Determination of fluorine in organofluorine compounds by combustion ion chromatography
Abstract
Fluorine determination as part of elemental analysis is an important step for characterization of organofluorine compounds. The purpose of this study is to demonstrate the capabilities of combustion ion chromatography for the fluorine determination in the main composition of organic compounds.
The objects of analysis are various fluoroaromatic compounds with fluorine in the range of 8-60%. Sample solutions for analysis were prepared by dissolving 0.5-3 mg samples in 10 ml of ethanol or hexane. To obtain reproducible results, if the fluorine content is 50% or higher, the sample weight should not exceed 1.5 mg. Then 10 μl of the sample solution was placed in a sampler boat and then introduced into the PAC Antek MultiTek combustion system. The sample was burned at 1050°C, the combustion products were absorbed with deionized water and analyzed by a Thermo Scientific Dionex Integrion HPIC ion chromatograph. A calibration curve was previously constructed using solutions prepared from pentafluorobenzoic acid (solvent – ethanol, fluorine concentration range 10-110 mg/l). Fluorine content in 6 compounds under study was determined; the results were consistent with theoretically calculated values. Accuracy was verified by analyzing an organic substance with a certified fluorine content value (13.56%) – 4-fluorobenzoic acid; precision was estimated by the relative standard deviation of 3-6 sample analysis results at three content levels – 8.79, 17.35, and 59.35%. The relative standard deviation was in the range 0.09-2.6%. The detection limit and the limit of quantification of fluorine were 0.6 and 2.1 mg/l, respectively.
Thus, the results presented in the work demonstrate the successful application of the combustion ion chromatography method for determining fluorine in the main composition of organofluorine compounds with an accuracy that meets the requirements of elemental organic analysis. The advantages of this method allow expanding its application for determining other heteroelements (Cl, Br, I, S, Se) both separately and simultaneously.
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