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  • 1
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 2 (1979), S. 31-35 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary, glass ; Surface deactivation, silylation ; Inertia stable to 350° ; Free acids and bases, simultaneous injection ; On-column injection ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A deactivation procedure is described based on a published method using hexamethyldisilazane in the gas phase. In addition to unusually high inertia and thermostability, the method produces truly neutral columns which allow simultaneous analysis of moderately strong free acids and bases. The silylated columns show their full potential only with on-column injection. Preliminary experimental directions are given; more elaborate directions will become available after extended optimization work.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
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  • 2
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary, glass ; Surface deactivation, persllylation ; Discussion of variable parameters ; Suggested practical procedure ; 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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  • 3
    Electronic Resource
    Electronic Resource
    Springer
    Chromatographia 18 (1984), S. 197-201 
    ISSN: 1612-1112
    Keywords: Capillary GC ; Co-injection ; Solvent effects
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Co-injection techniques (introducing additional pure solvent with the sample) were tested to eliminate peak distortion due to partial solvent trapping. Co-injections of solvent identical with the sample solvent were not successful, because first only partial solvent trapping of the strong type could be eliminated and second, there was no practicable method of placing a band of pure solvent ahead of the sample in the column inlet. Successful co-injections have to accept mixing of the sample with the pure solvent. Either the solvent trapping is improved by co-injection of a solvent which enhances solution of the critical solutes in the sample layer, or it creates a phase soaking effect in the stationary phase and reconcentrates broadened bands beyond the flooded inlet. The added solvent must have the appropriate polarity and some of it must remain in the column inlet at least until the sample solvent has completely evaporated.
    Type of Medium: Electronic Resource
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  • 4
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 2 (1979), S. 366-370 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary, glass ; Sampling problems by syringe needle temperature ; Technical solution of the problems by cooling and heating up minimized masses ; Discrimination and standard deviation measured with test mixtures C18-C38 ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: On-column injection into a hot gas chromatograph oven involves the danger that the bottom part of the needle is warmed up above the boiling point of the solvent in the sample. Consequently parts of the sample are evaporated out of the needle instead of being introduced as a liquid into the capillary column. This causes losses and hence discrimination of the less volatile parts of the sample which remain in the needle.A technical solution is proposed using a system for cooling the capillary during the injection, down to the injection point in the oven.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
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  • 5
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 3 (1980), S. 525-526 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary, glass ; Static coating ; Filling the column by pressure, not by vacuum ; Device for filling by pressure ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
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  • 6
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 3 (1980), S. 493-496 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary, glass ; Persilylation procedure ; Discussion of experimental parameters ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Persilylated glass capillary columns are the most universal GC columns available. They are relatively easy to prepare, but there is nevertheless a great need for helpful practical instructions. In the recent literature, methods and conditions for the preparation of persilylated columns have been recommended, but these might confuse the individual column maker, since they seem to originate from limited observations rather than from comprehensive investigation. They will hardly help to make column preparation safer. This paper attempts a summarized view of the present experience with persilylation and provides basic information for column makers.
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  • 7
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 5 (1982), S. 119-123 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary, glass ; Static coating ; Filling with mechanical closure ; Description of an easy and safe technique ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The static technique is commonly accepted as the most universal and scientific method of coating. At the same time, however, it is said to be experimentally demanding. Great efforts have therefore been made to render the method easier and safer, resulting in a wealth of recommendations confusing non-experts. Over a period of two years we have practically applied most of the reported procedures with the aim of studying their practical convenience. We do not doubt that most procedures are comparably suitable in the hands of expert users, i. e. once the initiation efforts have been forgotten, or are otherwise of little interest. We have attempted to describe a method which is specifically suited for easy and quick introduction to beginners. The method is based on mechanical column closure. The principles of the method are discussed, and a comprehensive description of its practical application is given.
    Additional Material: 5 Ill.
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  • 8
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    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
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
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  • 9
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    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.
    Additional Material: 5 Ill.
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  • 10
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 2 (1979), S. 527-528 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary, glass ; Leaching compared to etching ; Leaching by 20% HCI at 240°C ; Metal ions eliminated from glass surface ; Silica layer formed on leached surface ; 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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