A method is described for the determination of plutonium concentration in the presence of a bulk of other impurities by isotope dilution mass spectrometry /IDMS/ using239Pu as a spike. The method involves the addition of239Pu spike / 90 atom%/ to samples with239Pu / 70 atom%/ and vice versa. After ensuring chemical exchange between the sample and the spike isotopes, plutonium is purified by conventional anion exchange procedure in 7M HNO3 medium.239Pu/240Pu atom ratio in the purified spiked sample is determined with high precision /better than 0.1%/ using a thermal ionization mass spectrometer. Concentration of plutonium in the sample is calculated from the changes in239Pu/240Pu atom ratio in the spiked mixture. Results obtained on different plutonium samples using239Pu as a spike are compared with those obtained by the use of242Pu spike. Precision and accuracy comparable to those achieved by using242Pu are demonstrated. The method provides an alternative in the event of non-availability of enriched242Pu or244Pu required in IDMS of plutonium and at the same time, offers certain advantages over the use of242Pu or244Pu spike.