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Pereira RM, Costa VC, Hartwig CA, et al. Feasibility of halogen determination in noncombustible inorganic matrices by ion chromatography after a novel volatilization method using microwave-induced combustion. Talanta. 2015;147:76-81doi: 10.1016/j.talanta.2015.09.031.
Pereira, R. M., Costa, V. C., Hartwig, C. A., Picoloto, R. S., Flores, E. M., Duarte, F. A., & Mesko, M. F. (2016). Feasibility of halogen determination in noncombustible inorganic matrices by ion chromatography after a novel volatilization method using microwave-induced combustion. Talanta, 14776-81. https://doi.org/10.1016/j.talanta.2015.09.031
Pereira, Rodrigo M, et al. "Feasibility of halogen determination in noncombustible inorganic matrices by ion chromatography after a novel volatilization method using microwave-induced combustion." Talanta vol. 147 (2016): 76-81. doi: https://doi.org/10.1016/j.talanta.2015.09.031
Pereira RM, Costa VC, Hartwig CA, Picoloto RS, Flores EM, Duarte FA, Mesko MF. Feasibility of halogen determination in noncombustible inorganic matrices by ion chromatography after a novel volatilization method using microwave-induced combustion. Talanta. 2016 Jan 15;147:76-81. doi: 10.1016/j.talanta.2015.09.031. Epub 2015 Sep 13. PMID: 26592579.
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Talanta. 2016 Jan 15;147:76-81. doi: 10.1016/j.talanta.2015.09.031. Epub 2015 Sep 13.

Feasibility of halogen determination in noncombustible inorganic matrices by ion chromatography after a novel volatilization method using microwave-induced combustion.

Talanta

Rodrigo M Pereira, Vanize C Costa, Carla A Hartwig, Rochele S Picoloto, Erico M M Flores, Fabio A Duarte, Marcia F Mesko

Affiliations

  1. Centro de Ciências Químicas, Farmacêuticas e de Alimentos, Universidade Federal de Pelotas, 96160-000 Pelotas, RS, Brazil.
  2. Departamento de Química, Universidade Federal de Santa Maria, 97105-900 Santa Maria, RS, Brazil.
  3. Centro de Ciências Químicas, Farmacêuticas e de Alimentos, Universidade Federal de Pelotas, 96160-000 Pelotas, RS, Brazil. Electronic address: [email protected].

PMID: 26592579 DOI: 10.1016/j.talanta.2015.09.031

Abstract

A microwave-induced combustion (MIC) system based on the volatilization process was applied for subsequent halogen determination from noncombustible inorganic matrices. Portland cement samples were selected to demonstrate the feasibility of the proposed method, allowing the subsequent determination of Cl and F by ion chromatography (IC). Samples were mixed with high-purity microcrystalline cellulose, wrapped with a polyethylene film and combusted in quartz closed vessels pressurized with oxygen (20bar). Water and NH4OH (10, 25 or 50m mol L(-1)) were evaluated for Cl and F absorption, but water was selected, using 5min of reflux after volatilization. Final solutions were also suitable for analysis by pontentiometry with ion-selective electrode (ISE) for both analytes, and no difference was found when comparing the results with IC. The accuracy of the proposed method for Cl was evaluated by analysis of certified reference materials (CRMs), and agreement with certified values ranged from 98% to 103%. Results were also compared to those using the procedure recommended by the American Society of Testing and Materials (ASTM) for the determination of total chlorides (C114-13), and no difference was found. Volatilization by MIC using a mixture of cement, cellulose and a biological CRM was carried out in order to evaluate the accuracy for F, and recovery was about 96%. The proposed method allowed suitable limits of detection for Cl and F by IC (99 and 18mg kg(-1), respectively) for routine analysis of cement. Using the proposed method, a relatively low standard deviation (<7%), high throughput (up to eight samples can be processed in less than 30min) and lower generation of laboratory effluents, when compared to the ASTM method, were obtained. Therefore, the method for volatilization of Cl and F by MIC and subsequent determination by IC can be proposed as a suitable alternative for cement analysis.

Copyright © 2015 Elsevier B.V. All rights reserved.

Keywords: Cement analysis; Chlorine determination; Fluorine determination; Microwave-induced combustion; Sample preparation; Volatilization

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