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Synthesis and Fading of Eighteenth-Century Prussian Blue

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Synthesis and Fading of Eighteenth-Century Prussian Blue Missouri University of Science and Technology Scholars' Mine Chemistry Faculty Research & Creative Works Chemistry 01 May 2013 Synthesis and Fading of Eighteenth-century Prussian Blue Pigments: A Combined Study by Spectroscopic and Diffractive Techniques Using Laboratory and Synchrotron Radiation Sources Louise Samain Fernande Grandjean Missouri University of Science and Technology, [email protected] Gary J. Long Missouri University of Science and Technology, [email protected] Pauline Martinetto et. al. For a complete list of authors, see https://scholarsmine.mst.edu/chem_facwork/801 Follow this and additional works at: https://scholarsmine.mst.edu/chem_facwork Part of the Chemistry Commons Recommended Citation L. Samain et al., "Synthesis and Fading of Eighteenth-century Prussian Blue Pigments: A Combined Study by Spectroscopic and Diffractive Techniques Using Laboratory and Synchrotron Radiation Sources," Journal of Synchrotron Radiation, vol. 20, no. 3, pp. 460-473, International Union of Crystallography (IUCr), May 2013. The definitive version is available at https://doi.org/10.1107/S0909049513004585 This Article - Journal is brought to you for free and open access by Scholars' Mine. It has been accepted for inclusion in Chemistry Faculty Research & Creative Works by an authorized administrator of Scholars' Mine. This work is protected by U. S. Copyright Law. Unauthorized use including reproduction for redistribution requires the permission of the copyright holder. For more information, please contact [email protected]. research papers Journal of Synchrotron Synthesis and fading of eighteenth-century Prussian Radiation blue pigments: a combined study by spectroscopic ISSN 0909-0495 and diffractive techniques using laboratory and synchrotron radiation sources Received 4 January 2013 Accepted 16 February 2013 Louise Samain,a*‡2Fernande Grandjean,b,c Gary J. Long,c Pauline Martinetto,d Pierre Bordet,d Jana Sanyovae and David Strivaya aCentre Europe´en d’Arche´ome´trie, University of Lie`ge, Sart Tilman B15, Lie`ge 4000, Belgium, bFaculty of Sciences, University of Lie`ge, Sart Tilman B5, Lie`ge 4000, Belgium, cDepartment of Chemistry, Missouri University of Science and Technology, University of Missouri, Rolla, MO 65409-0010, USA, dInstitut Ne´el, CNRS et Universite´ Joseph-Fourier, BP 166, 38042 Grenoble, France, and eInstitut Royal du Patrimoine Artistique, Parc du Cinquantenaire 1, Brussels 1000, Belgium. E-mail: [email protected] Prussian blue, a hydrated iron(III) hexacyanoferrate(II) complex, is a synthetic pigment discovered in Berlin in 1704. Because of both its highly intense color and its low cost, Prussian blue was widely used as a pigment in paintings until the 1970s. The early preparative methods were rapidly recognized as a contributory factor in the fading of the pigment, a fading already known by the mid- eighteenth century. Herein two typical eighteenth-century empirical recipes have been reproduced and the resulting pigment analyzed to better understand the reasons for this fading. X-ray absorption and Mo¨ssbauer spectroscopy indicated that the early syntheses lead to Prussian blue together with variable amounts of an undesirable iron(III) product. Pair distribution functional analysis confirmed the presence of nanocrystalline ferrihydrite, Fe10O14(OH)2, and also identified the presence of alumina hydrate, Al10O14(OH)2,witha particle size of 15 A˚ . Paint layers prepared from these pigments subjected to accelerated light exposure showed a tendency to turn green, a tendency that was often reported in eighteenth- and nineteenth-century books. The presence of particles of hydrous iron(III) oxides was also observed in a genuine eighteenth- century Prussian blue sample obtained from a polychrome sculpture. # 2013 International Union of Crystallography Keywords: iron(III) hexacyanoferrate(II); archaeometry; pair distribution function; Printed in Singapore – all rights reserved light exposure fading; paint layers. 1. Introduction or Na+. Its intense blue color arises from an intervalence electron transfer between the iron(II) and iron(III) ions when The restoration of cultural heritage objects requires a good light is absorbed at 700 nm. understanding of the various long-term degradation processes Because of its low cost and its extremely high tinting of the materials used in paintings and related artistic efforts. strength, Prussian blue was widely used by artists from 1720 The interactions between pigments, binders and supports need until 1970 (Berrie, 1997). However, reports of the discolora- to be investigated in order to understand any possible tion or fading of Prussian blue pigments had already been alterations with time. In this context Prussian blue is a parti- noted in eighteenth-century and nineteenth-century books cularly interesting artistic pigment because of its popularity (Me´rime´e, 1830; Riffault, 1850; Regnier, 1855). Even though among artists and its variable light fastness, a fastness that had the preparative methods of the Prussian blue pigments were already been questioned by the mid-eighteenth century. rapidly recognized as a contributory factor in their fading Prussian blue was accidentally discovered in Berlin in 1704. (Kirby, 1993), to date, little attention has been devoted to It is now known to contain a hydrated iron(III) hexacyano- obtaining a scientific understanding of the intrinsic degrada- ferrate(II) anion, {FeIII[FeII(CN) ].xH O}À, with varying 6 2 tion processes associated with Prussian blue pigments in paint x + + values of up to 16, and with various cations, such as K ,NH4 layers (Kirby & Saunders, 2004; Samain et al., 2011, 2013). ‡ Present address: Department of Materials and Environmental Chemistry, Only two reagents are essential in the production of Prus- Stockholm University, Svante Arrhenius va¨g 16C, Stockholm 10691, Sweden. sian blue pigments by precipitation, an iron salt and an alkali 460 doi:10.1107/S0909049513004585 J. Synchrotron Rad. (2013). 20, 460–473 research papers hexacyanoferrate. However, the chemical stoichiometry and Table 1 structure of the starting materials and the resulting Prussian Reagent proportions for the two eighteenth-century recipes. blue pigments were unknown in the eighteenth century. At Reagents proportion in parts that time potassium hexacyanoferrate was indirectly obtained Alum, from the calcination of animal matter with an alkali. The Dried Alkali, Iron salt, KAl(SO4)2 Acid, residue of this calcination was boiled in water yielding, after Synthesis blood K2CO3 FeSO4.7H2O .12H2O HCl filtration, a pale yellow solution that presumably contained Dossie 3 1 1 2 4 or 0 potassium hexacyanoferrate. This solution was then mixed Le Pileur d’Apligny 8 8 3 4 4 or 0 with a solution of an iron(II) salt and alum, leading to the formation of a pale greenish precipitate that was filtered and, supplementary material.1 The major difference between the finally, treated with hydrochloric acid to yield Prussian blue. two methods is the proportion of the ingredients used (see In the mid-nineteenth century it became possible to Table 1). produce potassium hexacyanoferrate in bulk from gas purifi- In the above syntheses, dried blood that is sold and used cation products (Krafft, 1854). Consequently, Prussian blue as a garden fertilizer by DCM Corporation, Grobbendonk, pigments could be manufactured by a completely inorganic Belgium, was used as the organic matter. All other reagents process; these preparative methods are usually referred to as used herein for the syntheses of eighteenth-century Prussian modern methods in order to distinguish them from the blue pigments were of reagent-grade quality and obtained eighteenth-century methods that used an organic starting from Sigma-Aldrich, Steinheim, Germany. material. The modern inorganic manufacturing methods were Appropriate amounts of dried blood and potassium rapidly standardized and industrialized, a process that rapidly carbonate, K2CO3, were mixed in a porcelain crucible and led to the production of inexpensive high-quality Prussian heated in a Nabertherm furnace; the temperature was blue pigments (Buxbaum & Pfaff, 2005). increased from room temperature to 923 K in two hours. The The composition and quality of Prussian blue pigments mixture initially burned with an orange flame. At 723 K, after synthesized according to the early eighteenth-century 90 min heating, the crucible was removed from the furnace methods were much more variable because of the rather and its contents mixed. Upon further heating to 923 K, no empirical character of the process. Ingredients and their further combustion was observed and the contents of the proportions used in the eighteenth-century recipes have been crucible were reddish. The crucible was then removed from studied and indexed in detail by Kirby & Saunders (2004) and the furnace and the contents were dropped into 300 ml of Asai (2005). However, neither the underlying chemical reac- boiling deionized water and the mixture was subsequently tions nor the interactive factors that influenced the light boiled for 45 min. After filtration, the pale yellow filtrate was fastness of the pigments made in the eighteenth-century have collected and mixed with an aqueous solution of iron sulfate, been identified. FeSO4.7H2O, and alum, KAl(SO4)2.12H2O, previously Herein, Prussian blue pigments have been synthesized dissolved in deionized water. A pale-greenish precipitate according to two eighteenth-century recipes. The resulting immediately formed and was collected by filtration. A
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