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In this study, a new Ti3C2Tx‐coated fiber was synthesized and utilized as coatings for solid‐phase microextraction of seven polychlorinated biphenyls. The as‐produced multilayered Ti3C2Tx MXene was characterized by X‐ray diffractometer, thermos‐gravimetric analysis, scanning electron microscopy, and energy dispersive spectroscopy. It is noteworthy that the Ti3C2Tx showed some attractive features including...