Polímeros: Ciência e Tecnologia
Polímeros: Ciência e Tecnologia
Original Article

Characterization of additives in NR formulations by TLC-IR (UATR)

Murakami, Lidia Mattos Silva; Azevedo, Joyce Baracho; Diniz, Milton Faria; Silva, Leandro Mattos; Dutra, Rita de Cássia Lazzarinix

Downloads: 1
Views: 515


Abstract: It is a well-established fact that rubber accelerator is essential to provide solution in different sectors. However, there is a reversal process which can reduce the material performance. Sulfur accelerators donors and organic peroxides have been presented as a solution to the problem. The methodology development that can separate or characterize those components is a challenge and still allows gaps, explained by the application of conventional technique to reach this goal. This study aimed at contributing to the use of off-line coupling of thin layer chromatography (TLC)/infrared spectroscopy (IR) by Universal Attenuated Total Reflection (UATR) for analysis of N-cyclohexyl-2-benzotiazolsulfenamide (CBS), tetraethylthiuram disulfide (TMTD) and dicumyl peroxide (DCP), in natural poly-cis-isoprene (NR) formulations, containing naphthenic oil. The best results were obtained for the plasticizer and DCP, in formulations that had a greater proportion of these compounds. The separation of CBS and TMTD was made with less effectiveness, due to bands overlapping.


additives, characterization, NR, TLC, UATR


Ciência e Tecnologia da Borracha. Retrieved from in 2017, March 28, from http://ctborracha.com

Mohan, C. H. V. R., Ramanathan, J., Kumar, S., & Gupta, A. V. S. S. K. S. (2011). Characterization of Materials Used in Flex Bearings of Large Solid Rocket Motors. Defence Science Journal, 61(3), 264-269. http://dx.doi.org/10.14429/dsj.61.52.

Chemikeys. Retrieved from in 2017, April 18, from http://www.chemkeys.com/blog/wp-content/uploads/2008/09/polimeros.pdf

Grinson, E. C. (2010). Borrachas e seus aditivos - Componentes, Influências e Segredos. Porto Alegre: Ed. Letra & Vida.

D’Angelo, A. (2008). Peróxidos resistentes ao oxigênio para vulcanização contínua em túnel de ar quente. Revista Borracha Atual , 1-35. Retrieved in 2017, May 25, from Retrieved from http://www.retilox.com.br/astecnicos/download/peroxidos1.pdf

Reyneke-Barnard, C. P., Gradwell, M. H. S., & Mcgill, W. J. (2000). N,N’Pentamethylenethiuram disulfide- and N,N´´-Pentamethylenethiuram Hexasulfide-accelerated Sulfur Vulcanization. I. Interaction of Curatives in the Absence of Rubber. Journal of Applied Polymer Science, 77(12), 2718-2731. http://dx.doi.org/10.1002/1097-4628(20000919)77:12<2718::AID-APP200>3.0.CO;2-E.

Joseph, A. M., George, B., Madhusoodanan, K. N., & Alex, R. (2015). Current status of sulphur vulcanization and devulcanization chemistry: Process of vulcanization. Rubber Science, 28(1), 82-121.

Charoeythornkhajhornchai, P., Samthong, C., & Somwangthanaroj, A. (2017). Influence of sulfenamide accelerators on cure kinetics and properties of natural rubber foam. Journal of Applied Polymer Science, 134(19), 44822. http://dx.doi.org/10.1002/app.44822.

Kruželák, J., Sýkora, R., & Hudec, I. (2014). Peroxide vulcanization of natural rubber. Part I: effect of temperature and peroxide concentration. Journal of Polymer Engineering, 34(7), 617-624.

Dutra, R. C. L. (1996). Aplicação de técnica de TLC-IR em estudos de separação, identificação e quantificação de aditivos em borrachas. Polímeros: Ciência e Tecnologia , 6(2), 26-31.

Rodrigues, V. C., Diniz, M. F., Mattos, E. C., & Dutra, R. C. L. (2016). Separação e identificação de aditivos em tinta por TLC-IR/ UATR e extração seletiva. Polímeros: Ciência e Tecnologia, 26(Special Number), 68-74.

Damazio, D., Campos, E. A., Diniz, M. F., Mattos, E. C., & Dutra, R. C. L. (2016). TLC/IR (UATR) off-line coupling for the characterization of additives in EPDM rubber compositions. Polímeros: Ciência e Tecnologia, 26(1), 74-80.

Chauveau, S., Hamon, M., & Leleu, E. (1991). Separation and identification of various vulcanization agents and antioxidants in two types of rubber by chromatographic and spectrometric methods. Talanta, 38(11), 1279-1283. http://dx.doi.org/10.1016/0039-9140(91)80106-A. PMid:18965298.

Sanches, N. B., Cassu, S. N., Diniz, M. F., & Dutra, R. C. L. (2014). Characterization of additives typically employed in EPDM formulations by using FT-IR of gaseous pyrolyzates. Polímeros: Ciência e Tecnologia, 24(3), 269-275.

Mueller, D., Ferrão, M. F., Marder, L., Costa, A. B., & Schneider, R. C. S. (2013). Fourier Transform Infrared Spectroscopy (FTIR) and multivariate analysis for identification of different vegetable oils used in biodiesel production. Sensors, 13(4), 4258-4271. http://dx.doi.org/10.3390/s130404258. PMid:23539030.

Wake, W. C., Tidd, B. K., & Loadman, M. J. R. (1983). Analysis of rubber and rubber-like polymer (3rd ed.). New York: Applied Science.

Smith, A. L. (1979). Applied infrared spectroscopy. New York: John Wiley & Sons.

Wolfang, W. (1987). Tópicos de espectroscopia no infravermelho . São José dos Campos: ITA.

Sanches, N. B., Cassu, S. N., Diniz, M. F., & Dutra, R. C. L. (2015). TG/FT-IR characterization of additives typically employed in EPDM formulations. Polímeros: Ciência e Tecnologia, 25(3), 247-255.

5b7c6c8b0e8825be49896e51 polimeros Articles
Links & Downloads

Polímeros: Ciência e Tecnologia

Share this page
Page Sections