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Most of reported I-III-VI2 type chalcopyrites have been developed as indispensible materials for potential application in photovoltaic solar cells, magnetism or thermoeletrics. The exploration of its photoluminescence potentials has been very limited and the chemical sensing using fluorescence to signal a recognition event is realized by way of CuFeSe2 nanocrystals. A novel solution-based synthesis strategy has been developed for the preparation of CuFeSe2 quantum dots (QDs) via oleylamine and dodecanethiol as precursors. QDs possess an intense blue luminescence at 431 nm and excitation-dependent features are recorded. The nanocrystals exhibit transformation from ferromagnetism to paramagnetism state between 4 K and 298 K. Another distinct advantage of the quantum dots will be the signaling pathway in response to external analytes. It gives rise to a rapid and selective assay of Cr2O72- through an “on-off” switching process. A linear equation can be obtained in the range from 0 to 47.5 μM and the detection limit has been determined to be 0.46 μM. This cost-effective method will pave the way for the efficient synthesis of ternary chalcopyrites and provide suitable chemical routes for sensing purposes.