J Radioanal Nucl Chem (2010) 285:455–460
DOI 10.1007/s10967-010-0595-4
X-ray fluorescence analysis for the study of fragments pottery
excavated at Tell Jendares site, Syria, employing multivariate
statistical analysis
E. H. Bakraji • M. Itlas • A. Abdulrahman •
H. Issa • R. Abboud
Received: 8 February 2010 / Published online: 14 May 2010
Ó Akadémiai Kiadó, Budapest, Hungary 2010
Abstract X-ray fluorescence analysis study of 44
archaeological pottery samples collected from Tell Jend-
ares site north-west of Syria has been carried out. Four
samples of the total previous investigated samples were
obtained from the kiln found on Tell Jendares site. Sev-
enteen different chemical elements were determined. The
XRF results have been processed using two multivariate
statistical cluster and factor analysis methods in order to
determine the similarities and correlation between the
selected samples based on their elemental composition.
The methodology successfully separates the samples where
three distinct chemical groups were discerned.
Keywords X-ray  Pottery  Archaeology 
Multivariate analysis  Syria
Introduction
In view of the considerable Syrian heritage, special atten-
tion was given recently to physical instrumental analysis
science applications in archaeology, such as X-ray fluo-
rescence (XRF), particle induced X-ray emission (PIXE),
E. H. Bakraji (&)  H. Issa  R. Abboud
Department of Chemistry, Atomic Energy Commission,
P.O. Box 6091, Damascus, Syria
e-mail: cscientific@aec.org.sy
M. Itlas
Department of Scientific Service, Atomic Energy Commission,
P.O. Box 6091, Damascus, Syria
A. Abdulrahman
Director of Tell Jendares Mission, Albassel Centre for
Archaeological Training, Atomic Energy Commission,
P.O. Box 6091, Damascus, Syria
thermo luminescence (TL), etc. Archaeologists have been,
for many years, interested in the provenance of pottery
fragments, since pottery is the most abundant tracer in all
archaeological excavation. The analysis of pottery can
indeed supplement the information gathered from written
documents to produce a better knowledge of trade routes
linking populations of different areas, which is one of the
essential in gradients for the comprehension of their his-
tory. The microscopic properties of pottery such as
chemical composition may answer questions concerning
origin [1].
Chemical composition of pottery from major, minor and
trace elements provides a compositional ‘‘fingerprint’’ for
grouping together pottery made from the same raw mate-
rials and for distinguishing between groups of pottery made
from different raw material [2]. In the early days of
provenance studies using chemical analysis the principal
analytical techniques were instrumental neutron activation
analysis (INAA), and X-ray fluorescence (XRF). Since the
initial pottery study by Sayer and Dosden in 1957 [3],
many techniques have been widely exploited in the study
of archaeological pottery, such as INAA [4–6], XRF, PIXE
[7–13], and inductively coupled plasma emission analysis
[14]. The trace constituents-elements which are present in
amount below 1.000 ppm that provides the primary basis
for provenience analysis. XRF, a very sensitive non-
destructive method for analyzing the content of various
chemical elements in material, is an excellent tool for
investigations of historic relics, works of art and archaeo-
logical finds [15, 16]. The XRF method have been applied
in our laboratory to analyze different kind of samples,
among them archaeological pottery [12, 13]. XRF is low-
cost and rapid technique for the determining the major,
minor and trace element composition of pottery [17, 18],
XRF can analyze some 15–30 elements with atomic
123
456
numbers ranging from Z = 11 to Z = 41 and some of the
rare earth elements (REEs) [19, 20].
In this work, we applied the XRF technique to analyze
archaeological pottery recovered during the 2006 and 2007
field seasons of the Syrian–German Expedition to the Tell
Jendares site. Seventeen chemical elements were deter-
mined. These elemental concentrations have been pro-
cessed using statistical method in order to determine
similarity and correlation between the various samples. The
first aim of our study was to classify pottery into groups
having similar elemental composition, which are assumed
to correspond to the same provenance. The determination
of provenance of pottery is of special interest, as it gives
valuable insight into ancient trade connection. The second
aim was providing database on additional chemical com-
position of archaeological pottery in Syria. Provenance
studies based on chemical composition involve then the
analysis of a large number of samples. In selecting pottery
samples for analysis, it is important that the samples are
from a single period and site.
Description of area and materials
Tell Jendares is located north-west of Syria (36° 220 N, 40°
360 E), at the heart of this Tell exist the Alomek plain,
which represent a key milestone in this geographically part
of Syria. Alomek plain extends from the north-east to the
south-west among the Mont Simon in the east and moun-
tains Alomanus in the West.
The plain starts from the north of the Syrian–Turkish
border and ends at the south-west coast of the Mediterra-
nean, where the mouth of the Orontes river. The archaeo-
logical hill (Tell Jendares) exists in the south-west of the
Jendares town. Tell Jendares has a semi circular form and
the average diameter of the reminder of this Tell is about
450 m. Tell Jendares is located in plain at an altitude of
200 meters above sea level. The highest level of the Tell
Jendares is 31 m above the surrounding plain. Tell Jend-
ares contains consecutive settlements dating back to the
second millennium BC, where it is expected to be the
capital of Alomek plain and its name was ‘‘Anek’’ at that
time. In the first millennium BC, the Assyrian text indicates
that the name of the city Jendares was ‘‘Konaloa’’ at that
time, and it was the capital of Alomek area as well. It was
also mentioned that it was a rich city, has handed donations
and gifts to the Assyrian king Ashur Nasir Pal II, to avoid
the conflict with him.
All subsequent settlements belong to the classical per-
iod, which constitute recolonization since the Hellenistic
period to the Byzantine period, and the hill was called
‘‘Jindaros’’.
123
E. H. Bakraji et al.
The 44 samples analyzed are unglazed and not decorated
earthenware and fairly representative of Hellenistic-Roman
pottery made between 300 BC and 100 AD. Four samples
of the total samples derive from the kiln found on the site
(samples K41, K42, K43, and K44).
Experimental
Sample preparation
After removal of the surface deposit, pottery samples were
ground into a fine powder for 10–15 min, using an agate
motor. All samples powder were then dried at 105 °C for
24 h and stored in desiccators until they were measured,
where pellets from pressed powder were performed.
Instrumentation and measurements
The analyses of the thick pellets (25 mm diameter) from
pressed powder were performed using an EDXRF spec-
trometer assembled by the Syrian Atomic Energy Com-
mission. The unit is equipped with a Molybdenum X-ray
tube (Philips) with Mo secondary target, controller and
cooling system from (ItalStructures), Si(Li) detector and its
electronics (H.V. power supply, Amp., ADC and MCA)
from PGT, system 4000. The Si(Li) detector has an energy
resolution 140 eV at 5.9 keV for the Mn–Ka. The X-ray
tube was operated at 35 kV, 20 mA at 1000 s live time to
generate X-ray intensity ka, La lines data for the following
elements: bromine (Br) calcium (Ca), copper (Cu), chro-
mium (Cr), gallium (Ga), iron (Fe), lead (Pb) (from La),
manganese (Mn), nickel (Ni), potassium (K), rubidium
(Rb), strontium (Sr), titanium (Ti), and zinc (Zn). For the
elements niobium (Nb), yttrium (Y), and zirconium (Zr),
Ka line data were generated by using a cadmium (109Cd)
radioisotope source (*9 9 108 Bq) for 1000 s live time.
X-ray fluorescence outgoing from the samples were carried
out with qualitative and quantitative X-ray analysis pro-
gram (QXAS) from the International Atomic Energy
Agency (IAEA). The net peak intensities of the Ka and La
lines were calculated by fitting the spectra with the sub-
program AXIL (version 3.6) [21].
One of the implemented procedures in the QXAS
package is called elemental sensitivities in sub-program the
simple quantitative analysis (S.Q.A.), which is used to
determine the sensitivity of X-ray lines, taking into account
the X-ray attenuation in the standard used for calibration.
The standards used in our study to establish the sensitivity
curves are the following: Ti; Cr; Fe; Cu; Zn; Zr; as foils; S;
Ni; Se; as powder pure elements; KH2PO4; CaCO3; KCl;
KBr; As2O3 and SrCO3 as chemical compounds; for Ka
X-ray fluorescence
lines; Pt; Pb and U as foils; CsCl3; La2O3; Nd2O3; Gd2O3;
WO3 as chemical compounds; for La lines.
Soil-7 (IAEA); sediments SL-1 and SL-3 (IAEA) were
used as standards samples for testing the accuracy of sen-
sitivity curves. The S.Q.A. is then used to determine the
concentrations of the elements in the unknown samples
with the possibility to take X-ray attenuation into account.
More details about the S.Q.A. method are described in
[21]. All of the XRF data analyses were the results of
averaging three measurements for each pottery sample. The
repeated analyses of several samples showed that in each
case the relative standard deviation (RSD) was less than
5% for each element under investigation.
Statistical treatment
The Statistical 6.0 package was used in this work for all
statistical calculations. The final data which consists of
observations (samples) and variables (elements) have been
processed using two multivariate statistical methods,
cluster analysis (CA), and factor analysis (FA). Cluster
analysis is often used in the initial inspection of data
because it is a rapid and efficient technique for evaluating
relationships between a large numbers of samples, between
which distance measures have been calculated [22]. CA
classifies samples into distinct groups and the results are
commonly presented as dendrogram showing the order and
levels of clustering as well as the distances between indi-
vidual samples.
A primary goal of factor analysis is to extract a mini-
mum number of factors which explains an acceptable
amount of total variance of the data set. In order to explain
100% of the variance in the data set, the number of factors
retained should necessarily be equal to the number of
elements chosen for statistical analysis. In general we
choose a number of factors that explain at least 70% of the
total variance, and generally the three-first factors are
sufficient to reach this value. For the present work the
three-first factors were adequate to explain, as we will see
later, more than 70% of the total variance. The method for
factor extraction used in this study was principal compo-
nents; the method utilized for rotation was varimax.
Results and discussion
Table 1 lists the concentration of major, minor, and trace
elements found in the pottery analyzed. It is clear from this
table that there are large variations in the elemental con-
centrations among the samples. All the elements in the data
set with precision better than 10% were considered because
if an element is not measured with good precision it
can obscure real differences in concentration, and the
457
discriminating effect of other well-measured element tends
to be reduced. In the present work the precision was better
than 10% for all determined elements. In the other hand all
elements that have more than 25% missing values across
the samples set were not introduced in the data set for
multivariate analysis, this is the case of the elements gal-
lium (Ga) and bromine (Br). The procedure used to esti-
mate the missing values for other element in the data set
was to replace any missing value by the minimum detec-
tion limits (MDL) determined by XRF, this is the case of
the two elements niobium (Nb) and lead (Pb) were the
MDL is 10 ppm for these elements.
Based on the screening criteria, only 15 elements were
used in the subsequent data analysis. The final data set
consisted of 44 samples (observations) with 15 elements
(variables) for a total of 660 data entries. The cluster and
factor analysis were performed from the base log.10
transformed concentration values, to normalize element
distribution and reduce the impact of differences in mag-
nitude for some of the major elements.
Cluster analysis (CA)
The resulting dendrogram is shown in Fig. 1. It was found
using single linkage as grouping rule, according to
Euclidean distance. It is clear that there are two main
clusters. Cluster 1 contains 31 samples (70% of the
observations), cluster 2 contains eight samples, and there is
one small cluster, cluster 3 which contains only three
samples (C1, C5, and C6).
Factor analysis (FA)
Table 2 shows the factor loading for the three extracted
factors. As listed on Table 2, factor 1 explains 28.6% of the
total variance of the data set, factor 2 explains 27.5% and
finally factor 3 explains 14.8%. It is clear that the three
factors extracted in this study explain 70.9.% of the total
variance of the data set. The square of the factor loading of
an element for a given factor indicates the fraction of
variance of the element which can be explained by the
common variance of that factor. For example the loading of
manganese (Mn) in Table 2 on factor 1 for the data set is
0.92, thus (0.92)2 = 85% of the variance of Mn can be
explained by the common variance of factor 1. The squared
factor loading of a particular element summed over all
factors is the communality of that element. It is clear from
Table 2 that the communalities for 80% of the elements are
greater than 50%. Therefore, the FA fit to the data set is
good. In addition to factor loading, this analysis yields
factor scores, which quantify the relative intensities of
factor strength on each sample. Factor scores are very
helpful in interpreting and understanding factor analysis
123
458 E. H. Bakraji et al.

Table 1 Major, minor and trace elements concentrations data of pottery samples
Samples K% Ca% Ti% Cr Mn Fe% Ni Cu Zn Ga Br Rb Sr Y Zr Nb Pb

C1 1.2 20.0 0.2 138 437 2.8 103 98 98 12 10 29 513 17 126 11 12

C2 1.0 12.2 0.4 791 1342 4.3 545 56 105 13 33 428 19 98 13 27
C3 1.0 12.7 0.3 796 1197 3.8 346 46 91 14 29 379 20 88 11 29
C4 1.1 12.6 0.4 501 980 3.4 355 51 96 21 67 277 25 198 12 36
C5 1.4 20.2 0.3 155 545 2.7 108 88 105 14 12 35 553 21 101 12 13
C6 1.3 20.8 0.3 144 378 2.4 101 91 115 15 31 546 19 101 12 14
C7 1.2 12.2 0.4 490 1045 4.0 328 56 121 14 99 274 24 182 15 28
C8 1.2 12.5 0.4 764 1181 3.9 321 51 119 13 11 29 442 18 96 13 28
C9 1.2 16.2 0.3 578 952 4.0 487 54 117 14 38 480 16 98 11 28
C10 1.2 12.1 0.4 594 838 4.1 368 43 98 15 65 329 22 121 11 27
C11 1.0 13.0 0.3 780 1135 3.6 356 47 103 25 395 16 88 11 21
C12 1.3 14.5 0.4 614 915 3.4 344 61 111 28 354 17 106 12 29
C13 1.0 13.4 0.4 607 942 3.4 387 51 101 24 416 15 102 13 27
C14 1.3 12.4 0.4 617 1252 3.9 347 64 105 29 333 20 107 15 28
C15 1.2 10.1 0.2 273 699 2.0 188 28 47 16 279 11 100 14
C16 1.1 13.2 0.3 812 1318 2.8 407 46 102 35 309 20 100 11 25
C17 1.4 15.4 0.4 646 1021 3.1 420 44 115 26 295 16 102 11 26
C18 0.9 9.1 0.2 271 680 2.1 198 24 56 17 243 11 83
C19 1.3 13.3 0.3 610 940 3.3 355 54 106 24 352 17 96 14 28
C20 1.2 12.7 0.4 844 1188 3.8 350 54 103 28 381 19 100 22
C21 0.7 12.2 0.3 654 999 3.0 305 37 93 40 85 25 202 17 19
C22 2.2 14.4 0.4 879 1259 4.0 308 45 126 60 224 35 204 11 26
C23 1.0 10.4 0.2 301 704 2.0 201 27 55 14 244 13 94 11
C24 1.1 13.6 0.4 656 1069 4.6 337 50 104 90 212 30 193 14 30
C25 1.2 12.4 0.4 981 1279 4.6 331 64 123 44 417 25 130 16 27
C26 1.1 14.2 0.4 741 1413 5.0 357 54 107 20 98 224 35 204 15 33
C27 1.3 12.7 0.5 833 1259 4.6 349 65 140 16 71 314 29 178 15 24
C28 1.0 10.5 0.2 245 794 2.5 195 29 49 14 15 251 11 95 11
C29 0.8 10.1 0.3 302 794 2.0 204 30 50 12 17 257 13 102 16
C30 1.0 9.8 0.2 304 708 1.8 218 28 55 14 19 224 13 126 18
C31 1.3 15.6 0.4 458 1339 4.9 381 66 163 18 136 296 30 159 15 28
C32 1.0 8.8 0.2 309 677 2.1 217 32 52 15 222 10 103 11
C33 1.4 12.9 0.4 547 1112 5.0 405 63 128 16 65 401 20 101 11 25
C34 1.1 19.1 0.3 987 1093 3.7 517 64 91 29 410 15 70 12 24
C35 0.3 13.2 0.4 369 1026 5.2 510 41 95 13 5 115 14 27 11 17
C36 1.1 12.5 0.7 688 1302 4.0 480 52 108 14 13 28 308 17 141 15 29
C37 1.2 15.6 0.4 765 1025 5.5 504 62 130 15 101 257 22 118 11 24
C38 1.3 16.1 0.5 499 1394 4.8 501 58 135 16 87 282 29 86 14 30
C39 0.8 12.7 0.4 532 1055 2.2 407 47 103 16 343 11 199 11 21
C40 1.0 9.9 0.2 304 781 1.9 199 27 63 18 251 14 101 15
C41 1.4 14.6 0.5 402 1401 4.7 355 58 134 19 88 277 29 78 13 23
K42 1.3 17.5 0.3 701 987 4.4 425 61 120 18 11 69 365 19 77 12 32
K43 1.1 16.4 0.4 506 1024 4.7 465 67 107 13 59 336 17 109 12 29
K44 1.3 17.1 0.4 641 1002 3.8 501 59 115 14 63 367 22 141 11 34
All values are in lg/g except otherwise stated

results and can be helpful in finding errors that may exist in samples with the same factor score patterns can be grouped
the data set. In addition, factor scores may be utilized to together into these categories. Figures 2 and 3 present plots
identify grouping of the samples into particular categories, of factor score 1 against factor scores 2 and 3, respectively,

123
X-ray fluorescence 459

1.4 2.5
C6
2.0 C5
1.2 C1

1.5 C31
K41 C38
1.0 1.0 K42
K43 C37
C26
C27
C33
K44
C7 C24C35

Factor 2
0.8 0.5 C12
C34
C9 C25
C14
C19
C4 C22
C8
C10 C2
C36
0.0 C13 C17
C20
C11C3
C21
0.6 C16
-0.5

0.4 -1.0
C29
C40
C28
C30C23
-1.5 C15
C18
C32
0.2
-2.0 C39

0.0 -2.5
C_35
C_39
C_30
C_29
C_40
C_32
C_28
C_23
C_18
C_15
C_21
C_22
C_36
K_41
C_38
C_37
C_34
C_27
C_25
C_31
C_26
C_24
C_7
C_4
C_10
K_42
K_44
K_43
C_33
C_9
C_16
C_17
C_14
C_13
C_19
C_12
C_8
C_20
C_11
C_3
C_2
C_6
C_5
C_1
-3.5 -3.0 -2.5 -2.0 -1.5 -1.0 -0.5 0.0 0.5 1.0 1.5
Factor 1
Fig. 1 Grouping of pottery samples from Tell Jendares site by cluster
analysis Fig. 2 Factor score 1 versus factor score 2 of pottery samples

3
Table 2 Factor loading for fifteen elements in the data set for prin- C22
2
cipal component as factor analysis, and varimax as rotation C7 C26
C27
C31C24
C4
1 C30 C21
C25C39
Elements Factor 1 Factor 2 Factor 3 Communality C15C40 C14 K44
C10 C36
C1 C5 C29 K41 C33C38
C37
C6 C19 C8
0 C23C32
C28
C12
K43
C13
C17 C16
C9 C20
K42 C2
C18 C3
K 0.02 0.33 0.66 0.55 C11
Factor 3

-1 C34

Ca -0.03 0.85 -0.04 0.73

Ti 0.69 0.53 0.15 0.78 -2

Cr 0.93 0.04 0.14 0.88 -3

Mn 0.92 0.07 0.12 0.86 -4
Fe 0.33 0.64 -0.11 0.52 C35
-5
Ni 0.95 0.08 -0.13 0.92
-6
Cu 0.07 0.89 0.10 0.81 -3.5 -3.0 -2.5 -2.0 -1.5 -1.0 -0.5 0.0 0.5 1.0 1.5
Zn 0.50 0.77 0.18 0.87 Factor 1
Rb 0.31 0.60 0.61 0.83
Fig. 3 Factor score 1 versus factor score 3 of pottery samples
Sr -0.10 0.36 0.10 0.15
Y 0.34 0.68 0.47 0.79
Zr 0.07 -0.03 0.92 0.85 From Figs. 2 and 3 and returning to factor loading in
Nb -0.02 0.01 0.40 0.16 Table 2, it is clear that samples of group 1 have the highest
Pb 0.78 0.50 0.19 0.91 concentration of elements (Ti, Cr, and Mn) compared with
Variance explained 28.6 27.5 14.8 70.9 group 2 for the 15 elements used in data analysis (See Fig. 2).
by factors% It is also evident from these figures that group 2 differs from
groups 1 and 3 where the concentration of elements Ca, Cu,
Zn and Rb are lower than for groups 1 and 3. Table 3 sum-
for each of the 44 samples. A deep examination of Figs. 2 marizes these results by presenting the average elemental
and 3 indicates that the 31 samples identified as group 1 concentration and standard deviation for the samples in
from the cluster analysis in Fig. 1 follow a consistent groups 1, 2 and 3. This table illustrates the variation in ele-
pattern. We find the same notice for the eight samples and mental concentrations between the three categories.
the three samples, identified as groups 2 and 3, respectively It is evident, from this table, that categories 2 differs
from the CA in Fig. 1. Finally it is clear from Figs. 2 and 3 from the other categories since Pb did not detected and Cu,
that samples C35, and C39 do not follow a consistent and Rb have the lowest concentration in this category.
pattern with any group, which identifies these samples as
unique samples among the data set. The results obtained by
factor scores confirm that 100% of the pottery samples Conclusions
classified by cluster analysis are correctly classified. The
results confirm the existence of two major groups in In this paper, we used statistical classification, based on the
addition to a third small one. elemental composition of archaeological pottery. XRF

123
460 E. H. Bakraji et al.

Table 3 Mean values and standard deviation for the three chemical mainly on typology to classify material in fragmented
groups in the pottery condition.
Elements Group 1 (n = 31) Group 2 (n = 8) Group 3 (n = 3)
Mean ± SD Mean ± SD Mean ± SD Acknowledgements The author wishes to thank the International
Atomic Energy Agency (project ARASIA/1/010) and Prof. I. Othman
K 12000 ± 2000 10000 ± 1000 13000 ± 600 Director General of AEC of Syria and Dr. B. Jamous Director General
Ca 141000 ± 18000 98000 ± 6000 203000 ± 4000 of antiquity and museum in Damascus for their supporting of this
work.
Ti 3900 ± 800 2000 ± 300 2600 ± 400
Cr 700 ± 150 300 ± 23 140 ± 9
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