This research has been carried out to study the subjective symptoms related to toluene and xylene exposures in a paint manufacturing in Tehran and their relationships with the workers exposures to these solvents.This is a case-control study. Some 42 workers were selected from production sectors as case group and 43 individuals were chosen from administrative sector as the control group. Regarding work situation and the amount of pollutants exposure, the case group was divided into occupational subgroups. Totally some 175 samples were collected from individuals breathing zones by activated charcoal tubes as short and long term samples based on the standard method recommended by ASTM and NIOSH, and quantitatively determined by a gas chromatograph device. To study the subjective symptoms a reliable and valid questionnaire was used which had two parts: one was related to individual’s symptoms during the work performance and the other was concerned to the symptoms appeared outside the workplace during the previous year.The obtained results from breathing zone sampling suggested that the maximum amount of the solvents time weighted average (TWA) in the respiratory air of occupational groups in case group was equal to 76±39.9 percent of mixed threshold limit value that had no statistical significant difference with the workers exposure limit, but in other case subgroups were significantly lower than the threshold limit value (P<0.001). However in short term samples in some groups the exposure amounts were even 5 times of the mixed threshold limit vabes.The research findings revealed that during work performance there were significant relationships amongst workers exposure to toluene and xylene and the incidence of following symptoms : nasal and eye irritation, unusual odour sensation, face flashing, unusual taste (P<0.05), heavy feeling in head (P<0.005), and floating sensation(P<0.05).There were also significant relationships amongst the incidence or the following symptoms and workers exposure to toluene and xylene outside the workplace: hand skin sensitiveness (P<0.005), dyspenia, low appetite, tinnitus, feet skin sensitiveness, successive coughing (P<0.01), nightmare, anxiety, tachypenia, whole body numbness, xerostomia, skin roughness, and throat itching sensation (P<0.05).Considering the observed relationships among the symptoms and the workers exposure to the solvents, it can be concluded that the exposure limit or exposure to less than the threshold value does not guarantee safety and required measures should be done to eliminate the pollutants from workplace air. It is proposed to separate the high polluted sectors of the firm from other parts to prevent the incidence of symptoms and disorders.