Determination of Bromide, Chloride, and Fluoride in Cigarette Tobacco by Ion Chromatography after Microwave-Induced Combustion

Abstract

A microwave-induced combustion (MIC) method was applied for cigarette tobacco digestion and further determination of bromide (Br), chloride (Cl), and fluoride (F) by ion chromatography (IC). Samples (up to 500 mg) were combusted at 20 bar of oxygen. Combustion was complete in less than 30 s, and analytes were absorbed in (NH₄)₂CO₃ solutions. A reflux step, not available in other systems, was applied to improve analyte absorption. Absorbing solution with 50 mmol L⁻¹(NH₄)₂CO₃ was selected because it showed recovery close to 100% for samples containing spikes of halogens. Accuracy of the proposed procedure was evaluated by analysis of certified reference materials and the agreement was better than 97% for all analytes using 50 mmol L⁻¹ (NH₄)₂CO₃ as absorbing solution and 5 min of reflux. Temperature during combustion was higher than 1400°C and the residual carbon content was always lower than 1%. With the use of the MIC system, up to eight samples could be processed simultaneously, and a single absorbing solution was suitable for all analytes. Limits of quantification by MIC and further IC determination were 0.50, 0.20, and 0.10 µg g⁻¹ for Br, Cl, and F, respectively.

Keywords:

• Bromide
• Chloride
• Cigarette tobacco
• Fluoride
• Ion chromatography
• Microwave-induced combustion

Acknowledgments

The authors are grateful to INCT-Bioanalitica/CNPq and Fapergs for supporting this study. The authors also thank to Metrohm AG (Switzerland and partner in Brazil) for IC support.

Notes

^a Informed value.