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II. La fabrique du noir

Black Carolingian inks under examination. Part 1: recipes and literature survey

Un examen des encres noires carolingiennes. Première partie : recettes et panorama de la littérature
Zina Cohen, Oliver Hahn et Ira Rabin
p. 90-95

Résumés

L’emploi des différents types de matériaux d’écriture noirs et leurs compositions ont varié selon les époques et les régions. Nous souhaitons ici contribuer à leur étude en répertoriant et en analysant les recettes d’encres de calligraphie noires en circulation dans l’Empire carolingien, ainsi qu’en procédant au référencement des analyses archéométriques des encres noires utilisées dans les manuscrits. Faisant appel aux sciences humaines et aux sciences naturelles, ces analyses apportent un éclairage nouveau sur la manière dont les savants du haut Moyen Âge organisaient les manuscrits.

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Introduction

  • 1 The project C08 (2015-2019) focussed on a particular class of medieval manuscripts, namely “East Fr (...)
  • 2 This second paper will be published in Technè 56 (December 2023).

1In the framework of two parallel projects on Carolingian manuscripts at Hamburg University1, we have been interested in the question of materiality in Carolingian manuscripts. To this day, the question of early European inks has barely been discussed in view of the existing recipes. In her seminal work, in 1981, Zerdoun pointed out that iron-gall ink seems to have conquered Europe very early which is to be contrasted with the scarcity of the recipes. Our interest in the early European inks evolved from the transition of carbon ink to iron-gall ink. To address the question of the materiality and of the production process of manuscripts in a scriptorium, we first reviewed ink recipes and the results found in scientific analytical literature. In a second article2, we will report the results obtained from the analysis of 63 manuscripts written between the 8th and 10th centuries in the Carolingian Empire.

Carolingian manuscripts in the context of ink studies

2Today, the term “black ink” is often applied to all non-coloured writing inks, i.e. it includes inks that appear black or in various shades of brown. This is because it has been known for many years, that the colour of ink results from many factors such as the recipe, particular ingredients, ageing and degradation processes as well as restoration. From a chemical point of view, three types of typologically different black inks were used in Medieval Europe:

  • carbon ink, which consists of a fine dispersion of carbon pigments in a water-soluble binder such as a protein glue or gum arabic;

    • 3 Gall nuts are abnormal growths that form on the young branches or twigs of plants in response to in (...)

    plant or tannin inks, which constitute extracts from tree bark or gall nuts3;

  • iron-gall ink that results from the reaction of iron (II) and gallic/tannic acids contained in tree bark and gall nuts.

  • 4 Schopen, 2006; Ghigo et al., 2020; Cohen, 2021, p. 202; Nehring et al., 2021.
  • 5 Brown, Clark, 2004.

3We would like to add a fourth type that presents a mixture of carbon ink with an iron-gall or plant one. This last ink type is not only found in many medieval recipes in the Islamic and Jewish worlds but has also been identified in a considerable number of documentary and literary texts in Greek, Coptic, and Jewish manuscripts4. This last ink has been also suggested in the report on the ink studies of several Anglo-Saxon manuscripts from the 8th to the 11th centuries CE5.

  • 6 Díaz Hidalgo et al., 2018; Hahn et al., 2021.
  • 7 Karpenko, Norris, 2002.
  • 8 It should be noted that while we know that this term does indeed refer to vitriol in the 16th centu (...)
  • 9 Karpenko, Norris, 2002.

4It seems that only two ink types are significant for the manuscripts produced in Europe in the period under scrutiny: plant and iron-gall ink. Various possible sources for tannins and iron in these inks have recently been discussed in depth6. It suffices to say here that, independently of geographic area, at least two sources of iron have been experimentally identified in the iron-gall inks used in the Late Antiquity and early Middle Ages. To stress the difference, we named the inks vitriolic iron-gall and non-vitriolic iron-gall inks, depending on their main source of iron. The first ones are based on hydrated iron sulphate, derived from a mixture of hydrated metal sulphates, often called vitriol7. The second subtype’s iron source is metallic iron dissolved in an acid such as vinegar. The recipes for the inks based on metallic iron circulated in the Medieval Islamic world, while vitriol seems to have been well known since Late Antiquity and through medieval times, albeit under various names such as chalchantum, atramentum sutorium, atrament, atramentum, atramenta8, or copperas9.

  • 10 Hahn et al., 2021.

5To be able to map the appearance and spread of the new inks, i.e. the inks based on tannins (and iron-gall inks belong to this category), we need to approach the task from two different sides. The first one deals with the transmitted records of the recipes, while the other uses “reversed engineering”, i.e. reconstructing the recipes by analysing the manuscripts produced prior to the appearance of a large number of recipes. We would like to point out that the second approach has many limitations. One of them is due to the fluid transition between plant and iron-gall ink, because a tiny amount of iron (II) added to a plant ink would transform the latter into an iron-gall one. Here, the main problem consists in understanding whether the metal entered the inks accidently or on purpose. In our previous work, we observed that the amount of iron in the inks of the manuscripts produced before the 10th century was extremely low and suggested that this low iron content was a characteristic feature of these inks10.

  • 11 Ghigo, Rabin, 2020; Ghigo et al., 2020; Cohen, 2021.
  • 12 For example, see Roger, Barrandon, 2010. However, it should be noted that these inks were not named (...)
  • 13 Karpenko, Norris, 2002. Furthermore, analysis of late inks leads us to believe that the purificatio (...)

6In previous studies, we noticed the existence of non-vitriolic iron-gall inks, i.e. inks containing no other metallic element than iron11. Curiously enough, no explanation was put forward before 2020, though such inks were already observed a decade earlier12. This fact is even more surprising since vitriol consisting of a single iron sulphate is not known and even vitriol purification, which did not start before the 16th century13, would not produce an ink bare of the metallic satellites.

Recipes

  • 14 Vitruvius, 1847, bk. 7, sec. 10.
  • 15 Zerdoun Bat-Yehouda, 1983, p. 81-83; Pliny (the Elder), n.d., sec. 25.
  • 16 Zerdoun Bat-Yehouda, 1983, p. 80; Dioscorides Pedanius, secs. 182-183.
  • 17 Preisendanz, 1931, p. 83; Zerdoun Bat-Yehouda, 1983, p. 94. The papyrus V of Leiden was found in a (...)
  • 18 Theophilus, 1986, XXXIII. Moreover, it is difficult to establish the true chronological limit of th (...)
  • 19 The bibliography on the subject is extremely exhaustive and has been analysed in numerous works, fo (...)
  • 20 Zerdoun Bat-Yehouda, 1983, p. 143-214.

7In Antiquity, several recipes were recorded in the texts of Vitruvius14, Pliny the Elder15, Dioscorides16, and the Papyrus V of Leyden17. But it was not until the high Middle Ages that ink recipes reappeared in Europe18. Moreover, even when the recipes appeared in the European region, they presented a rather uniform picture with vitriol as the only iron source among the ingredients for preparing iron-gall ink. In contrast, ink recipes for carbon, plant, iron-gall, and mixed inks proliferated in the contemporary Islamic world from the 9th century onwards19. Let us now briefly review the ink recipes for the black writing inks that existed in Late Antiquity and the early Middle Ages in Europe20.

  • 21 Zerdoun Bat-Yehouda, 1983, p. 81-83; Pliny (the Elder), n.d., sec. 25.
  • 22 Vitruvius, 1847, bk. 7, sec. 10.
  • 23 Zerdoun Bat-Yehouda, 1983, p. 80; Dioscorides Pedanius, 2000, p. 182-183.
  • 24 Zerdoun Bat-Yehouda, 1983, p. 143-214.

8Among the oldest extant recipes of carbon ink, the best known are recorded by Pliny the Elder in his Natural History21 (written during the 1st century CE), and by Vitruvius22 (written during the 1st century BCE). In both recipes, the carbon ink is prepared by mixing soot and gum Arabic. Another recipe, by Dioscorides (from the 1st century CE), suggested adding a copper compound to the soot, and seems to be the earliest indication of inks prepared by mixing carbon pigments and metals23. Zerdoun suggests that carbon inks were not used for writing anymore and that the recipes for carbon ink in Medieval Europe were mere copies of those circulated in Antiquity, when mostly carbon inks were used24. To support her view, she presents three recipes:

    • 25 Zerdoun Bat-Yehouda, 1983, p. 144-146.

    One given by Cetius Faventinus (around the 4th century). In his Liber artis architectonicae, he describes a recipe for carbon ink, identified by Zerdoun as having close links with that given by Vitruvius25.

    • 26 Zerdoun Bat-Yehouda, 1983, p. 147-148.

    The second recipe is taken from the Etymologies of Isidore of Seville (6th-7th century), which Zerdoun says has strong links with the recipes given by Vitruvius and Pliny the Elder26.

    • 27 Zerdoun Bat-Yehouda, 1983, p. 148-150.

    Finally, the third one, De coloribus et artibus romanorum, by Eraclius, copied between the 12th and the 13th century, could be a copy of Vitruvius and Cetius Faventinus27.

  • 28 Garlan, 1974.
  • 29 Zerdoun Bat-Yehouda, 1983; Nehring et al., 2021.

9Plant inks, whose appearance is usually ascribed to the Middle Ages, seem to have had a much longer history. They are mentioned in an extant recipe for a secret ink recorded by Philo of Byzantium as early as the 3rd century BCE28. In this recipe, a text written with a gallnut extract on felt stays invisible until its “activation” by “chalcanthum”. The discussion of the possible meanings of the term “chalcanthum” and whether this ink can be considered a predecessor of iron-gall ink is beyond the scope of this work because this recipe does not seem to have influenced the development of the ink in Europe. An interested reader is referred to the detailed reviews by Zerdoun and the recent work by Nehring et al.29. We derive the important information that writing with gallnut extract co-existed with writing with carbon ink in Late Antiquity.

  • 30 An edition of this text is available in Preisendanz, 1931, p. 83; Zerdoun Bat-Yehouda, 1983, p. 94.
  • 31 The interpretation of those terms is an open discussion. For more details, see Christiansen, 2017.

10Another Greek ink recipe from Late Antiquity, albeit dated to a much later period, namely ca. the 3rd century CE recorded in the Papyrus V of Leyden30, has been also frequently associated with the appearance of iron-gall inks. It lists the following ingredients: “Myrrh 1 drachma, misy 4 drachmas, chalcanthum 4 drachmas, gallnut 2 drachmas, gum 3 drachmas.” Though the impossibility of a secure identification of the meaning of both chalcanthum and misy precludes an unambiguous interpretation, it admits their correlation with metallic salts31.

  • 32 Capellae, n.d., sec. 225.

11We find the next recipe in the work of Martianus Capella from Carthage dating to ca. the 5th century CE32. Here in Latin, the author indicates that a mixture of gallnuts and gum (gallarum gummeosque commixtio) is used for writing. Curiously, this recipe was considered to be among the first iron-gall ink recipes though no metal or metallic salt is mentioned. It is, therefore, a good example of a recipe for a plant ink.

  • 33 Theophilus, 1986, XXXIII.
  • 34 Zerdoun Bat-Yehouda, 1983, p. 156-165.

12And at last, we arrive at the recipe from the Diversis artibus of Theophilus33 that appears some 700 years later and is believed by many a scholar to be the first explicitly European recipe for iron-gall ink. In great detail, it describes the preparation of a plant ink from a hawthorn bark and wine. The ink is then left to dry in the sun and kept in dry form in small bags made of parchment. Before using it for writing, the dry ink should be mixed with wine and a small amount of atramentum. At the end of the recipe, it is suggested to add a piece of incandescent iron to the mixture, if the ink is not black enough. The resulting ink can therefore be interpreted as either an iron-gall one if atramentum is translated as vitriol or a European example of mixed ink if atramentum is translated as carbon ink34. We have no unequivocal solution here, because there is no precise data on the transformation of the meaning of atramentum from carbon ink (Late Antiquity) to vitriol (Middle Ages). To supplement our overview, we have gathered the relevant information in Table 1.

Table 1. Overview of ink types given in literary sources with a description of their historical and geographical contexts

Author, work

Century

Location

(modern names)

Language

Ink type

Philo of Byzantium, Μηχανικὴ Σύνταξις

3rd BCE

Egypt?

Greek

Invisible ink/vitriolic ink?

Vitruvius, De Architectura

1st BCE

Italy

Latin

Carbon

Pliny the Elder, Naturalis Historia

1st

Italy

Latin

Carbon, also vitriolic (?*)

Dioscorides, Περὶ ὕλης ἰατρικῆς

1st

Turkey?

Greek

Carbon and mixed

Papyrus V of Leyden

3rd

Egypt?

Greek

Iron-gall (with vitriol?)

Cetius Faventinus, Liber artis architectonicae

4th

Italy

Latin

Carbon (close connection with the recipe given by Vitruvius)

Martianus Capella, De Nuptiis Philologiae et Mercurii

5th

Tunis

Latin

Plant?

Isidore de Séville, Etymologies

6th-7th

Spain

Latin

Carbon (copy of Vitruvius and Pliny)

Theophilus, Diversis artibus

12th

Germany?

Latin

Iron-gall (with vitriol)

Eraclius, De coloribus et artibus romanorum

12th-13th

Greece or Italy

Latin

Carbon (copy of Vitruvius and Cetius Faventinus)

* See note 8.

Published results of ink analysis

  • 35 Hahn et al., 2021.

13To compensate for the gap left by the scarcity of written European recipes in our possession, we are left with the reverse engineering though a complete reconstruction is not possible using non-destructive analysis alone. Moreover, degradation of the organic components might preclude a reliable reconstruction even if destructive analysis is permitted. Therefore, the collected information usually refers to the type of the inks found in a manuscript. Furthermore, except for the publication of Hahn et al.35, none of the articles listed in Table 2 differentiates between vitriolic and non-vitriolic inks. The authors only note the presence of iron (Fe) and possibly other elements such as calcium (Ca) or potassium (K). We interpret the absence of metallic elements commonly present in vitriol (Cu, Zn, Mn) as evidence that the ink was prepared with a source of iron II other than vitriol.

Table 2. Examples of manuscripts whose ink has been analysed prior to this work with a description of their historical-geographical context and the result obtained

Manuscript or collection

Number of manuscripts analysed

Location

Century

Ink type

Analytical techniques

Vercelli Gospelsa

1

Northern Italy

4th

Vitriolic

XRF, FTIR, Raman

St Paul de Lavanttalb

2 fragments

Northern Italy

5th

Non-vitriolic (vivianite?)

Reflectography, XRF

2

Northern Italy and/or south of France

7th-9th

Vitriolic

ÖNB Cod. Ser. n. 2065c

1

Mondsee Abbey (Austria)

Late 8th

Non-vitriolic

Reflectography, XRF

Fleuryd

13

Fleury (France)

8th-12th

Non-vitriolic

Diffuse reflectance spectroscopy (DRS), XRF

Codex Millenarius Maior and Minor (inv. No CC Cim 1&2)e

2

Mondsee Abbey (Austria)

Ca. 800

Non-vitriolic

XRF, FTIR, Raman

ÖNB Cod. 808f

1

Salzburg (Austria)

Early 9th

Non-vitriolic

Reflectography, XRF

St Paul de Lavanttalg

4

Reichenau and surrounding (Germany)

9th

Non-vitriolic

Reflectography, XRF

Bibl. mun. 295h

1

Reims (France)

845-899

Non-vitriolic

DRS, XRF

Bibl. mun. 127i

1

Winchcombe (England)

945-999

Non-vitriolic

DRS, XRF

St-Michelj

50

Mont St-Michel (France)

990-1100

Non-vitriolic

XRF

Brussels, KBR 10066-10077k

1

North of France

11th

Non-vitriolic / vitriolic (cover sheets 4 to 6)

XRF

Manuscripts kept in the Troyes libraryl

3

Paris (France)

1140-1190

Non-vitriolic

DRS, XRF

3

Clairvaux (France)

1140-1200

Non-vitriolic

1

1170-1180

Vitriolic (at least two different compositions)

3

Troyes (France)

1160-1180

Non-vitriolic

1

Ca. 1190

Vitriolic

a. Aceto et al., 2008.
b. Hahn et al., 2021.
c. Rabin et al., 2019.
d. Roger, Bosc, 2008.
e. Frühmann et al., 2018.
f. Rabin et al., 2019.
g. Hahn et al., 2021.
h. Roger, Bosc, 2008.
i. Roger, Bosc, 2008.
j. Robinet, Lecouteux, 2021.
k. van Bos, Watteeuw, 2014.
l. Roger, Barrandon, 2010.

  • 36 Hahn et al., 2021; Cohen, Rabin [to be published].
  • 37 Roger, Bosc, 2008; Roger, Barrandon, 2010; Lecouteux et al., 2020; Robinet, Lecouteux, 2021.
  • 38 Roger, Barrandon, 2010.
  • 39 Clark, van der Weerd, 2004; Denoël et al., 2018.
  • 40 Clark, van der Weerd, 2004; Aceto et al., 2008, 2017; Bioletti et al., 2009.

14The results presented in the studies listed in Table 2 show the almost systematic use of non-vitriolic iron-gall ink36 in Northern Europe from the 8th to the 12th centuries37. At Troyes and Clairvaux, however, the end of the 12th century marked the arrival of metallic impurities associated with vitriol in the composition of the ink38. In contrast, vitriol seems to have been used in Northern Italy and Southern France at a much earlier date. In parallel, two studies of the manuscripts of Tours from the Carolingian period focused on the coloured illuminations and other polychrome representations, unfortunately without paying much attention to the writing inks39. Black pigment has been analysed only when it was present in the miniatures of certain manuscripts, with a focus on Gospels written between the 4th and the very beginning of the 9th century40; however, such analyses are rare, and even rarer is their comparison with the inks used in the same manuscript (both in terms of their nature and composition). This lack of data creates a gap in our understanding of the use of black writing and drawing materials in the medieval period.

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Bibliographie

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Notes

1 The project C08 (2015-2019) focussed on a particular class of medieval manuscripts, namely “East Frankish manuscripts containing collections of formulae” and the project Coenotur focussed on the production of manuscripts associated with the scriptorium of Tours. The two projects are associated by their geographical (Francia), chronological (Early Middle Ages) and institutional settings (the monastery and its written culture) of manuscript production. The Coenotur corpus however is much more localised by focusing on the city and environs of the city of Tours, whereas the Formulae manuscripts cover large parts of the Frankish Empire.

2 This second paper will be published in Technè 56 (December 2023).

3 Gall nuts are abnormal growths that form on the young branches or twigs of plants in response to infestation by certain types of insects and by the deposition of their eggs. Those growth are rich in tannins.

4 Schopen, 2006; Ghigo et al., 2020; Cohen, 2021, p. 202; Nehring et al., 2021.

5 Brown, Clark, 2004.

6 Díaz Hidalgo et al., 2018; Hahn et al., 2021.

7 Karpenko, Norris, 2002.

8 It should be noted that while we know that this term does indeed refer to vitriol in the 16th century, notably in Agricola’s De natura fossilium, which shows an interchangeable use of the two terms, we cannot be so sure for the medieval period. Pliny the Elder uses the term as a synonym for “cobbler’s black”, which appears to be used for vitriol, Rabin, 2017. The word “vitriol”, on the other hand, is used in the 8th (Compositiones ad tingenda) and 13th centuries (Book of Minerals by Albertus Magnus). This confusion has been noted by many researchers who have tried to make sense of it, Peckham, 1941.

9 Karpenko, Norris, 2002.

10 Hahn et al., 2021.

11 Ghigo, Rabin, 2020; Ghigo et al., 2020; Cohen, 2021.

12 For example, see Roger, Barrandon, 2010. However, it should be noted that these inks were not named so; the researchers simply noted the absence of metallic contaminants usually present in vitriol. However, we can speculate that non-vitriolic inks might have been easy to prepare since they do not require vitriol, a material that was apparently imported at the time.

13 Karpenko, Norris, 2002. Furthermore, analysis of late inks leads us to believe that the purification process was probably not sufficient to remove all iron satellite elements in the ink. Giuntini et al., 1995; Del Carmine et al., 1996; Lucarelli, Mandò, 1996.

14 Vitruvius, 1847, bk. 7, sec. 10.

15 Zerdoun Bat-Yehouda, 1983, p. 81-83; Pliny (the Elder), n.d., sec. 25.

16 Zerdoun Bat-Yehouda, 1983, p. 80; Dioscorides Pedanius, secs. 182-183.

17 Preisendanz, 1931, p. 83; Zerdoun Bat-Yehouda, 1983, p. 94. The papyrus V of Leiden was found in a tomb in Thebes in the early 19th century by an adventurer, Jean d’Anastasi, and dates to the 3rd century CE.

18 Theophilus, 1986, XXXIII. Moreover, it is difficult to establish the true chronological limit of this gap since the majority of the recipes that circulate are copies and variations of ancient texts, in particular those by Vitruvius, Pliny and Dioscorides.

19 The bibliography on the subject is extremely exhaustive and has been analysed in numerous works, for some references, see Levey, 1962; Zerdoun Bat-Yehouda, 1983, p. 123-142; Chabbouh, 1995; Schopen, 2006; Raggetti, 2016; Colini, 2018, 2021; Cohen, Rabin [to be published].

20 Zerdoun Bat-Yehouda, 1983, p. 143-214.

21 Zerdoun Bat-Yehouda, 1983, p. 81-83; Pliny (the Elder), n.d., sec. 25.

22 Vitruvius, 1847, bk. 7, sec. 10.

23 Zerdoun Bat-Yehouda, 1983, p. 80; Dioscorides Pedanius, 2000, p. 182-183.

24 Zerdoun Bat-Yehouda, 1983, p. 143-214.

25 Zerdoun Bat-Yehouda, 1983, p. 144-146.

26 Zerdoun Bat-Yehouda, 1983, p. 147-148.

27 Zerdoun Bat-Yehouda, 1983, p. 148-150.

28 Garlan, 1974.

29 Zerdoun Bat-Yehouda, 1983; Nehring et al., 2021.

30 An edition of this text is available in Preisendanz, 1931, p. 83; Zerdoun Bat-Yehouda, 1983, p. 94.

31 The interpretation of those terms is an open discussion. For more details, see Christiansen, 2017.

32 Capellae, n.d., sec. 225.

33 Theophilus, 1986, XXXIII.

34 Zerdoun Bat-Yehouda, 1983, p. 156-165.

35 Hahn et al., 2021.

36 Hahn et al., 2021; Cohen, Rabin [to be published].

37 Roger, Bosc, 2008; Roger, Barrandon, 2010; Lecouteux et al., 2020; Robinet, Lecouteux, 2021.

38 Roger, Barrandon, 2010.

39 Clark, van der Weerd, 2004; Denoël et al., 2018.

40 Clark, van der Weerd, 2004; Aceto et al., 2008, 2017; Bioletti et al., 2009.

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Zina Cohen, Oliver Hahn et Ira Rabin, « Black Carolingian inks under examination. Part 1: recipes and literature survey »Technè, 55 | 2023, 90-95.

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Zina Cohen, Oliver Hahn et Ira Rabin, « Black Carolingian inks under examination. Part 1: recipes and literature survey »Technè [En ligne], 55 | 2023, mis en ligne le 16 novembre 2024, consulté le 14 février 2025. URL : http://journals.openedition.org/techne/17603 ; DOI : https://doi.org/10.4000/techne.17603

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Auteurs

Zina Cohen

Bundesanstalt für Materialforschung und -prüfung, Berlin (BAM), 4.5 Kunst- und Kulturgutanalyse (zina.cohen[at]bam.de).

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Oliver Hahn

Bundesanstalt für Materialforschung und -prüfung, Berlin (BAM), 4.5 Kunst- und Kulturgutanalyse ; Centre for the Study of Manuscript Cultures (CSMC), Universität Hamburg (oliver.hahn[at]bam.de).

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Ira Rabin

Bundesanstalt für Materialforschung und -prüfung, Berlin (BAM), 4.5 Kunst- und Kulturgutanalyse ; Centre for the Study of Manuscript Cultures (CSMC), Universität Hamburg (ira.rabin[at]bam.de).

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