MediterraneanArchaeologyandArchaeometry,Vol.11,No.2,pp.

9198
Copyright2011MAA
PrintedinGreece.Allrightsreserved.

ANALYTICALINVESTIGATIONOFPIGMENTS,GROUND
LAYERANDMEDIAOFCARTONNAGEFRAGMENTS
FROMGREEKROMANPERIOD
HalaA.M.Afifi
ConservationDepartment,FacultyofArchaeologyCairoUniversity,PostCode:12613,Egypt

Received:31/07/2011
Accepted:12/09/2011

Correspondingauthor:halaafifi11@hotmail.com

ABSTRACT
Some cartonnage fragments from Hawara, Fayoum Excavation were examined to identify pig
ments, media and grounds. It belonged to the GreekRoman period. They were studied by Xray
diffraction(XRD),EnergydispersiveXrayanalysis(EDS)equippedwithScanningelectronmicros
copy (SEM) and Fourier transform infrared spectroscopy (FTIR). These techniques were used to
identifythecompositionandmorphologyofgrounds,natureofpigments andmediausedincar
tonnagefragments.Thecoarsegroundlayerwascomposedofcalciteandtracesofquartz.Thefine
ground layer used under the pigments directly was composed of calcite only. Carbon black was
usedasblackpigmentwhileleadoxideasredpigment,showingtheinfluenceofRomanandGreek
pigments on Egyptian art in these later periods. Blue colorant was identified as cuprorivaite and
yellowpigmentwasgoethite.Animalgluewasusedinthefourpigmentsasmediumcolored.

KEYWORDS:Fayoum,Hawara,Cartonnage,Pigments,FTIR

HALAA.M.AFIFI

92

1.INTRODUCTION
Analytical investigations of archaeological
objects bring us much information on the de
velopment and propagation of technologies on
cultures.Toconserveandrestorethesevaluable
andscarceobjects,itisindispensabletounder
stand their chemical constituents and crystal
structures.
The EgyptianPolish archaeological Excava
tiontoHawarrapyramidarea,Fayoum(Fig.1A)
coveredmanyarchaeologicalmaterialssuchas,
many pieces of human bones, various skulls,
two skeletons of sacred crocodiles, terracotta,
and one gilded mask with many fragments of
colored cartonnage. These fragments decorated
withreligiousgods.HawarraLabyrinthsiteisa
unique combination of buildings and artefacts
from two different eras and cultures: an Egyp
tian pyramid complex, and Roman period
cemeteries (Shaw, 2000; Verner, 2001; Vila,
1976).
During late Pharonic times, cartonnage was
usedtomaketheinnercoffinsformummies.It
wasmoldedtotheshapeofthebody,forminga
one piece shell. It was often highly decorated
with various geometric designs, an assortment
of deities and inscriptions, which included
versesfromtheBookoftheDead(Picton,etal.,
2007) colored with different pigments. Ancient
Egyptian pigments have been analyzed exten
sivelyinlaboratorystudies(Barbierietal.1974;
Riederer 1974; Jaksch et al. 1983; Goresy et al.
1986;Saleh1987;Riederer1988;LucasandHar
ris1989).
It is selfevident that nondestructive and
noncontact analysis in the field is indispensa

bleforinvestigatingancientremains.Theproc
ess,ofcreatinganentiremummiformcoffinout
of cartonnage, was a time consuming and ex
pensiveprocess.
During Ptolemaic times, a new, simpler
method of mummy decoration was adopted.
Instead of encasing the mummy in a onepiece
mummiform shell, it would be covered with
four to six separate pieces of decorated carton
nage. These would be attached to the outer
mummy wrappings and could easily be mass
produced. These separate sections of carton
nageconsistedofamaskcoveringtheheadand
shoulders,apectoral,anapronforthelegsand
afootcasing.
Sometimes, two additional pieces were
added to cover the ribcage and stomach. The
cartonnage pieces which covered the ribcage
andstomachoftendepictedthewingedbabird.
These sections wouldoften be cut tothe shape
ofthefigure.Sometimes,theimageofawinged
scarab was also depicted. On some of these
pieces, a small, generally square section of the
cartonnage would be left undecorated or
paintedaneutralcolor(Stewart,1986).
This work analyzed some fragments from
the painted cartonnage of a mummy that was
discovered in Hawara pyramid excavation Fig.
1(B)toestablishitselementalcompositionand
toverifyifthepigmentsusedinthedecorative
paintingsareinaccordancewiththoseusedby
Egyptian craftsmen in the Roman period
(Liritzis et al., 1997). These cartonnage frag
ments consist of two ground layers; coarse
groundlayerandfineorpaintinggroundlayer
Fig.1(C).

Fig.1(A)HawaraPyramidandtheareaofexcavationwork,Fayoum,Egypt.(B)Studiedexcavatedcartonnage
fragments.(C)Twopaintinggroundlayersofcartonnagefragment.

ANALYTICALINVESTIGATIONOFPIGMENTS,GROUNDLAYERANDMEDIAOFCARTONNAGEFRAGMENTSFROMGREEKROMANPERIOD

93

Fig.2(A),(B),(C)ThreeofHawaracartonnagefragmentsrepresentedtheexaminedpigments

2. METHODS OF ANALYSIS AND IN

VESTIGATIONS
Different analytical techniques have been
performed to characterize pigments, grounds,
and binding media employed in a number of
verysmallcartonnagefragmentsFig2(A,B,C).
2.1Opticalmicroscopy
Samples wereobserved by aWildM8 stereo
microscope, a Olympus BX51 optical microscope
andrecordedwithaphotocamera.Thecrosssec
tionswerepreparedbyembeddingthesamplein
apolyesterresin,coldpolymersablewiththead
ditionofacatalyst,andthenpolishedwithaStru
ers DAPV machine by using SiC paper discs
with a decreasing granulometry (600, 1200, 2400
and4000gritsize),untilthecrosssectionsurface
became smooth and specular (Liritzis and Poly
chroniadou, 2007). These preparation processes
wereappliedintheGeologyDepartment,Faculty
ofScience,CairoUniversity).
2.2Scanningelectronmicroscopeequippedwith
energydispersivexrayanalysis
SampleswereinvestigatedbyPhilips(XL30)
microscopy, equipped with EDS micro
analytical system to obtain the total element
contentqualitativelyandquantitativelybyEDX
unit in the samples. It was useful for semi
quantitative elemental analysis to make up for
thedeficienciesofXRD(Hanlan,1975).Insome
cases, doubt arose about specific minerals that
could not be readily identified by XRD (Perdi
katsis,etal.,2000).
2.3Xraydiffractionanalysis
Xray diffraction analysis carried out with
Phillips Xray diffraction equipment model

pw/1840 with Ni filter, Cu radiation 1.54056 A

at 40 KV, 25mA, 0.05 /sec. Highresolution
graphitemonochromator,rotatingsampleholder
andaproportionaldetector.Measurementswere
carried out on powders of the samples, in the
range0<2<70withastepof0.02.
2.4Fouriertransforminfraredspectroscopy
Samples were analysed as KBr pellets by
JASCO FT\IR 460 plus spectrometer, in the
transmissionmode(Bikiaris,etal.,1999,Grigar,
2003).Thepowderedsamplewasexaminedbe
tween(4004000cm1,4cm1resolution).

3.RESULTS
To conserve and restore, it is indispensable
to understand the chemical constituents and
crystalstructures.Thetechnologyofthemateri
als used in the fabrication of ancient Egyptian
cartonnage is still not fully investigated.
(Daniels, 2007; Scott et al., 2003; Scott et al.,
2009).
Among archaeological objects, pigments are
most attractive targets for scientific study be
cause their colors are yardsticks of a sense of
beauty, and they provide a means for estimat
ing ancient technologies ability to prepare
pigmentsartificially(Green1995;Nagashimaet
al. 1996; Goresy 1997; Uda 1999, Uda et al.
2000a; Uda et al. 2000b; Yoshimura et al. 2002;
Goresyet.,al1986).
3.1.Groundlayers
From visual inspection and analysis of sam
ples by X ray diffraction (XRD), energy disper
siveXrayanalysisequippedwithscanningelec
tron microscope analysis (SEM) are character
izedbytwopreparationlayersorgroundpaint

HALAA.M.AFIFI

94

ing layers. The preparation technique used

seems to have been to pour the first layer of a
coarse ground layer directly on the linen
mummy bandages. This coarse layer covered
withanothersmoothlayerpreparedforpainting
process. These twolayered structures of plaster
were observed on all fragments. Based on ex
perimental results obtained, XRD analysis re
vealed that the inner coarse ground layer is
composedofcalciteCaCO3asamajorwithsmall
amountsofquartz(SiO2)(Fig.3A).Thematerial

compositionofthefinegroundlayerusedunder
the pigments directly was composed of calcite,
CaCO3 only Fig. 3 B). This result agreed with
(UDA, 1999). EDX data of ground layers (Fig. 3
C,D)respectively,showedthefinegroundlayer
that composed of Ca that exhibited the highest
concentrations80.86%and11.14%ofC.Thisre
sultindicatesthatthelayerisconsistsofcalcite.
The coarse ground layer is composed of Ca, C,
Si, agreed with the result of XRD data that is
composedofcalciteandquartz.

Fig.3(A,B,C,D)XRD,EDXpatternsoftheinternalandexternalgroundlayersofthecartonnagefragments.(A)
XRDdataofinternalgroundlayerthatconsistedofcalciteandquartz.(B)XRDdataofexternalgroundlayerthat
containedcalciteonly.(C)EDXpatternofinternalgroundlayer.(D)EDXdataofexternalgroundlayer

3.2.Pigments
3.2.1Redpigment
Themajorityofredpigmentsusedinancient
Egypt were earthen based colors containing
iron oxide. Hematite (Fe2O3) was very com
mon (Green 2001, M. Uda, et al 2000). This Fe
based colors are longer lasting and light faster
than others, and are sometimes of astonishing
brilliance.Twofurtherredpigmentshavebeen
imported to Egypt by the Romans: Red lead
(Pb3O4)andVermillion(HgS).Ifthesepigments
arefoundonancientobjects,itcanbeassumed
tobeproducednotearlierthanthefirstcentury
B.C. Mineralogical analysis conducted by XRD
showedintheFig.(4A).Itpresentedcalciteasa
painting ground layer, lead oxide Pb3O4 as red
pigment with carbon as black. This result
agreedwith(Burgioetal.,2007;RoccoMazzeo,

etal.,2004).Calciteandleadoxideweredeter
mined by SEMEDS. Pb, Ca, with minor com
ponentofSi(Fig.4B).
3.2.2Bluepigment
In 3000 BC, Egyptian craftsmen created the
firstsyntheticpigmentproducedbyman,Egyp
tianblue,whichwaswidelyusedduringantiq
uity, spreading all around the Mediterranean
basin until the 7th century AD. The Egyptian
green pigment, also called green frit, appeared
shortly after, presenting the same chemical
elementsandaturquoisecolor.Thesetwopig
ments have been confused for a long time
(Mazzochin, 2004; Page`s 2003; Daniels, 2007).
In many cases, Egyptian blue was added in
smallamountstoenhancethebrillianceofother
colors. It was reported by (Mazzochin 2003;
Mazzochin ,et al., 2003). XRD data of blue pig

ANALYTICALINVESTIGATIONOFPIGMENTS,GROUNDLAYERANDMEDIAOFCARTONNAGEFRAGMENTSFROMGREEKROMANPERIOD

ment in Fig. 3C, which identified cuprorivaite,

CaCuSi4O10, the major constituent in Egyptian
blue.Cu,Ca,SiwereidentifiedbyEDXpattern
as showed in Fig 4D. The result verified the
XRDdata(seee.g.Katsarosetal.,2011).
3.2.3Yellowpigment
In the Fig 4E, the yellow pigment is con
firmedbyXRDpatternasagoethiteFe2O3.H2O
(Fig4F).ThiswasconfirmedbyEDXdata.Cais
the main component of ground layer, Si, as
quartz and Fe represent goethite as yellow

95

pigment this result agreed with (Perdikatsis et

al2000;Brecoulaki,et.al.,2006).
3.2.4Blackpigment
The only black pigment identified is carbon
black.Itistheprincipalblackattestedandused
from ancient Egyptian periods. Its use is very
frequent both as an homogeneous paint layer
and mixed with other pigments to produce
darker tones (Mazzochin ,et al., 2003). SEM ob
servationrevealedthechemicalcompositionthat
wascharacterizedbyagreatamountofcarbon.

Fig4(A,B,C,D,E,F)XRDandEDXofpigmentsamples.Fig3(A)XRDdataofredandblackpigmentsshowed
thatredpigmentconsistedofleadoxidePbO3andblackascarbon.Fig3(B)EDXdataoftheredandblackpig
ments.Fig3(C)XRDofblueandblackpigmentsdataexplainedthecuprorivaite,CaCuSi4O10asblueandblack
wascarbon.Fig3(D)EDXdataoftheblueandblackpigments.Fig3(E)XRDdatashowedthatgoethite
Fe2O3.H2Owasyellowpigmentusedonthecartonnagefragments.Fig3(F)EDXdataofyellowpigment

3.3.Bindingmedia
The spectroscopic study was essentially ad
dressed to characterize the colouring medium
usedinthecartonnagefragments.Inalltheana
lysed samples, the stretching vibrations of cal
ciumcarbonate,CaCO3,peakedat1409,705and
611cm1wereidentifiedsincethesubstratewas
just a calcarenite (Griffith 1987). In particular,
we evidenced the typical hydroxyl bands cen
tredat3694,3669,3652andat3620cm1,theSi
OSi band peaked at 1032 cm1, the SiOAl at
1009cm1andfinallytheAlOHbandsat938
and 914 cm1. The use of animal glue is also
showninthisIRspectrumbythepresenceofa
bandat1540cm1associatedwiththedeforma
tion vibration of the NH link in the protein

(Carbo,1997). In the four pigments, the same

medium and working technique were found.
(Schiegletal.,1989;Mazureketal.2008;Scottet
al., 1996; Hodgins and Hedges, 2000; Schilling
etal.,2000).

4.CONCLUSION
Thepresentstudyhasshownthecharacteri
zation of painted cartonnage fragments from
HawaraexcavationinFayoumthatbelongedto
theGreekRomanperiod,Egypt.
The technology of cartonnage making,
ground layers composition, pigments constitu
entsandcolormediumwereidentifiedbyusing
differentanalyticalmethodsasXRD,EDX,SEM
andFTIR.

96

Two preparation or ground painting layers

are applied; the inner coarse ground layer is
composed of calcite CaCO3 as a major with
smallamountsofquartz(SiO2).Thefineground
layer used under the pigments directly was
composedofonlycalciteCaCO3.Readpigment
that used is red lead (Pb3O4). Blue pigment is
cuprorivaite, CaCuSi4O10. Goethite Fe2O3.H2O
used as yellow pigment. The only black pig
ment identified is carbon black. In the four
pigmentsanimalglueisfoundasthesameme

HALAA.M.AFIFI

dium in the working technique. The well pre

served state of the pigments on the cartonnage
fragmentsisattributedtothefactthattheybur
iedandthereforewerenotexposedtotheopen
environment; soon after being excavated the
fragmentswerepackedincratesandkeptinthe
conservation lab of the excavation until this
study was undertaken. The results of the pig
ment analysis shed important light on the pig
ments that applied on the cartonnage frag
ments.

ACKNOWLEDGEMENTS
The author gratefully acknowledges the help of the Egyptianpolish excavation members. The
helpofProf.Dr.AllaElDienShaheenpreviousDeanofFacultyofArchaeology,CairoUniversity
andProf.Dr.MohamedAbdElHadyProf.ofConservationandRestorationmonumentsinFaculty
ofArchaeology,CairoUniversitywasinvaluableforhelpfuldiscussions.

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