A RNAA procedure is described for the determination of trace Ir in Precambrian-Cambrian boundary samples. After irradiation, the powdered sample is transferred to a graphite crucible to expel the massive silicon with mixed acid (HF–HCl–HNO3) by heating. The residue is then fused with mixed fusion (Na2O2–NaOH) in a muffle furnace at 700°C for 15 minutes. After cooling, the fused mixture is leached with hot water. The final solution is adjusted to pH 1.5–2.0 and then passed through a column filled with thiourea type chelate resin. The resin absorbed with192Ir is measured for 4000–10 000 s by means of SCORPIO-3000 multi-channel computer — Ge(Li) detector system. Experiments with radioactive tracer are carried aout for checking radiochemical separation yield. The accuracy and precision of the method are evaluated by the analysis of U.S. geological SRMs DTS-1 and AG-Bohor-1. The method is used for the determination of trace Ir in several sets of Precambrian-Cambrian boundary samples collected from Yunnan province in China and the Ir anomaly is observed.