The determination of trace elements, particularly rare earth elements, in uranium ore concentrates (UOCs) is important as the pattern can be indictive ore characteristics. Presented here is a methodology for accurately quantifying rare earth elements (REE) in UOCs. To improve the measurement uncertainty, isotope dilution mass spectrometry (IDMS) was utilized over other quantification techniques such as external calibration or standard addition. The isotopic determinations were measured by inductively coupled plasma-mass spectrometry (ICP-MS). To obtain high-fidelity isotopic measurements, separation of the REE from the uranium matrix was achieved by high-performance ion chromatography (HPIC), reducing the isobaric interferences. After separation, the target analytes were analyzed in two different modalities. For high precision analysis, the separated analytes were collected and measured by ICP-MS in an “offline” fashion. For a rapid approach, the separated analytes were sent directly into an ICP-MS for “online” analysis. These methods have been demonstrated to accurately quantify the REE content in a well-characterized UOC sample.