| Abstract: | Organic phosphonates are widely used, and in general, they are not easily biodegradable. Therefore, our interest was focussed on the development of an analytical method for the trace-level determination of organic phosphonates in water. Our method combines preconcentration of the analytes by evaporating the water sample with the methylation of the phosphonates using diazomethane. Analysis of the totally methylated phosphonates is done by liquid chromatography coupled with mass Spectrometry by the particle-beam interface. The derivatives could be clearly identified by their electron impact mass spectra as well as their chemical ionisation mass spectra. The totally methylated phosphonates can be separated by liquid chromatography using a 125 mm × 4 mm LiChrospher 100 Diol column and a gradient mobile phase containing n-hexane and isopropyl alcohol. After optimizing preconcentration and derivatization procedures as well as all particle-beam and mass spectra conditions, detection limits in the low ppb range were attained. |
