This study investigated the relationship between conceptual understanding of inorganic Analysis and performance in volumetric analysis among secondary school students in Kafachan, Nigeria. The sample consisted of a total of 75 students drawn from five secondary schools in Kafanchan zone. The samples were randomly selected using balloting. Two instruments were used for data collection, Test of Understanding of Qualitative Analysis (TUQA) and Test of Practical Skill (TOPS). TUQA was first administered after which TOPS was administered. The Data collected were analysed and the hypotheses stated were tested using pearsons product moment correlation and t-test statistical techniques at 0.05 level of significance. The major findings revealed that significant relationship exist between students? conceptual knowledge of inorganic chemistry qualitative analysis and performance in volumetric analysis. It also revealed that there is no significant difference between students? performance in Qualitative Analysis and volumetric analysis. The study also revealed that there is no significant difference between the performance of male and female students in conceptual understanding of inorganic chemistry qualitative analysis. The researcher recommended that effort should be made to ensure that attention is given to conceptual instruction to enhance meaningful learning of qualitative analysis concepts. Based on this it was concluded that, conceptual knowledge of qualitative analysis relates high with the performance of students in volumetric analysis.