal of Polymer Science: Polymer Chemistry Edition 21 (1983), S. 147-154 
    ISSN: 0360-6376
    Keywords: Physics ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: It has been found that when hydrophobic monomers are polymerized in the presence of highly hydrophilic polymer seed particles, the second-stage hydrophobic polymers form cores surrounded by the first-stage hydrophilic polymers, resulting in “inverted” core-shell latexes. The formation of core-shell morphology by this inversion process has been found to be dependent on the hydrophilicity and molecular weight of the first-stage hydrophilic polymers and the extent of phase separation between the two polymers involved. Particle morphology has been examined by electron microscopy, surface acid titration, alkali swelling of particles, and surface reactivity.
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    Journal of Polymer Science: Polymer Chemistry Edition 21 (1983), S. 155-163 
    ISSN: 0360-6376
    Keywords: Physics ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The structure of polymeric microemulsions, viz. toluene/water/PS-PEO graft copolymer/2-propanol, has been studied by 1H-NMR spectroscopy. Results show that at low water contents, the copolymer adopts a rather diffuse micellar structure in which the rotational mobility of the ethylene oxide units is little affected by the ternary solvent mixture. Above a critical water concentration (ca. 4%), a restriction in mobility of the ethylene oxide chains is observed which has been related to the formation of an inverse micellar structure with water solubilized within the particles. The study of the chemical shifts and linewidths of water protons indicates that initially most of the water is hydrogen bonded to the hydrophilic part of the copolymer, then is present in its free form in water aggregates. These results confirm previous data obtained by dialysis equilibrium experiments.
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    Journal of Polymer Science: Polymer Chemistry Edition 21 (1983), S. 751-760 
    ISSN: 0360-6376
    Keywords: Physics ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The concept of piezoelectric and pyroelectric effects in amorphous polymers is presented, with experimental results, details on sample preparation, and activity evaluation. Most evaluations were performed on 25-30 mol% tributyltin methacrylate/methyl methacrylate copolymers, which possessed good piezoelectric activity, antifouling properties, and paint-formulation characteristics. Solvent-induced orientation effects that lead to piezoelectric activity in amorphous, unpoled, polymers are also described.
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    Journal of Polymer Science: Polymer Chemistry Edition 21 (1983), S. 737-750 
    ISSN: 0360-6376
    Keywords: Physics ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The physical state of the material obtained during the various stages of preparation of a typical MgCl2-supported, high-mileage propylene polymerization catalyst was studied by BET, mercury porosimetry, and x-ray diffraction techniques. The starting MgCl2 and the substance after HCl treatment have negligible BET surface areas. Mercury porosimetry showed that they have large pores with radii 〉 200 nm which are probably crevices between MgCl2 crystallites. The most pronounced physical changes occur during dry porcelain ball milling in the presence of ethyl benzoate. After 60 h or more of ball milling the material had a 5.1-7.3 m2 g-1 BET surface area, twice the pore surface area, and a smaller pore radius than before ball milling and a large reduction in crystallite sizes to almost ultimate dimensions. The crystallites were probably held together by complexation with ethyl benzoate in the form of large agglomerates. Subsequent reactions with p-cresol and triethyl aluminum had minor effects in further reduction of the MgCl2 crystallite size but efficiently brokeup the agglomerates. The final refluxing with TiCl4 increased the BET surface area to 110-150 m2 g-1 but may have increased the crystallite size somewhat due to cocrystallization of TiCl3 and AlCl3 with MgCl2. There may have been only 8-10 crystallites in each catalyst particle. The surface structure of the catalyst resembled those of the classical Ziegler-Natta γ-TiCl3·0.33 AlCl3 catalyst.
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  • 75
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    Journal of Polymer Science: Polymer Chemistry Edition 21 (1983), S. 111-120 
    ISSN: 0360-6376
    Keywords: Physics ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The reactions of 4-aminophthalonitrile (APN) with 3,3′,4,4′-benzophenone tetracarboxylic dianhydride (BPTDA), and with 1,2,3,4-benzenetetracarboxylic dianhydride (PMDA) have been studied to optimize the conditions for the synthesis of monomeric thermosetting bisphthalonitrile compound. Suitable procedures for the synthesis of the two monomers are presented. Elemental analyses, IR spectra, dynamic thermogravimetric analyses, differential scanning calorimetry, 1H-NMR, and mass spectral studies have been used to characterize these compounds. Preliminary observations show that these materials can be polymerized to give high-temperature-resistant materials.
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  • 76
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    Journal of Polymer Science: Polymer Chemistry Edition 21 (1983), S. 141-145 
    ISSN: 0360-6376
    Keywords: Physics ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: This article is a report of the investigation of the influence of monomer composition within optimum limits on the light-transmitting properties of MBS terpolymers obtained by the mass-suspension method. The high and nearly constant light-transmitting properties of the MS copolymer matrix have no effect on the light-transmitting properties of MBS with a MMA content up to about 20 mol % higher than that at the azeotropic point. The refractive index of the MS copolymers decreases uniformly as the mole ratio of MMA increases and becomes equal to the index of the SBR. Particle concentration in sizes up to 0.6μm increases as the MMA content increases to a given point at which the concentration remains constant as MMA continues to increase. The light-transmitting properties of MBS with a MMA content of 57 mol % are improved significantly. This fact is explained by a decrease in variation on the refractive index between the two phases to 0.0014 and by the increasing percentage of particles with sizes smaller than 0.6 μm up to 70%.
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  • 77
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    Journal of Polymer Science: Polymer Chemistry Edition 21 (1983), S. 175-181 
    ISSN: 0360-6376
    Keywords: Physics ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: It was found that aromatic aldehydes and ketones could be reduced smoothly at room temperature by sodium dithionite using viologen derivatives as an electron transfer catalyst to obtain the corresponding alcohols in good yields. Viologens (methyl viologen and polymer) acted catalytically and active species in the reduction were quinoid forms which were obtained by two-electron reduction of viologens.
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  • 78
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    Journal of Polymer Science: Polymer Chemistry Edition 21 (1983), S. 953-960 
    ISSN: 0360-6376
    Keywords: Physics ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: For a fundamental study of the electrochemical behavior of electroactive polymers a series of poly(3-vinyl-10-methylphenothiazine) (polyMPT), copolymers of 3-vinyl-10-methylphenothiazine and methyl methacrylate (MMA) (copolyMPT), and 3-ethyl-10-methylphenothiazine (EMPT) (a related monomer model) were prepared. The methylphenothiazine groups in these compounds showed reversible, one-electron oxidation waves in the triangular-were voltammograms. From a detailed comparison of the voltammograms between these polymers and EMPT it was revealed that the electroactive groups in poly MPT were not the “noninteracting” centers in the strict sense, whereas those in copolyMPT, in which the centers are spaced with the MMA segments, were typically noninteracting in nature; that is, in polyMPT the oxidation takes place at the potential 40 m V lower than that of EMPT and copolyMPT exhibited a wave identical to that of EMPT in shape and potential. The exhaustive electron transfer occurred from polyMPT to the electrode. On the other hand, a significant number of centers remained unoxidized in copolyMPT. The self-exchange electron transfer within the polymer coil facilitates the exhaustive oxidation. For this event the proximity of the centers was an essential factor.
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  • 79
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    Journal of Polymer Science: Polymer Chemistry Edition 21 (1983), S. 969-983 
    ISSN: 0360-6376
    Keywords: Physics ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Substantial hole transport can be achieved in organic polymers simply by incorporating aromatic amine groups into the monomer. Hole mobilities similar to or greater than those in poly(N-vinyl-carbazole) (PVK) were measured in a series of high molecular weight arylamine-substituted polymethacrylates. The hole transport in these polymers is electric-field-dependent as in PVK, varying between E and E2 within a range of 4 × 104 - ∼9 × 105 V/cm. The polymers also exhibit carrier generation in ultraviolet (UV) light in the range of absorption. Synthesis of the monomers, their polymerization, and the general properties of these polymers are discussed.
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  • 80
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    Journal of Polymer Science: Polymer Chemistry Edition 21 (1983), S. 1025-1032 
    ISSN: 0360-6376
    Keywords: Physics ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Thermally stable poly(metal phthalocyanine)imide copolymers were prepared with metal(11) 4,4′,4″,4‴ -phthalocyanine tetraamines, 4,4′ -diamino diphenyl ether, and 3,3′,4,4′ -benzophenone tetracarboxylic dianhydride. Variables such as molar concentrations of the reagents, solvents, and temperature were investigated to optimize the conditions of the polymerization. Inherent viscosity, and infrared (IR) spectral and thermogravimetric analysis (TGA) studies were done to characterize the polymers. These polymers are stable and thier decomposition temperatures both in air and nitrogen are greater than 500°C. Their char yields at 800°C in nitrogen varied between 60 and 76%, depending on the type and concentrations of the metal phthalocyanine tetraamines. These polymers can be used to produce heat-stable films, fibers, varnishes, and adhesives.
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  • 81
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    Journal of Polymer Science: Polymer Chemistry Edition 21 (1983), S. 923-936 
    ISSN: 0360-6376
    Keywords: Physics ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The influence of the reaction conditions (time, temperature, concentrations of the monomer, and the initiator) on the amount and composition of the oligomers and high molecular products formed during the heterogeneous anionic polymerization of ∊-caprolactone was investigated. The polymerization was initiated by KC24 in xylene or tetrahydrofuran. Conditions were found under which intra- and intermolecular transesterification was strongly suppressed, thus providing the opportunity for the formation of polyesters with viscometric molecular masses of more than 300,000 and good yields (80% and higher). The total quantity of products with a viscometric molecular mass below 2500 did not exceed 15%; that of the cyclic dimer was not in excess of 5%. Peculiar features of the KC24 initiated polymerization are the insignificant rise in the number of oligomers and the formation of high polymers even in strongly diluted solutions of ∊-caprolactone (0.2 mol/L and lower). The quantity and molecular mass of the polymers obtained decreased as the temperature increased. It was also established that the polymerization of the cyclic dimer of ∊-caprolactone is not initiated by KC24.
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  • 82
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    Journal of Polymer Science: Polymer Chemistry Edition 21 (1983), S. 1151-1157 
    ISSN: 0360-6376
    Keywords: Physics ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Polyaromatic either-sulfone-ketones containing fluoro-substituted p-cyclophane units were prepared from isophthaloyl chloride, terephthaloyl chloride, diphenyl ether, diphenoxydiphenyl sulfone, and a small amount of 1,1,2,2,9,9,10,10-octafluoro-[2,2]-p-cyclophane (type A) or pseudo-p-1,12,2,9,9,10,10-octafluoro-[2,2]-p-cyclophane bis-acid chloride (type B) by Friedel-Crafts-type polymerization. The p-cyclophane units were incorporated as crosslinking sites. Crosslinking was achieved by curing polymers at 300-350°C for several days. The polymers obtained, containing 1-10 wt % fluoro-substituted p-cyclophane units, were moderately soluble in dichloromethane, DMF, and sulfuric acid with inherent viscosities between 0.4 and 0.6. Laminates on glass fiber were made with excellent thermal stability.
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  • 83
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    Journal of Polymer Science: Polymer Chemistry Edition 21 (1983), S. 1289-1303 
    ISSN: 0360-6376
    Keywords: Physics ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The esterification of the carboxyl group in copoly(γ-benzyl-L-glutamyl-L-glutamic acid) was carried out using N-hydroxysuccinimide and dicyclohexylcarbodimide to yield the activated site for the coupling reaction with amino compounds. The α-helix stability of the reactive copolymer thus obtained is remarkably affected in the presence of succinimide ring. This copolymer was proved to react nearly completely with amino alcohols such as 2-aminoethanol, 3-aminopropanol, and diethanolamine. The copoly(N5-hydroxyalkyl-L-glutamine) thus prepared is insoluble in water, since the benzyl ester remains in this copolymer. The copoly(α-amino acids) having another functional group were also prepared using aminoalkylsilane. Crosslinked poly(α-amino acids) were prepared by the reaction of the reactive copolymer with a low-molecular-weight polymer of PBLG having one amino group on each end of its main chain which was obtained from the corresponding NCA using p-diaminobenzene as an initiator. Another crosslinked polymer was prepared using an alkyl diamine such as 1,6-diaminohexane or 1,12-diaminododecane as a crosslinking reagent. The crosslinked copoly(α-amino acids) bearing the activated site are able to further react with various compounds having amino groups.
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  • 84
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    Journal of Polymer Science: Polymer Chemistry Edition 21 (1983), S. 1417-1422 
    ISSN: 0360-6376
    Keywords: Physics ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The reversible isomerization of poly(chloromethylthiirane) and poly(3-chlorothietane) represents a new kind of polymer reaction and a new method of copolymer synthesis. In chloroform, in dichloromethane, or in nitrobenzene the reaction is well described by reversible first-order kinetics. A rate increase of ca. 40% on changing the solvent from chloroform to nitrobenzene is consistent with an isomerization mechanism that involves a rate-determining attack of the backbone sulfur atom on the neighboring carbon-chlorine bond and rapid ring-opening of the thiiranium ion intermediate by chloride ion.
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  • 85
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    Journal of Polymer Science: Polymer Chemistry Edition 21 (1983), S. 609-613 
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    Keywords: Physics ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 86
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    Journal of Polymer Science: Polymer Chemistry Edition 21 (1983), S. 633-634 
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    Keywords: Physics ; Polymer and Materials Science
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  • 87
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    Journal of Polymer Science: Polymer Chemistry Edition 21 (1983), S. 1819-1829 
    ISSN: 0360-6376
    Keywords: Physics ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A detailed magic angle spinning 13C-NMR investigation of the intractable polymer prepared by plasma polymerization of toluene and isotopically labeled toluene led to a proposed model for the structure of the polymer and suggested some of the likely processes that occur in the gas phase leading to film formation. From the 13C spectra four resolved resonances permitted the determination of the contribution of nonprotonated and protonated unsaturated as well as methyl and other aliphatic carbons to the polymer structure. Specific 13C isotopic labeling of the methyl and phenyl C-1 toluene carbons in the injected liquid vapor allowed the destination of these carbons in the deposited polymer to be traced. The dominant structure is derived primarily from two precursors: benzyl radical and toluene itself. The 13C data further requires a net saturation of ca. 30% of the toluene double bonds and a net displacement of hydrogen by carbon on ca. 20% of the toluene ring carbons.
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  • 88
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    Journal of Polymer Science: Polymer Chemistry Edition 21 (1983), S. 803-810 
    ISSN: 0360-6376
    Keywords: Physics ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The free radical polymerization of acrylonitrile (AN) initiated by Cu(II) 4-anilino 2-one [Cu(II) ANIPO] Cu(II), 4-p-toluedeno 3-pentene 2-one [Cu(II) TPO], and Cu(II) 4-p-nitroanilino 3-pentene 2-one [Cu(II) NAPO] was studied in benzene at 50 and 60°C and in carbon tetrachloride (CCl4), dimethyl sulfoxide (DMSO), and methanol (MeOH) at 60°C. Although the polymerization proceeded in a heterogeneous phase, it followed the kinetics of a homogeneous process. The monomer exponents were ≥2 at two different temperatures and in different solvents. The square-root dependence of Rp on initiator concentration and higher monomer exponents accounted for a 1:2 complex formation between the chelate and monomer. The complex formation was shown by ultraviolet (UV) study. The activation energies, kinetics, and chain transfer constants were also evaluated.
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  • 89
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    Topics: Chemistry and Pharmacology
    Notes: N-Methylacrylamide (NMAAm) was polymerized quantitatively by using di-tert-butyl peroxide as photosensitizer to be, for the most part, incorporated in living poly(NMAAm) radical. The living polymer radical reacted effectively with acrylate monomers to yield block copolymer. Longer alkyl chain of the acrylate monomer caused a decrease in the conversion of the second monomer. Methacrylate monomers, such as methyl methacrylate and cyclohexyl methacrylate, showed relatively low reactivities in comparison with acrylates. Styrene exhibited a much lower conversion. The resulting block copolymers showed different thermochromic behaviors in methyl benzoate from that of poly(NMAAm). This is explained on the basis of the difference between refractive indexes of the block copolymers and poly(NMAAm).
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  • 90
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    Journal of Polymer Science: Polymer Chemistry Edition 21 (1983), S. 865-881 
    ISSN: 0360-6376
    Keywords: Physics ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Polyimide films based on either 3, 3′, 4, 4′-benzophenone tetracarboxylic acid dianhydride or pyromellitic dianhydride with 4,4′-oxydianiline have been doped with copper(I) and copper(II) complexes. High-quality, flexible, glass-cast films have been obtained which exhibit increased softening temperatures and lower polymer decomposition temperatures. The atmosphere and glass sides of the films are quite different. The copper(I) dopant is oxidized on the air side of the film, while the glass side contains predominantly copper (I). In the copper(II) case most of the copper appears on the air side as a silvery substance in the Cu(II) state. Chemical as well as ion etching can remove this material. Electrical resistivity of the copper(II)-doped films is decreased by three to five orders of magnitude relative to the polymer alone.
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  • 91
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    Journal of Polymer Science: Polymer Chemistry Edition 21 (1983), S. 883-890 
    ISSN: 0360-6376
    Keywords: Physics ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The synthesis of two phenylated bifunctional monomers, dimethyl 4-(4-(p-aminophenoxy)phenyl)-3,5,6-triphenylphthalate and dimethyl 4-(4-(4-(p-aminophenoxy)phenoxy)phenyl)-3,5,6-triphenylphthlate, was accomplished. Polymerization in solution or by a bulk polymerization procedure yielded a series of low molecular weight phenylated polyimides. The polymers were soluble in chlorinated hydrocarbons and exhibited thermal stabilities comparable to other polyimide systems.
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  • 92
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    Journal of Polymer Science: Polymer Chemistry Edition 21 (1983), S. 937-941 
    ISSN: 0360-6376
    Keywords: Physics ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The structural changes in the potassium graphitide KC24 in its interaction with ∊-caprolactone, γ-butyrolactone and pivalolactone are examined by profilometric measurement and electron scanning microscopy. The interaction of KC24 with a nonpolymerizable lactone-γ-butyrolactone proceeds without delamination of the graphitide. The polymerization of ∊-caprolactone and pivalactone in the interlayer spaces of KC24 leads to destruction of the initiators structure. An increase in the temperature and monomer concentration enhances the delamination of the graphitide.
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  • 93
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    Keywords: Physics ; Polymer and Materials Science
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    Topics: Chemistry and Pharmacology
    Notes: A procedure was developed by which polymer colloids can be prepared by polymerizing aerosol droplets of monomers with an initiator in the vapor state. This work describes the formation of poly(p-tertiarybutylstyrene) particles by exposing the corresponding monomer droplets to trifluoromethanesulfonic acid. It was found that the monomer-to-initiator mass ratio is the critical factor in determining the uniformity and morphology of the particles. Under ideal conditions spheres of narrow size distribution are obtained. Otherwise porous particles or soft particles with whiskers may develop. The aerosol was prepared in a falling film generator, but other procedures for producing monomer droplets may be used.
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  • 94
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    Journal of Polymer Science: Polymer Chemistry Edition 21 (1983), S. 999-1012 
    ISSN: 0360-6376
    Keywords: Physics ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Polycondensation of the diacid chloride of 2-(3-carboxy vinyl)phenyl-1,3-dioxoisoindoline-5-carboxylic acid with m-phenylenediamine and the diacid chloride of 2-(4-carboxy phenyl)-1,3-dioxoisoindoline-5-carboxylic acid with 1,5-bis(3-aminophenyl)1,4-pentadien-3-one was carried out in polar solvents to produce new unsaturated polyamide-imides. The solution and the thermal, electrical, and a few other properties of the polymers were studies. The polymers were soluble in highly polar solvents. The solubility parameter of the polymers was calculated from the Small's group contribution. The polymers were fairly thermostable and underwent crosslinking creaction when heated, preferably in the presence of a suitable catalyst. The crosslinked polymers were in soluble even in highly polar solvents and possessed higher thermal stability. The swelling behavior of the polymers was studied and the molecular weight between two consecutive crosslinks was determined. X-ray diffraction and the dielectric properties of the polymers and their crosslinked products were also studied.
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  • 95
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    Journal of Polymer Science: Polymer Chemistry Edition 21 (1983), S. 1013-1024 
    ISSN: 0360-6376
    Keywords: Physics ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Crosslinked polystyrene particles were prepared by Friedel-Crafts suspension crosslinking of polystyrene using 2,4-dichloromethyl-2,5-dimethyl benzene as crosslinking agent. The polymer was dissolved in nitrobenzene and reaction occurred in a 70 wt % aqueous solution of ZnCl2 with poly(vinyl alcohol) as a suspending agent. The spherical particles produced were swollen in toluene, chloroform, and tetrahydrofuran to determine their equilbrium polystyrene volume fraction. Analysis of the crosslinked macromolecular structure gave values of number-average molecular weight between crosslinks of M̄c = 900-5900 increasing as the nominal crosslinking ratio X decreased from 0.75 to 0.0625 mol of crosslinking agent per mole of polystyrene repeating unit. Porosimetric analysis contributed to the understanding of the importance of the pore structure for swelling behavior.
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  • 96
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    Keywords: Physics ; Polymer and Materials Science
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    Topics: Chemistry and Pharmacology
    Notes: An efficient kinetic method of reactivity ratio measurement for binary copolymerization of gaseous monomers4 that does not require the measurement of copolymer composition and can be applied to the data obtained in a single copolymerization run was modified and applied to olefin copolymerization with heterogeneous Ziegler-Natta catalysts. Estimated r1 and r2 values for pairs like ethylene-propylene and propylene-1-butene agree favorably with published data.
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  • 97
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    Journal of Polymer Science: Polymer Chemistry Edition 21 (1983), S. 1097-1110 
    ISSN: 0360-6376
    Keywords: Physics ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A new redox couple based on the copper-catalyzed reduction of diaryliodonium salts with benzoins has been used to initiate cationic polymerizations of cyclic ethers and esters. A proposed mechanism for initiation by this redox couple is based on its stoichiometry and on the nature of the products. It was concluded that initiation of polymerization occurs both by direct arylation of the monomer and by protonation by strong Brønsted acids. The polymerization of several typical cationically polymerizable monomers using this new redox initiator were studied.
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  • 98
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    Journal of Polymer Science: Polymer Chemistry Edition 21 (1983), S. 1125-1137 
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    Keywords: Physics ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A regenerable dihydronicotinamide immobilized on a macroreticular polystyrene carrier was developed and used in an aqueous medium for the reduction of trifluoroacetophenone to the corresponding alcohol. It was shown that the second-order rate constant for the polymer-bound reagent is significantly lower than that of the low-molecular-weight analog 1-benzyldihydronicotinamide. The observed reaction rate, however, was of the same order of magnitude as that due to enrichment of substrate in the polymeric pores. It was possible to depress the undesired side reactions to 10-15% per reaction cycle, thereby allowing reutilization of the functionalized polymer.
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  • 99
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    Journal of Polymer Science: Polymer Chemistry Edition 21 (1983), S. 2451-2461 
    ISSN: 0360-6376
    Keywords: Physics ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The 337.1-nm emission of a pulsed nitrogen laser was shown to initiate the crosslinking polymerization of epoxy-acrylate photoresists effectively. We evaluated the extent of curing from the amount of insoluble polymer formed and by the decrease in infrared (IR) absorption of the reactive double bond at 810 cm-1. With the large power density available in the laser pulse (0.5 MW cm-2) rates of polymerization as high as 108 mol L-1 s-1 were observed in the presence of air. Quantum yield measurements indicated that each photon absorbed can create as many as 450 crosslinks; the kinetic chain length was calculated as ca. 4000 double bonds polymerized per initiating radical. During the induction period due to oxygen inhibition each photoinitiator radical consumed 1 O2 molecule. The influence of the monomer and photoinitiator used on the sensitivity of the resin was examined; the best performing formulation contained the epoxy-acrylate oligomer, pentaerythritol triacrylate, as monomer and 2,2 dimethoxy-2-phenyl-acetophenone as photoiniatior. All the formulations studied can be cured by a single 500-kW laser pulse of 8 ns duration, provided that the irradiation is carried out in an inert atmosphere or with a focused laser beam.
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  • 100
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    Journal of Polymer Science: Polymer Chemistry Edition 21 (1983), S. 2491-2501 
    ISSN: 0360-6376
    Keywords: Physics ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Values calculated for the activation volume for chain propagation, ΔV
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