Improvements in the sample preparation for the determination of ruthenium in catalysts by different spectrometric...

The sample preparation steps of two analytical methods for the determination of ruthenium in carbon supported catalysts with flame atomic absorption spectrometry (FAAS) or UV-vis spectrophotometry, were carefully optimised. As a first step, the carbon support is ignited in air at 450 degrees C then the residue is fused with potassium hydroxide and potassium nitrate to convert ruthenium into ruthenate anion RuO4(2-). The melt is dissolved in water with potassium persulphate and potassium hydroxide as stabilisers. Ruthenium may be directly estimated by measuring the UV-vis molecular absorption of ruthenate at the isosbestic point of the ruthenate-perruthenate mixture or by FAAS. In the latter case, an aliquot of the sample solution is added to the concentrated hydrochloric acid to obtain hexachlororuthenate RuCl6(2-), that is nebulized into the flame after proper dilution. This novel procedure allows to determination of ruthenium without the sensitivity loss (-66%) which occurs in the alkaline media resulting from the fusion. The relative standard deviation is 1.1% for FAAS and 1.3% for UV-vis, at 5% Ru (n = 7). The detection limit (3sB) is 0.07% Ru for FAAS and 0.02% Ru for UV-vis. Both methods were applied to the analysis of a commercial sample and a statistical comparison was carried out.