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The purpose of this study was to develop an instrument performance assessment tasks and rubrics in conventional titration (asidi-alkalimetri, argentometry, permanganometry, complexometry, iodometry). The Instrument has several skills, they are weighing, making solution, titrant preparation, pipette, and titration. This study using four phases based on Development and Validation methods are: preliminary study, instrument development, validation, and field testing. Phase 1, describe purpose of study and identification titration skill. Phase 2, development tasks and rubrics for assess performance of students. Phase 3, instrument was validated by five validators and then instrument was revised and modified become valid instrument with CVI=0.98. Phase 4, field testing was conducted at Vocational School Chemical Analysis program in Bandung with 30 students were divided into three groups assessed by four observers using the inter-rater method with statistical measurements are Intra-class correlation coefficient (ICC) and Krippendorff-s alpha (Kalpha). First group consisted five students has reliability value are ICC=0.92 and Kalpha=0.96, second group 10 students has reliability value are ICC=0,85 and Kalpha=0.80, and third group 15 students has reliability value are ICC=0.75 and Kalpha=0.66. Result of data analyisis can be concluded instrument has been developed are valid and reliable. Reliability in small group has higher than other group.