Abstract: This paper describes the quantitative determination of Fe, Ni, Sr, Mo, Ba, Pb in hair standard material by isotope dilution spark soruce mass spectrometry. The sensitivity of this method is about n ppb. The precision is better than 5%, and the accuracy is better than 8%. Several methods to deal with the sample, choice of spectrum and the best adding amount of tracer agent are studied. An extremely effective method of forming small amount sample into electrode has also been discussed.