A proper reference material is crucial for accurate measurement of isotope ratios. This paper deals with the preparation of a new reference material with basaltic matrix for Cu, Fe and Zn isotope measurement, which is named CAGSR-1. The substanceselected for preparation of CAGSR-1 is a certified primary standard for analysis of rock and minerals, which is named GBW07105 and composed of basaltic powder. The preparation of the new reference material was carried out strictly in accord with the stipulation of the State Metrological Technical Standard for primary reference material, which includes homogeneity and stability tests, and certification analyses. The certificated values and uncertainty at 95% confidence level are as follows: δ65CuSRM976（‰）=0.10±0.02δ56FeIRMM014（‰）=0.12±0.02；δ66ZnRomil（‰）=745 ±0.01.This newly certified reference material can be used in such aspects asthe assessment of isotope fractionation during chemical separation of geological and environmental samples, the instrumental calibration for Cu, Fe and Zn isotope measurement, and the data quality evaluation in the whole process of sample preparation and isotope measurement. 