Abstract
A simple, rapid and non-destructive method for the detection and determination of phosphines and phosphine oxides in solution by 1H and 31P NMR spectroscopy is proposed. Diphenylphosphine (DPP) and diphenylphosphine oxide (DPPO) mixtures in C6D6 chosen as model system were studied in wide ranges of concentration (10−2 to 4 mol/l). The detection of DPP and DPPO in solution by 1H NMR was based on the presence of two doublets (hydrogen directly bonded to phosphorus, HP) originating from P-H and P(O)H groups with one bond coupling constant 1JPH of 216.08 and 476.12 Hz. 31P NMR signals at −40.07 and +18.26 ppm additionally proved the presence of DPP and DPPO in solution. A linear dependence of the measured HP and ortho-proton integral intensity on the concentration of DPP and DPPO was found. The content of DPP and DPPO evaluated by 31P without adding Cr(acac)3 and by 1H NMR agreed with the quoted amounts within 1 to 3%.
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