Physical Study of Cucuteni Pottery Technology

8102019 Physical Study of Cucuteni Pottery Technology

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Physical study of the Cucuteni pottery technology

Florica Matau ab Valentin Nica a Petronel Postolache a Irina Ursachi a Vasile Cotiuga bcAlexandru Stancu a

a Faculty of Physics ldquo Alexandru Ioan Cuzardquo University of Iasi Boulevard Carol I 11 700506 Iasi Romaniab Department of Sciences ARHEOINVEST Platform of Interdisciplinary Research in Archaeology ldquo Alexandru Ioan Cuzardquo University of Iasi Lascar Catargi St 54 700107 Iasi Romaniac Faculty of History ldquo Alexandru Ioan Cuzardquo University of Iasi Boulevard Carol I 11 700506 Iasi Romania

a r t i c l e i n f o

Article history

Received 20 December 2011Received in revised form1 August 2012Accepted 22 August 2012

Keywords

Cucuteni culturePottery technologyMagnetic measurementsFORC diagramRietveld analysis

a b s t r a c t

Most of our knowledge concerning the Cucuteni pottery is based on traditional archaeological methods(typology style and context analysis) and only a few interdisciplinary studies have been published Asthere is a strong interest in revealing the basic pottery technology used by the Cucuteni communities wehave investigated a signi1047297cant number of pottery samples from 22 archaeological sites located in EasternRomania by several physical analysis techniques X-ray diffraction (XRD) and by magnetic measure-ments including a 1047297rst-order reversal curve (FORC) diagram study on the samples showing a hystereticbehavior The main results presented in this study are discussed and compared with actual knowledge onthe ancient Cucuteni pottery

2012 Elsevier Ltd All rights reserved

1 Introduction

Archaeological research based on the examination of wareshape color decoration and overall fabric provides a wealth of information concerning typological stylistic and functional issuesTo complement such taxonomy schemes archaeologists oftenresort to an interdisciplinary approach involving physical sciences

The physical properties of the potteries like color texture andsize of the clay particles composing them can be used in order todetermine the technology of manufacture and method of 1047297ringadopted by the Cucuteni communities The estimation of the 1047297ringtemperatures throws light on the pyro-technological abilities of theCucuteni artisans and on the pottery production scale during theChalcolithic period in South-Eastern Europe In the pottery

production process the heating rate and length of exposure time toheat (the soaking time) appear to be the most suitable parametersfor understanding the 1047297ring technology For this reason the esti-mate 1047297ring temperature on potshards is evaluated as equivalent1047297ring temperature which may not be the same with the 1047297ringtemperature set initially (Gosselain 1992 Livingstone Smith2001) From the knowledge of the equivalent 1047297ring temperature

one may be able to conclude how the 1047297ring process evolved andhow the raw clay was tempered and used to model the vessels

We are targeting the Cucuteni culture area which was not yetsystematically studied with modern physical characterization toolsThis objective is obviously very ambitious and requires time andresources and cannot be accomplished in one step or studyAccordingly this paperrsquos aim is to start this project by analyzinga signi1047297cant sample of Cucuteni culture pottery (50 potshards)from a wide geographical area within Romania X-ray diffraction(XRD) and magnetic measurements including a 1047297rst-order reversalcurve (FORC) study are the main physical techniques presented inthis paper to estimate the 1047297ring temperature

Examples of studies covering similar topics using differentresearch techniques can be found in the literature (Maniatis and

Tite 1981 Maggetti et al 2011 Tudisca et al 2011) Previousresearch has included mostly measurements of the susceptibilityand intensity of natural magnetization of archaeological samplessaturation isothermal remanence and also anhysteretic remanentmagnetization (ARM) intensities (McDougall et al 1983) Most of these studies have applied rock magnetic characterization toobsidian samples from Eastern Mediterranean region (McDougallet al 1983) Argentinian and Chilean Patagonia (Vasquez et al2001) and central Mexico (Urrutia-Fucugauchi 1999) Mooneyet al (2003) employed magnetic susceptibility and isothermalremanence measurements to provenance studies of archaeologicalochre quarries from Australia In order to identify clay sources and

Corresponding author Fax thorn40 232 201205E-mail address alstancuuaicro (A Stancu)

Contents lists available at SciVerse ScienceDirect

Journal of Archaeological Science

j o u r n a l h o m e p a g e h t t p w w w e l s e vi e r c o m l o c a t e j a s

0305-4403$ e see front matter 2012 Elsevier Ltd All rights reserved

httpdxdoiorg101016jjas201208021

Journal of Archaeological Science 40 (2013) 914e925





conditions as well as the use of high 1047297ring temperature and theconstruction of elaborate up-draught kilns (Ellis 1984)

This study focuses on the Cucuteni pottery in Romania but itshould be remembered that closely related prehistoric communi-ties lived in Ukraine and the designation CucutenieTrypillia oftenis used to refer to the entire cultural tradition

3 Sampling and analytical methods

31 Sample selection

The data set for this investigation contains 50 pottery fragmentssampled to represent the stylistic and technological diversity of theCucuteni culturersquos potshards (see Fig 2 and Table 1) These pot-shards were selected from twenty-two archaeological sites (seeFig 3) Samples were taken from the body of the pottery fragmentsavoiding 1 mm surface layer

32 XRD analysis

All the solid samples were ground in an agate mortar and gentlyside-pressed intoa top-loaded holder in order to minimize preferredorientation XRD patternswere recorded using Shimadzu LabX XRD-6000 powder diffractometer with a diffracted beam graphitemonochromator of CuKa radiation (l frac14 15406 A) The specimensmounted in re1047298ection mode were analyzed in ambient atmosphereover the range 2q frac14 2e100 with scanning angle rate of 003 anda 2 sstep count time Qualitative analysis was automaticallyperformed (Shimadzu LabX software) by comparison with thereference powder patterns included in ICDD Powder DiffractionFile (PDF2-2004) Mineral phase quanti1047297cation was made by theRietveld method

The software Diffrac plus TOPAS Version 21 (Bruker AXS GmbHGermany 2003) which implements fundamental parametersapproach (FPA) (Cheary and Coelho1992) was used forquantitativephase analysis by Rietveld re1047297nement The FPA uses a convolution-

based pro1047297le 1047297tting calculated from the emission pro1047297le instru-mental and sample contributions without a reference sample Theglobal factors included the scale factor 2q zero error correctionLorentz polarization factor Chebyshev polynomials of background1047297tting and crystal linear absorption coef 1047297cient were re1047297ned for allthe patterns Positions occupancy factors and overall isotropicdisplacement parameters of individual atoms for all phases exceptfor general atomic positions of quartz were 1047297xed during phaseanalysis The effect of preferred orientation for some crystallinephase (eg mica) was taken into account using the MarcheDollasefunction (Dollase 1986) Lattice parameters and mean crystallitesize of the mineral phases were also optimized in order to providethe best pattern1047297tting (Young1993) The starting values for atomicparameters were extracted from the Inorganic Crystal Structure

Database (ICSD) (ICSD 2011)The Rietveld re1047297nement method uses a non-linear least squares

approach to simulate the measured pattern pro1047297le (Rietveld 1969)The quality of the 1047297tting procedure is indicated by a weightedsum of squares of deviations between the calculated and the

experimental diffraction patterns (Rwp) and an estimation of thebest possible Rwp pro1047297le based on the statistical noise of themeasured diffraction pattern (Rexp) The quality of the 1047297t is deter-mined from the expected and weighted pro1047297le R-factorsGOF frac14 (RwpRexp)2 that for the best 1047297tting should be equal to 1(Young 1993) The relative mineralogical phase compositionsexpressed as weight percent (wt) of crystalline phases with cor-responding standard deviation and the GOF obtained from theRietveld re1047297nement are listed in Table 2

33 Magnetic measurements

Magnetization curves of the powdered pottery fragments weremade with a vibrating sample magnetometer (Princeton Measure-ments Co MicroMag VSMampAGM 2900-3900) The maximum 1047297eldapplied was 12 T Measurements were carried out at roomtemperatures with less than 1 s averaging time per point Thismeasurement system is very good especially when a large numberof data are required like in the FORC technique that contains typi-cally about 10000 experimental points for one diagram

4 Results and discussion

41 XRD measurements

Technological issues are revealed by mineralogical studiesaiming to determine the type of raw clays and tempering materialsused as well as the 1047297ring temperature and atmosphere to whichthey have been submitted For the reconstruction of the Cucutenipottery technology what becomes important is not the high-temperature thermal behavior of individual clay minerals but thetransformations at high temperatures of the various phases Thesephases can be the result of the decomposition of the clay mineralsthemselves and also of any non-plastic inclusions which might bepresent such as carbonates or even organic material (Pollard andHeron 2008)

The XRD results showed different mineralogical and phasecontents for all the selected Cucuteni shards Quartz [SiO2] clayminerals illitemuscovite [(K H3O)Al2Si3AlO10(OH)2][KAl2Si3A-lO10(OH)2] and kaolinite [Al2Si2O5(OH)4] feldspars (K-feldspar(KAlSi3O8) and plagioclase albite [NaAlSi3O8] and anorthite[Ca(Al2Si2O8)]) carbonated minerals calcite [CaCO3] pyroxenesdiopside [CaMg(Si2O6)] and augite [(Ca Na) (Mg Fe Al Ti) (SiAl)2O6] clinochlore [Al2Mg5Si3O10(OH)8] and iron mineralshematite [a-Fe2O3] and magnetite [Fe3O4] were identi1047297ed (Table 3)The study of the present mineralogical contents of the Cucutenipottery samples enables to estimate the equivalent 1047297ring temper-ature We noted that the process of 1047297ring does not necessarilyachieve a mineral assemblage which is at thermodynamic equi-librium and this must be remembered in any attempt to predict the

1047297ring properties (Rathossi et al 2004) The melting point of variousphases becomes critical in high temperature reactions sinceimpurities in the clay usually mean that suf 1047297cient 1047298uxes are presentto melt (or sinter) at least some of the phases (Pollard and Heron2008)

Fig 2 Representative samples of the Cucuteni painted pottery

F Matau et al Journal of Archaeological Science 40 (2013) 914e925916



The mineralogical composition of most of the selected pottery

samples determined within the XRD analysis due to the hightemperatures they have been 1047297red do not provide signi1047297cantinformation on the mineralogical composition of the clay that hasbeen used for their production The destruction of the pre-existingmatrix structure does not occur instantaneous ( Jordaacuten et al 1999)The now-existing pottery matrix was obtained through the 1047297ringprocess in which these crystalline phases once they exceed theirstability limits partially decompose and simultaneously others arebeing formed ( Jordan et al 2008)

The ceramic materials from the studied pottery samples can bede1047297ned as illitic clays withhighsandcontent except samples 9D and12E in which kaolinite is present together with illitemuscovite Theresults from the XRD analysis of the mineralogical transformationsshow the persistence of illitemuscovite up to at least 900 C

(Rathossi et al 2004 Jordan et al 2008 Iumlssi et al 2011) in samples

These correspond with the phyllosilicates evolution upon 1047297ring

which starts with the dehydroxylation of the illitemuscovite phaseat700 C till it disappears at 900 C (Cultrone et al2001) Accordingto Papachristodoulou et al (2006) the complete destructionof illitemuscovite ranges between 950 C and 1000 C and depending onthe composition of the ceramic body ensures the development of diopside andalso gives increment to iron oxides such as hematite If the 1047297ring temperature does not exceed this range these mineralsstill continue to exist as can be observed in 42 potshards

Quartz remains the main abundant phase at any 1047297ringtemperature except in samples 7D 17G 20H 26J 27J 28J 34M39P and 40P in which K-feldspar is the dominant phase Newphases develop in the pottery samples upon 1047297ring diopside andaugite appear at 800e900 C and show a signi1047297cant increase inquantity and in the main diffraction peak at higher temperatures

(Iumlssi et al 2011)

Table 1

Archaeological analysis of the Cucuteni pottery samples

Sample Siteacronym

Paste Kneading Coarse size Firing atmosphere Style

Fine Medium Poor Fine Poor Small Different sizes Oxidizing Reducing Cucuteni A Cucuteni AeB Cucuteni B Cucuteni C

Complete Incomplete

1 A 2 A

3 B 4 B 5 C 6 C 7 D 8 D 9 D 10 D 11 E 12 E 13 E 14 F 15 F 16 F 17 G 18 G 19 G 20 H 21 H 22 I 23 I 24 B 25 B 26 J 27 J 28 J 29 K 30 K 31 K 32 K 33 L 34 M 35 M 36 N 37 O

38 O 39 P 40 P 41 Q 42 R 43 R 44 S 45 S 46 S 47 T 48 U 49 U 50 V

F Matau et al Journal of Archaeological Science 40 (2013) 914e925 917



Calcite decomposition into CaO and CO2 begins at a tempera-ture of 650 C and this phase disappears at 900 C giving rise tonew high temperature calco-silicates and alumino-calco-silicates

such as the members of the pyroxene group (diopside) and someof the plagioclase feldspars (anorthite) (Riccardi et al 1999Cultrone et al 2001 Papachristodoulou et al 2006 Iumlssi et al2011) Calcite is present in samples 8D 14F and 25B in variousamount ranging from 169 in sample 8D to 251 in sample 14F

and 473 in sample 25B as it was determined by the Rietveldquantitative analysis The absence of diopside in sample 8D

indicates that calcite is of primary origin and not a result of post-burial deposition processes allowing to consider that the shardwas submitted to a low 1047297ring temperature below 800 C(Papachristodoulou et al 2006) The high amount of calcite insamples 14F and 25B could be explained by the crushed shellsused as temper in the Cucuteni C pottery type (Dodd-Opritescu1982) The presence of diopside (1) in sample 25B indicates

that the 1047297ring temperature was of at least 850

C (Maggetti et al2011 Papachristodoulou et al 2006)Iron minerals found in the samples may also help assessing the

1047297ring temperature and atmosphere (Iumlssi et al 2011) Hematite ispresent in different quantities ranging from 05 (sample 49U) upto 39 (sample 26J) in 45 of the selected samples Besides hema-tite 11 pottery samples (5C 13E 16F 19G 24B 28B 32K 33L 36N40P and 50V ) contain different amounts of magnetite (from 19 insample 24B up to 79 in sample 50V ) Samples 35M (2) and 48U

(79) have only magnetite as iron minerals For the shards con-tainingonly hematite we estimate that the1047297ring cycle was ended inoxidative atmosphere (Papachristodoulou et al 2006 Iumlssi et al2011) The association of hematite with magnetite is due to theincomplete reduction phase of Fe3thorn compounds during the

reducing phase of 1047297

ring (Mangone et al 2008)

The neo-mineral formation temperatures may be affected by1047297ring type such as pit or kiln 1047297ring Calcite decomposition endsaround 825 C in kiln 1047297ring but tends to 875 C in pit 1047297ring

conditions (Maritan et al 2006) These mineralogical trans-formations are related to peak 1047297ring temperature soaking timeabundance and type of mineralphases present 1047297ring atmospherepressure and the speci1047297c area of components (Iumlssi et al 2011) Alsothese are in1047298uencedby the surface area from where the sample wasselected (Maggetti et al 2011)


The use of magnetic measurements on potshards was suggestedmanyyears ago(Coey et al 1979) and its importance was especiallydue to the variety of the magnetic properties shown by samples of pottery (Schmidt 2007) Magnetic measurements were used ininvestigation of the source materials (Evans 1979 McDougall et al

1983 Urrutia-Fucugauchi 1999 Rasmussen 2001 Vasquez et al2001 Mooney et al 2003 Linford 2005) manufacture tech-niques used (Coey et al 1979 van Klinken 2001 Constanzo-Alvarez et al 2006 Beatrice et al 2008 Rada et al 2008 RadaTorres et al 2011) or in archaeomagnetic dating of archaeolog-ical sites (Kovacheva et al 2001 Zananiri et al 2007 Suteu et al2008 Spassov et al 2008 Catanzariti et al 2008 de Marco et al2008 Herries et al 2008)

Essentially these methods are built on the idea that themagnetic properties of pottery samples can be correlated not onlywith the composition of the clay but also with the thermal processused during the production The magnetic characterization tech-niques speci1047297c to these studies are originated in the paleomagneticstudies targeted on the magnetic carriers of remanent magnetiza-

tion and on the various magnetization processes responsible for the

Fig 3 Distribution map of the Cucuteni sites from where the pottery samples were selected for analysis Legend A Ghelaiesti Neamt county B Lunca Neamt county C Tolici

Neamt county D Trusesti Botosani county E Izvoare Neamt county F Solca Suceava county G Valeni Neamt county H Bodesti Neamt county I Raucesti Neamt county J

Tg Ocna Bacau county K Poduri Bacau county L Dumestii Noi Vaslui county M Rafaila Vaslui county N Bacesti Vaslui county O Malusteni Vaslui county P Vorniceni

Botosani county Q Scanteia Iasi county R Fetesti Suceava county S Cucuteni Iasi county T Sangeorgiu de Mures Mures county U Ariusd Covasna county V Malnas Covasna

county






magnetization of rocks We mention for example the use of naturalremanent magnetization the bulk magnetic susceptibility and theintensity of isothermal remanent magnetization (McDougall et al

(1983) for samples from Mediterranean region Vasquez et al(2001) for samples from Argentina and Chilean Patagonia) AFdemagnetization of the saturation isothermal remanent magneti-zation was reported in Urrutia-Fucugauchi (1999) for samples fromCentral Mexico Rasmussen (2001) added Magnetic Susceptibilityand Luminescence measurements for provenance studies of pottery at three different sites in Denmark To distinguish betweendifferent ochre sources from Australia Mooney et al (2003) addedthe anhysteretic remanent magnetization to the previously usedmagnetic parameters (susceptibility and isothermal remanence)Beatrice et al (2008) for tile samples from Pompeii and Gravina diPerugia (Italy) combined magnetic properties with colormeasurements Constanzo-Alvarez et al (2006) and Rada Torreset al (2011) for samples from Venezuelan islands associated

dielectric measurements to magnetic parameters

Two main dif 1047297culties in the simpler interpretation of themagnetic data are always recognized by the researchers workingin paleomagnetism and these problems are mentioned also in thepreviously cited articles One is the size dependence of themagnetic properties of particles and the other is the strongin1047298uence of the inter-particle magnetic interaction on anymagnetization process used for the characterization It is recog-nized that very small ferromagnetic particles can show a super-paramagnetic behavior with no remanence in zero applied1047297eld asthe thermal energy is bigger than the energy barrier betweenstable equilibrium states The bigger particles can have a rema-nent moment but this remanence depends on the size of theparticles Small blocked particles have a single-domain behaviorsimilar to the one described by the well-known StonereWohlfarthmodel (Stoner and Wohlfarth 1948) but as the volume increasesa pseudo single domain state or even a multidomain state can beobserved in the particles Methods to separate these differentstates were studied intensely (Dunlop and Oumlzdemir 1997) but theresults are not always credible As mentioned for example byTauxe (2002) ldquophysical interpretation of hysteresis loops is morecomplex and simple plots of the ratios alone are virtually mean-inglessrdquo We also mention that the characterization by single

parameters (like remanence coercivity other similar) have theinherent problem that canrsquot discriminate in a unique formbetween different contributions of particles from differentmaterials with various anisotropies easy axes orientationvolumes shape etc The other problem that is avoided carefullyby most of the mentioned studies is the problem of inter-particlemagnetic (mostly magnetostatic) interactions As the particledensity is not the same in all the samples and consequently theeffect of interactions is unknown in the performed experimentsthis adds errors dif 1047297cult to evaluate in the global magnetic char-acterization process As a 1047297nal remark on the problems related toclassical magnetic studies we mention the complex behavior of the reversible component of magnetization in ensembles of ferromagnetic particles especially when some of the particles are

superparamagnetic and others with bigger volumes are blockedThe coupling by interactions between the reversible and irre-versible (related only to moment switching) make the problemeven more complicated (see for example Bodale et al 2011) Thereversible component is present in all the susceptibilitymeasurements and consequently should be accounted correctly inthis type of measurement Again the correct account of interac-tions is of paramount importance for the magnetic characteriza-tion The need for new magnetic characterization techniques ableto provide the kind of information not given by the classicaltechniques is evident

About one decade ago the use of another magnetic character-ization technique namely the 1047297rst-order reversal curves (FORC)diagram method was proposed by Pike et al (1999) from the

Department of Geology University of Davis California In thementioned paper and in the subsequent publications (Pike et al1999 Roberts et al 2000 Pike et al 2001a 2001b Pike 2003Stancu et al 2003a) it was shown that this technique can offer notonly accurate information concerning the inter-particle interac-tions in particulate ferromagnetic media but also the distribution of the particles as a function of the coercive1047297eld As the potshards areessentially particulate media a logical consequence would be theuse of this method in archaeomagnetic studies as well

The FORC technique was in fact described for the 1047297rst time byMayergoyz (1991) before the publication of the mentioned paperof Pike et al (1999) The method was designed to identify thePreisach distribution (the distribution of coercive and interaction1047297elds) for systems correctly described by the classical Preisach

model (CPM) (Preisach 1935) As stated by Mayergoyz (1991) in

Table 3

The results of magnetic measurements

Sample S Mass Saturation Hc M s

Units g emu Oe emug

1 029 002 002 15041 0822 010 002 000 7191 0213 022 004 002 10239 0474 010 003 001 4600 027

5 032 002 001 14954 0676 011 003 001 5149 0227 016 002 001 7425 0528 006 006 001 5545 0109 009 001 000 4457 02110 014 001 001 5490 04111 010 002 001 6777 02512 010 001 000 5850 03813 030 003 002 11457 08314 008 003 001 4362 02415 013 003 001 6540 03816 022 002 001 14890 03617 037 002 002 11933 08918 003 002 000 3646 00819 039 001 000 69519 02720 005 001 000 4480 01821 009 003 001 5513 021

22 015 002 001 7752 03923 014 004 002 5567 05124 004 002 000 3047 01125 010 005 001 6180 02726 012 003 001 4545 02627 024 002 001 7563 05528 016 004 001 17044 02229 025 001 000 14633 03530 010 002 000 5639 01731 028 003 002 10839 08232 024 003 002 8877 06433 012 003 001 8491 02034 022 002 001 8360 04435 021 003 004 8889 13536 023 002 001 9858 06037 020 003 002 6891 04838 015 002 000 5692 03039 022 002 000 26814 01740 043 001 001 19961 12341 005 004 001 2905 01642 014 001 001 6657 04143 028 004 002 13184 05344 032 002 002 12102 09045 020 002 001 11076 02846 005 002 000 3997 01147 020 002 001 15239 03648 012 001 000 8888 01849 015 005 003 6379 04850 024 002 001 10577 048




the representation theorem the systems should obey to wiping-out and congruency properties in order to be described by theCPM As a consequence of this theorem one 1047297rst has to checkexperimentally if the samples show wiping-out and congruencyproperties and then to apply an identi1047297cation technique based onFORCs measurement The wiping-out property can be tested bymeasuring minor hysteresis loops and observing if these loops areclosing perfectly Most magnetic samples have this property Thecongruency property is more dif 1047297cult to be experimentally provenas it requires to see if the minor loops measured between thesame 1047297eld limits (regardless of the way one obtains the initialpoint on the minor loop) are congruent (if one translates the loopsalong the moment axis the minor loops should be identical) Thisproperty is dif 1047297cult to be checked extensively as it requires a largenumber of measurements Theoretically a system obeyingcongruency property should have a distribution of interaction1047297elds not dependent on themagneticstate of the sample which inreal systems is dif 1047297cult to imagine Systematic studies of inter-action 1047297eld distribution in correlation with the congruencyproperty were at the origin of modi1047297ed Preisach models (DellaTorre 1999)

What is really important in the paper published by Pike and

collaborators (Pike et al 1999) was the proposal to use the FORCmethod as a purely experimental technique which will providea distribution named FORC distribution that will be an approxi-mation of the Preisach distribution and will be characteristic to themeasured sample In time many laboratories have followed thisidea and gradually a large number of typical diagrams were iden-ti1047297ed for speci1047297c magnetic samples (Stancu et al 2003aMuxworthy et al 2004 Sagnotti et al 2005 Wehland et al 2005Carvallo et al 2006 Smirnov 2006) and characteristic featureswere linked to physical properties of the samples It has beenshown that some of the typical features observed on experimentalFORC diagrams can be explained within the modi1047297ed Preisachmodels and that the real distributions of interaction and coercive1047297elds can be calculated from FORC experimental data (Stancu et al

2003a Postolache et al 2003 Stancu et al 2006) The FORCdiagram method is now one of the most popular methods tocharacterize magnetic hysteresis in various systems ferromagnetic(recording materials (Stancu et al 2000 Muxworthy and Dunlop2002 Sagnotti et al 2005 Smirnov 2006) natural magneticsamples e geophysics (Muxworthy 2001 Wehland et al 2005Roberts et al 2010) and even in very complex nanomagneticstructured media (Muxworthy and Williams 2005 Carvallo et al2006)) non-ferromagnetic (spin-transition materials) (Enachescuet al 2005 Tanasa et al 2005) ferroelectric (Stancu et al2003b) and in other hysteretic systems (Carvallo and Muxworthy2006)

The 1047297rst-order magnetization curve can be measured startingin a point from the major hysteresis loop One can use points on

the descending or ascending branches of the major loop If onediscusses the FORCs starting from the descending branch of themajor hysteresis loop the measurement starts after the sample ispositively saturated and then a smaller 1047297eld is applied to thesample (usually applied in the negative direction) This 1047297eld iscalled reversal 1047297eld and is the starting point of one FORCmeasurement (see Fig 4) Instead of continuing the measurementtowards the negative saturation as in the classical measurement of the descending branch of the major hysteresis loop starting withthe reversal 1047297eld H r the 1047297eld is increased gradually until thepositive saturation is obtained again One FORC is measuredbetween the reversal 1047297eld and the 1047297eld suf 1047297cient to saturate thesample in the positive direction again As the major loop isconsidered conventionally as a zero order magnetization curve the1047297

rst-order magnetization curve is theone that has theinitial point

on the zero-order curve and for which the 1047297eld value changes in

the opposite direction to the measurement on the zero-ordercurve As we have discussed in our example on the descendingbranch of the major loop the 1047297eld is decreasing but on the FORCstarting from H r the 1047297eld is increasing In a similar manner if ata certain moment one interrupts the measurement on the FORC ina 1047297eld H r1 and instead of increasing the 1047297eld one starts decreasingit we shall obtain a second-order magnetization curve What isessential to mention is that the magnetization measured in onepoint on the FORC is dependent on two 1047297elds (H H r) where H isthe actual 1047297eld in the experimental point It can be rather easilyshown that the second order mixed derivative of the momentmeasured on the FORC m

FORCethH H rTHORN is proportional to the FORCdistribution

rFORCethH H rTHORN frac14 12v2mFORCethH H rTHORN

vH vH r

which for the CPM systems is identical with the Preisach distri-bution as we have already mentioned

When applied to experimental data one has to cover the major-hysteresis loop with FORCs (typically 100 experimental curves) andwith a numerical algorithm one evaluates the derivative andobtains the FORC distribution As shown in Fig 5 1047297nally onerepresents the contour plot of the FORC distribution in (H H r)coordinates If one rotates the system with 45 one can representthe diagram in (H c H s) coordinates (where H c frac14 (H H r)2 is thecoercive 1047297eld and H s frac14 (H thorn H r)2 frac14 H i is the 1047297eld shift that is theinteraction 1047297eld H i with the opposite sign) In the Preisach model

terms the elementary hysteresis (the hysteron) is a rectangularhysteresis loop and the interactions are shifting the loops along the1047297eld direction In this representation one obtains the distribution of the coercive 1047297eld along the abscissa and the distribution of inter-actions along the ordinate It is recommended to show one or moresections along the two coordinates especially around themaximum value of the distribution (see Fig 6)

The magnetic properties of the potshards selected from theCucuteni culture may differ greatly as we can observe from Table 3In Table 3 it may be seen that M s is very small (010 emug) insamples 8D and 18G but continues to increase until reaches135 emug in sample 35M The selected pottery samples showalso distinctive coercivity values H c is 50 Oe for nine potterysamples 50e100 Oe for twenty three potshards and 200 Oe for

seventeen ware samples As an exception the pottery sample 19G

Fig 4 First-order reversal curve (FORC) and minor closed loop with one branch from

the FORC and the other a second-order reversal curve (SORC)




has a very high coercivity (695 Oe) compared to the rest of thepotshards

In the case of potshards from Cucuteni we have measured themajor loops forall thesamplesand for thesomeselectedsampleswealsohave measured the FORCs and calculated the FORC distributions

In Fig 8 one shows the most typical plot used in archaeomagnetismwhich consist in the representation of the major loop rectangularityS frac14 (M rM s) where M s is the saturation and M r the remanentmagnetic speci1047297c moments of the sample respectively

This graphic presentation of the data (Fig 8) shows the possi-bility of clustering the data in three major group The potshardsbelonging to the1047297rst contain calcite as were determined by the XRDanalysis and has low values for M rM s and H c The second groupbrings together most of the pottery samples which have different

amounts of hematite magnetite and diopside in their compositionand shows moderate values for M rM s and H c The third groupincludes only few samples having hematite and diopside in theirmineralogical structure and high values for M rM s and H c

The general aspect of the loops is rather diverse and inagreement with previous studies performed on archaeologicaltiles from Pompei (Beatrice et al 2008) (see Fig 7) In our caseone can relate rather well the magnetic measurements with theother physical analyses presented in this paper By the measure-ment of magnetic properties which relate the para- andor ferro-magnetic attributes of the pottery with the 1047297ring-induced irontransformations it is possible to obtain information on the basis of an almost unique combination of properties related to 1047297ringprotocol and mineralogical phase transformations revealed by the

XRD measurements

Fig 6 Experimental FORC diagram (sample 1A ) in rotated coordinates On the abscissa

is represented the coercive 1047297eld of the particles and on the ordinate the interaction

1047297eld (equivalent to a shift of the hysteron along the

1047297eld axis)

Fig 7 Typical magnetic hysteresis loops from Cucuteni pottery samples (samples 2A

5C 18G )

Fig 5 Experimental set of FORCs (sample 1A ) and the FORC diagram (below) in

Preisach-type (H H r) coordinates The experimental points presented in the inset are

used in the evaluation of the second-order mixed derivative which is proportional to

the FORC distribution






to 1047297ring technology From this point of view three distinct ceramicsgroups attributed to different 1047297ring temperatures have beendifferentiated in a coherent grouping which supports this conclu-sion The magnetic measurementrsquos resultsseemto be in1047298uenced bythe soaking time the modality of cooling and by the clay compo-sition and homogeneity

The analysis of magnetic properties provides new informationwhich help understanding the mineralogical transformations dueto the 1047297ring process In terms of pottery technology the magneticmeasurements con1047297rm the mineralogical transformations detectedby XRD analysis and suggest a certain degree of standardization inthe pottery production

The magnetic measurements provide archaeologists with thepotential to test hypotheses concerning ceramic manufacture thathas not previously been achieved in traditional Cucuteni ceramicstudies A larger database of both clays and shards from multiplesites along with better chronological control is necessary to thor-oughly take advantage of this potential

The increased 1047297ring temperature is related to a large scale

production process This was determined by a possible change inthe scale or ldquomoderdquo of pottery production during the Chalcolithicperiod with possible shifts from household to workshop industry

However we consider it is too early to conclusively determine suchan issue on the basis of this study alone What is clear at this stage isthat the pyro-technological abilities (use of high 1047297ring tempera-tures) seems to have remained quite the same indicating a veryhigh technological skill and a very traditional potterrsquos techniquewith very little change occurring over time

In the next stage of our research we hope to be able to moreexplicitly relate these phenomena to changes in the social organi-zation of the CucutenieTrypillia communities during the respectiveperiods Such a study will also have to take into account otheraspects such as the distribution of the relevant pottery typesproduction modes and technologies something which is clearlybeyond the scope of this present study

Acknowledgments

This paper is a result of the research project Physical methods

applied in archaeology which is 1047297nancially supported by theSectorial Operational Programme Human Resources Development2007e2013 within the project Transnational Network for Integrated

Management of Postdoctoral Research in Communicating SciencesInstitutional building (postdoctoral school) and fellowships program

(CommScie) e POSDRU8915S63663The authors would like to thank Dr Neculai Bolohan and Dr Dan

Monah for fruitful discussions We would also like to express ourgratitude to Dr Roxana Munteanu (Neamt County Museum)Lacramioara Istina (Bacau County Museum) Dr George Bodi DrMagda Lazarovici and Bogdan Minea (Institute of Archaeology

Romanian Academy Iasi Branch) dr Aurel Melniciuc (BotosaniCounty Museum) Dr Bogdan Niculica (Suceava County Museum)Ciprian Lazanu (Vaslui County Museum) and Dr Sandor Jozsef Sztancsuj (Szekely National Museum Sfantu Gheorghe CovasnaCounty) for providing the pottery samples The 1047297nal version wasimproved within the valuable comments and suggestions of twoanonymous reviewers

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Butzureano GC 1891 Notes sur Coucouteni et plusieurs autres stations de laMoldavie du Nord In Congregraves International drsquoAnthropolgie et drsquoArcheacuteologiePreacutehistoriques Compte-rendu de la dixiegraveme session agrave Paris 1889 pp 299e307

Buzgar N Bodi G Buzatu A Apopei AI Astefanei D 2010 Raman and XRDstudies of black pigment from Cucuteni ceramics Analele Stiinti1047297ce ale Uni-versitatii ldquoAl I Cuzardquo Iasi Geologie LVI (2) 95e108

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Young R 1993 The Rietveld Method Oxford University Press Oxford

Zananiri I Batt CM Lanos P Tarling DH Linford P 2007 Archaeomagneticsecular variation in the UK during the past 4000 years and its application toarchaeomagnetic dating Physics of the Earth and Planetary Interiors 160 (2)97e107









31 Sample selection


32 XRD analysis










41 XRD measurements
















Table 1


Sample Siteacronym



Complete Incomplete

1 A 2 A


38 O 39 P 40 P 41 Q 42 R 43 R 44 S 45 S 46 S 47 T 48 U 49 U 50 V

























county
















Table 3



Units g emu Oe emug

1 029 002 002 15041 0822 010 002 000 7191 0213 022 004 002 10239 0474 010 003 001 4600 027

5 032 002 001 14954 0676 011 003 001 5149 0227 016 002 001 7425 0528 006 006 001 5545 0109 009 001 000 4457 02110 014 001 001 5490 04111 010 002 001 6777 02512 010 001 000 5850 03813 030 003 002 11457 08314 008 003 001 4362 02415 013 003 001 6540 03816 022 002 001 14890 03617 037 002 002 11933 08918 003 002 000 3646 00819 039 001 000 69519 02720 005 001 000 4480 01821 009 003 001 5513 021

22 015 002 001 7752 03923 014 004 002 5567 05124 004 002 000 3047 01125 010 005 001 6180 02726 012 003 001 4545 02627 024 002 001 7563 05528 016 004 001 17044 02229 025 001 000 14633 03530 010 002 000 5639 01731 028 003 002 10839 08232 024 003 002 8877 06433 012 003 001 8491 02034 022 002 001 8360 04435 021 003 004 8889 13536 023 002 001 9858 06037 020 003 002 6891 04838 015 002 000 5692 03039 022 002 000 26814 01740 043 001 001 19961 12341 005 004 001 2905 01642 014 001 001 6657 04143 028 004 002 13184 05344 032 002 002 12102 09045 020 002 001 11076 02846 005 002 000 3997 01147 020 002 001 15239 03648 012 001 000 8888 01849 015 005 003 6379 04850 024 002 001 10577 048















vH vH r

















XRD measurements




1047297eld axis)


5C 18G )

















Acknowledgments







References




197








































































































Table 1


Sample Siteacronym



Complete Incomplete

1 A 2 A


38 O 39 P 40 P 41 Q 42 R 43 R 44 S 45 S 46 S 47 T 48 U 49 U 50 V

























county
















Table 3



Units g emu Oe emug

1 029 002 002 15041 0822 010 002 000 7191 0213 022 004 002 10239 0474 010 003 001 4600 027

5 032 002 001 14954 0676 011 003 001 5149 0227 016 002 001 7425 0528 006 006 001 5545 0109 009 001 000 4457 02110 014 001 001 5490 04111 010 002 001 6777 02512 010 001 000 5850 03813 030 003 002 11457 08314 008 003 001 4362 02415 013 003 001 6540 03816 022 002 001 14890 03617 037 002 002 11933 08918 003 002 000 3646 00819 039 001 000 69519 02720 005 001 000 4480 01821 009 003 001 5513 021

22 015 002 001 7752 03923 014 004 002 5567 05124 004 002 000 3047 01125 010 005 001 6180 02726 012 003 001 4545 02627 024 002 001 7563 05528 016 004 001 17044 02229 025 001 000 14633 03530 010 002 000 5639 01731 028 003 002 10839 08232 024 003 002 8877 06433 012 003 001 8491 02034 022 002 001 8360 04435 021 003 004 8889 13536 023 002 001 9858 06037 020 003 002 6891 04838 015 002 000 5692 03039 022 002 000 26814 01740 043 001 001 19961 12341 005 004 001 2905 01642 014 001 001 6657 04143 028 004 002 13184 05344 032 002 002 12102 09045 020 002 001 11076 02846 005 002 000 3997 01147 020 002 001 15239 03648 012 001 000 8888 01849 015 005 003 6379 04850 024 002 001 10577 048















vH vH r

















XRD measurements




1047297eld axis)


5C 18G )

















Acknowledgments







References




197





















































































































county
















Table 3



Units g emu Oe emug

1 029 002 002 15041 0822 010 002 000 7191 0213 022 004 002 10239 0474 010 003 001 4600 027

5 032 002 001 14954 0676 011 003 001 5149 0227 016 002 001 7425 0528 006 006 001 5545 0109 009 001 000 4457 02110 014 001 001 5490 04111 010 002 001 6777 02512 010 001 000 5850 03813 030 003 002 11457 08314 008 003 001 4362 02415 013 003 001 6540 03816 022 002 001 14890 03617 037 002 002 11933 08918 003 002 000 3646 00819 039 001 000 69519 02720 005 001 000 4480 01821 009 003 001 5513 021

22 015 002 001 7752 03923 014 004 002 5567 05124 004 002 000 3047 01125 010 005 001 6180 02726 012 003 001 4545 02627 024 002 001 7563 05528 016 004 001 17044 02229 025 001 000 14633 03530 010 002 000 5639 01731 028 003 002 10839 08232 024 003 002 8877 06433 012 003 001 8491 02034 022 002 001 8360 04435 021 003 004 8889 13536 023 002 001 9858 06037 020 003 002 6891 04838 015 002 000 5692 03039 022 002 000 26814 01740 043 001 001 19961 12341 005 004 001 2905 01642 014 001 001 6657 04143 028 004 002 13184 05344 032 002 002 12102 09045 020 002 001 11076 02846 005 002 000 3997 01147 020 002 001 15239 03648 012 001 000 8888 01849 015 005 003 6379 04850 024 002 001 10577 048















vH vH r

















XRD measurements




1047297eld axis)


5C 18G )

















Acknowledgments







References




197












































































































Table 3



Units g emu Oe emug

1 029 002 002 15041 0822 010 002 000 7191 0213 022 004 002 10239 0474 010 003 001 4600 027

5 032 002 001 14954 0676 011 003 001 5149 0227 016 002 001 7425 0528 006 006 001 5545 0109 009 001 000 4457 02110 014 001 001 5490 04111 010 002 001 6777 02512 010 001 000 5850 03813 030 003 002 11457 08314 008 003 001 4362 02415 013 003 001 6540 03816 022 002 001 14890 03617 037 002 002 11933 08918 003 002 000 3646 00819 039 001 000 69519 02720 005 001 000 4480 01821 009 003 001 5513 021

22 015 002 001 7752 03923 014 004 002 5567 05124 004 002 000 3047 01125 010 005 001 6180 02726 012 003 001 4545 02627 024 002 001 7563 05528 016 004 001 17044 02229 025 001 000 14633 03530 010 002 000 5639 01731 028 003 002 10839 08232 024 003 002 8877 06433 012 003 001 8491 02034 022 002 001 8360 04435 021 003 004 8889 13536 023 002 001 9858 06037 020 003 002 6891 04838 015 002 000 5692 03039 022 002 000 26814 01740 043 001 001 19961 12341 005 004 001 2905 01642 014 001 001 6657 04143 028 004 002 13184 05344 032 002 002 12102 09045 020 002 001 11076 02846 005 002 000 3997 01147 020 002 001 15239 03648 012 001 000 8888 01849 015 005 003 6379 04850 024 002 001 10577 048















vH vH r

















XRD measurements




1047297eld axis)


5C 18G )

















Acknowledgments







References




197











































































































vH vH r

















XRD measurements




1047297eld axis)


5C 18G )

















Acknowledgments







References




197






































































































XRD measurements




1047297eld axis)


5C 18G )

















Acknowledgments







References




197









































































































Acknowledgments







References




197






























































































Physical Study of Cucuteni Pottery Technology

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Transcript of Physical Study of Cucuteni Pottery Technology