Abstract: This study assessed the extent of senior secondary school student’:s acquisition of science process skills in volumetric analysis in Ondo State, Nigeria. Two research questions and one null hypothesis guided the study. The study adopted a descriptive survey design. A sample of 240 students was used for the study. The instrument used for data collection was a 20-item rating scale. The research questions were answered using means while the hypothesis was tested using t-test statistic. The findings revealed that the level of senior secondary school student’s acquisition of science process skills in volumetric analysis is low. Also, it was revealed that senior secondary school male students demonstrated high level of science process skills acquisition in volumetric analysis than female students. The need for training chemistry teachers on science process skills is recommended in order to make their teaching more practical oriented.