New hints on Maya Blue formation process by PCA-assisted in situ XRPD/PDF and optical spectroscopy

Caliandro, Rocco; Toson, Valentina; Palin, Luca; Conterosito, Eleonora; Aceto, Maurizio; Boccaleri, Enrico; Gianotti, Valentina; Dooryhee, Eric; Milanesio, Marco

doi:10.1002/chem.201901932

Title: New hints on Maya Blue formation process by PCA-assisted in situ XRPD/PDF and optical spectroscopy

Journal Article · 25 June 2019 · Chemistry - A European Journal

DOI: https://doi.org/10.1002/chem.201901932 · OSTI ID:1543407

Caliandro, Rocco ^[1]; Toson, Valentina ^[1]; Palin, Luca ^[1]; Conterosito, Eleonora ^[1]; Aceto, Maurizio ^[1]; Boccaleri, Enrico ^[1]; Gianotti, Valentina ^[1]; Dooryhee, Eric ^[2]; Milanesio, Marco ^[1]

Univ. del Piemonte Orientale, Alessandria (Italy)
Brookhaven National Lab. (BNL), Upton, NY (United States)

The exact recipe to prepare the ancient Maya Blue (MB), an incredibly resistant and brilliant pigment prepared from indigo (dye) and Paligorskite (clay), is lost to the ages. To unravel the key features of the MB formation process, several inorganic-dye couples were heated to 200°C and cooled to RT, to investigate their reactivity and the diffusion and degree of sequestration of the dye into the inorganic host. In situ XRPD/PDF and fiber optic reflectance spectroscopy (FORS) data, sided by TGA, provided a comprehensive overview on MB formation mechanism. XRPD/PDF gave information on long/short range behaviors of water desorption/adsorption and indigo sequestration, while TGA and in situ FORS gave information on mass and optical changes within temperature. Ex situ dye removal was used to understand the sample stability after the thermal treatments. A statistical approach based on Principal Component Analysis was exploited to efficiently and jointly analyze the ~3000 collected patterns. MB formation starts below 110°C with disordered distribution of indigo within the channels, reaching maximum reaction speed and higher ordering at 150°C. Above 175°C, color changes and a stronger sequestration of indigo into framework channels are observed, while the affinity for water is dramatically reduced. The origin of different colors, hues and stability in historical MB samples can then explained in term of different thermal history of the starting mechanical indigo-palygorskite mixture.

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Research Organization:: Brookhaven National Laboratory (BNL), Upton, NY (United States)

Sponsoring Organization:: USDOE Office of Science (SC), Basic Energy Sciences (BES)

Grant/Contract Number:: SC0012704

OSTI ID:: 1543407

Report Number(s):: BNL-211886-2019-JAAM

Journal Information:: Chemistry - A European Journal, Vol. 25, Issue 49; ISSN 0947-6539

Publisher:: ChemPubSoc EuropeCopyright Statement

Country of Publication:: United States

Language:: English

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