Download e-book for iPad: Analytical Reaction Gas Chromatography by Viktor G. Berezkin

By Viktor G. Berezkin

ISBN-10: 1468407090

ISBN-13: 9781468407099

ISBN-10: 1468407112

ISBN-13: 9781468407112

The so much common and powerful process for the research of complicated multicomponent combos of risky ingredients is gasoline chromatography. notwithstanding, there are many boundaries asso­ ciated with the classical edition of this method which retard its improvement and the additional enlargement of its program: 1) the id of the elements of a fancy combine­ ture of unknown composition is in itself a posh and hard challenge, until the homologous sequence of the part of be pointed out is understood; 2) the overlapping of chromatographic peaks for a number of compounds makes it tricky, and in a couple of situations very unlikely, to hold out qualitative and quantitative research of those elements, and ends up in the need of utilizing a number of columns of alternative polarities or to using columns with very excessive potency; three) the direct research of volatile and nonvolatile compounds is very unlikely; four) the trouble of quantitative chromatographic research utilizing thermal conductivity detectors raises with the need of deciding upon person reaction (calibration) components; the insensitivity of the flame ionization detector to a couple of components (inorganic gases) results in the need of introducing extra operations (prelimi­ nary focus of hint elements) in reference to thermal conductivity detectors. vii viii FOREWORD The directed use of chemical conversion of the compounds analyzed often makes it attainable to take away the constraints pointed out above.

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Lille [8] developed methods for analysis of unsaturated hydrocarbons in shale gasolines with boiling points up to 150°C using vapor phase hydrogenation in a microreactor placed in front of the chromatographic column. Reduced nickel (20% on diatomite) was 56 ANALYSIS OF COMPLEX MIXTURES >E I 2 I 2 e:- ... 0 lJ ~ f 1I If 5 "5 8 7 .. ~ 1II IlfZ 9 10 13 8 If ~ 0 lJ 41 0:: 0 5 10 0 5 10 0 Time, min 5 10 f5 20 Fig. 11. Chromatograms for the original samp~e (I), and for the products of hydrogenation at 200·C (II) and dehydrogenation at 325·C (III) [6].

He showed that it is not difficult to carry out selective hydrogenation of aromatic hydrocarbons and olefins as a group reaction. 4% platinum on aluminum oxide) containing a halogen is best for this purpose. 5 g; temperature, 299°C; flow rate of helium (hydrogen), 60-70 ml/min. Dehydrogenation is a more complex process, which is often accompanied by side reactions. Cyclopentane homologs are converted into aromatic hydrocarbons to a much lesser degree than the cyclohexane homologs. As general methods for the analysis of complex hydrocarbon mixtures, Rowan suggested carrying out dehydrogenation of a mixture of isoparaffins and naphthenes for the selective determination of the concentration of cyclohexanes with the help of the peaks cor- HYDROGENATION AND DEHYDROGENATION 55 responding to the aromatic hydrocarbons formed, and also the utilization of hydrogenation at room temperature for the selective conversion of the olefins to the corresponding paraffins.

Yanovskii, Kinetika iKataliz, 5:490 (1964). 1. Semenenko, S. Z. Roginskii, and M. 1. Yanovskii, Kinetika i Kataliz, 6:320 (1965). 12. 13. 14. 15. 16. 17. 18. 19. 20. 21. R. J. Kokes, H. Tobin, and P. H. Emmett, J. Am. Chem. , 77:5860 (1955). J. Kallen and E. Heilbronner, Helv. Chim. Acta, 43:489 (1960). E. Glueckauf, Trans. , 51:34 (1955). A. Klinkenberg and F. Sjenitzer, Chem. Eng. , 5:258 (1956). V. G. Berezkin, V. S. Kruglikova, and V. E. Shiryaeva, Neftekhimiya, 6:630 (1966). B. D. Blaustein and G.

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