Halogen Determination in Polymeric Waste of Electrical and Electronic Equipment: Overcoming Limitations in Sample Preparation

Sample preparation of polymers for halogen determination requires special attention because they are difficult to bring into solution and due to the risk of analyte losses when using acid digestion. A method using microwave-induced combustion (MIC) was optimized for accurate determination of halogens in polymeric parts obtained in waste of electrical and electronic equipment. Results were compared with those by using microwave-assisted extraction (MAE) with alkaline solution and microwave-assisted wet digestion (MAWD) using concentrated nitric acid, which are common choices for sample preparation. In this particular case, the MAE method was not suitable and underestimated results were obtained, showing the necessity for the complete digestion. Even with the use of MAWD under high temperature and pressure, incomplete digestion and high acid content were obtained, which were unsuitable for analysis and resulted in poor recovery. Only by using MIC (diluted ammonia as absorbing solution) acceptable recoveries (95 to 104%) and agreement with certified values for the certified reference materials (CRMs) of polymers were obtained. Thus, a suitable method for all halogen to be determined by ion chromatography (IC) or inductively coupled plasma mass spectrometry (ICP-MS), with the exception of F, was obtained in agreement with the requirements by the Restriction of the Use of Certain Hazardous Substances (RoHS) European directive.