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  • 1
    Electronic Resource
    Electronic Resource
    Co-injections to avoid peak distortion due to partial solvent trapping in capillary gas chromatography (GC) (1984)
    Springer
    Chromatographia 18 (1984), S. 197-201 
    Details
    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
    URL: http://dx.doi.org/10.1007/BF02276732
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  • 2
    Electronic Resource
    Electronic Resource
    Capillary columns with immobilized stationary phases. Part 4: A moderately polar phase, OV-1701 (1982)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 5 (1982), S. 13-18 
    Details
    ISSN: 0935-6304
    Keywords: Gas chromatography, capillary ; Column preparation ; Immobilization of stationary phases ; Procedure for polar phases ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Whereas the immobilization of apolar silicone phases is essentially understood and mastered, the corresponding treatment of even moderately polar phases remains problematical. Upon attack by peroxide radicals, these phases respond by forming active transformation products rather than by bonding to the support surface or to neighboring molecules. OV-1701 is at present the most polar stationary phase which can reasonably be immobilized. An essential feature of the practical procedure is the prevention of film breakage after coating the inert support surface and before immobilization. Two ways of overcoming this problem are presented.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/jhrc.1240050103
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  • 3
    Electronic Resource
    Electronic Resource
    Loop-type interface for concurrent solvent evaporation in coupled HPLC-GC. Analysis of raspberry ketone in a raspberry sauce as an example (1986)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 9 (1986), S. 518-523 
    Details
    ISSN: 0935-6304
    Keywords: Coupled HPLC-GC ; Concurrent solvent evaporation ; Loop-type interface ; Raspberry ketone ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Presently, two coupling techniques are used for directly introducing HPLC fractions into capillary GC: The retention gap technique (involving negligible or partially concurrent solvent evaporation) and fully concurrent solvent evaporation. While the former involves use of a conventional on-column injector, it is now proposed that concurrent solvent evaporation technique be carried out using a switching valve with a built-in sample loop. The technique is based on the concept that the carrier gas pushes the HPLC eluent into the GC capillary against its own vapor pressure, generated by a column temperature slightly exceeding the solvent boiling point at the carrier gas inlet pressure. Further improvement of the technique is achieved by flow regulation of the carrier gas (accelerated solvent evaporation) and backflushing of the sample valve (improved solvent peak shape).Concurrent solvent evaporation using the loop-type interface is easy to handle, allows transfer of very large volumes of HPLC eluent (exceeding 1 ml), and renders solvent evaporation very efficient, allowing discharge of the vapors of 1 ml of solvent through the column within 5-10 min.
    Additional Material: 6 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/jhrc.1240090906
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  • 4
    Electronic Resource
    Electronic Resource
    Solvent effects in on-column injection of large sample volumes (1986)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 9 (1986), S. 405-407 
    Details
    ISSN: 0935-6304
    Keywords: Capillary GC ; Solvent effects ; Solvent trapping ; Phase soaking ; Large sample volumes ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/jhrc.1240090708
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  • 5
    Electronic Resource
    Electronic Resource
    Capillary columns with immobilized stationary phases. Part 3: The basic influence of vinyl groups (1981)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 4 (1981), S. 491-494 
    Details
    ISSN: 0935-6304
    Keywords: Gas chromatography, capillary ; Column preparation ; Immobilization of stationary phases ; Influence of vinyl groups ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: This article presents a preliminary description of the influence exerted by vinyl groups on the process and on the result of immobilization. Vinyl groups may occur in the stationary phase (e. g. in SE-54) or may be bound to the support surface by persilylation with divinyltetramethyldisilazane. In the first case they promote the crosslinking process in the stationary phase. In the second case bonding to the solid surface is intensified. We have observed that vinyl groups in both situations contribute with comparable efficiency to the final non-extractability of the stationary phase. A further, yet entirely independent influence of surface-bonded vinyl groups concerns the acidity of the column. Whereas regular persilylation produces slightly acidic columns, a substantial shift to basic column behavior is observed after persilylation with a vinyl-containing reagent. The potential future importance of both kinds of influence is discussed.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/jhrc.1240041003
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  • 6
    Electronic Resource
    Electronic Resource
    Analysis of petroleum fractions by on-line micro HPLC-HRGC coupling, involving increased efficiency in using retention gaps by partially concurrent solvent evaporation (1985)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 8 (1985), S. 601-606 
    Details
    ISSN: 0935-6304
    Keywords: Coupled HPLC-GC ; Retention gap ; Partially concurrent solvent evaporation ; Gasoline ; Group-type separation ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Two-dimensional chromatography of gasoline by on-line coupled HPLC-HRGC, as described in this paper, allows separate GC analysis of paraffins and aromatics. The GC system contains a retention gap of only 10 m length for introducing HPLC fractions of 100 μl volume. This becomes possible through evaporation of part of the solvent during introduction of the HPLC eluent. This “partially concurrent solvent evaporation” technique allows transfer of large volumes of HPLC eluent into relatively short retention gaps, maintaining the full efficiency of the solvent effects in reconcentrating the bands of the early eluted solutes.
    Additional Material: 7 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/jhrc.1240080925
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  • 7
    Electronic Resource
    Electronic Resource
    Coupled HPLC-GC for determining PCBs in fish (1987)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 10 (1987), S. 416-417 
    Details
    ISSN: 0935-6304
    Keywords: Coupled HPLC-GC ; Loop-type interface ; Concurrent solvent evaporation ; PCBs in fish ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/jhrc.1240100713
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  • 8
    Electronic Resource
    Electronic Resource
    GC column effluent splitter for problematic solvents introduced in large volumes: Determination of di-(2-ethylhexyl) phthalate in triglyceride matrices as an application (1988)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 11 (1988), S. 135-139 
    Details
    ISSN: 0935-6304
    Keywords: Solvents and GC detectors ; Coupled HPLC-GC ; Column effluent splitter ; Di-(2-ethylhexyl) phthalate ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Introduction of solutions of up to several milliliters by on-column injection of large volumes or by coupled HPLC-GC may cause problems with GC detectors (FID, AFID, MS). For instance, dichloromethane forms large amounts of hydrochloric acid and carbon black in FIDs.A column effluent splitter was developed for keeping the major portion of the solvent vapors away from the detector; approximately 99% of the vapor is vented while the remaining 1% of vapor is used for detecting the widths of the solvent peaks. During analysis, the split ratio is reversed by a strong increase of the resistance to the gas flow through the split exit line.The system was used for the determination of di-(2-ethylhexyl)-phthalate (DEHP) in triglyceride matrices of various foods. Direct determination by HPLC is not sufficiently sensitive, whereas direct analysis by GC is hindered by the triglycerides. Solutions of fats or oils were pre-separated on a silica column using dichloro-methanelcyclohexane 1:l with addition of 0.05 % acetonitrile as eluent. The HPLC fraction containing the DEHP was transferred to GC through a loop-type interface using concurrent solvent evaporation. Detection limits were around 0.1 ppm.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/jhrc.1240110135
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  • 9
    Electronic Resource
    Electronic Resource
    Concurrent solvent evaporation for on-line coupled HPLC-HRGC (1986)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 9 (1986), S. 95-101 
    Details
    ISSN: 0935-6304
    Keywords: Coupled HPLC-capillary GC ; Concurrent solvent evaporation ; Retention gap ; Solvent effects ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A technique is proposed which allows introduction of very large volumes of liquid (10 ml were tested) into capillary columns equipped with short (1-2 m long) retention gaps. It is based on concurrent solvent evaporation, i.e. evaporation of the solvent during introduction of the sample. The technique presupposes high carrier gas flow rates (at least during sample introduction) and column temperatures near the solvent boiling point. The major limitation of the method is the occurrence of peak broadening for solutes eluted up to 30°, in some cases up to 100°, above the injection temperature. This is due to the absence of solvent trapping and a reduced efficiency of phase soaking. Therefore, use of volatile solvents is often advantageous. Application of the concurrent solvent evaporation technique allows introduction of liquids which do not wet the retention gap surface. However, the method is still not very attractive for analysis of aqueous or water-containing solutions (reversed phase HPLC).
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/jhrc.1240090208
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  • 10
    Electronic Resource
    Electronic Resource
    Co-solvent effects for preventing broadening or loss of early eluted peaks when using concurrent solvent evaporation in capillary GC. Part 1: Concept of the technique (1988)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 11 (1988), S. 388-394 
    Details
    ISSN: 0935-6304
    Keywords: Solvent effects ; Co-solvent effects ; Concurrent solvent evaporation ; Large sample volumes ; Coupled HPLC-GC ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The concept and some first results of a method are described for evaporating large volumes of solvent in a relatively short pre-column (retention gap) in such a way that solvent trapping retains volatile components in the inlet up to completion of solvent evaporation. The method was developed for transferring large volumes (easily exceeding 1 ml) of HPLC eluent to GC when using on-line coupled HPLC-GC, but is equally suited for injecting large sample volumes (at least some 50 μl) and could be particularly useful for introducing aqueous solutions.Concurrent solvent evaporation allows introduction of very large volumes of liquid into GC. However, peaks eluted up to some 40-80° above the column temperature during introduction of the liquid are strongly broadened due to the absence of solvent trapping. On the other hand, previous retention gap techniques involving solvent trapping were not suited for transferring very large volumes of liquid into GC. Using a relatively high boiling co-solvent added to the sample or the HPLC eluent, advantages of concurrent solvent evaporation can be combined with solute reconcentration by solvent effects, allowing elution of sharp peaks starting at the column temperature during introduction of the sample.
    Additional Material: 6 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/jhrc.1240110506
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