A membrane deposition–laser ablation sampling system was developed, in which the generated dry aerosol was introduced into an inductively coupled plasma mass spectrometer (ICP-MS). Based on this system, a micro-sampling method was established for the determination of gadolinium (Gd), dysprosium (Dy), and ytterbium (Yb) in high-purity cerium oxide. The gas composition in the ablation cell, carrier-gas flow rates, and laser spot sizes were systematically optimized. Carrier gas 1 was argon (Ar) at 1.0 L/min, and carrier gas 2 was helium (He) at 1.1 L/min. An optical aperture diameter of 2.75 mm was found to provide optimal performance. The membrane-deposition efficiency was evaluated from the ratio of the generated analyte mass to the mass determined post-deposition by ICP-MS/MS. Results showed that when the sampling volume was 100 μL and the cerium (Ce) matrix concentration exceeded 100 mg/L, the deposition efficiency approached 100 %. Internal-standard correction was applied to minimize fractionation and matrix effects, and the most suitable internal standards were identified. Under these optimized conditions, the detection limits for Gd, Dy, and Yb were 0.52, 0.18, and 0.21 ng/g, respectively. Analysis of three high-purity CeO2 samples showed that this method produced significantly lower Gd and Yb values than conventional ICP-MS, effectively eliminated hydroxide and oxide interferences, exhibited superior resistance to spectral interference, and provided results consistent with those from ICP-MS/MS.


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