In the presented work it is proposed the development of an analytical method for sulfur determination by high-resolution continuum source graphite furnace molecular absorption spectrometry (HR-CS GF MAS). The samples were prepared by acid dissolution and the calibration standards containing sulfate, thiourea, L-cysteine were studied as a function of their different thermal stabilities and its capability for matrix matching. The HR-CS GF MAS technique is an interesting alternative for sulfur determination, since its capability to perform an interference-free analysis due to its high resolution monochromator that allows to overcome the spectral overlapping and by the use of the graphite furnace as atomizer which minimizes the matrix effects before the analytical measurement. The aim of this work is to develop an analytical method for sulfur determination in hair samples by HR-CS GF MAS, in order to evaluate the levels of this element in the human body and to compare them with the results obtained by ICP OES. The chosen conditions for pyrolysis and vaporization temperatures were 1000 C degrees and 2400 C degrees, respectively, using 800 micrograms of W as permanent modifier combined with 15 micrograms and 10 micrograms, respectively, of Pd(plus)Mg mixture as modifier in solution. The value determined for S concentration in the certified reference material NSC DC73347a (human hair) was in agreement with those reported in its certificate, as well as sulfur concentrations determined in 14 hair samples, which are in agreement with those determined by ICP-OES according to the t-paired test (95 percent level of confidence), which proves the good accuracy of the proposed method.