Abstract: Through the experiments of sampling, sizegrading, screening, splitting and homogeneity test for the native copper ore samples from northeast Yunnan province, a sample processing procedure was established. After rough and medium crushing and screening out the grains with grain size 2 mm screen (>95% is native copper), the sample was rod grinded, passing through 0.246 mm（60 mesh） screen, splitting and prepared to 0.074 mm（200 mesh）. Atomic absorption spectrometry, iodimetry and iodinefluorine methods were selected for copper analysis with good accuracy, reliability and economical efficiency.