Two sets of calibration standards for134Cs and137Cs were prepared by small serial dilution of a natural matrix standard reference material, IAEA-154 whey powder. The first set was intended to screen imported milk powders which were suspected to be contaminated with134Cs and137Cs. Therefore the concentration range of the calibration standards were about 40–400 Bq/kg. The precision of the preparation of the standard with about 7 Bq/kg of134Cs and 39 Bq/kg of137Cs at measurement time was 7.4% and 3.2%, respectively. The preparation of a similar standard by spiking the matrix with radioisotope solutions resulted in a poorer precision, about double that of the former technique. The other set of calibration standards was prepared to measure the environmental levels of137Cs in commercial Venezuelan milk powders. Their concentration ranged from 3–10 Bq/kg of137Cs. The accuracy of these calibration curves was checked by using IAEA-152 and A-14 milk powders. Their measured values were in good agreement with their certified values. Finally, it is shown that these preparation techniques by serial dilution of a standard reference material were simple, rapid, precise, accurate and cost-effective.