Simple, rapid and non-destructive detection and determination of phosphines and phosphine oxides in solution by1H and31P NMR

摘要

A simple, rapid and non-destructive method for the detection and determination of phosphines and phosphine oxides in solution by1H and31P NMR spectroscopy is proposed. Diphenylphosphine (DPP) and diphenylphosphine oxide (DPPO) mixtures in C6D6chosen as model system were studied in wide ranges of concentration (10−2to 4 mol/l). The detection of DPP and DPPO in solution by1H 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 constant1JPHof 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 HPand ortho-proton integral intensity on the concentration of DPP and DPPO was found. The content of DPP and DPPO evaluated by31P without adding Cr(acac)3and by1H NMR agreed with the quoted amounts within 1 to