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Maya blue is a pigment found in different archaeological sites of different cultures from Mesoamerica, and also in colonial buildings in Mexico and Cuba. The pigment is made from a thermally treated mixture of indigo and palygorskite. Pigment samples from Aztec and non‐Aztec archaeological sites as well as reference Yucatecan palygorskites were studied in this paper to assess their differences. The characterization of the samples was carried out by a combination of a crystal–chemical‐point analyses using electron microscopy to obtain the structural formulae of the palygorskite crystals, and studied using high‐resolution X‐ray diffraction. The data show evidence that the palygorskite used by non‐Aztec cultures, such as the Maya, is compatible with palygorskite from known sources in the Yucatan Peninsula, while the palygorskite used by the Aztec culture is different in its structure and has an origin that is still unknown. [ABSTRACT FROM AUTHOR]