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burgio2007
burgio2007
Lucia Burgio, Shayne Rivers, Catherine Higgitt, Marika Spring & Ming Wilson
To cite this article: Lucia Burgio, Shayne Rivers, Catherine Higgitt, Marika Spring & Ming Wilson
(2007) Spherical Copper Resinate on Coromandel Objects: Analysis and Conservation of Matt
Green Paint, Studies in Conservation, 52:4, 241-254
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An unusual green pigment was found on a seventeenth-century kuan cai (Coromandel) lacquer screen at the Victoria and Albert
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Museum, London.The particles are perfectly spherical and translucent, with the appearance of green fish roe. Analysis revealed
that the pigment is a copper resinate, produced by reacting a copper salt with a resin, probably one from a Pinus species.The
binding medium for the pigment is proteinaceous.The unusual spherical morphology of the particles results from the method of
manufacture. A pigment with the same microscopic appearance was also found on two other Coromandel objects from the same
collection. In light or olive green areas, where the pigment is mixed with lead white, the paint is glossy and well preserved. In
contrast, in the dark green areas where the pigment was used alone, the paint is matt and powdery and there is significant paint
loss and abrasion.The problem of consolidation of the powdery paint, while still preserving the matt appearance of the surface, was
resolved by the use of immiscible solvents and consolidant.
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242 L. BURGIO, S. RIVERS, C. HIGGITT, M. SPRING AND M. WILSON
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early eighteenth-century France [1, 2]. The front of the while the more brightly coloured glossy areas, such as
kuan cai screen examined in this study is decorated with the deer and flowers, advance into the foreground.
a pastoral scene of animals and birds among trees and A limited range of pigmented lacquer was produced
flowers alongside waves topped with spindrift, while the prior to the nineteenth century, typically black, brown,
back is characterized by incised fan-shaped and square red and yellow [3]. There are two reasons for this limited
cartouches inscribed with extracts from the works of palette. First, the drying of lacquer occurs through
well-known poets, an allusion to the screen-owner’s a combination of oxidation and enzyme-catalysed
literary knowledge. Both front and back are bordered (therefore pH-specific) cross-linking and many pigments
with the ‘hundred antiques’ design depicting flower disrupt the curing process [4]. Second, pigments used in
vases, urns and animals such as dogs, terrapins, dragons combination with lacquer must have the ability to mask
and phoenix. the natural dark brown colour of this binding medium,
The artistic quality of kuan cai can be judged by the so it is not possible to make white lacquer, for example.
intricacy and conception of the overall design, while A wider range of colours, including the greens, whites,
craft skill is evident in the execution of the decoration. and blues typical of kuan cai polychromy, are possible if
Fine-lined and smooth-flowing curves are the most other binding media are used.
technically difficult incised decoration to produce. Texts on Chinese lacquer, historical documentary
The large areas given over to the depiction of fine sources and contemporary conservation literature give
bundles of coniferous needles and waves are testament little information on kuan cai, while the materials and
to the exceptionally high quality of this screen. The techniques used to create it rarely warrant more than a
polychrome decoration utilizes a wide range of colours single sentence (see for example [5]).Typical descriptions
in combination with delicate glazes, which are used for of the polychromy technique refer to the use of oil as
both pictorial detail and graduated shadowing. Matt the binding medium, or lacquer for certain colours,
and gloss paint are juxtaposed to create an impression although two authors refer to the use of water-based
of three-dimensionality in the design. The combination colours [6, 7].
of fine line incised work with matt muted colour in The sixteenth-century Chinese lacquerist Huang
the coniferous needle bundles, for example, causes the Cheng listed kuan cai along with 90 other lacquering
overhanging tree greenery to recede within the design, techniques in Xiu Shi Lu (The Lacquering Handbook)
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SPHERICAL COPPER RESINATE ON COROMANDEL OBJECTS 243
OPTICAL MICROSCOPY
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244 L. BURGIO, S. RIVERS, C. HIGGITT, M. SPRING AND M. WILSON
mixed with a translucent dark green spherical pigment malachite, and is more frequently observed when
(see the Appendix and Figure 4). The spheres ranged preparing dispersions of copper-containing glaze paint
from approximately 2 to 100 µm in diameter. In the sam- where verdigris has reacted with oil. In addition, emerald
ples from the matt areas a thick layer composed of the green and spherical malachite yield distinctive Raman
same translucent green spheres was always present, used spectra, unlike the green pigment from the Coromandel
alone rather than with lead white, giving the appearance screen (only fluorescence was observed with 514.5 and
under the microscope of green fish roe. The pigment in 632.8 nm excitation).
these areas was very leanly bound and there were voids Other occurrences of a green pigment described
between the spherical particles. In a few areas there as resembling fish roe have been reported on Chinese
was a layer of malachite over the layer containing the objects, but the pigment is either not discussed in
translucent green spherical pigment, and in these places detail [20], or it is described, based on its microscopic
the matt green paint is in better condition (Figure 5). appearance rather than on analytical results, as a synthetic
The appearance and colour of the translucent form of malachite, ‘showing a white centre surrounded
green pigment was typical of a copper-containing by a shell of green’ [21].
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Figure 4 Photomicrograph of a cross-section of a sample from a pale, Figure 5 Photomicrograph of a cross-section of a sample from a matt
glossy green area on the Coromandel screen, showing translucent, dark green area on the Coromandel screen showing a layer of malachite on top
green spheres of variable size embedded in a lead white matrix. of a layer of translucent, dark green spheres.
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SPHERICAL COPPER RESINATE ON COROMANDEL OBJECTS 245
are particularly clear in the glossy green areas because of copper-containing pigments such as malachite. In the
the strong contrast with the lead white in which they are backscattered images of some of the cross-sections there
embedded (Figures 7 and 8). is a more highly scattering feature in the centre of the
The EDX spectra confirm that the spherical green largest spheres (Figure 9), in which some chlorine was
pigment contains copper, although at a relatively low detected in association with copper.
level compared to the background, which is more
typical of copper salts of organic acids than other
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Figure 6 Tabletop electron microscope backscattered electron images of an unmounted sample from a matt green area on the Coromandel screen, at
two different magnifications.
Figure 7 SEM backscattered electron image of a cross-section of a Figure 8 Tabletop electron microscope backscattered electron image
sample from a pale, glossy green area on the Coromandel screen. of an unmounted sample from a glossy green area on the Coromandel
screen.
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246 L. BURGIO, S. RIVERS, C. HIGGITT, M. SPRING AND M. WILSON
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SPHERICAL COPPER RESINATE ON COROMANDEL OBJECTS 247
Table 1 Results of the analysis of a green sample from the Coromandel screen by GC-MS
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248 L. BURGIO, S. RIVERS, C. HIGGITT, M. SPRING AND M. WILSON
Coromandel craftsmanship. The term ‘copper resinate’ is brush marks. White accretions along the edges of many
more commonly encountered in the context of Western incised areas were identified as paraffin wax [34]. The
European easel painting, where it has traditionally been varnished surface had a greenish-white autofluorescence
used for green translucent copper-containing glazes, under ultraviolet (UV) illumination, which is consistent
although recent work has shown that these glazes in with several Western natural resin varnishes. By contrast,
fact generally consist of verdigris which has wholly or photo-degraded black oriental lacquer frequently
partially reacted and dissolved in the oil binding medium. exhibits a muted orange autofluorescence [35]. These
A small amount of varnish was sometimes added to these factors, combined with the solubility characteristics,
glazes, so that some ‘copper resinate’ can be present, but suggested the presence of a wax–resin varnish.
formed through reaction with the resin on ageing of the Although alcohols and ketones would usually be used
paint rather than by deliberate reaction [22, 23, 31]. to remove this type of varnish, contact with such solvents
The unusual morphology of the copper resinate often causes blanching in photo-degraded oriental
particles on the Coromandel screen suggests that it did lacquer. The more light-damaged the lacquer and the
not simply result from the reaction of a copper pigment longer it is exposed to these solvents, the more likely it
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with an organic binding medium but is a deliberately is that significant blanching will occur [36]. Solvent tests
manufactured copper resinate pigment. It seems likely on the varnish demonstrated that aromatic hydrocarbon
that the molten copper resinate mix was quenched solvents caused sufficient swelling to allow removal of
in water and that the spherical green particles then the varnish from the lacquer using a combination of
separated out of the emulsion as the copper resinate solvent and mechanical action.
cooled and solidified. Such a method of production Solubility tests on the matt green copper resinate
would account for the shape and the variable size of paint were undertaken using small samples viewed
the pigment particles. Where the copper resinate has under 100–200× magnification. The pigment was
not been mixed with lead white, the lean proteinaceous readily soluble in ethanol and acetone and insoluble in
binder does not fill the voids between the large pigment deionized water, aliphatic and aromatic hydrocarbon
particles, explaining why the paint appears rather matt solvents. The overlapping solubility parameters of
and is very powdery and brittle. The lighter green areas pigment and varnish combined with the friability of the
contain the same pigment and also have a proteinaceous paint layer meant that no attempt was made to remove
binding medium, but contain lead white, which fills the the Western varnish from the matt paint. However, it was
voids between the green particles giving a glossier, more still necessary to consolidate the matt paint decoration
durable paint. without further altering its appearance.
The aims of the consolidation treatment for the
CONSERVATION matt paint on the screen were to introduce enough
consolidant to prevent further loss of pigment, ideally
In contrast to the gloss painted areas, which were largely without altering the appearance of the paint, and to allow
intact, areas of matt painted decoration were powdery for the possibility of future re-treatment without damage
and friable and had suffered significant losses, as is to the paint or adjacent lacquer. Common approaches
typical of matt paints with their high ratio of pigment for the consolidation of matt paint include reducing the
volume to binder volume [32, p. xxxix]. Adhesive failure concentration of consolidant, using multiple applications
had occurred both within the paint layer, which is of very dilute consolidant solutions (sometimes less than
0.5–1.5 mm thick, and at the interface with the white 1%) or using a nebulizer [37] or ultrasonic mister [38];
preparation layer. SEM images showed that this paint had increasing penetration of consolidant into the paint layer
a rough surface, was poorly bound and contained large by means of a slow-evaporating solvent [39] or a vapour-
voids. This paint presented a particular challenge, since saturated atmosphere [40]; the use of additives such as
any conservation treatment that alters these properties matting agents in the consolidant and experimentation
will cause a marked change in the appearance of such with traditional materials in new ways, for example
paint, due to a reduction in the diffuse reflection of light funori, an alginate used in Japanese conservation [37, 41,
from the surface of the paint [33, p. 164]. 42]. Several methods and materials were tested, including
Both the front and rear of the screen had been ParaloidTM B72 in dilute solutions and in the slow-
varnished in the past, probably in an attempt to unify the evaporating aromatic solvent diethylbenzene, a range of
appearance of wax repairs and the adjacent lacquer. The cellulose ethers, and the use of fumed silica as a matting
semi-matt varnish was characterized by thick, uneven agent. All were unsuccessful, providing either insufficient
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SPHERICAL COPPER RESINATE ON COROMANDEL OBJECTS 249
adhesion or darkening the matt green paint. However, forming a coherent film on top of the pigment particles.
during informal discussions of this consolidation problem, By the time the white spirit has evaporated, the isinglass
colleagues from the V&A sculpture conservation studio has gelled below the surface. The low concentration of
referred to their use of immiscible solvents to prevent the isinglass provides sufficient adhesion within the paint
penetration of aqueous cleaning agents into uncoated layer without filling the voids and darkening the paint.
porous plaster surfaces during cleaning [43]. Typically Consolidation of the fr iable matt paint using
the plaster surface was wetted with a hydrocarbon immiscible solvents facilitated the rapid treatment of
solvent (white spirit) which acted as a barrier to prevent substantial areas of matt paint on the Coromandel
water-soluble dirt being carried further into the porous, screen. These vertical surfaces have suffered no further
water sensitive plaster surface as the surface was cleaned loss in the years since the screen was redisplayed at the
with a dampened swab. The use of immiscible solvent V&A in a gallery where relative humidity ranges from
combinations has been reported for aqueous cleaning 32 to 57%. Two other matt painted objects, a small
of paintings (hydrocarbon solvent layer/ammonium eighteenth-century Chinese polychrome sculpture and
hydroxide–water solution [44]) and paper objects with a nineteenth-century Japanese ceiling panel, have also
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water-sensitive media (cyclododecane barrier layer [45]). been treated successfully using this method.
There is only a single anecdotal reference to the use
of immiscible solvents for consolidation of matt paint CONCLUSION
(footnoted as Futernick, personal communication):
‘sensitive flaking paint has been successfully adhered The green areas of the Coromandel screen contain
with acrylic emulsions while the paint was saturated a translucent dark green pigment with an unusual
with toluene… the toluene was allowed to dry, leaving spherical particle form. It was identified using FTIR
the flaking paints still porous but adhered’ [32, p. lvi]. microscopy and GC-MS as copper resinate, which had
These experiences with porous materials prompted been deliberately prepared as a pigment using resin that
consolidation tests following a similar approach. was probably from a species of pine. This is the first
An acrylic dispersion, PrimalTM WS24 (5% solids), time to the authors’ knowledge that a pigment of this
and isinglass 5% w/v were tested. First, drops of a description, which was used extensively in the green
hydrocarbon solvent (white spirit) were applied to the areas on the screen, has been reported. A pigment with
friable paint from a pipette, followed by application of the same microscopic appearance has also been found on
the consolidant, drawn off by capillary action from a two other Coromandel objects, a casket and a cabinet
fine sable brush touched to the surface. Once dry, the dating from the late seventeenth century, which were
treatment was evaluated by brushing lightly over the sampled for comparison (Figure 12). It seems likely that
surface with a dry sable brush while observing the effect further analysis of Coromandel objects will uncover
under low magnification. No loose pigment particles more examples of its use.
were observed when isinglass was used, but 5% PrimalTM The paint was glossy, hard and well preserved where
WS24 was insufficient to secure the pigment. In both the spherical green pigment was used in admixture with
cases, the appearance of the surface was unchanged. lead white, and matt and porous where it was not. The
After further successful trials, isinglass was selected binding medium was identified as proteinaceous in both
as the consolidant for the matt painted areas of the cases, which contradicts historical sources that document
Coromandel screen. Some collagen-derived adhesives the materials and techniques used to create Coromandel
can offer long-term stability if natural contaminants are lacquer. Consolidation of the matt paint was achieved
minimized, relative humidity fluctuations limited and without altering the appearance of the paint using a
high light levels avoided [33, p. 165]. combination of the immiscible materials white spirit and
The most likely explanation for the effectiveness of isinglass.
the treatment is simple displacement. Isinglass used on
its own as a consolidant forms a thin layer on the surface
APPENDIX – EXPERIMENTAL
that saturates and darkens matt paint. Pre-wetting the
surface with a hydrophobic solvent such as white spirit Optical microscopy
prevents this. As the isinglass is applied, the white spirit is
displaced and forms a layer at the surface of the paint, on Samples were embedded in clear casting polyester
top of the isinglass. The hydrophobic white spirit layer resin, polished and examined under visible and UV
acts as a barrier that repels the isinglass and prevents it illumination with a Leica Aristomet microscope and a
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250 L. BURGIO, S. RIVERS, C. HIGGITT, M. SPRING AND M. WILSON
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Figure 12 Photomicrograph of a cross-section of a sample from a matt green area on the Coromandel cabinet (V&A accession number FE.39-1981)
showing a layer of green spheres. Image width: approximately 0.8 mm.
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SPHERICAL COPPER RESINATE ON COROMANDEL OBJECTS 251
and Julia Hutt for discussions on Coromandel lacquer; to 12 November 1993, ed. K. Nishikawa, Tokyo National Research
Edgar Mantz, Barbara Schertel and Nanke Schellmann Institute of Cultural Properties, Tokyo (1993) 49–62.
for assistance with German texts. Rian Kanduth and 13 Piert-Borgers, B., ‘Aspects and problems of the application of
Alice Kleyboldt contributed to the conservation of the Urushi in the restoration of objects from European collections’,
in International Symposium on the Conservation and Restoration of
screen.
Cultural Property: Conservation of Urushi Objects, 10–12 November
1993, ed. K. Nishikawa, Tokyo National Research Institute of
Cultural Properties, Tokyo (1993) 147–165.
MATERIALS
14 Bresinsky, H., ‘Montierter Lack’ (Mounted oriental lacquer:
ParaloidTM B72 and PrimalTM WS24: Conservation Resources, 18th century French furniture made with East Asian lacquer
1 Pony Road, Cowley, Oxford OX4 2RD, www.conservation work), Restauro 94 (1988) 195–210 [in German].
resources.com. 15 Breidenstein, I., ‘Considerations regarding the restoration of a
Chinese lacquer screen’, in Japanese and European Lacquerware,
Clear casting polyester resin: Alec Tiranti Ltd, 27 Warren Street, Arbeitshefte des Bayerischen Landesamtes für Denkmalpflege,Vol. 96,
London W1T 5NB, UK. ed. M. Kühlenthal, Lipp Verlag, Munich (2000) 561–585.
16 Fiedler, I., and Bayard, M.A., ‘Emerald green and Scheele’s
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252 L. BURGIO, S. RIVERS, C. HIGGITT, M. SPRING AND M. WILSON
27 Mills, J.S., and White, R., The Organic Chemistry of Museum 41 Michel, F., Geiger, T., Reichlin, A., and Teoh-Sapkota, G.,
Objects, 2nd edn, Butterworth-Heinemann, Oxford (1994). ‘Funori, Ein Japanisches Festigungsmittel für Matte Malerei’,
28 Watts, S., and de la Rie, E.R., ‘GC-MS analysis of triterpenoid Zeitschrift für Kunsttechnologie and Konservierung 16 (2002)
resins: In situ derivatization procedures using quaternary 257–275 [in German].
ammonium hydroxides’, Studies in Conservation 47 (2002) 42 Geiger, T., and Michel, F., ‘Studies on the polysaccharide
257–272. JunFunori used to consolidate matt paint’, Studies in Conservation
29 van den Berg, K.J., Boon, J.J., Pastorova, I., and Spetter, L.F.M., 50 (2005) 193–204.
‘Mass spectrometric methodology for the analysis of highly 43 Hubbard, C., and Kosinova, A., Victoria and Albert Museum,
oxidized diterpenoid acids in Old Master paintings’, Journal of personal communication (1997).
Mass Spectrometry 35 (2000) 512–533. 44 Hook, J., ‘The use of immiscible solvent combinations for
30 Hilditch, T.P., and Williams, P.N., The Chemical Constitution of the cleaning of paintings’, Journal of the American Institute for
Natural Fats, 4th edn, Chapman and Hall, London (1964). Conservation 27 (1988) 100–104.
31 Spring, M., and Higgitt, C., ‘Analyses reconsidered: The 45 Brückle, I., Thornton, J., Nichols, K., and Strickler, G.,
importance of the pigment content of paint in the interpretation ‘Cyclododecane: Technical note on some uses in paper
of the results of examination of binding media’, in Medieval and objects conservation’, Journal of the American Institute for
Painting in Northern Europe, ed. J. Nadolny, K. Kollandsrud, Conservation 38 (1999) 162–175.
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SPHERICAL COPPER RESINATE ON COROMANDEL OBJECTS 253
CATHERINE HIGGITT graduated in chemistry from the Institute in Cambridge in 1991. She joined the Scientific
University of York in 1994 and completed a PhD degree Department in the National Gallery in 1991. Her
in chemistry at the same institution in 1998. After one principal interests are the study of historical painting
year working for the Historic Scotland Conservation technique and materials, particularly pigments, and
Centre in Edinburgh, she joined the Scientific research into the mechanisms of their deterioration.
Department at the National Gallery in London in 1999, She is currently senior scientific officer at the National
working with Raymond White. Here she specialized Gallery. Scientific Department, The National Gallery,
in the study of natural organic materials in old master Trafalgar Square, London WC2N 5DN, UK. Email: marika.
paintings using spectroscopic, chromatographic and spring@ng-london.org.uk
spectrometric methods. The study described in this
paper was undertaken while she was senior organic MING WILSON, Chinese by birth, has an MA degree from
analyst at the National Gallery. At the beginning of 2007 the School of Oriental and African Studies, London
Catherine moved to the British Museum to take up the University. She joined the Victoria and Albert Museum
post of head of the Science Group. Address: Department in 1994 and is now a senior curator in the Asian
Department, where she is responsible for the collection
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Résumé — Un pigment vert inhabituel a été trouvé dans un paravent laqué kuan cai (Coromandel) du XVIIe siècle du
Victoria and Albert Museum, à Londres. Les particules sont parfaitement sphériques et translucides et ont l’apparence d’œufs de
poisson. Les analyses ont montré que le pigment est un résinate de cuivre produit par la réaction d’un sel de cuivre avec une résine,
probablement de l’espèce Pinus. Le liant pour ce pigment est protéinique. La morphologie sphérique inhabituelle des particules est
due à la méthode de fabrication. Un pigment d’apparence semblable a aussi été trouvé sur deux autres objets Coromandel de la
même collection. Dans les zones vert clair ou vert olive, où le pigment est mélangé avec du blanc de plomb, la peinture est brillante
et bien conservée. En revanche, dans les zones vert sombre, où le pigment est utilisé seul, la peinture est mate et pulvérulente et
on observe des lacunes et des zones d’abrasion. L’emploi de solvants non miscibles entre eux et d’un consolidant a permis de
consolider la peinture pulvérulente tout en préservant l’aspect mat de la surface.
Zusammenfassung — Auf einer kuan cai (Coromandel) Lacktafel des 17. Jahrhunderts aus dem Besitz des Victoria
and Albert Museum, London wurde ein ungewöhnliches Grünpigment gefunden. Die Partikel sind perfekt sphärisch und
durchscheinend und haben das Aussehen von grünen Fischrogen. Analytisch konnte das Pigment als Kupferresinat bestimmt
werden, das durch Reaktion eines Kupfersalzes mit einem Harz, wahrscheinlich aus einer Pinus – Species, entstanden ist.
Das Bindemittel des Pigmentes ist proteinisch. Die ungewöhnliche sphärische Morphologie des Pigmentes ist Ergebnis des
Herstellungsprozesses. Ein Pigment des gleichen mikroskopischen Aussehens wurde auf zwei anderen Coromandel Objekten
derselben Sammlung gefunden. In den hellgrünen bzw. olivgrünen Bereichen, wo das Pigment mit Bleiweiß ausgemischt ist, ist
die Malschicht glänzend und gut erhalten. Im Gegensatz dazu sind die dunkelgrünen Bereiche, in denen das Pigment alleine
verwendet wurde, matt und abgepudert und ein Malschichtverlußt sowie Abrieb ist feststellbar. Das Problem der Konsolidierung
der pudernden Malerei unter gleichzeitigem Erhalt des matten Oberflächencharakters wurde durch die Verwendung von
unmischbaren Lösungs- und Konsolidierungsmitteln.
Resumen — Un pigmento verde inusual fue identificado en un panel de laca kuan cai (Coromandel), del siglo XVII,
perteneciente al Victoria and Albert Museum, Londres. Las partículas son perfectamente esféricas y translúcidas, con la apariencia
de huevos de pescado verdes. Los análisis revelaron que el pigmento es un resinato de cobre producido por la reacción de la sal
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254 L. BURGIO, S. RIVERS, C. HIGGITT, M. SPRING AND M. WILSON
de cobre con una resina, probablemente una de la especie Pinus. El aglutinante para este pigmento es proteínico. La inusual
morfología de las partículas es fruto del proceso de elaboración. Un pigmento con la misma apariencia microscópica se detectó en
otros dos objetos Coromandel de la misma colección. En las áreas claras o de color verde oliva, donde el pigmento está mezclado
con blanco de plomo, la pintura es brillante y está bien presentada. Por el contrario, en las zonas de verde oscuro, donde el
pigmento se ha empleado puro, la pintura se presenta mate y pulverulenta con abundantes pérdidas y abrasión. El problema de
la consolidación de la pintura pulverulenta manteniendo la apariencia mate se resolvió con el uso de disolventes inmiscibles y de
consolidante.
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