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The application of gas chromatography (GC) to the analysis of lanthanides as mixed ligand complexes with hexafluoroacetylacetone (HFAA) and tri- n -octylphosphine oxide (TOPO) is investigated. Thermogravimetric studies indicate that these complexes are volatile without decomposition at low temperature (100–200°C). The volatility of mixed chelates is found to increase with the decreasing radius of the trivalent lanthanide ion. Trivalent lanthanide ions are found to be quantitatively extractable with HFAA, a neutral donor, and TOPO as a mixed ligand complex in the pH range 2–7. The organic extract can be directly fed into a GC for separation and estimation. The optimum conditions for the estimation of lanthanides using GC are established. Chromatograms of lanthanides at different concentration ratios illustrate the possibility of the estimation of one lanthanide ion when as much as a 10-fold excess of other lanthanide ions is present in a mixture. Calibration curves of each of the individual lanthanides and their mixtures are studied in the concentration range 0.2–25 µg/mL

journal of chromatographic science

Separation and Estimation of Lanthanides as Mixed-Ligand Complexes with Hexafluoroacetylacetone and Tri- n -octylphosphine Oxide Using Solvent Extraction and Gas Chromatography