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AMS radiocarbon dating and scientific examination of high historical value manuscripts: Application to two Chinese manuscripts from Dunhuang
Journal of Cultural Heritage 11 (2010) 398–403
Original article
AMS radiocarbon dating and scientific examination of high historical value manuscripts: Application to two Chinese manuscripts from Dunhuang Pascale Richardin a,∗ , Franc¸oise Cuisance b,1 , Nathalie Buisson c,2 , Victoria Asensi-Amoros d,3 , Catherine Lavier a,4 a
Laboratory of Centre of Research and Restoration of the Museums of France, LC2RMF – CNRS UMR, 171, Palais-du-Louvre, 14, quai Franc¸ois Mitterrand, 75001 Paris, France National Library of France, Manuscripts Department, Conservation studio, Oriental Section, 58, rue de Richelieu, 75002 Paris, France National Library of France, Laboratory, 58, rue de Richelieu, 75002 Paris, France d Xylodata, 4, place Violet, 75015 Paris, France b c
a r t i c l e
i n f o
Article history: Received 26 March 2010 Accepted 13 May 2010 Available online 13 July 2010 Keywords: Dunhuang manuscripts Inks Wood identification Accelerator Mass Spectrometry Radiocarbon dating Scanning electron microscopy with energy dispersive x-ray analysis (SEM-EDX) Butterfly bookbinding Whirlwind bookbinding
a b s t r a c t In order to develop their restoration, a material study was undertaken on two Chinese manuscripts, shaped like binded codex (Chinese Pelliot 2547 and 2490), supposed to be dated from 8th and 10th centuries, and belonging to the Pelliot collection of the National Library of France in Paris. It allowed a better knowledge of the making technique of their bindings together with some of their components. We undertook the identification of the inks, and pigments used for calligraphy, and the dating of the wood and of the binding of the documents. Microsamples of inks were characterised by scanning electron microscopy (SEM) and the results of the x-ray microanalysis of particular interest are the presence of hematite and ochre in red samples, and carbon black and traces of bone black in the black inks. The taxon of wood has been identified on thin strips by the classical techniques used in xylology: the two scrolls were identified as Tamarix sp. (Tamaricaceae). The AMS radiocarbon dating of the manuscripts was also carried out on the wooden sticks which hold the paper sheets. Comparison of the potential calendar age distributions indicates probability distributions in the region between 662–781 cal AD and 862–994 cal AD for CP2547 and CP2490 respectively, which corresponds to the expected values. These results allowed to bring wider knowledge on the inks and the paintings and, in particular, have led to propose a date for the making of the binding of the CP2547, which confirms ideas proposed by book historians. © 2010 Elsevier Masson SAS. All rights reserved.
1. Introduction and research aim Since the end of the 19th century, Central Asia has been the objective of numerous scientific explorations organized by several countries (Russia, England, then Germany, Norway, Japan). Professor Paul Pelliot, from the French School of Oriental Studies, was in charge of a mission in this region from 1906 till 1908, which led him to the oasis of Shazou and the whole buddhist caves near Dunhuang [1]. The mission set its camp near the site of Mogaoku including some 500 caves dug in a loess cliff, collectively called “Caves of
∗ Corresponding author. Tel.: +33 (0) 1 40 20 24 65; fax: +33 (0) 1 47 03 32 46. E-mail addresses: [email protected] (P. Richardin), [email protected] (F. Cuisance), [email protected] (N. Buisson), [email protected] (V. Asensi-Amoros), [email protected] (C. Lavier). 1 Tel.: +33 (0) 1 53 79 86 07. 2 Tel.: +33 (0) 1 53 79 86 22. 3 Tel.: +33 (0) 1 45 79 90 21. 4 Tel.: +33 (0) 1 45 79 90 21; fax: +33 (0) 1 47 03 32 46. 1296-2074/$ – see front matter © 2010 Elsevier Masson SAS. All rights reserved. doi:10.1016/j.culher.2010.05.001
the thousand Buddha” (Qianfodong). They are decorated with wall paintings, in fairly good state of preservation and dating from the 6th to the 10th century. Pelliot began to inventory methodically the inside of each of the caves after being allowed to penetrate into the “Cave to manuscripts” (cavern-library or cave 17 according to the current numbering of the Art Institute of Dunhuang), where he discovered 15.000 and 20.000 scrolls and booklets and also paintings on silk, hemp or on paper. From his mission, he brought in particular 6000 manuscripts and a few printed matters dated before 1035 which were stored at the Manuscripts Department of the National Library of France (BNF) [2], some coins dated from 621 to 783 entrusted to the Department of coins and medals of the BNF, where they have been preserved since 1910, 200 paintings preserved at the Guimet museum, statues and archaeological matters, nowadays belonging to the collections of the Louvre museum. They include works ranging from religion and philosophy (Taoism, Buddhism, Nestorianism, Judaism – one document is in Hebrew) to history and mathematics, and even folk songs and dance. Others are archive documents of local interest. The study of these manuscripts appears as a remarkable breakthrough in the
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Fig. 1. Photographs (a, c) (©P. Salinson, BNF) and binding technique (b and d) (©C. Sarrion and J.-M. Karchi, BNF) of the two manuscripts CP2547 and CP2490.
understanding of medieval Chinese history, society, literature, religion and culture [3]. The manuscripts whose studies are being presented in this paper come from the cavern-library (cave no. 17). They are inventoried at the BNF under the name of ‘Pelliot chinois 2547 et 2490’. For their restoration and their future digitization and in the framework of the International Dunhuang Project [4], a material study was developed on these two codices, in order to know the nature of materials of their composition and the making of their interesting bindings, types of so-called butterfly or whirlwind bindings [5,6]. We worked out these analyses using a few workable fragments of wood, ink, pigments and papers [7]. The manuscript CP2547 (Fig. 1a) , entitled Zhaiwan wen (texts of purification and lament), is a booklet of ‘texts and formulae used for various rituals’ according to its anonymous author. Probably, the texts were composed between 647 and 788, and it is estimated that this copy was written between 728 and 744 [8]. This manuscript written on mulberry paper was initially scroll-shaped. At a very early period, it was cut out in 15 bifolios, which were mounted on guards. The mounting is fastened by stitches made with a hemp thread to a small Tamarisk wood branch previously covered with a red-brown glossy substance and cut into two pieces in length (Fig. 1b). We do not know if the leaves were wound on the branch originally [9], but by convenience, we will call the branch “roller” along this paper. The second manuscript CP2490 (Fig. 1c) is an incomplete calculation manual for the reckoning of farming areas entitled Bu shui xi jie (Farming Table). It is made up of six folios of a rough textile fibre paper mounted on guards and pasted onto a roller on their right, in a kind of whirlwind booklet (Fig. 1d) and it bears the date 952 on the recto of the fourth one [7]. The leaves bear a regular squaring, made of a red painting slightly thick, where characters are inscribed. The roller, rather thin, is not circular but has facets in relation with the way it was cut. In both cases, the mounting on guards has allowed the manuscript leaves to be fastened to a roller. Book historians explain
that texts and forms have a relationship and regarding these kinds of reference books, the form of booklet, easier to handle and to consult, seems to have been imperative [5]. Since the end of the 20th century, the analysis of the morphology of the Dunhuang manuscripts provides new elements to the history of paper and allow reaching a convenient method of dating [10–12]. Many scientific studies on the materials used have been undertaken, like e.g. the in situ analysis of few dyes and colorants by different analytical techniques [13–16], or the identification of trace elements by Pixe [17]. We undertook a study of the inks, pigments and wood used for the making of these manuscripts. We had the opportunity to make microsamples of inks which we have identified by scanning electron microscopy (SEM). The radiocarbon dating of the two manuscripts was carried on the wooden rollers, which held the paper sheets. Finally, the taxon of wood has been identified on thin strips of wood, by the classical techniques used in xylology. 2. Experimental part 2.1. Ink analysis The examination of CP2490 and CP2547 was carried out using a Zeiss stereomicroscope. Four ink samples (Table 1) were taken Table 1 Localisation and brief description of the ink samples. Manuscrits
Sample name
Sample localisation
Colour
CP2547
PE1 PE2
Red Black
CP2490
PE3 PE4
Sheet 2, 5th column Indeterminate sheet, last column, 8th pictogram Sheet 4, 7th red line Sheet 5, 3rd red line, 3rd column
Red Black
400
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from documents. The samples were mounted in embedding resin and examined as polished cross-section using microscopic methods that included UV microscopy and light microscopy. As samples were embedded in a polyester resin (H59 Sodemi, France), they were coated with a thin layer of carbon to improve conductivity and to prevent accumulation of charge. The crosssections were then examined with x-ray microanalysis using a JEOL JSM 840 SEM operating at 20 kV. Elemental analyses were performed at various points throughout the cross-sections by measuring the emitted x-rays with an energy dispersive x-ray system equipped with a Si/Li detector. 2.2. Wood identification Very thin samples were removed from the two rollers. We have followed standard procedures for the optico-microscopical examination and wood identification [18]. The samples were prepared to examine the transverse, radial and tangential sections through microscope (Carl Zeiss Jena), Xylodata SARL. Photographs of samples were taken by a camera attached to the microscope. Comparisons were made with our own scientific reference collection and that of the Laboratory of Palaeobotany and Palaeoecology of the Pierre and Marie Curie University (Paris VI, France). 2.3. Radiocarbon measurements 2.3.1. Sampling During the sampling session, the wooden stick was dissociated from CP2490 manuscript and we observed that it was partially covered with a thick layer of glue. That could induce a true problem of contamination by exogenous carbon for the radiocarbon dating. For this reason, about 10 very thin splinters (Fig. 2a) were collected with tweezers from the extremity of the stick which was a little disintegrated (total weight inferior at 20 mg). For the manuscript CP2547, a wooden fragment was broken loose from one extremity of the stick. A sample (7 × 1 × 3 mm, 15 mg) was cut with a sterilized scalpel blade. It was completely covered with a varnish or a coloured matter (Fig. 2b), which needed to be extracted from the wood during the sample preparation. 2.3.2. Sample preparation All the glassware was washed with a particular protocol used to avoid any pollutions and contaminations. After boiling 20 minutes with diluted TFD4 detergent (Franklab SA, France), all the glass pieces are rinsed with demineralised water, placed 48 hours in a 10% solution of hydrochloric acid (prepared from 30% HCl, technical grade from VWR International), and then rinsed a last time with ultrapure water (Direct-Q system from Millipore). At least, all pieces are put in a high-temperature oven at 450 ◦ C during 5 hours and stored in aluminium foil before used. The samples were cut into smaller fragments and processed separately. In order to eliminate all insoluble impurities (dust, textile fibres due to the manipulating of the documents. . .), the two samples were weighed into a clean 30 mL glass centrifuge tube, and washed twice in an ultrasonic bath (10 min) with ultrapure water. After this preliminary washing, they have undergone the classical Acid-Alkali-Acid procedure, previously described [19]. First, they have been treated with a 0.5 M HCl solution (VWR International, used as received) for 1 hour at 80 ◦ C. After removing the supernatant with a glass pipette, the remaining fragments have been rinsed with warm water, until neutral washing waters. A similar treatment was achieved with a fresh NaOH 0.05N aqueous solution (prepared from a sodium hydroxide solution at 0.1N from VWR International), followed by rinsing with ultrapure water. At least, another acidic treatment (similar to the first one) was done to remove atmospheric carbon added during the alkali treatment. During the sample prepa-
Fig. 2. Binocular observation of the CP2490 sample (a) and CP2547 sample (b) (©P. Richardin, C2RMF).
ration, the extraction of exogenous organic matter is followed by binocular observation. Finally, the clean samples were allowed to dry overnight in a low vacuum (100 mbar) oven at 60 ◦ C. The organic fraction has been then combusted at high temperature (5 hours at 850 ◦ C) under high vacuum (at 10-6 torr) on a semiautomatic combustion bench based on that of the Laboratoire des Sciences du Climat et de l’Environnement (LCSE) radiocarbon laboratory [20]. A portion of the processed samples (2 to 2.5 mg) was combusted in a quartz tube with 500 mg CuO (Cu(II) oxide on Cu(I) oxide heart for analysis, VWR International) and Ag wire (99.95%, Aldrich). The combustion gas (H2 O and CO2 ) were separated by cryogenic purification and the CO2 is collected in a sealed tube. The graphitization [21] of the obtained CO2 was achieved by direct catalytic reduction with hydrogen, using Fe powder (average particle size 10 m) as catalyst at 600 ◦ C and with excess of H2 (H2 /CO2 = 3). During this process, the carbon is deposited on the iron and the whole powder is mechanically pressed into a flat pellet. 2.3.3. AMS radiocarbon measurement All the measurements have been achieved through the Artemis AMS facility of Saclay (France). The radiocarbon activity is calculated by comparing the measured intensities of the 14 C, 13 C and 12 C beams from each sample with those of CO standards prepared 2 with HOx (I) oxalic acid reference, in pMC (percent Modern carbon) normalized with a ␦13C at −25 ‰. The radiocarbon ages are calculated [22] with correcting the isotope fractionation ␦13 C, calculated
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Table 2 Description and elemental analysis of the inks samples. Sample name
Description
Results
PE1
Red and yellow grains; layer firmly bound to the paper fibres; impossible to separate from substrate
Al, Si, Fe (Mg, K, Ti) Fe, O Ca, S Ca
PE2
Black, thin layer; very firmly bound to the paper fibres
C Al, Si, Fe (Mg, K, Ca)
PE3
Red and yellow grain, layer firmly bound to the paper fibres
Al, Si, Fe, (K, Ti) Fe, O Ca, Mg
PE4
Black with some red grains; thin layers, very firmly bound to the paper fibres
C Al, Si, Fe (K, Ca, Mg) Ca, P
from AMS measurements of the 13 C/12 C ratio. We have measured one sample for CP2490 and two for CP2457. 3. Results and discussion 3.1. Inks analysis The results of the x-ray microanalysis of inks are listed in Table 2. The results are of particular interest because they highlight the presence of hematite and red ochre in PE1 and PE3 samples and carbon black and traces of bone black in PE2 and PE4. Cross-sections of red inks analyzed in both CP2547 and CP2490, consist of a mixture of hematite (red iron oxide Fe2 O3 ) and red and yellow ochres. Ochres are characterized on a chromatic basis by ferric iron oxide: goethite for yellow ochre and hematite for red ochre. Furthermore, ochres are mainly composed of a large part of uncoloured minerals such as clay and quartz [23]. These pigments belong to a group of main red pigments used in the early historical periods. There are many reports and publications on the use of red earth for the decoration of skulls or skeletons in Palaeolithic and Neolithic Chinese graves [24,25]. Analysis of pigments from mural paintings in the Mogao grottoes, near Dunhuang, indicates that red ochre was used in such works from all the periods examined [26]. Ochres were also used as a coloring matter for red Chinese ink, as well as natural cinnabar, synthetic vermilion, red lead or organic red [27]. These red pigments were mixed with a little of calcium carbonate and sulphate carbonate for CP2547. Low quantities of quartz, double carbonate of calcium and magnesium and calcium carbonate was added to the red ink of CP2490. Carbon is the major element found in the black ink samples. Considering the colour and the composition of these two inks, it would appear that they are composed of carbon black, like in Chinese ink. This last, known as “Mo” in China and “Sumi” in Japan, refers to the black paint used almost every where in painting and calligraphy from East Asia for 2 millennia [28]. To these black inks was added ochre, calcium carbonate and a little of quartz and kaolinite (white earth). Kaolinite is a mineral composed of hydrated aluminium silicate (Al2 Si2 O5 OH)4 from the ¯ líng phylosilicates family. This name comes from the Chinese “gao t” which means “soil from the high hills” [29,30]. A small amount of bone black (Ca, P) was also detected. Its presence in these inks is not yet explained because it is not a common constituent of Chinese ink. 3.2. Wood identification The wood used for the two rollers were identified as Tamarix sp. (Tamaricaceae). The growth ring boundaries are difficult to dis-
Fig. 3. Photograph of the wooden roller of the butterfly booklet binding PC 2547 showing the endgrain (©S. Meziache, BNF), and photo-micrograph of a transverse section ( × 10) of Tamarix sp. (©V. Asensi-Amoros).
tinguish because it is a diffuse porous tree (Fig. 3a) . Vessels are solitary or diagonally arranged in multiples of 2 or 3 and in small clusters; their diameter is around 50 m. Vessels perforations are simple and the intervessel pitting alternates while pits are small with slit-like openings. Furthermore, the vessel-ray pits present distinct borders and the fibers are medium thick-walled (Fig. 3b). The axial parenchyma is paratracheal, vasicentric, confluent; the cell type is fusiform. The number of rays per millimetre is 3 to 4. The ray width is mostly five to 10 cells wide and the height reaches 1.5 mm. The composition of the rays is heterocellular, with procumbent, square and upright cells. Vessels and parenchyma elements are storied. The wood we have identified is a Tamarix species, which seems to confirm that this document has been made locally. Indeed, Tamarix spp. is distributed in the desert area Taklamakan. This area is under the influence of cold temperatures and of high pressures. These areas consist mainly of floating dunes. Because of the
402
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Table 3 Radiocarbon measurements conditions and results for the two samples. Pelliot
ArNa
␦13 Cb
14C age (yr BP)
954% (2) cal age ranges (cal AD)
Relative area under distribution (%)
CP2490
SacA 8716
−28.10
1120 ± 30
784–787 824–842 862–994
0.3 1.7 98
CP2547
SacA 8718 SacA 8719
−27.00
1275 ± 30 1280 ± 30
662–781 790–809 662–779 794–801
97.4 2. 99 1
a b
−26.50
Artemis run number. ␦13 C value measured by AMS (‰).
depth of underground water, salt content in the water and different types of deserts, the vegetation types also differ with communities dominated by Populus euphratica, Haloxylon persicum and H. ammodendron, Elaeagnus angustifolia, Tamarix spp., Caragna spp. in association with Calligonum spp., Artemisia spp. and especially Salix spp. The Tamarix are trees or tall shrubs with very small scale-like leaves. Numerous Tamarix species can be found in China and in the Dunhuang area. In Dunhuang vicinity, they are (and were) naturally distributed on sand dunes and sandbanks. The wood of the two rollers could be, anatomically speaking, Tamarix ramosissima and/or Tamarix taklamakanensis [31]. Unfortunately, the samples were too small, in order to confirm the species. Beside, this result could indicate that the binding of these manuscripts might have been done locally. 3.3. AMS radiocarbon dating Table 3 reports the isotope fractionation ␦13 C, measured by AMS and the age as radiocarbon age (in year BP: before present). The calibrated ages (cal age) have been calculated with the program Calib Rev 6.0.0 [32] and with the more recent calibration data [33]. The results are considered, by international conventions, in an interval of 2, with a level of confidence of 95.4%. The units are done in year’s cal BC or cal AD. The Fig. 4 displays the possible calendar age ranges and the probability for each value using the relevant portion of the calibration curve for each measurement. Comparison of the potential calendar age distributions indicates probability distributions in the region between 662–781 cal AD and 862–994 cal AD for CP2547 and CP2490, respectively, which corresponds to the expected value. 4. Conclusion
Fig. 4. Radiocarbon age and calculated calendar age range probability from each measured sample (a) CP2490 – SacA8716; (b) CP2547 – SacA8718.
These results are a new contribution to the research on materials used in making of the most ancient Chinese books. The microanalyses of inks are of particular interest because they show the presence of hematite and red ochre in red samples, and carbon black and traces of bone black in the black ones. The wood of the two rollers is a Tamarix species, which could indicate a local making of the bookbindings. If the texts have been probably composed between 647 and 788, it is estimated that this copy was written between 728 and 744. In fact, according to the sinologist Hélène Vetch, the date can be postponed to 762, if we take into account the limitation of 15 year’s for re-using such a document [7]. Moreover, the very regular longitudinal section of the young branch in two halves could be done only little time after being detached from the tree. So, the radiocarbon dating obtained for the roller is in accordance with these dates. All these information lead to think that the working out of this binding could be placed in the period between 762 and the beginning of the occupation of this region by the Tibetans (786–848) in which these
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texts were probably not used. Accordingly, it should be one of the first examples, and may be the first, of a kind of ‘butterfly’ binding. Being a roller transformed into a codex, this booklet witnesses the evolution of the book form in China, from roller to codex. Pictures of these manuscripts will be available on the Internet website of the British Library in the framework of the International Dunhuang Project. Initiated in 1994, this Project is an international collaboration to provide information and images of all manuscripts, paintings, textiles and artefacts from Dunhuang and archaeological sites of the Eastern Silk Road, freely available on Internet and to encourage their use through educational and research programs. Acknowledgements Thanks to T. Delcourt, director of the Manuscript’s Department (National Library of France) for the facilities he bring us for the present study. Our gratitude to Professor J. Broutin, director of the Laboratory of Palaeobotany and Palaeoecology of the Pierre and Marie Curie University (Paris VI) for the access he gives us to the wood collection. The authors want also to thank S. Couvreur (C2RMF) for the samples preparation. We thank E. Kaltnecker, J.F. Tannau at LSCE (Gif-sur-Yvette, France) and B. Moignard (C2RMF) for their collaboration on sample preparation and for the construction of our combustion bench. We wish to thank also C. Moreau (LMC14, CEA Saclay) for the radiocarbon measurements. References [1] J.P. Drège, Paul Pelliot: de l’histoire à la légende, Lettre du Collège de France, 25, 2009. [2] M. Cohen, in: A. Berthier (Ed.), Manuscrits, xylographes, estampages. Les collections orientales du département des Manuscrits, Bibliothèque nationale de France, 2000, pp. 91–117. [3] P. Pelliot, Catalogue des manuscrits chinois de Touen-Houang. Fonds Pelliot chinois de la Bibliothèque nationale, I, Fondation Singer-Polignac, Paris, 1983, pp. IX–XXI. [4] S.B. Brysac, The virtual Silk Road (The International Dunhuang Project, an interactive web database of manuscripts), Archaeology 53 (4) (2000) 72–74. [5] J.P. Drège. Papillons et tourbillons, in: De Dunhuang au Japon, Études chinoises et bouddhiques offertes à Michel Soymié, 31, Hautes Études orientales II, École pratique des Hautes Études, Sciences historiques et philologiques, collège de France, institut des Hautes Études chinoises, Ed. Droz, Genève, 1996, pp. 162–176. [6] J.P. Drège. Les transformations du livre chinois (viiie –xiie siècle), in: Les Trois Révolutions du livre, CNAM, Paris, 2002. [7] F. Cuisance, Undoing Old and Doing New Conservation on Pelliot Chinois 2547 and 2490, IDP News 33 (2009) 4–7. [8] P. Magnin. Donateurs et joueurs en l’honneur du Buddha, in: De Dunhuang au Japon, Études chinoises et bouddhiques offertes à Michel Soymié, 31, Hautes Études orientales II, École pratique des Hautes Études, Sciences historiques et philologiques, Collège de France, institut des Hautes Études chinoises, Ed. Droz, Genève, 1996, pp. 103–40.
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Original article
AMS radiocarbon dating and scientific examination of high historical value manuscripts: Application to two Chinese manuscripts from Dunhuang Pascale Richardin a,∗ , Franc¸oise Cuisance b,1 , Nathalie Buisson c,2 , Victoria Asensi-Amoros d,3 , Catherine Lavier a,4 a
Laboratory of Centre of Research and Restoration of the Museums of France, LC2RMF – CNRS UMR, 171, Palais-du-Louvre, 14, quai Franc¸ois Mitterrand, 75001 Paris, France National Library of France, Manuscripts Department, Conservation studio, Oriental Section, 58, rue de Richelieu, 75002 Paris, France National Library of France, Laboratory, 58, rue de Richelieu, 75002 Paris, France d Xylodata, 4, place Violet, 75015 Paris, France b c
a r t i c l e
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Article history: Received 26 March 2010 Accepted 13 May 2010 Available online 13 July 2010 Keywords: Dunhuang manuscripts Inks Wood identification Accelerator Mass Spectrometry Radiocarbon dating Scanning electron microscopy with energy dispersive x-ray analysis (SEM-EDX) Butterfly bookbinding Whirlwind bookbinding
a b s t r a c t In order to develop their restoration, a material study was undertaken on two Chinese manuscripts, shaped like binded codex (Chinese Pelliot 2547 and 2490), supposed to be dated from 8th and 10th centuries, and belonging to the Pelliot collection of the National Library of France in Paris. It allowed a better knowledge of the making technique of their bindings together with some of their components. We undertook the identification of the inks, and pigments used for calligraphy, and the dating of the wood and of the binding of the documents. Microsamples of inks were characterised by scanning electron microscopy (SEM) and the results of the x-ray microanalysis of particular interest are the presence of hematite and ochre in red samples, and carbon black and traces of bone black in the black inks. The taxon of wood has been identified on thin strips by the classical techniques used in xylology: the two scrolls were identified as Tamarix sp. (Tamaricaceae). The AMS radiocarbon dating of the manuscripts was also carried out on the wooden sticks which hold the paper sheets. Comparison of the potential calendar age distributions indicates probability distributions in the region between 662–781 cal AD and 862–994 cal AD for CP2547 and CP2490 respectively, which corresponds to the expected values. These results allowed to bring wider knowledge on the inks and the paintings and, in particular, have led to propose a date for the making of the binding of the CP2547, which confirms ideas proposed by book historians. © 2010 Elsevier Masson SAS. All rights reserved.
1. Introduction and research aim Since the end of the 19th century, Central Asia has been the objective of numerous scientific explorations organized by several countries (Russia, England, then Germany, Norway, Japan). Professor Paul Pelliot, from the French School of Oriental Studies, was in charge of a mission in this region from 1906 till 1908, which led him to the oasis of Shazou and the whole buddhist caves near Dunhuang [1]. The mission set its camp near the site of Mogaoku including some 500 caves dug in a loess cliff, collectively called “Caves of
∗ Corresponding author. Tel.: +33 (0) 1 40 20 24 65; fax: +33 (0) 1 47 03 32 46. E-mail addresses: [email protected] (P. Richardin), [email protected] (F. Cuisance), [email protected] (N. Buisson), [email protected] (V. Asensi-Amoros), [email protected] (C. Lavier). 1 Tel.: +33 (0) 1 53 79 86 07. 2 Tel.: +33 (0) 1 53 79 86 22. 3 Tel.: +33 (0) 1 45 79 90 21. 4 Tel.: +33 (0) 1 45 79 90 21; fax: +33 (0) 1 47 03 32 46. 1296-2074/$ – see front matter © 2010 Elsevier Masson SAS. All rights reserved. doi:10.1016/j.culher.2010.05.001
the thousand Buddha” (Qianfodong). They are decorated with wall paintings, in fairly good state of preservation and dating from the 6th to the 10th century. Pelliot began to inventory methodically the inside of each of the caves after being allowed to penetrate into the “Cave to manuscripts” (cavern-library or cave 17 according to the current numbering of the Art Institute of Dunhuang), where he discovered 15.000 and 20.000 scrolls and booklets and also paintings on silk, hemp or on paper. From his mission, he brought in particular 6000 manuscripts and a few printed matters dated before 1035 which were stored at the Manuscripts Department of the National Library of France (BNF) [2], some coins dated from 621 to 783 entrusted to the Department of coins and medals of the BNF, where they have been preserved since 1910, 200 paintings preserved at the Guimet museum, statues and archaeological matters, nowadays belonging to the collections of the Louvre museum. They include works ranging from religion and philosophy (Taoism, Buddhism, Nestorianism, Judaism – one document is in Hebrew) to history and mathematics, and even folk songs and dance. Others are archive documents of local interest. The study of these manuscripts appears as a remarkable breakthrough in the
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Fig. 1. Photographs (a, c) (©P. Salinson, BNF) and binding technique (b and d) (©C. Sarrion and J.-M. Karchi, BNF) of the two manuscripts CP2547 and CP2490.
understanding of medieval Chinese history, society, literature, religion and culture [3]. The manuscripts whose studies are being presented in this paper come from the cavern-library (cave no. 17). They are inventoried at the BNF under the name of ‘Pelliot chinois 2547 et 2490’. For their restoration and their future digitization and in the framework of the International Dunhuang Project [4], a material study was developed on these two codices, in order to know the nature of materials of their composition and the making of their interesting bindings, types of so-called butterfly or whirlwind bindings [5,6]. We worked out these analyses using a few workable fragments of wood, ink, pigments and papers [7]. The manuscript CP2547 (Fig. 1a) , entitled Zhaiwan wen (texts of purification and lament), is a booklet of ‘texts and formulae used for various rituals’ according to its anonymous author. Probably, the texts were composed between 647 and 788, and it is estimated that this copy was written between 728 and 744 [8]. This manuscript written on mulberry paper was initially scroll-shaped. At a very early period, it was cut out in 15 bifolios, which were mounted on guards. The mounting is fastened by stitches made with a hemp thread to a small Tamarisk wood branch previously covered with a red-brown glossy substance and cut into two pieces in length (Fig. 1b). We do not know if the leaves were wound on the branch originally [9], but by convenience, we will call the branch “roller” along this paper. The second manuscript CP2490 (Fig. 1c) is an incomplete calculation manual for the reckoning of farming areas entitled Bu shui xi jie (Farming Table). It is made up of six folios of a rough textile fibre paper mounted on guards and pasted onto a roller on their right, in a kind of whirlwind booklet (Fig. 1d) and it bears the date 952 on the recto of the fourth one [7]. The leaves bear a regular squaring, made of a red painting slightly thick, where characters are inscribed. The roller, rather thin, is not circular but has facets in relation with the way it was cut. In both cases, the mounting on guards has allowed the manuscript leaves to be fastened to a roller. Book historians explain
that texts and forms have a relationship and regarding these kinds of reference books, the form of booklet, easier to handle and to consult, seems to have been imperative [5]. Since the end of the 20th century, the analysis of the morphology of the Dunhuang manuscripts provides new elements to the history of paper and allow reaching a convenient method of dating [10–12]. Many scientific studies on the materials used have been undertaken, like e.g. the in situ analysis of few dyes and colorants by different analytical techniques [13–16], or the identification of trace elements by Pixe [17]. We undertook a study of the inks, pigments and wood used for the making of these manuscripts. We had the opportunity to make microsamples of inks which we have identified by scanning electron microscopy (SEM). The radiocarbon dating of the two manuscripts was carried on the wooden rollers, which held the paper sheets. Finally, the taxon of wood has been identified on thin strips of wood, by the classical techniques used in xylology. 2. Experimental part 2.1. Ink analysis The examination of CP2490 and CP2547 was carried out using a Zeiss stereomicroscope. Four ink samples (Table 1) were taken Table 1 Localisation and brief description of the ink samples. Manuscrits
Sample name
Sample localisation
Colour
CP2547
PE1 PE2
Red Black
CP2490
PE3 PE4
Sheet 2, 5th column Indeterminate sheet, last column, 8th pictogram Sheet 4, 7th red line Sheet 5, 3rd red line, 3rd column
Red Black
400
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from documents. The samples were mounted in embedding resin and examined as polished cross-section using microscopic methods that included UV microscopy and light microscopy. As samples were embedded in a polyester resin (H59 Sodemi, France), they were coated with a thin layer of carbon to improve conductivity and to prevent accumulation of charge. The crosssections were then examined with x-ray microanalysis using a JEOL JSM 840 SEM operating at 20 kV. Elemental analyses were performed at various points throughout the cross-sections by measuring the emitted x-rays with an energy dispersive x-ray system equipped with a Si/Li detector. 2.2. Wood identification Very thin samples were removed from the two rollers. We have followed standard procedures for the optico-microscopical examination and wood identification [18]. The samples were prepared to examine the transverse, radial and tangential sections through microscope (Carl Zeiss Jena), Xylodata SARL. Photographs of samples were taken by a camera attached to the microscope. Comparisons were made with our own scientific reference collection and that of the Laboratory of Palaeobotany and Palaeoecology of the Pierre and Marie Curie University (Paris VI, France). 2.3. Radiocarbon measurements 2.3.1. Sampling During the sampling session, the wooden stick was dissociated from CP2490 manuscript and we observed that it was partially covered with a thick layer of glue. That could induce a true problem of contamination by exogenous carbon for the radiocarbon dating. For this reason, about 10 very thin splinters (Fig. 2a) were collected with tweezers from the extremity of the stick which was a little disintegrated (total weight inferior at 20 mg). For the manuscript CP2547, a wooden fragment was broken loose from one extremity of the stick. A sample (7 × 1 × 3 mm, 15 mg) was cut with a sterilized scalpel blade. It was completely covered with a varnish or a coloured matter (Fig. 2b), which needed to be extracted from the wood during the sample preparation. 2.3.2. Sample preparation All the glassware was washed with a particular protocol used to avoid any pollutions and contaminations. After boiling 20 minutes with diluted TFD4 detergent (Franklab SA, France), all the glass pieces are rinsed with demineralised water, placed 48 hours in a 10% solution of hydrochloric acid (prepared from 30% HCl, technical grade from VWR International), and then rinsed a last time with ultrapure water (Direct-Q system from Millipore). At least, all pieces are put in a high-temperature oven at 450 ◦ C during 5 hours and stored in aluminium foil before used. The samples were cut into smaller fragments and processed separately. In order to eliminate all insoluble impurities (dust, textile fibres due to the manipulating of the documents. . .), the two samples were weighed into a clean 30 mL glass centrifuge tube, and washed twice in an ultrasonic bath (10 min) with ultrapure water. After this preliminary washing, they have undergone the classical Acid-Alkali-Acid procedure, previously described [19]. First, they have been treated with a 0.5 M HCl solution (VWR International, used as received) for 1 hour at 80 ◦ C. After removing the supernatant with a glass pipette, the remaining fragments have been rinsed with warm water, until neutral washing waters. A similar treatment was achieved with a fresh NaOH 0.05N aqueous solution (prepared from a sodium hydroxide solution at 0.1N from VWR International), followed by rinsing with ultrapure water. At least, another acidic treatment (similar to the first one) was done to remove atmospheric carbon added during the alkali treatment. During the sample prepa-
Fig. 2. Binocular observation of the CP2490 sample (a) and CP2547 sample (b) (©P. Richardin, C2RMF).
ration, the extraction of exogenous organic matter is followed by binocular observation. Finally, the clean samples were allowed to dry overnight in a low vacuum (100 mbar) oven at 60 ◦ C. The organic fraction has been then combusted at high temperature (5 hours at 850 ◦ C) under high vacuum (at 10-6 torr) on a semiautomatic combustion bench based on that of the Laboratoire des Sciences du Climat et de l’Environnement (LCSE) radiocarbon laboratory [20]. A portion of the processed samples (2 to 2.5 mg) was combusted in a quartz tube with 500 mg CuO (Cu(II) oxide on Cu(I) oxide heart for analysis, VWR International) and Ag wire (99.95%, Aldrich). The combustion gas (H2 O and CO2 ) were separated by cryogenic purification and the CO2 is collected in a sealed tube. The graphitization [21] of the obtained CO2 was achieved by direct catalytic reduction with hydrogen, using Fe powder (average particle size 10 m) as catalyst at 600 ◦ C and with excess of H2 (H2 /CO2 = 3). During this process, the carbon is deposited on the iron and the whole powder is mechanically pressed into a flat pellet. 2.3.3. AMS radiocarbon measurement All the measurements have been achieved through the Artemis AMS facility of Saclay (France). The radiocarbon activity is calculated by comparing the measured intensities of the 14 C, 13 C and 12 C beams from each sample with those of CO standards prepared 2 with HOx (I) oxalic acid reference, in pMC (percent Modern carbon) normalized with a ␦13C at −25 ‰. The radiocarbon ages are calculated [22] with correcting the isotope fractionation ␦13 C, calculated
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Table 2 Description and elemental analysis of the inks samples. Sample name
Description
Results
PE1
Red and yellow grains; layer firmly bound to the paper fibres; impossible to separate from substrate
Al, Si, Fe (Mg, K, Ti) Fe, O Ca, S Ca
PE2
Black, thin layer; very firmly bound to the paper fibres
C Al, Si, Fe (Mg, K, Ca)
PE3
Red and yellow grain, layer firmly bound to the paper fibres
Al, Si, Fe, (K, Ti) Fe, O Ca, Mg
PE4
Black with some red grains; thin layers, very firmly bound to the paper fibres
C Al, Si, Fe (K, Ca, Mg) Ca, P
from AMS measurements of the 13 C/12 C ratio. We have measured one sample for CP2490 and two for CP2457. 3. Results and discussion 3.1. Inks analysis The results of the x-ray microanalysis of inks are listed in Table 2. The results are of particular interest because they highlight the presence of hematite and red ochre in PE1 and PE3 samples and carbon black and traces of bone black in PE2 and PE4. Cross-sections of red inks analyzed in both CP2547 and CP2490, consist of a mixture of hematite (red iron oxide Fe2 O3 ) and red and yellow ochres. Ochres are characterized on a chromatic basis by ferric iron oxide: goethite for yellow ochre and hematite for red ochre. Furthermore, ochres are mainly composed of a large part of uncoloured minerals such as clay and quartz [23]. These pigments belong to a group of main red pigments used in the early historical periods. There are many reports and publications on the use of red earth for the decoration of skulls or skeletons in Palaeolithic and Neolithic Chinese graves [24,25]. Analysis of pigments from mural paintings in the Mogao grottoes, near Dunhuang, indicates that red ochre was used in such works from all the periods examined [26]. Ochres were also used as a coloring matter for red Chinese ink, as well as natural cinnabar, synthetic vermilion, red lead or organic red [27]. These red pigments were mixed with a little of calcium carbonate and sulphate carbonate for CP2547. Low quantities of quartz, double carbonate of calcium and magnesium and calcium carbonate was added to the red ink of CP2490. Carbon is the major element found in the black ink samples. Considering the colour and the composition of these two inks, it would appear that they are composed of carbon black, like in Chinese ink. This last, known as “Mo” in China and “Sumi” in Japan, refers to the black paint used almost every where in painting and calligraphy from East Asia for 2 millennia [28]. To these black inks was added ochre, calcium carbonate and a little of quartz and kaolinite (white earth). Kaolinite is a mineral composed of hydrated aluminium silicate (Al2 Si2 O5 OH)4 from the ¯ líng phylosilicates family. This name comes from the Chinese “gao t” which means “soil from the high hills” [29,30]. A small amount of bone black (Ca, P) was also detected. Its presence in these inks is not yet explained because it is not a common constituent of Chinese ink. 3.2. Wood identification The wood used for the two rollers were identified as Tamarix sp. (Tamaricaceae). The growth ring boundaries are difficult to dis-
Fig. 3. Photograph of the wooden roller of the butterfly booklet binding PC 2547 showing the endgrain (©S. Meziache, BNF), and photo-micrograph of a transverse section ( × 10) of Tamarix sp. (©V. Asensi-Amoros).
tinguish because it is a diffuse porous tree (Fig. 3a) . Vessels are solitary or diagonally arranged in multiples of 2 or 3 and in small clusters; their diameter is around 50 m. Vessels perforations are simple and the intervessel pitting alternates while pits are small with slit-like openings. Furthermore, the vessel-ray pits present distinct borders and the fibers are medium thick-walled (Fig. 3b). The axial parenchyma is paratracheal, vasicentric, confluent; the cell type is fusiform. The number of rays per millimetre is 3 to 4. The ray width is mostly five to 10 cells wide and the height reaches 1.5 mm. The composition of the rays is heterocellular, with procumbent, square and upright cells. Vessels and parenchyma elements are storied. The wood we have identified is a Tamarix species, which seems to confirm that this document has been made locally. Indeed, Tamarix spp. is distributed in the desert area Taklamakan. This area is under the influence of cold temperatures and of high pressures. These areas consist mainly of floating dunes. Because of the
402
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Table 3 Radiocarbon measurements conditions and results for the two samples. Pelliot
ArNa
␦13 Cb
14C age (yr BP)
954% (2) cal age ranges (cal AD)
Relative area under distribution (%)
CP2490
SacA 8716
−28.10
1120 ± 30
784–787 824–842 862–994
0.3 1.7 98
CP2547
SacA 8718 SacA 8719
−27.00
1275 ± 30 1280 ± 30
662–781 790–809 662–779 794–801
97.4 2. 99 1
a b
−26.50
Artemis run number. ␦13 C value measured by AMS (‰).
depth of underground water, salt content in the water and different types of deserts, the vegetation types also differ with communities dominated by Populus euphratica, Haloxylon persicum and H. ammodendron, Elaeagnus angustifolia, Tamarix spp., Caragna spp. in association with Calligonum spp., Artemisia spp. and especially Salix spp. The Tamarix are trees or tall shrubs with very small scale-like leaves. Numerous Tamarix species can be found in China and in the Dunhuang area. In Dunhuang vicinity, they are (and were) naturally distributed on sand dunes and sandbanks. The wood of the two rollers could be, anatomically speaking, Tamarix ramosissima and/or Tamarix taklamakanensis [31]. Unfortunately, the samples were too small, in order to confirm the species. Beside, this result could indicate that the binding of these manuscripts might have been done locally. 3.3. AMS radiocarbon dating Table 3 reports the isotope fractionation ␦13 C, measured by AMS and the age as radiocarbon age (in year BP: before present). The calibrated ages (cal age) have been calculated with the program Calib Rev 6.0.0 [32] and with the more recent calibration data [33]. The results are considered, by international conventions, in an interval of 2, with a level of confidence of 95.4%. The units are done in year’s cal BC or cal AD. The Fig. 4 displays the possible calendar age ranges and the probability for each value using the relevant portion of the calibration curve for each measurement. Comparison of the potential calendar age distributions indicates probability distributions in the region between 662–781 cal AD and 862–994 cal AD for CP2547 and CP2490, respectively, which corresponds to the expected value. 4. Conclusion
Fig. 4. Radiocarbon age and calculated calendar age range probability from each measured sample (a) CP2490 – SacA8716; (b) CP2547 – SacA8718.
These results are a new contribution to the research on materials used in making of the most ancient Chinese books. The microanalyses of inks are of particular interest because they show the presence of hematite and red ochre in red samples, and carbon black and traces of bone black in the black ones. The wood of the two rollers is a Tamarix species, which could indicate a local making of the bookbindings. If the texts have been probably composed between 647 and 788, it is estimated that this copy was written between 728 and 744. In fact, according to the sinologist Hélène Vetch, the date can be postponed to 762, if we take into account the limitation of 15 year’s for re-using such a document [7]. Moreover, the very regular longitudinal section of the young branch in two halves could be done only little time after being detached from the tree. So, the radiocarbon dating obtained for the roller is in accordance with these dates. All these information lead to think that the working out of this binding could be placed in the period between 762 and the beginning of the occupation of this region by the Tibetans (786–848) in which these
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texts were probably not used. Accordingly, it should be one of the first examples, and may be the first, of a kind of ‘butterfly’ binding. Being a roller transformed into a codex, this booklet witnesses the evolution of the book form in China, from roller to codex. Pictures of these manuscripts will be available on the Internet website of the British Library in the framework of the International Dunhuang Project. Initiated in 1994, this Project is an international collaboration to provide information and images of all manuscripts, paintings, textiles and artefacts from Dunhuang and archaeological sites of the Eastern Silk Road, freely available on Internet and to encourage their use through educational and research programs. Acknowledgements Thanks to T. Delcourt, director of the Manuscript’s Department (National Library of France) for the facilities he bring us for the present study. Our gratitude to Professor J. Broutin, director of the Laboratory of Palaeobotany and Palaeoecology of the Pierre and Marie Curie University (Paris VI) for the access he gives us to the wood collection. The authors want also to thank S. Couvreur (C2RMF) for the samples preparation. We thank E. Kaltnecker, J.F. Tannau at LSCE (Gif-sur-Yvette, France) and B. Moignard (C2RMF) for their collaboration on sample preparation and for the construction of our combustion bench. We wish to thank also C. Moreau (LMC14, CEA Saclay) for the radiocarbon measurements. References [1] J.P. Drège, Paul Pelliot: de l’histoire à la légende, Lettre du Collège de France, 25, 2009. [2] M. Cohen, in: A. Berthier (Ed.), Manuscrits, xylographes, estampages. Les collections orientales du département des Manuscrits, Bibliothèque nationale de France, 2000, pp. 91–117. [3] P. Pelliot, Catalogue des manuscrits chinois de Touen-Houang. Fonds Pelliot chinois de la Bibliothèque nationale, I, Fondation Singer-Polignac, Paris, 1983, pp. IX–XXI. [4] S.B. Brysac, The virtual Silk Road (The International Dunhuang Project, an interactive web database of manuscripts), Archaeology 53 (4) (2000) 72–74. [5] J.P. Drège. Papillons et tourbillons, in: De Dunhuang au Japon, Études chinoises et bouddhiques offertes à Michel Soymié, 31, Hautes Études orientales II, École pratique des Hautes Études, Sciences historiques et philologiques, collège de France, institut des Hautes Études chinoises, Ed. Droz, Genève, 1996, pp. 162–176. [6] J.P. Drège. Les transformations du livre chinois (viiie –xiie siècle), in: Les Trois Révolutions du livre, CNAM, Paris, 2002. [7] F. Cuisance, Undoing Old and Doing New Conservation on Pelliot Chinois 2547 and 2490, IDP News 33 (2009) 4–7. [8] P. Magnin. Donateurs et joueurs en l’honneur du Buddha, in: De Dunhuang au Japon, Études chinoises et bouddhiques offertes à Michel Soymié, 31, Hautes Études orientales II, École pratique des Hautes Études, Sciences historiques et philologiques, Collège de France, institut des Hautes Études chinoises, Ed. Droz, Genève, 1996, pp. 103–40.
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