Abstract
A simple ion chromatographic method has been applied to the determination of anionic impurities chloride, bromide, nitrate, and sulfate in hexafluorotitanic acid and hexafluorozirconic acid samples. Industrial samples analyzed may contain high levels of fluorinated species at pH values lower than 1.0, which represents a handicap for the instrumental analysis of these matrixes. Up to now, these samples have been analyzed by chemical methods, which have interferences, involving detection of the final point in chloride determination by volumetry and coprecipitation in sulfate determination by gravimetry. The optimization of the method was carried out using industrial samples. In order to obtain the best chromatographic resolution, the dilution factor of the samples, flow rate, and eluent concentration were studied using isocratic elution. The ion chromatographic method was suitable for the determination of anionic impurities in acidic matrixes, except for chloride in hexafluorozirconic acid. The analytes were separated in hexafluorotitanic acid and hexafluorozirconic acid, without using any sample treatment apart from dilution, with good linearity with correlation coefficients higher than 0.99 and inter- and intra-day repeatability lower than 15 percent, expressed in terms of the relative standard deviation.
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