Abstract
Chromatographic separation and detection of four kinds of oxoanions were investigated. Ion-exchange chromatography and ion-pair chromatography with tetrabutylammonium hydroxide (TBA-OH) and with cetyltrimethylammonium bromide (CTMA-Br) as the ion interaction reagent (IIR) were compared. By using a carbon column, 1–3 m M solution of Na 3PO 4 as the eluent, and a permanent coating technique, these oxoanions could be separated satisfactorily without any influence of common anions. A solution of CTMA-Br in water–acetonitrile was allowed to flow through a carbon column (100×4.6 mm) until equilibration. Effective ion-exchange capacity can be controlled with the water–acetonitrile ratio of the solvent in which CTMA-Br is dissolved. The ion-exchange capacity of a column was 40 μequiv. when 2 m M CTMA-Br of 25% CH 3CN solution was used for the coating. Once coated, the column could be used for a long time without complement of the IIR. UV-absorbance detection showed fairly good sensitivity. If a multi-wavelength detector is used, ion identification is more reliable. The addition of H 2O 2 to the sample solution causes the vanadate peak to elute later. As an application example, Mo, V, W, and Cr in Hastelloy C-276 and ceramic pigments were determined after decomposition with Na 2O 2 in a zirconium crucible.
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