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Two-tier multiple choice instrument is an instrument consisting of two tiers, the first tier is the choice of the answer from a question and the second tier is the choices of reason for an answer at the first level. The two-tier instrument can be used to measure students-science process skill. This study aims to analyze contents validity two-tier instument multiple choice to measure students- thinking skills in a statistics fluid. The method used in this research is a descriptive analyze a method for content validation based on Formula Aikens. Data of content validation was obtained from 8 experts, consisting of 4 lecturers who had doctorates and 4 high school physics teacher of the senior high school in Madiun. Based on the results and discussion, can be concluded that 14 item question of multiple choices instrument to measure students science process skills in heat and temperature are declared valid based on Aiken Validity.