微波诱导燃烧样品处理技术测定氟材料中的痕量元素

An effective approach to the digestion of fluoropolymers for the determination of Ag, Ca, Cd, Co, Cr, Cu, Fe, K, Mg, Mn, and Ni impurities has been developed using microwave-induced combustion (MIC) in closed quartz vessels pressurized with oxygen. Samples that were examined included the following: polytetrafluorethylene (PTFE); polytetrafluoroethylene with an additional modifier, perfluoropropylvinylether (PTFE-TFM); and fluorinated ethylene propylene (FEP). A quartz device was used as a sample holder, and the influence of the absorber solution was evaluated. Determination of trace elements was performed by inductively coupled plasma−optical emission and mass spectrometry. Neutron activation analysis (NAA) was used for validation purposes. Results were also compared to those obtained using microwave-assisted acid extraction in high-pressure closed systems. Dilute nitric acid (5 mol L−1), which was selected as the absorbing medium, was used to reflux the sample for 5 min after the combustion. Using these conditions, agreement for all analytes was better than 98% when compared to values determined by NAA. The residual carbon content in the digests was lower than 1%, illustrating the high efficiency of the method. Up to 8 samples could be digested within 30 min using MIC, providing a suitable throughput, taking into account the inertness of such samples.