Journal of Archaeological Science: Reports xxx (2015) xxx–xxx

JASREP-00140; No of Pages 8

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Journal of Archaeological Science: Reports

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PXRF analysis of pigments in decorations on ceramics in the East Mediterranean: Atest-case on Cypro-Geometric and Cypro-Archaic Bichrome ceramics at Tel Dor, Israel

Shlomo Shoval a,b,⁎,1, Ayelet Gilboa c

a Geology Group, Department of Natural Sciences, The Open University of Israel, The Dorothy de Rothschild Campus, 1 University Road, Raanana 43537, Israelb The Freddy and Nadine Herrmann Institute of Earth Sciences, The Hebrew University of Jerusalem, Edmund J. Safra Campus, Jerusalem 91904, Israelc Zinman Institute of Archaeology and the Department of Archaeology, University of Haifa, Mount Carmel, Haifa 3498838, Israel

⁎ Corresponding author at: Geology Group, DepartmenUniversity of Israel, The Dorothy de Rothschild Campu43537, Israel.

E-mail address: shovals@openu.ac.il (S. Shoval).1 Sabbatical Year status at The Freddy and Nadine Herrm

The Hebrew University of Jerusalem, Edmund J. Safra Cam

http://dx.doi.org/10.1016/j.jasrep.2015.08.0112352-409X/© 2015 Elsevier Ltd. All rights reserved.

Please cite this article as: Shoval, S., Gilboa, ACypro-Geometric and Cypro-Archaic B..., Jou

a b s t r a c t

a r t i c l e i n f o

Article history:Received 31 October 2014Received in revised form 2 April 2015Accepted 13 August 2015Available online xxxx

Keywords:Cypriot potteryEast-Mediterranean potteryIron AgeIron-based pigmentManganese-based pigmentOchre orePaint pigmentUmber ore

As part of an attempt to identify the provenances and technology of pottery in Cypro-Geometric and Cypro-Archaic Bichrome styles at Tel Dor, Israel, the black and the red paint pigments and the ceramic body wereanalysed chemically by using a pXRF apparatus in a handheld configuration. This method enables analysis ofthe thin painted decoration directly on the surface of the vessels. As a comparison, we also analysed the fabricof the vessels, as well as comparative potential Cypriot pigment ores. The analyses reveal that the black paintsconsist of manganese-based pigments comprising manganese and iron. The red paints consist of iron-based pig-ments rich in iron and poor inmanganese. In contrast, the ceramic body of the vessels is rich in silica and aluminaand contains lesser concentrations of iron and only traces of manganese. The results demonstrate the utilizationof Cypriot pigment ores (black umber and red ochre) for the painted decoration on these ceramics. Beyond thespecific Tel Dor case, the results are intended to initiate a compositional data-base of pigments on East Mediter-ranean ceramics in the Bronze and Iron Ages. We argue that to serve this end the chemical data should be pre-sented in detail, in order to enable future comparative studies.

© 2015 Elsevier Ltd. All rights reserved.

1. Introduction

1.1. Cypriot and Cypriot-style pottery at Dor

Dor is situated on the East Mediterranean seaboard, on Israel's Car-mel coast, about 30 km south of Haifa (Gilboa and Sharon, 2008). Itwas one of the main port sites along the southern Levantine littoraland its material culture through most of the late 2nd and 1st millenniaBC can be defined as Phoenician (Gilboa, 2005; Nitschke et al., 2011;Sharon and Gilboa, 2013). Among other commodities, imported Cypriotpottery, especially in the early Iron Age, occurs there more than in anyother site outside Cyprus (preliminarily for the Iron Age, Gilboa, 1989,1999).

Most of the Cypriot-style pottery at Dor dates to the Iron Age 1b–Iron 2a chronological range of Phoenicia, paralleling the Cypro-Geometric (CG) I–III periods in Cyprus, the 11th–9th centuries BC.These vessels belongmostly to CypriotWhite Painted (I–III) and CypriotBichrome (I–III) wares. Respectively, these are vessels where the

t of Natural Sciences, The Opens, 1 University Road, Raanana

ann Institute of Earth Sciences,pus, Jerusalem 91904, Israel.

., PXRF analysis of pigmentsrnal of Archaeological Science

designs are painted only in shades of black (grey and brown as well)on a light background, or with the addition of paint in various shadesof red (Gjerstad, 1948). In this period, there is also evidence for localproduction of pottery in Cypriot style (e.g., Gilboa, 1999: Fig. 5:7;Yellin, 1989; A. Georgiadou, personal communication), but currently itis unclear how extensive this phenomenon might have been. Lesserquantities of Cypriot pottery imports at Dor, of Types IV–V, belongmainly to the Iron Age 2c (7th century BC), paralleling part of theCypro-Archaic (CA) I period, and even smaller numbers originate fromcontexts of the Persian period (5th/4th centuries BC), equaling grossomodo late Cypro-Archaic II and the beginning of the Cypro-Classic(CC) period.

1.2. XRF analysis of pottery

X-ray Fluorescence Spectroscopy (XRF) is one of the methods usedfor chemical analysis of archaeological ceramics and other cultural her-itage artefacts (Liritzis and Zacharias, 2011; Goren et al., 2011; Frahmand Doonan, 2013). It provides quantitative chemical data regardingmajor elements, as well as regarding several trace elements in the com-position of ceramics (Speakman et al., 2011), slips (Scarpelli et al., 2014)and paints (Stos-Fertner et al., 1979; Hochleitner et al., 2003; Centenoet al., 2012; Attaelmanan and Yousif, 2012; Kaplan et al., 2014). How-ever, this method does not detect several ‘light’ major elements andthe detection of Al, Si, S and P, for example, requires analysis under

in decorations on ceramics in the East Mediterranean: A test-case on: Reports (2015), http://dx.doi.org/10.1016/j.jasrep.2015.08.011

http://dx.doi.org/10.1016/j.jasrep.2015.08.011shovals@openu.ac.ilhttp://dx.doi.org/10.1016/j.jasrep.2015.08.011http://www.sciencedirect.com/science/journal/http://ees.elsevier.com/jasrephttp://dx.doi.org/10.1016/j.jasrep.2015.08.011

Table 1List of Dor's Bichrome pottery studied. CG = Cypro-Geometric; CA = Cypro-Archaic; Ir = Iron Age.

Sample no. Vessel type Area/locus Reg. no. Cypriot classification Horizon

CD-64 Bichrome deep bowl B/7746 77481 CG; Bichr III UnstratifiedCD-153 Bichrome jug B/3341 33377 CG; Bichr III? Ir2aCD-121 Bichrome deep bowl B/7189 71899 CG- CA; Bichr III–IV UnstratifiedCD-223 (CYI-14) Bichrome plate D2/5251 52195 CG- CA; Bichr III–IV Ir2a?CD-272 (CYI-45) Bichrome jar D2/surface find 150957/1 CA; Bichr IV UnstratifiedCD 273 (CYI-5) Bichrome jar? D2/06D2-040 06D2-0369 CA; Bichr IV Ir2a late?CD-274 (CYI-44) Bichrome- red amphora? D2/unstratified 104837 CA; Bichr IV–V UnstratifiedCD-275 (CYI-48) Bichrome amphora D2/15213 151563 CA; Bichr IV–V Ir2b–Ir2cCD-178 (CYI-27) Bichrome-red amphora D5/10D5-219 10D5-2603 CA; Bichr IV–V? Ir2cCD-183 (CYI-41) Bichrome amphora D4/11D4-791 11D4-8276 CA; Bichr IV–V? Ir2c?CD-177 (CYI-1) Bichrome barrel jug? D5/09D5-456 09D5-8709/2 CA; Bichr IV–V? Ir2c–HellenisticCD-182 (CYI-47) Bichrome amphora D4/04D4-510 09D4-5197 CA; Bichr IV–V? PersianCD-185 (CYI-43) Bichrome trefoil jug D1/16664 168648/1 CA; Bichr V Ir2c–PersianCD-157 (CYI-8) Bichrome amphora D5/09D5-409 09D5-8743/1 CA; Bichr V Persian–Hellenistic

2 S. Shoval, A. Gilboa / Journal of Archaeological Science: Reports xxx (2015) xxx–xxx

vacuum. As well, trace elements can be measured by this method ingood accuracy (in ppm) only when they appear in sufficientconcentrations.

Another obstacle when employing on-surface pXRF specifically forthe study of decoration on pottery lies in the thinness of the paintedbands/lines. The penetration-depth of the radiation, and concomitantlythe contributions from the ceramic body substrate to the analysis de-pend on the thickness and contiguousness of the paint bands, as wellas on the atomic number Z of the detected element (Aloupi et al.,2001). For some ways to overcome this problem, at least partially, seebelow.

In the study presented here we used a portable X-ray Fluores-cence apparatus (pXRF) in a handheld configuration. The major ad-vantage of pXRF for ancient artefacts is that the method is cheap,rapid, and non-destructive and therefore can be used on a largescale. The equipment is easily movable and thus is instrumental in

Fig. 1. Examples of Dor's Cypro-Geometric and Cypro-Archaic Bichrome pottery studied: (a) bichtwo views).

Please cite this article as: Shoval, S., Gilboa, A., PXRF analysis of pigmentsCypro-Geometric and Cypro-Archaic B..., Journal of Archaeological Science

investigating artefacts that cannot be moved, such as in museums(Karydas et al., 2005).

1.3. PXRF analysis of paint on decorated pottery in the East Mediterranean

XRF analyses of paint pigment on ceramics of the ancient East Med-iterranean are still a rarity (but see, for example, Kaplan et al., 2014). Es-pecially relevant for the study presented here are in situ XRF analyses ofvarious Cypriot archaeological media, including ceramics (reported inAloupi, 2001; Aloupi et al., 2000, 2001). In Aloupi et al. (2000, 2001),this method was used for analysing the black and red paint pigmentson Cypriot decorated pottery in the Cyprus Museum (Nicosia), from avery long time-span. Interestingly, Aloupi and her co-investigators con-cluded that from ca. 5000 BC to the Middle Bronze Age, the dark(‘black’) painted decorationwas essentially based on iron-richminerals.Only from the end of the Late Bronze Age onwards (ca. 1050–325 BC;

rome barrel jug (CD-177); (b) bichromebowl (CDI-223); (c) bichrome amphora (CD-157;

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Table 2PXRF analyses (major elements in %; trace elements in ppm; each analysis is normalized to 100%) of the black paint pigments on Dor's Bichrome pottery. For the black painted bands ofeach fragment we present data of the measurements that have the highest concentration of manganese.

Black paint pigments CD-64B CD-153B CD-121B CD-223B CD-272B CD 273B CD-274B CD-275B CD-178B CD-183B CD-177B CD-182B CD-185B CD-157B

Al2O3% 25.83 22.95 21.48 24.86 31.65 27.29 27.58 18.47 27.50 14.03 13.19 20.82 26.05 24.93SiO2% 44.85 43.56 41.31 21.61 45.83 36.55 36.45 30.61 35.76 18.72 17.65 21.95 25.98 23.90P2O5% 0.22 0.15 0.17 0.21 0.49 0.16 0.23 0.17 0.26 0.39 0.39 0.22 0.11 0.23SO3% 1.67 1.62 2.09 1.57 2.36 1.81 1.57 2.66 1.62 1.18 1.89 1.57 1.88 1.34K2O% 1.98 2.17 1.29 2.06 0.97 3.49 2.81 1.26 2.88 1.30 1.49 1.15 1.31 1.53CaO% 8.32 10.17 13.49 4.93 1.85 17.50 3.50 29.89 8.88 12.09 28.82 12.71 11.89 7.52TiO2% 0.37 0.38 0.45 0.39 0.20 0.51 0.56 0.35 0.44 0.60 0.44 0.48 0.41 0.39MnO% 4.18 5.23 5.66 33.54 8.56 1.51 11.55 4.49 9.46 39.36 23.81 30.5 22.49 29.71Fe2O3% 12.32 13.58 13.79 10.54 7.94 10.91 15.45 11.88 12.93 11.88 12.05 10.16 9.64 10.17V ppm 657 352 574 610 162 338 536 390 526 829 527 567 427 482Cr ppm 388 395 558 727 182 202 991 279 571 1127 355 1714 416 561Co ppm 32 33 33 19 29 29 35 26 30 20 22 19 20 20Ni ppm 40 39 40 21 25 36 37 32 35 24 27 22 25 23Cu ppm 482 374 364 249 846 414 382 415 473 255 351 271 366 348Zn ppm 780 588 574 431 317 801 660 626 799 390 652 387 742 648Ga ppm 52 42 45 30 79 52 44 46 49 35 45 32 44 36As ppm 226 174 183 116 351 222 157 190 191 139 210 121 175 134

Table 3PXRF analyses (major elements in %; trace elements in ppm; each analysis is normalized to 100%) of the red paint pigments on Dor's Bichrome pottery. For the red painted bands of eachfragment we present data of the measurements that have the highest concentration of iron.

Red paint pigments CD-64R CD-153R CD-121R CD-223R CD-272R CD 273R CD-274R CD-275R CD-178R CD-183R CD-177R CD-182R CD-185R CD-157R

Al2O3% 24.05 24.96 26.83 23.29 28.74 29.90 29.29 24.55 25.12 18.67 17.47 25.66 28.32 24.36SiO2% 35.81 33.94 33.51 38.21 31.77 33.74 39.34 34.61 42.23 34.27 29.49 36.27 32.26 36.44P2O5% 0.24 0.22 0.29 0.19 0.24 0.17 0.15 0.26 0.28 0.45 0.45 0.01 0.14 0.05SO3% 2.54 1.83 2.20 2.07 3.25 1.56 1.62 1.96 1.16 1.45 2.17 1.99 2.26 2.17K2O% 1.38 1.82 1.40 1.45 1.96 3.97 2.87 1.68 3.17 1.23 1.61 1.92 1.13 1.79CaO% 12.88 14.73 9.47 14.47 10.77 12.69 7.06 17.06 9.08 16.65 28.16 14.75 14.15 16.25TiO2% 0.40 0.37 0.37 0.43 0.46 0.53 0.58 0.38 0.44 0.57 0.48 0.52 0.39 0.39MnO% 0.35 0.36 0.38 0.42 0.32 0.20 0.58 0.39 0.36 0.99 0.60 0.47 0.66 0.55Fe2O3% 22.08 21.54 25.22 19.29 22.18 17.07 18.3 18.88 17.94 25.37 19.31 18.21 20.45 17.77V ppm 698 522 814 442 742 345 359 415 363 788 571 474 612 311Cr ppm 601 582 1210 455 549 171 446 302 231 667 194 289 367 632Co ppm 52 51 60 48 53 32 48 38 35 58 46 46 48 43Ni ppm 55 51 55 55 57 39 55 46 42 59 56 53 51 46Cu ppm 352 339 328 393 644 485 436 513 607 426 500 453 505 384Zn ppm 553 507 414 559 1274 888 684 795 1102 1256 909 738 726 620Ga ppm 46 45 42 48 51 53 50 54 67 56 64 53 52 44As ppm 175 157 152 193 199 217 199 225 303 211 283 228 206 169

Table 4PXRF analyses (major elements in %; trace elements in ppm; each analysis is normalized to 100%) of the ceramic body of Dor's Bichrome pottery.

Ceramic body CD-64C CD-153C CD-121C CD-223C CD-272C CD 273C CD-274C CD-275C CD-178C CD-183C CD-177C CD-182C CD-185C CD-157C

Al2O3% 23.52 24.10 22.52 27.22 28.51 24.99 24.20 20.77 25.94 21.81 25.62 27.31 21.81 28.02SiO2% 46.65 40.59 42.57 43.43 42.20 36.62 40.73 35.93 43.62 44.57 43.52 38.83 41.47 42.02P2O5% 0.01 0.19 0.16 0.19 0.22 0.18 0.21 0.20 0.27 0.18 0.21 0.19 0.12 0.27SO3% 1.77 2.11 1.56 2.01 2.96 1.99 1.81 2.31 1.63 1.51 1.80 2.34 1.66 1.90K2O% 1.93 1.55 1.66 1.66 2.18 1.76 1.88 1.43 1.89 1.84 1.71 1.88 1.69 1.96CaO% 14.62 19.65 16.79 15.26 15.28 27.19 20.85 31.11 17.90 18.22 15.82 18.70 23.59 16.76TiO2% 0.38 0.41 0.45 0.39 0.40 0.41 0.45 0.34 0.42 0.50 0.47 0.51 0.39 0.41MnO% 0.10 0.09 0.11 0.10 0.05 0.06 0.09 0.07 0.08 0.10 0.09 0.07 0.11 0.09Fe2O3% 10.86 11.15 13.95 9.58 8.03 6.66 9.66 7.68 8.10 11.11 10.59 9.91 9.05 8.44V ppm 266 341 359 371 356 270 287 226 349 330 347 368 125 307Cr ppm 287 281 774 317 173 150 151 168 234 254 257 987 165 127Co ppm 27 38 44 b10 23 12 31 19 24 38 37 34 19 26Ni ppm 307 298 266 227 256 222 230 317 260 232 229 262 202 173Cu ppm 105 65 66 21 b10 93 b10 65 b10 b10 b10 49 34 37Zn ppm 27 92 18 44 310 123 36 122 b10 45 188 154 140 104Ga ppm 61 51 53 59 56 52 51 52 53 50 52 52 58 52As ppm 333 321 252 313 367 336 330 338 385 289 289 267 321 357

3S. Shoval, A. Gilboa / Journal of Archaeological Science: Reports xxx (2015) xxx–xxx

Please cite this article as: Shoval, S., Gilboa, A., PXRF analysis of pigments in decorations on ceramics in the East Mediterranean: A test-case onCypro-Geometric and Cypro-Archaic B..., Journal of Archaeological Science: Reports (2015), http://dx.doi.org/10.1016/j.jasrep.2015.08.011

http://dx.doi.org/10.1016/j.jasrep.2015.08.011

Table5

PXRF

analyses

(major

elem

entsin

%;traceelem

entsin

ppm;e

achan

alysisisno

rmalized

to10

0%)of

compa

rative

Cypriotp

igmen

tores:blackCy

prus

umbe

r(1)

from

theKam

biaminean

dredan

dye

llow

Cyprus

ochre(2,3)from

theSk

ouriotissa

and

Mitsero-Kok

kino

pezoulamines,respe

ctively.

Forea

chraw

material,wepresen

tda

tafrom

2mea

suremen

ts.

Pigm

entores

Cyprus

blackum

ber(1

a)Cy

prus

blackum

ber(1

b)Cy

prus

redoc

hre(2

a)Cy

prus

redoc

hre(2

b)Cy

prus

yello

woc

hre(3

a)Cy

prus

yello

woc

hre(3

b)

Al 2O3

18.88

27.32

17.45

18.37

24.64

18.92

SiO2

25.81

25.43

33.82

27.65

34.67

17.75

P 2O5

0.50

0.32

0.57

0.52

0.31

0.42

SO3

1.55

2.30

1.87

7.18

2.62

1.50

K2O

0.40

0.31

0.20

0.22

0.08

0.07

CaO

5.36

4.84

1.38

0.99

1.50

12.20

TiO2

0.25

0.14

0.23

0.44

0.03

0.25

MnO

23.17

19.36

0.71

0.38

0.56

0.44

Fe2O3

23.77

19.77

43.45

44.02

35.28

48.16

Vpp

m33

523

272

073

610

0398

2Cr

ppm

1335

985

931

770

758

740

Copp

m51

4210

210

990

110

Nip

pm30

2785

8764

79Cu

ppm

255

259

960

258

829

225

Znpp

m21

720

455

340

342

038

5Gapp

m28

2457

5742

53Aspp

m82

6925

017

310

514

6

4 S. Shoval, A. Gilboa / Journal of Archaeological Science: Reports xxx (2015) xxx–xxx

Please cite this article as: Shoval, S., Gilboa, A., PXRF analysis of pigmentsCypro-Geometric and Cypro-Archaic B..., Journal of Archaeological Science

roughly paralleling the time-span investigated in our study) are thedark paint pigments composed of minerals with various concentrationsof manganese (expressed as Mn3O4), and also iron (expressed a Fe2O3).They suggested that themanganese pigment originates from the Cyprusumber ore and that the red decoration was achieved through the use ofiron-based redpigment. Both in this study, and in Aloupi (2001), the po-tential of the analysis of the pigments for questions of technology andprovenience of the pottery, and to more general cultural issues inCyprus and beyond has been well illustrated. The results of these veryimportant studies, however, were presented in a very general manner.For example, in Aloupi et al. (2000), one spectrum each for the blackand red paint pigments has been published (Fig. 6 there) and no typo-logical or compositional data for specific vessels (see more on thisbelow). Similarly, Daniel et al. (2007), in a study on CA pottery fromAmathus in southern Cyprus, and applying Scanning Electron Micros-copy and Raman Spectroscopy, suggest that black pigments composedof manganese oxides were extensively employed on ceramics of thissite. There too, only a qualitative SEM spectrum of one vessel has beenpresented.

1.4. Aims of the present study

The study presented here is a first step in a wider investigation ofpigments on Bronze and Iron Age pottery in the Levant and their cul-tural meanings (see below, Future Prospects). We started with the pig-ments on Dor's Cypriot-style ceramics since concurrently we have alsoembarked on a detailed examination of this pottery, which involves sty-listic, compositional and technological aspects, and is intended to shedlight on Cypro-Phoenician interactions in the Iron Age. We began withan attempt to differentiate between genuine Cypriot vessels and localproducts in Cypriot style and to identify the specific production centresin Cyprus represented atDor, inter alia by studying the pigments.We in-deed perceive this study as preliminary. Beyond addressing the specificquestions we posed regarding Dor's pottery, the results are meant tolaunch a compositional data-base of pigments on East Mediterraneanceramics, to be used and further elaborated by ourselves and by others(cf. Hochleitner et al., 2003). We consider some aspects of pXRF opera-tions, analysis andmode of presentation of the results whichmay servethis end.

2. Materials and methods

2.1. Pottery

Table 1 lists Dor's Bichrome pottery studied. We analysed Bichromepottery only (and not WP), in order to compare between the black andred paint pigments on the same vessels. This means that the periodsrepresented in this study are only those when the Bichrome mode ofdecoration was prevalent, namely (at Dor), CG III and CA I (Gjerstad'sTypes III–V). Fig. 1 illustrates some examples of the material studied.

2.2. Potential comparative Cypriot pigment ores

In order to start to determine the sources of the ores used for thepainted decoration, we also analysed examples of some comparativeCypriot pigment ores, chosen rather randomly. The comparative Cypriotpigment ores are black Cyprus umber from the Kambia mine and redand yellow ochre from the Skouriotissa and Mitsero-Kokkinopezoulamines, respectively.

2.3. Method

The on surface pXRF analysis was conducted with a portable BrukerTracer III–V handheld XRF spectrometer of the Institute of Earth Sci-ences, The Hebrew University, Jerusalem. This apparatus is equippedwith a SiPIN Detector and excitation Source of X-ray tube Rh target

in decorations on ceramics in the East Mediterranean: A test-case on: Reports (2015), http://dx.doi.org/10.1016/j.jasrep.2015.08.011

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Fig. 2. PXRF spectral patterns of themajor elements and ‘lowmass’ trace elements (Ka1 peaks) of the black and the red paint pigments (a, b) and the ceramic body (c) in fragments CD-185and CD-223.

5S. Shoval, A. Gilboa / Journal of Archaeological Science: Reports xxx (2015) xxx–xxx

standard. For general analysis we used 40 kV, 9mA for a 60-second live-time count under vacuum. The analysis under vacuum allows the detec-tion of light elements such asAl, Si, S and P. The apparatus is operated bythe Bruker HH Programs (S1 pXRF) software. Concentrations of the ele-ments were calculated following Rowe et al. (2012). The spot size of theapparatus is ca. 4 mm in diameter.

We attempted to choose the segments where the paint pigmentswere best preserved. This was first performed visually. Since, however,it is clear that on the micro-scale the paint bands are fragmented andnot continuously distributed, at least five measurements were per-formed for each segment of paint chosen. Below we present for eachblack band the measurement that had the highest Mn concentration,and for the red bands the onewith the highest Fe concentration. It is ex-pected that the highest concentrations of these elements represent thesegments in which the paint bands are thicker and the pigments are ofhigher quality or have been better preserved. It is also expected thatanalysing thicker paint bands eliminates, or at least significantly reducesthe penetration of the radiation into the ceramic body. In order to partiallycontrol the differential effects of the atomic number Z of the detected ele-ments (see above) on the penetration of the radiation into the ceramicbody substrate, from among the trace elements we calculated and presentin the present work only the concentrations of ‘low mass’ ones (Tables 2,

Please cite this article as: Shoval, S., Gilboa, A., PXRF analysis of pigmentsCypro-Geometric and Cypro-Archaic B..., Journal of Archaeological Science

3). The elements analysed where the same as for the body of the potteryvessels and for the comparative Cypriot pigment ores (Tables 4, 5).

We analysed the concentrations of the following nine major ele-ments: Al, Si, P, S, K, Ca Ti, Mn and Fe and the following nine ‘lowmass’ trace elements: V, Cr, Co, Ni, Cu, Zn, Ga and As. We present themajor elements as oxides in % and the trace elements in ppm(Tables 2–5; for similar presentations, see for example Ravisankaret al., 2014; Scarpelli et al., 2014).

3. Results and discussion

3.1. General

PXRF spectra of the black and red paint pigments and the ceramicbody of representative sherds of Dor's Cypriot-style Bichrome potteryare shown in Fig. 2. Tables 2–4 present the concentrations of themajor elements (%) and the trace elements (ppm) in the paint pigmentsand the ceramic body of the vessels examined and Table 5 shows thesame for the Cypriot pigment ores. Concentrations of the elementswere calculated from the Ka1 peaks of the elements in the pXRF spectra;in each analysis the concentrations are normalized to 100%. For conve-nience, the results of 10 out of the 14 sherds analysed and those of the

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Fig. 3. The compositional patterns of themajor elements (represented as oxides in percentages; each analysis is normalized to 100%) of the black and the red paint pigments (a–b), and theceramic body (c) of 10 representative Bichrome sherds (data from Tables 2–5), aswell as of comparative Cypriot pigment ores (d): black Cyprus umber (1) from the Kambiamine and redand yellow Cyprus ochre (2, 3) from the Skouriotissa and Mitsero-Kokkinopezoulamines, respectively.

6 S. Shoval, A. Gilboa / Journal of Archaeological Science: Reports xxx (2015) xxx–xxx

Cypriot ores are also presented in a graphic manner (Fig. 3 for major el-ements and Fig. 4 for trace elements).

3.2. Compositional patterns

3.2.1. The ceramic bodyFigs. 3c and 4c illustrate the compositional patterns of the elements

in the ceramic body of the examined potsherds. In contrast to thepainted decoration (below), the ceramic body is rich in silica and alu-mina (36–47% SiO2 and 21–29% Al2O3; Table 4) and it contains lesserconcentrations of iron and only traces of manganese (7–14% Fe2O3and b0.1% MnO). The amounts of these oxides represent the composi-tion of the fired-clay ceramic (Shoval et al., 2006). The high concentra-tion of Ca (Table 4) reveals the use of light-coloured calcareous clays(Shoval, 2003; Fabbri et al., 2014), which accentuated the colours ofthe painted decoration without the need of applying, for example, anunderlying light slip. Among the trace elements, concentrations of Crand Ni are noteworthy in the ceramic body (127–987 ppm Cr and173–317 ppm Ni; Table 4), with commonly less amounts of Cu and Zn(b10–105 ppmCu and b10–310ppmZn). These compositional patternsare in accordancewith theutilization of Cypriot clays (Dikomitou, 2007)for the production of the investigated vessels.

3.2.2. The paint pigmentsFig. 3(a, b) and Fig. 4(a, b) illustrate the compositional patterns of

the pigments on Dor's Cypriot-style pottery. The black bands consist ofmanganese-based pigments, comprising manganese and iron (2–39%MnO and 8–15% Fe2O3; Table 2). The red bands consist of iron-basedpigments rich in iron and poor in manganese (17–25% Fe2O3 and b1%MnO; Table 3). Both red and black paint pigments also contain themajor elements Al, Si, K and Ti. These elements either originate fromthe ore sources and/or are contributed by the ceramic body. Amongthe trace elements, concentrations of Cu and Zn are noteworthy in the

Please cite this article as: Shoval, S., Gilboa, A., PXRF analysis of pigmentsCypro-Geometric and Cypro-Archaic B..., Journal of Archaeological Science

paint pigments (249–846 ppm Cu and 317–801 ppm Zn in the blackpaint pigments; Table 2, and 328–644 ppm Cu and 414–1274 ppm Znin the red paint pigments; Table 3).

3.3. Comparison of the composition of the pigments to those of Cypriot ores

The high concentrations of manganese and/or iron in the paint pig-ments indicate the utilization of pigments from ore sources (Barnettet al., 2006). Since most (but not all, see above) Cypriot-style vesselsat Dor were likely genuine imports from Cyprus we investigated thepossibility that Cypriot pigment ores were utilized for producing thedecoration on the specific sherds examined. Figs. 3d, 4d illustrate thecompositional patterns of the elements in comparative Cypriot pigmentores. It is expected that the chemical signature of the paint pigmentswill be similar to that of the distinct manganese and iron ore sourcesthat were used to produce them.

3.3.1. The black pigmentsThe compositions of the black paint pigments indicate the utilization

of black ferromanganese pigment ore. In general, globally, manganeseores are not widespread (but see further below, Future Prospects), how-ever in Cyprus they are found in association with the copper deposits(the Cypriot umber ore; Robertson and Hudson, 1973; Ravizza et al.,2001). The compositional patterns of the black paint pigments on theDor fragments are indeed compatible with a utilization of Cyprusumber for the black decoration. Similar to the composition of theblack pigments (Table 2), the Cyprus umber we examined containsmanganese and iron oxides (approximately 19–23% MnO and 20–24%Fe2O3, Table 5). In the black paint of several sherds the concentrationof Fe2O3 is higher than that of MnO and in others the opposite is true(Table 2, Fig. 3a). These differences are probably related to the utiliza-tion of ores from different Cypriot provenances.

in decorations on ceramics in the East Mediterranean: A test-case on: Reports (2015), http://dx.doi.org/10.1016/j.jasrep.2015.08.011

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Fig. 4. The compositional patterns of ‘low mass’ trace elements (in ppm) of the same ceramic samples illustrated in Fig. 3, as well as of comparative Cypriot pigment ores: black Cyprusumber (1) from the Kambia mine and red and yellow Cyprus ochre (2, 3) from the Skouriotissa and Mitsero-Kokkinopezoulamines, respectively.

7S. Shoval, A. Gilboa / Journal of Archaeological Science: Reports xxx (2015) xxx–xxx

3.3.2. The red pigmentsThe compositions of the red paint pigments indicate the utilization

of red ferruginous pigment ore. In general, iron pigment ores are glob-ally very common (Barnett et al., 2006). Examples in Cyprus are ochreores (Ravizza et al., 2001) and other iron-rich deposits (Hradil et al.,2003). The compositional patterns of the red pigments on the Dor frag-ments are in accordance with a utilization of Cypriot ores: similar to thecomposition of the red paint pigments (Table 3), the examined redCyprus ochre ore is rich in iron and poor in manganese (approximately43–44% Fe2O3 and b0.7% MnO, Table 5). The lower concentrations ofFe2O3 in the red paint pigments (Table 3) with respect to the redochre ore (Table 5) may stem from dilution (with clays) during thepreparation of the pigment or from the utilization of iron-rich de-posits with concentrations of iron that are lower than those in theochre.

Among the trace elements, concentrations of Cu and Zn in the pig-ment ores are noteworthy (255–259 ppm Cu and 204–217 ppm Zn inthe Cyprus black umber ore, and 258–960 ppm Cu and 403–553 ppmZn in the Cyprus red ochre ore; Table 5). These compositional patternsare in accordance with the utilization of Cypriot pigment ores for thepainted decorations of the investigated vessels.

Thus, the analysis of the ceramic body and the painted decorationconfirms that at least the examined Cypriot-style Bichrome ceramicsfrom Dor are genuine imports from the Island. As mentioned, sincethe pXRFmethod is easily implementedwe intend to employ it to inves-tigate Dor's Cypriot ceramics on a much larger scale.

4. Future prospects: comparative studies

As mentioned in our introduction, we perceive our study as a smallstep in a wide-scale comparative investigation of pigments employedon ceramics in the EastMediterranean. For example, preliminary resultsof an analysis we conducted on Late CypriotWhite Slip vessels from Tellel-Assawir on Israel's Sharon plain shows that though the black bands

Please cite this article as: Shoval, S., Gilboa, A., PXRF analysis of pigmentsCypro-Geometric and Cypro-Archaic B..., Journal of Archaeological Science

on them are starker (and ‘nicer’) than those on the CG–CA vessels pre-sented here, the Mn ratios in the former are in fact generally lower. Aswell, black bands on decorated Canaanite vessels from Late BronzeAge contexts at the same site indeed reveal significant lower Mn ratiosthan those on the Cypriot wares, but still high enough to indicate thatthe pigments were not procured in the site's vicinity. Possible sourcesare, for example, the Mn-rich copper deposits of Timna and Feinan inthe Aravah plain, several hundreds of km away (e.g., Yahalom-Macket al., 2014); other (also rather far) locales in the Levant; and indeedCyprus. This means that the possibility of inter-regional trade inpigments should be considered. As well, our analysis shows thateven among the Cypriot potsherds examined here, general similaritiesin the compositions of pigments notwithstanding, there is stillconsiderable variability between the compositions of the paints onthe different vessels (Tables 2, 3). This may indicate different Cypriotprovenances and/or various technological choices. As a complementarymethod of analysis for the pigments we intend to use Laser AblationInductively Coupled Plasma Mass Spectrometry (LA-ICP-MS), which isa more accurate method, but much more expensive, destructive tosome extent, and cannot be performed on objects that are more thana few cm large. It therefore cannot be used on a large scale and willnot completely replace XRF. We submit that only a detailed investiga-tion and presentation of the chemical compositions of pigments andtheir potential sources (including various sources in Cyprus)will enablefuture comparative research that will elevate the study of pigments onEastern Mediterranean pottery to a regionally-meaningful avenue ofcultural inquiry.

Acknowledgements

This research is supported by the Israel Science Foundation(grant no. 209/14) and by the Research Funds of the Open Univer-sity of Israel (grant no. 31016). These supports are gratefullyacknowledged. This work was partially carried out while the firstauthor was on sabbatical at the Institute of Earth Sciences of The

in decorations on ceramics in the East Mediterranean: A test-case on: Reports (2015), http://dx.doi.org/10.1016/j.jasrep.2015.08.011

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Hebrew University, Jerusalem. The first author expresses his appre-ciation to Prof. Oded Navon of this Institute for his collaborationand to Prof. Yigal Erel for the permission to use the XRF apparatus.We thank Dr. Costas Xenophontos for providing us with Cypriotumber and Cypriot ochre. We are grateful to Prof. Ilan Sharon, co-director of the Tel Dor excavations, to Dr. Anna Georgiadou forher comments on the vessels analysed and to Paula Waiman-Barak for her help in various aspects of this research. The prelimi-nary Tell el-Assawir results are mentioned courtesy of Dr. Shai Barand Golan Shalvi.

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PXRF analysis of pigments in decorations on ceramics in the East Mediterranean: A test-case on Cypro-Geometric and Cypro-...1. Introduction1.1. Cypriot and Cypriot-style pottery at Dor1.2. XRF analysis of pottery1.3. PXRF analysis of paint on decorated pottery in the East Mediterranean1.4. Aims of the present study

2. Materials and methods2.1. Pottery2.2. Potential comparative Cypriot pigment ores2.3. Method

3. Results and discussion3.1. General3.2. Compositional patterns3.2.1. The ceramic body3.2.2. The paint pigments

3.3. Comparison of the composition of the pigments to those of Cypriot ores3.3.1. The black pigments3.3.2. The red pigments

4. Future prospects: comparative studiesAcknowledgementsReferences