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

• MIC was used for halogen volatilization from noncombustible inorganic matrices.
• Cl and F were volatilized using microcrystalline cellulose as combustion aid.
• Only water was necessary for analyte absorption after volatilization by MIC.
• IC and ISE were suitable for analyte determination.
• Volatilization by MIC allowed a high sample throughput and low waste generation.

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 (20 bar). Water and NH4OH (10, 25 or 50 mmol L−1) were evaluated for Cl and F absorption, but water was selected, using 5 min 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 18 mg 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 30 min) 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.

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