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A combined synchrotron powder diffraction and vibrational study of the thermal treatment of palygorskite–indigo to produce Maya blue

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Abstract

The heating process (30–200 °C) of a palygorskite-indigo mixture has been monitored in situ and simultaneously by synchrotron powder diffraction and Raman spectroscopy. During this process, the dye and the clay interact to form Maya blue (MB), a pigment highly resistant to degradation. It is shown that the formation of a very stable pigment occurs in the 70–130 °C interval; i.e., when palygorskite starts to loose zeolitic water, and is accompanied by a reduction of the crystallographic a parameter, as well as by alterations in the C=C and C=O bonds of indigo. Mid- and near-infrared spectroscopic work and microporosity measurements, employed to study the rehydration process after the complex formation, provide evidence for the inhibition of the rehydration of MB as compared with palygorskite. These results are consistent with the blocking of the palygorskite tunnel entrance by indigo molecules with a possible partial penetration inside the tunnels. The surface silanols of palygorskite are not perturbed by indigo, suggesting that MB is not a surface complex.

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References

  1. 1.

    Arnold DE, Bohor BF (1975) Archaeology 28:23

  2. 2.

    Gettens RJ (1962) Am Antiquity 7(4):557

  3. 3.

    Shepard AO (1962) Am Antiquity 27:565

  4. 4.

    Gómez-Romero P, Sanchez C (2005) N J Chem 29:57

  5. 5.

    Doménech A, Doménech-Carbo MT, Vázquez de Agredos Pascual ML (2006) J Phys Chem B 110(12):6027

  6. 6.

    Hubbard B, Kuang W, Moser A, Facey GA, Detellier C (2003) Clays Clay Miner 51(3):318

  7. 7.

    Reinen D, Köhl P, Müller C (2004) Zeitschrift für anorganische und allgemeine Chemie 630(1):97

  8. 8.

    Sanchez del Rio M, Martinetto P, Reyes-Valerio C, Dooryhée E, Suárez M (2006) Archaeometry 48(1):115

  9. 9.

    Bauer H, Kowski K, Kuhn H, Lüttke W, Rademacher P (1998) J Mol Struct 445(1–3):277

  10. 10.

    Klessinger M (1982) Dyes Pigm 3:235

  11. 11.

    Süsse P, Steins M, Kupcik V (1988) Z Kristallogr 184:269

  12. 12.

    Chryssikos GD, Gionis V, Kacandes GH, Stathopoulou ET, Suarez M, Garcia-Romero E, Sanchez del Rio M (2009) Am Miner 94(1):200

  13. 13.

    Chiari G, Giustetto R, Ricchiardi G (2003) Eur J Miner 15(1):21

  14. 14.

    Chisholm JE (1992) Can Miner 30:61

  15. 15.

    Post JE, Heaney PJ (2008) Am Miner 93(4):667

  16. 16.

    Van Olphen H (1966) Science 154:645

  17. 17.

    Kleber R, Masschelein-Kleiner R, Thissen J (1967) Stud Conserv 12(2):41

  18. 18.

    Chianelli RR, Perez De la Rosa M, Meitzner G, Siadati M, Berhault G, Mehta A, Pople J, Fuentes S, Alonzo-Nunez G, Polette LA (2005) J Synchrotron Radiat 12(2):129

  19. 19.

    Chiari G, Giustetto R, Druzik J, Doehne E, Ricchiardi G (2008) Appl Phys A Mater Sci Process 90(1):3

  20. 20.

    Fuentes ME, Contreras BPC, Montero AL, Chianelli R, Alvarado M, Olivas R, Rodríguez LM, Camacho H, Montero-Cabrera LA (2008) Int J Quantum Chem 108(10):1664

  21. 21.

    Manciu FS, Reza L, Polette LA, Torres B, Chianelli RR (2007) J Raman Spectrosc 38(9):1193

  22. 22.

    Polette-Niewold LA, Manciu FS, Torres B, Alvarado M Jr, Chianelli RR (2007) J Inorg Biochem 101(11–12):1958

  23. 23.

    Fois E, Gamba A, Tilocca A (2003) Microporous Mesoporous Mater 57(3):263

  24. 24.

    Giustetto R, Levy D, Chiari G (2006) Eur J Miner 18:629

  25. 25.

    Giustetto R, Llabrés i Xamena FX, Ricchiardi G, Bordiga S, Damin A, Gobetto R, Chierotti MR (2005) J Phys Chem B 109(41):19360

  26. 26.

    Tilocca A, Fois E (2009) J Phys Chem C 113(20):8683

  27. 27.

    Doménech A, Doménech-Carbó MT, Sánchez del Río M, Vázqued de Agredos Pascual ML (2009) J Solid State Electrochem 13:869

  28. 28.

    Doménech A, Doménech-Carbó MT, Vázqued de Agredos Pascual ML (2007) J Solid State Electrochem 11(9):1335

  29. 29.

    Doménech A, Doménech-Carbo MT, Vázquez de Agredos Pascual ML (2007) J Phys Chem C 111(12):4585

  30. 30.

    Doménech A, Doménech-Carbo MT, Vázquez de Agredos Pascual ML (2007) Anal Chem 79(7):2812

  31. 31.

    Doménech A, Doménech-Carbó MT, Sánchez del Río M, Goberna S, Lima E (2009) J Phys Chem C 113:12118

  32. 32.

    Doménech A, Doménech-Carbo MT, Sánchez del Río M, Vázquez de Agredos Pascual ML, Lima E (2009) N J Chem. doi:10.1039/b901942a

  33. 33.

    Boccaleri E, Carniato F, Croce G, Viterbo D, van Beek W, Emerich H, Milanesio M (2007) J Appl Crystallogr 40(4):684

  34. 34.

    Sanchez del Rio M, Suarez M, Garcia-Romero E (2009) Archaeometry 51(2):214

  35. 35.

    Reyes-Valerio C (1993) De Bonampak al Templo Mayor. El azul maya en Mesoamerica. Colección America Nuestra, vol 40. Siglo XXI Editores, Mexico D.F., p 157

  36. 36.

    Gionis V, Kacandes GH, Kastritis ID, Chryssikos GD (2006) Am Miner 91:1125

  37. 37.

    Suarez M, Garcia Romero E, Sanchez del Rio M, Martinetto P, Dooryhee E (2007) Clay Miner 42:287

  38. 38.

    Hayashi H, Otsuka R, Imai N (1969) Am Miner 53:1613

  39. 39.

    VanSoyoc GE, Serna CJ, Ahlrichs JL (1979) Am Miner 64:215

  40. 40.

    McKeown DA, Post JE, Etz ES (2002) Clays Clay Miner 50(5):667

  41. 41.

    Witke K, Brzezinka K-W, Lamprecht I (2003) J Mol Struct 661–662:235

  42. 42.

    Sanchez del Rio M, Picquart M, Haro-Poniatowski E, van Elslande E, Uc VH (2006) J Raman Spectrosc 37:1053

  43. 43.

    Tatsch E, Schrader B (1995) J Raman Spectrosc 26(6):467

  44. 44.

    Nagasawa Y, Taguri R, Matsuda H, Murakami M, Ohama M, Okada T, Miyasaka H (2004) Phys Chem Chem Phys 6:5370

  45. 45.

    Leona M, Casadio F, Bacci M, Picollo M (2004) JAIC 43:39

  46. 46.

    Gionis V, Kacandes GH, Kastritis ID, Chryssikos GD (2007) Clays Clay Miner 55:543

  47. 47.

    Jones BF, Galán E (1998) In: Bailey SW (ed) Hydrous phyllosilicates (exclusive of micas). Mineralogical Society of America, USA

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Acknowledgements

We acknowledge the ESRF for beamtime used for this experiment, and the experimental staff of BM01B for technical support and helpful discussions. Financial support from the Spanish CICYT (project CGL2006-09843) and Italian PRIN edition 2007 is also acknowledged.

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Correspondence to Manuel Sánchez del Río.

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Sánchez del Río, M., Boccaleri, E., Milanesio, M. et al. A combined synchrotron powder diffraction and vibrational study of the thermal treatment of palygorskite–indigo to produce Maya blue. J Mater Sci 44, 5524–5536 (2009) doi:10.1007/s10853-009-3772-5

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Keywords

  • Raman Spectrum
  • Indigo
  • Sepiolite
  • Attapulgite
  • Tunnel Entrance