A method was developed for the determination by inductively coupled plasma mass spectrometry of germanium, arsenic and selenium in urine and blood after microwave acid digestion and on-line anion-exchange separation. After acid digestion, the analytes exist mainly as H2GeO3, H3AsO3, H3AsO4, H2SeO3 and H2SeO4 in the resulting sample solution. Separation of the analytes is achieved by adsorption of the analytes as anionic species on the column in relatively alkaline media with subsequent desorption of the analytes from the column as undissociated neutral species in acidic media. By loading the digested sample, adjusted to about pH 11.5, onto the column of the on-line separation system, the analytes as well as Cl and S, which may cause spectral interference in the inductively coupled plasma mass spectrometric determination, are retained on the column. In the subsequent elution step with eluent of about pH 1.6, the analytes are desorbed from the column while Cl and S are still retained. With this on-line analytical system, the determination of 72Ge and 75As could be completely free from the interference caused by 35Cl37Cl and 40Ar35Cl, respectively. By following the established microwave digestion and on-line separation process, the detection limits obtained for Ge, As and Se were as low as 0.07, 0.13 and 0.3 ng ml-1, respectively. The analytical reliability of the proposed method was evaluated by analysing commercially available urine and whole blood standards, and the results obtained were found to be in reasonably good agreement with the literature values.
- Inductively coupled plasma mass spectrometry
- On-line removal of interference