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Evaluation of sample preparation methods for elastomer digestion for further halogens determination

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Abstract

In this work, three sample preparation methods were evaluated for further halogen determination in elastomers containing high concentrations of carbon black. Samples of nitrile-butadiene rubber, styrene-butadiene rubber, and ethylene-propylene-diene monomer elastomers were decomposed using oxygen flask combustion and microwave-induced combustion (MIC) for further Br and Cl determination by ion chromatography (IC), inductively coupled plasma optical emission spectrometry (ICP OES), and inductively coupled plasma mass spectrometry (ICP-MS). Extraction assisted by microwave radiation in closed vessels was also evaluated using water or alkaline solution. Digestion by MIC was carried out using 50 mmol l−1 (NH4)2CO3 as the absorbing solution. The effect of the reflux step was also evaluated. Accuracy was evaluated using certified reference materials with polymeric matrix composition and by comparison of results using neutron activation analysis. Agreement for Br and Cl was better than 95% by MIC using 5 min of reflux, and no statistical difference was found using IC, ICP OES, and ICP-MS for determination of both analytes. For MIC, the relative standard deviation (RSD) was lower than 5%. Using extraction in closed vessels, a high amount of residues was observed, and recoveries were lower than 45% for both analytes. For oxygen flask combustion, the agreement was similar using MIC but RSD was higher (20%). The residual carbon content, an important parameter used to evaluate the digestion efficiency, was always below 1% for MIC. Using MIC, it was possible to digest elastomers with high efficiency, resulting in a single solution suitable for halogen determination by different techniques.

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Acknowledgments

The authors are grateful for fellowships provided by CAPES, CNPq ,and Fapergs and to Metrohm AG (Switzerland and partner in Brazil) for IC support. The authors also thank Dr. Marco Aurélio Zezi Arruda (UNICAMP) for lending the infrared thermometer.

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Authors and Affiliations

  1. Departamento de Química, Universidade Federal de Santa Maria, 97105-900, Santa Maria, RS, Brazil

    Diogo P. Moraes, Juliana S. F. Pereira, Liange O. Diehl, Valderi L. Dressler, José Neri G. Paniz & Érico M. M. Flores

  2. Instituto de Química e Geociências, Universidade Federal de Pelotas, 96010-610, Pelotas, RS, Brazil

    Márcia F. Mesko

  3. Micro-and Radiochemistry Graz University of Technology, Technikerstrasse 4, 8010, Graz, Austria

    Guenter Knapp

Authors
  1. Diogo P. Moraes
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  2. Juliana S. F. Pereira
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  3. Liange O. Diehl
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  4. Márcia F. Mesko
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  5. Valderi L. Dressler
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  6. José Neri G. Paniz
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  7. Guenter Knapp
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  8. Érico M. M. Flores
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Correspondence to Érico M. M. Flores.

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Moraes, D.P., Pereira, J.S.F., Diehl, L.O. et al. Evaluation of sample preparation methods for elastomer digestion for further halogens determination. Anal Bioanal Chem 397, 563–570 (2010). https://doi.org/10.1007/s00216-010-3478-1

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  • DOI: https://doi.org/10.1007/s00216-010-3478-1

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