Two luminescent coordination polymers (CPs), {[Cd2L2(H2O)4]·H2O}n (1) and {[Zn2L2(H2O)4]·H2O}n (2) (H2L = 5-(1H-1,2,4-triazol-1-yl)isophthalic acid) are reported herein. The CPs reveal readily dispersible two-dimensional (2D) layer structures with considerable stability in aqueous media within a wide pH range (pH = 2-12). Sensing experiments indicate that they can serve as highly selective and sensitive fluorescent probes toward CrVI-anions (CrO42- and Cr2O72-).