Using microwave plasma atomic emission spectrometry for the determination of phosphorus in arylphosphines and their metal complexes
S. YU. PETRAKOVA, V. D. TIKHOVA
Vorozhtsov Novosibirsk Institute of Organic Chemistry, Siberian Branch of the Russian Academy of Sciences, Novosibirsk, Russia
Keywords: organophosphorus compounds, microwave plasma atomic emission spectrometry, Agilent 4100, phosphorus determination, arylphosphines
Abstract
Elemental analysis in general, and phosphorus determination in particular, is an important step necessary for establishing the purity of newly synthesised organophosphorus compounds. It has been shown that phosphorus determination by classical spectrophotometry is difficult due to the need to convert all phosphorus to orthophosphate. Microwave plasma atomic emission spectrometry is proposed for determining phosphorus in arylphosphine ligands and their metal complexes after oxidative decomposition of these compounds. This method allows for the determination of total phosphorus regardless of its form. Two approaches were used for mineralisation of the compounds: oxygen flask combustion (Schoeniger method) for arylphosphines and acidic microwave digestion for metal complexes. The atomic emission spectrometer was calibrated using solutions prepared from triphenylphosphine by microwave digestion or by the Schoeniger method. Using this method, 11 arylphosphines of various structures and three nickel complexes with phosphorus contents ranging from 4 to 12% were analysed. The absolute error of determination did not exceed 0.3 wt%. The detection limit and limit of quantification of phosphorus were 0.2 and 0.7 mg/L, respectively; the calculated minimum detectable phosphorus content using the Schöniger decomposition method was 1.5 %.
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