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In order to develop new reference materials for microanalytical nuclear techniques, scanning proton microprobe(SPM) technique was used to determine homogeneity level within 100x200 μm2 micro-area on the small pieces of IAEA urban dust reference materials. The experimental methods were described in detail. The results show that IAEA-396A/M Vienna urban dust is homogeneous enough for small sample analysis of standard reference material (SRM).