RESUMO
Pyrohydrolysis is a well-established separation method, and it is being used as a sample preparation method for several materials for further determination of non-metals such as halogens, boron, and sulfur. Analytes are retained in a diluted solution that is suitable for carrying out analysis by several determination techniques and minimizing the use of concentrated reagents. Pyrohydrolysis separation of metals has not been reported yet. The present study demonstrates the pyrohydrolysis separation of Mo as MoO4(2-) from uranium materials and its subsequent determination using ion chromatography coupled with suppressed conductivity detector. With use of TGA and XRD the volatilization behavior of Mo was studied. Important parameters for the pyrohydrolysis method required for the quantitative separation of Mo were evaluated. The precision of the method was better than 5% at 25 ppm of Mo. The accuracy was evaluated by analysis of a CRM (U3O8-ILCE-IV). The method was applied to determine Mo in ammonium diuranate samples, where the conventional methods suffer from the loss of Mo.