Composition and microstructure of the lead white pigment in Masters paintings using HR Synchrotron XRD

González, Víctor; Calligaro, Thomas; Wallez, Gilles; Eveno, Myriam; Toussaint, Kathleen; Menu, Michel

doi:10.1016/j.microc.2015.11.005

Cited by 50 publications

(44 citation statements)

References 18 publications

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“…1488–1576) but owing to temporal and spatial distances between the two painters, they may have used different techniques. For what concerns Dutch Golden Age paintings, Rembrandt used materials traditionally available on the 17th century Dutch color market, namely the lead white pigment (a mixture of hydrocerussite Pb 3 (CO 3 ) 2 (OH) 2 (HC) and cerussite PbCO 3 (C) obtained by corrosion of metallic lead in acetic acid vapor‐ and CO 2 ‐rich conditions) and small amounts of organic media (mainly linseed oil) . However, the precise recipe that Rembrandt used to obtain his characteristic impastos from those constituents still remains unknown.…”

Section: Figurementioning

confidence: 99%

Unraveling the Composition of Rembrandt's Impasto through the Identification of Unusual Plumbonacrite by Multimodal X‐ray Diffraction Analysis

et al. 2019

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Rembrandt (1606–1669) is renowned for his impasto technique, involving his use of lead white paint with outstanding rheological properties. This paint was obtained by combining lead white pigment (a mixture of cerussite PbCO3 and hydrocerussite Pb3(CO3)2(OH)2) with an organic binding medium, but the exact formulation used by Rembrandt remains a mystery. A powerful combination of high‐angle and high‐lateral resolution x‐ray diffraction was used to investigate several microscopic paint samples from four Rembrandt masterpieces. A rare lead compound, plumbonacrite (Pb5(CO3)3O(OH)2), was detected in areas of impasto. This can be considered a fingerprint of Rembrandt's recipe and is evidence of the use of an alkaline binding medium, which sheds a new light on Rembrandt's pictorial technique.

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Section: Figurementioning

confidence: 99%

Unraveling the Composition of Rembrandt's Impasto through the Identification of Unusual Plumbonacrite by Multimodal X‐ray Diffraction Analysis

et al. 2019

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“…'Lead white', also named 'ceruse' has been synthesized since antiquity. The generic term 'lead white' refers to different pigments with varying compositions and microstructures, including mainly hydrocerussite (2PbCO 3 ,Pb(OH) 2 ) and cerussite (PbCO 3 ) in various proportions (Welcomme et al, 2007;Gonzalez et al, 2016). Its continued presence over centuries reflects its continued use in paintings.…”

Section: Identification Of Metal Soaps In Paintings: a Dramatic Evolumentioning

confidence: 99%

Lead soaps in paintings: Friends or foes?

Cotte

Checroun

Nolf

et al. 2016

Studies in Conservation

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The origin(s) and role(s) of metal soaps in paints are a worldwide concern today. These hybrid compounds, containing both fatty acid chains and metals associated with a carboxylate function, are increasingly identified in paints. As reviewed in the first part of this work, the presence of metal soaps in paints is differently interpreted in scientific publications: metal soaps are sometimes considered to play a positive role as anchor points, during paint drying processes; they can also be considered as responsible for many degradation processes (protrusions, efflorescences, darkening, etc.). Their origins are also interpreted in various ways. In some paintings (in particular from the twentieth century), they have sometimes introduced on purpose, as additives, to modify the physical properties of the painting materials. In older paintings, metal soaps are usually thought to result from an uncontrolled reaction of oil with lead-based pigments, in particular lead white, red lead, and lead tin yellow. In the second part of this work, the review of historical recipes of lead-based paint shows an important number of recipes based on controlled mixing of oil with lead driers. In the third part, the experimental reproduction of such traditional recipes using walnut oil and litharge (PbO) shows that lead soaps can be formed, both in about one hour at ∼100°C, or in about one month at room temperature. It shows as well that after a few years, litharge is no longer detected in the paint medium, while different lead carbonates are. Finally, the micro-infrared spectroscopy and micro-X-ray diffraction re-analysis of protrusions from a nine-year model painting shows together with lead soaps, the presence of Pb 5 (CO 3 ) 3 (OH) 2 O ('synthetic plumbonacrite'), an unusual phase recently observed in a protrusion from a painting by Vincent Van Gogh. This work highlights (i) the multiple origins and roles of metal soaps in paints and (ii) the importance of combining the analysis of fragments from historical paintings with the analysis and reproduction of historical recipes. In particular, we show that the components detected today in historical paintings may severely differ from those originally used or prepared by the painter, complicating the assessment of the painter's intentions. More than the presence of metal soaps, the key questions to be tackled should be about their origins and (re)mobilization.

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“…Laboratory reconstructions of ancient synthesis processes and of post-synthesis treatments permitted an investigation of their effects on the composition and microstructure of the pigment. [22] For example,h eatingt he pigmenti nw ater induces the transformation of cerussite into hydrocerussite, with the newly formed hydrocerussite crystallites exhibiting large sizes (dimensions up to 5 mm insteado f< 1 mm without this process). Conversely, the treatmentw ith an acidic solution (such as vinegar) leads to the formationo fs mall( < 100 nm) cerussite crystallites,f ollowing ar ecrystallization process.S R-mXRD andM A-XRPD both allow to estimate the hydrocerussite to cerussite ratios and the dimensions of crystallites in microsamples or paintings, thus revealing the variousg rades of lead white used by the Old Masters, such as Vermeer.…”

Section: Impurities In Natural Compoundsmentioning

confidence: 99%

“…This technique was recently employedt oc haracterize different lead white pigments amples. [22] It usually relies on millimetric X-ray beamsa nd ac ontinuous rotationo ft he sample, which makes it incompatible with X-ray microscopy.U sing XRD microscopes, the angular resolution of the diffraction signals is usually much poorer (for experimental reasons) and the beam size can be comparable to the crystallite size leading to discrete diffraction spots (Figure 2b). In this case, Scherrer broadening mays till be qualitatively estimated by averaging 2D diffractionp atterns from al arge number of pixels over areas of similar composition.…”

Section: Impurities In Natural Compoundsmentioning

confidence: 99%

X‐ray Diffraction Mapping for Cultural Heritage Science: a Review of Experimental Configurations and Applications

González

Cotte

Vanmeert

et al. 2019

Chemistry A European J

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X-ray diffraction (XRD) mapping consists in the acquisition of XRD patterns at each pixel (or voxel) of an area (or volume). The spatial resolution ranges from the micrometer (mXRD) to the millimeter (MA-XRD)s cale, making the technique relevant for tiny samples up to large objects. Although XRD is primarily used for the identification of different materials in (complex) mixtures, additional information regarding the crystallite size, their orientation, and their indepth distribution can also be obtained. Through mapping, these different types of information can be located on the studied sample/object. Cultural heritage objects are usually highly heterogeneous, and contain both original and later (degradation, conservation) materials. Their structural characterization is required both to determine ancient manufacturing processes and to evaluate their conservation state. Togetherw ith other mapping techniques, XRD mapping is increasingly used for these purposes. Here, the authors review applicationsa sw ell as the various configurations for XRD mapping (synchrotron/laboratory X-ray source, poly-/monochromatic beam,micro/macro beam, 2D/3D, transmission/reflectionm ode). On-going hardware and software developments will further establish the technique as ak ey tool in heritage science.[a] Dr.

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Composition and microstructure of the lead white pigment in Masters paintings using HR Synchrotron XRD

Cited by 50 publications

References 18 publications

Unraveling the Composition of Rembrandt's Impasto through the Identification of Unusual Plumbonacrite by Multimodal X‐ray Diffraction Analysis

Unraveling the Composition of Rembrandt's Impasto through the Identification of Unusual Plumbonacrite by Multimodal X‐ray Diffraction Analysis

Lead soaps in paintings: Friends or foes?

X‐ray Diffraction Mapping for Cultural Heritage Science: a Review of Experimental Configurations and Applications

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