This paper reports the development of a method of simultaneous determination of iron and nickel in fluoropolymers by high-resolution continuum source graphite furnace atomic absorption spectrometry (HR-CS GF AAS) with direct solid sampling. In order to carry out simultaneous measurements, both the main resonance line of nickel (232.003nm) and the adjacent secondary line of iron (232.036nm) were monitored in the same spectral window. The proposed method was optimized with a perfluoroalkoxy (PFA) sample and was applied to the determination of iron and nickel in fluorinated ethylene propylene (FEP) and modified polytetrafluoroethylene (PTFE-TFM) samples. Pyrolysis and atomization temperatures, as well as the use of Pd and H2 (during pyrolysis) as chemical modifiers, were carefully investigated. Compromise temperatures for pyrolysis and atomization of both analytes were achieved at 800 and 2300°C, respectively, using only 0.5Lmin(-1) H2 as chemical modifier during pyrolysis. Calibration curves were performed with aqueous standards by using a single solution which contained both analytes. Limits of detection were 221 and 9.6ngg(-1) for iron and nickel, respectively. Analyte concentrations in all samples ranged from 3.53 to 12.4µgg(-1) for iron and from 37 to 78ngg(-1) for nickel, with relative standard deviation less than 19%. Accuracy was evaluated by comparing these results with those obtained by inductively coupled plasma mass spectrometry after sample digestion by microwave-induced combustion and no significant statistical difference was observed.

Arsenic speciation in seafood after several culinary treatments was performed and AsB, As(iii), DMA, MMA and As(v) species were determined by LC-ICP-MS/MS.

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In this work, a method for sample preparation of high-purity polyimide was proposed for halogens and sulfur determination by ion chromatography (IC) with conductivity detection and, alternatively, by inductively coupled plasma mass spectrometry (ICP-MS). A relatively high polyimide mass (600mg) was completely digested by microwave-induced combustion (MIC) using 20bar of O2 and 50mmolL(-1) NH4OH as absorbing solution. These conditions allowed final solutions with low carbon content (<10mgL(-1)) and suitable pH for analysis by both IC and ICP-MS. The accuracy was evaluated using a certified reference material of polymer for Cl, Br and S and spike recovery experiments for all analytes. No statistical difference (t-test, 95% of confidence level) was observed between the results obtained for Cl, Br and S by IC after MIC and the certified values. In addition, spike recoveries obtained for F, Cl, Br, I and S ranged from 94% to 101%. The proposed method was suitable for polyimide decomposition for further determination of halogens and sulfur by IC and by ICP-MS (Br and I only). Taking into account the lack of methods and the difficulty of bringing this material into solution, MIC can be considered as a suitable alternative for the decomposition of polyimide for routine quality control of halogens and sulfur using IC or ICP-MS.

In this study, the microwave-induced combustion (MIC) method was evaluated for the sample preparation of the most consumed mushroom species in Brazil (Champignon, Shiitake, and Shimeji) and further halogen determination by ion chromatography (IC). For this, sample mass, combustion aid mass, and absorbing solution (H2O and 50 mmol·L−1, 100 mmol·L−1, or 150 mmol·L−1 NH4OH) were evaluated. Bromine and iodine concentrations, determined by IC, were lower than the limits of detection (LODs, Br: 6 mg·kg−1 and I: 24 mg·kg−1). Inductively coupled plasma mass spectrometry (ICP-MS) was also used for Br and I determination, and the LODs were lower (Br: 0.066 mg·kg−1 and I: 0.014 mg·kg−1) than those obtained by IC. Concentrations of Cl, obtained by IC, ranged from 523 mg·kg−1 to 13053 mg·kg−1 with LOD of 40 mg·kg−1. In turn, Br and I concentrations, obtained by ICP-MS, ranged from 2.49 mg·kg−1 to 5.50 mg·kg−1 and from <0.014 mg·kg−1 to 0.047 mg·kg−1, respectively. Fluorine concentrations, determined by IC, were always lower than LOD (23 mg·kg−1). The trueness of the proposed methods was evaluated by recovery tests using standard solutions and a reference material (RM NIST 8435). When using the standard solution, recoveries ranged from 95% to 103% for halogen determination by IC and from 105% to 109% for Br and I determination by ICP-MS. When using the RM, recoveries of 102% for Cl by IC and of 87% and 86% for Br and I by ICP-MS, respectively, were obtained.