Investigation of structural homogeneity of oligomers by a method of two-detector high effective liquid chromatography

  • Nazim Rauf oglu Bektashi Associate Professor of the Laboratory of Physical-Chemical Analysis, Institute of Polymer Materials National Academy of Sciences of Azerbaijan, nazimbektash@gmail.com
Keywords: isomers, molecular-weight distribution, oligomers, structural homogeneity, exclusion liquid chromatography

Abstract

In this work it has been presented a short review of works devoted to the investigation of various types of heterogeneity of macromolecules in the various polymer systems by a method of two-detector liquid chromatography. It has been shown based on results of analysis of literary sources that practically there is no information about division of polymers on isomer composition. The aim of this work consists in study of the structural heterogeneity of amination products of a-hexene in the synthesized redox system NH2OH×HCl-TiCl3 and in revealing by the methods of two-detector exclusion and reversed-phase HPLC of possible types of division on chemical composition of products. The results of the investigations of amination reaction of hexene by the methods of two-detector adsorption and exclusion HPLC and observations for dynamics of change of composition and structure of the amination products have been presented. It has been shown that in the composition of the prepared products besides purposeful individual amines the oligomers, molecular-weights changing approximately within the limits of Mn = 460-800 are detected. By a method of two-detector reversed-phase adsorption chromatography in composition of oligomers, besides division on molecular weight it has been also established the division on isomer composition, a formation of which occurs during migration to various carbon atoms. So it has been noted that at refractometric detection a division is observed only on molecular weight, and in a case of UV-detector in adsorption regime a division of fraction is also fixed on isomer composition. It has been concluded on multiplicity that in the investigated process during proton migration to various carbon atoms it occurs a formation of radicals with various reactivity; hereupon the oligomers with various molecular weights are respectively formed.  The structure of amination products has been studied and confirmed by the methods of IR- and NMR-spectroscopy

Downloads

Download data is not yet available.

References

1. Rafikov S.R., Pavlova S.A., Tverdokhlebova I.I., Metody opredeleniya molekulyarnykh vesov i polidispersnosti vysokomolekulyarnykh soyedineniy. M., Izd-vo Akademii Nauk SSSR, 1963, 336 p.
2. Sovremennoe sostoyaniye jidkostnoy khromatografii, Ed. D. Kirkland, M., Mir, 1974, 325 p.
3. Jidkostnaya kolonochnaya khromatografiya, ed. Z. Dale, K. Matzek, J. Yanaka, per. with English., t. 1-3, M., Mir, 1978, 428 p.
4. Ekstraktzionnaya khromatografiya, ed. T. Brown et al., Trans. with English., M., Mir, 1978, 627 p.
5. Batzer H., Zahir S.A., Journal of Applied polymer science, 1975, Vol. 19, pp. 585-600, 601-607, 609-617.
6. Dondos A., Benoit H., Die Makromolekulare Chemie, 1974, Vol. 175, pp. 1659-1663.
7. Servotte A., De Bruil R., Die Makromolekulare Chemie, 1975, Vol. 176, pp. 203-212.
8. Entelis S.G., Soros Educational J., 1996, No 7, pp. 59-66.
9. Entelis SG, Evreinov V.V., Kuzayev A.I., Reaksionnosposobnye oligomery. Moscow, Chemistry, 1985, 304 p.
10. Blagodatskikh I.V. Diss. doc. chem. sciences. M., 2008, 21 p.
11. Rozdina I.G., Filatova N.N., Gorshkov A.V., Evreinov V.V., Journal of High Molecular Chemistry Series A, 2013, Vol. 55, No 1, pp. 62-65.
12. Rozdina I.G., Filatova N.N., Gorshkov A.V., Evreinov V.V., Journal of High Molecular Chemistry Series A, 2013, Vol. 55, No 6, pp. 764-772.
13. Gorshkov A.V., Gorshkov M.V., Rozdina I.G., Tarasova I.A. et al., Journal of High Molecular Chemistry Series A, 2010, Vol. 52, No 3, pp. 478-486.
14. Gorshkov A.V., Evreinov V.V., Tarasova I.A, Gorshkov M.V., Journal of High Molecular Chemistry. Series B, 2007, Vol. 49, No 4, pp. 732-749.
15. Bektashi N.R., Alieva R., Dzalilov R.A., Ragimov A.V., Polymer Science. Ser. B, 2000, Vol. 42. No 9-10, pp. 276-281.
16. Crompton T.R. Polymer referans book, United Kingdom. Rapra Technology Ltd., 2006, pp. 273-278.
17. Bektashi N.R., Dzhafarov V.D., Chalyabiev Ch.A., Azadalieva G.N. et al., Az.khim jur., 2001, No 3, pp. 52-56.
18. Bektashi N.R., Djafarov V.C., Azadaliyeva G.N., Efendiyev A.A. İnternational Workshop - Conference, HPLC procedures for seperation of macromolecules, Slovakia, Bratislava, 200, pp.11-12.
19. Guliev S.A., Bektashi N.R., Sharifov G.S., Efendiev A.A., Az.khim jur., 2002, No 4, pp. 35-39.
20. Bektashi N.R., Dzafarov V.A., Polymer Science, Ser. A. of vysokomolekuliarnye soedineniya, 2004, Vol. 46, pp.1239-1244.
21. Bektashi N.R, Mustafaev A.M, Guseinov İ.A, and. Dzafarov V.D., Russian J. of Applied Chemistry, 2011, Vol. 84, No 7, pp.1281-1285.
22. Bektashi N.R. "Recent scientific achievements -2013", IX Interdisciplinary and practical conference Bulgaria, Sofia, 2013. No 18, pp. 61-67.
23. Aslanov T.A, Mustafayev R.I., Petrochemistry, 1988, Vol. 27, No 4, pp. 541-546.
24. Veliyev M.G., Salmanov M.A., Bektashi N.R., Aliyeva S.R. et al., J. Analyt. Chem., 2013, Vol. 1, No 2, pp. 7-11.
25. Styskin EL, Itzikson LB, Braude E.B. Prakticheskaya vysokoeffektivnaya jidkostnaya khromatografiya, M., Chemistry, 1986, 313 p.
26. Deroom E. Sovremennye metody YMR dlya khimicheskikh issledovaniy, M., Mir, 1992, 403p.
Published
2018-02-27
How to Cite
Bektashi, N. R. oglu. (2018). Investigation of structural homogeneity of oligomers by a method of two-detector high effective liquid chromatography. Sorbtsionnye I Khromatograficheskie Protsessy, 18(1), 64-72. https://doi.org/10.17308/sorpchrom.2018.18/466