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Spectrochimica Acta Part A 86 (2012) 299–304

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Spectrochimica Acta Part A: Molecular and


Biomolecular Spectroscopy
journal homepage: www.elsevier.com/locate/saa

The function of prehistoric lithic tools: A combined study of use-wear analysis


and FTIR microspectroscopy
Stella Nunziante Cesaro a,∗ , Cristina Lemorini b
a
Istituto per lo Studio dei Materiali Nanostrutturati (ISMN-CNR) c/o Chemistry Department, University of Rome “Sapienza”, P.le A. Moro 5, 00185 Rome, Italy
b
Dipartimento di Scienze dell’Antichità, University of Rome “Sapienza”, P.le A. Moro 5, 00185 Rome, Italy

a r t i c l e i n f o a b s t r a c t

Article history: The application of combined use-wear analysis and FTIR micro spectroscopy for the investigation of the
Received 3 December 2010 flint and obsidian tools from the archaeological sites of Masseria Candelaro (Foggia, Italy) and Sant’Anna
Received in revised form 13 June 2011 di Oria (Brindisi, Italy) aiming to clarify their functional use is described. The tools excavated in the former
Accepted 14 October 2011
site showed in a very high percentage spectroscopically detectable residues on their working edges. The
identification of micro deposits is based on comparison with a great number of replicas studied in the
Keywords:
same experimental conditions.
FT-IR
FTIR data confirmed in almost all cases the use-wear analysis suggestions and added details about the
Microspectroscopy
Use-wear
material processed and about the working procedures.
Prehistory © 2011 Elsevier B.V. All rights reserved.
Lithic tools

1. Introduction Nowadays, the microscopic observation of a variety of traces, here-


after referred as use-wear analysis, based on the evidence that each
The study of prehistoric stone tools aiming to infer their use worked material induces distinctive alteration on lithic artefacts, is
gives an important contribution to the knowledge of economic, a well established method.
social and symbolic aspects of ancient communities life. The presence of microscopic amounts of the worked material
The interest towards prehistoric activities induced archaeolo- entrapped in the micro-cavities of the irregular surface of lithic
gists, at the end of the 19th century, to analyze the polishes induced tools edges was ascertained in the late 70s and reported in a number
by the worked material on prehistoric stone tools and compare of papers sometimes aiming to understand the formation process
them to traces observed on replicas [1,2] or on ethnographic items of use-wear whose genesis is still an open problem [9 and refs.
whose function was known [2]. The interest engendered by the therein]. In this view the pioneer morphological and/or chemical
translation of the Semenov’s book “Prehistoric Technology” [3] analysis of residues [10,11] of the material worked opened new
encouraged many western scholars to deal with use-wear analysis. perspectives of research alongside the more traditional use-wear
Lithic tools were usually analyzed by means of low powered micro- analysis. Although residues can suffer morphological and chemi-
scopes in reflected light looking principally at the micro-fractures cal degradation in the archaeological deposits still the detection of
developed on the working edge-profiles [4–6]. surviving residues with a variety of experimental procedures gave
The use of high powered microscopes was introduced by Keeley encouraging results in the last decades [9,12].
[7] and allowed to gain information on polishes defined as visible Scanning electron microscopy (SEM), electron dispersive X-ray
alteration of the stone tool surface influencing its reflectivity when (EDX) and ion beam analysis (IBA) techniques, for example, were
viewed through the microscope. extensively applied to determine the elemental composition of
The capability of the low or high powered microscopic analy- residues and allowed to distinguish between bone or wood deposits
sis was controversial until the methodological settlement reached from the relative abundance of calcium and phosphor [13–15]. In
only in 1989 at the Conference “The interpretative possibilities of addition, it was possible to estimate for many residues a surface
micro-wear studies” held in Uppsala (Sweden) where the valid- density of few ␮g/cm2 and a thickness ranging from few ␮g/cm2
ity and complementarity of both methods was recognized [8]. up to 1 mg/cm2 . This means that thick deposits are not simple over-
layers but diffuse into the stone and this fact explains their survival
since prehistoric periods [15].
∗ Corresponding author. Tel.: +39 0649913962; fax: +39 0649913951. More recently, organic residues of animal and vegetable origin
E-mail addresses: stelluccia.nunziante@ismn.cnr.it (S. Nunziante Cesaro), were identified by means of gas chromatography–mass spectrom-
cristina.lemorini@uniroma1.it (C. Lemorini). etry (GC–MS) after extraction via Fatty Acid methyl Ester (FAME)

1386-1425/$ – see front matter © 2011 Elsevier B.V. All rights reserved.
doi:10.1016/j.saa.2011.10.040
300 S. Nunziante Cesaro, C. Lemorini / Spectrochimica Acta Part A 86 (2012) 299–304

technique [16, 17 and refs. therein] or studied adopting the cross- Table 1
List of the lithic replicas and material worked.
over immune electrophoresis (CIEF) method [18].
Up till now FTIR micro-spectroscopy was never adopted for non- Replicas Raw material Material worked Replicas with
invasive identification of residues on archaeological lithic tools detectable residues
although this technique does not require chemical or mechani- 2 Obsidian Antler 2
cal pre-treatment of the sample investigated and can distinguish 3 Flint Antler 1
between organic and inorganic samples. 2 Obsidian Bone 0
7 Flint Bone 6
In order to test the advantages and the limits of this technique
6 Obsidian Fleshy tissues 5
and to combine two independent methods we carried out a system- 1 Flint Fleshy tissues 1
atic use-wear analysis of lithic assemblages from well preserved 1 Obsidian Fleshy tissues + bone 0
prehistoric sites. All items showing micro-traces were therefore 7 Flint Fleshy tissues + bone 4
11 Flint arrowhead Fleshy tissues + bone 6
spectroscopically analyzed to ascertain the presence of residues.
1 Flint Fleshy tissues + bone 1
These were identified by comparison with a reference collection of boiled + marrow
replicas that worked a wide selection of animal, plants and mineral 9 Obsidian Hide 3
materials. 20 Flint Hide 18
The procedure here proposed can introduce a new perspec- 6 Flint Hide + brain 4
1 Flint Hide + salt + brain 1
tive in the functional study of lithic industries. Since stone tools
1 Flint Hide + fleshy tissues 1
were used for a variety of activities including butchering, hide, 4 Flint Tendons 4
bone and wood-working, harvesting, etc., we are providing a data- 2 Obsidian Shell 0
base where inferences drawn by the mentioned approaches are 1 Flint Shell 1
1 Flint Teeth 1
reported and critically compared. In this paper results related
to the activities involving contact with animal materials are
presented.
2.3. Optical analysis of archaeological use-wear

2. Experimental Use-wear analysis was performed with both low and high-
power approach using respectively a stereomicroscope SMZ
2.1. Samples (Nikon) with objective 0.5×, oculars 10× and magnification range
0.75×–7.5× and a metallographic microscope Eclypse (Nikon) with
699 archaeological flint tools and 53 obsidian tools were oculars 10× and objectives 10× and 20×. Both microscopes were
selected for use-wear analysis. They represent the knapped lithic used in reflected light.
assemblage of two Neolithic sites from Southern Italy dating from
VII to VI millennium BP. 2.4. FTIR spectroscopy
628 flint tools come from the three layers of the Middle
Neolithic deposit of Masseria Candelaro (Foggia), one of the few Reflectance spectra were obtained using the last generation
entrenched villages characterizing the Neolithic period of the infrared microscope Hyperion (Bruker) in the frequency range
wide plain bordering eastwards the Adriatic Sea called “Tavoliere” 4000–600 cm−1 at a resolution of 2 cm−1 or better cumulating at
[19]. least 200 scans to achieve an optimal signal-to-noise ratio. Spots of
267 lithic tools had use-wear; out of them 72 showed traces 100 × 100 ␮ were normally selected. All archaeological and experi-
attributable to animal materials processing [20]. mental items were analyzed both on regions not showing use-wear,
71 flint tools and 53 obsidian tools come from the Neolithic set- in order to have a suitable reference (‘blank’ spectra) and on many
tlement of Sant’Anna di Oria (Brindisi) consisting of two huts, the points of the used edges in order to individuate the micro-residues
more recent built over the remains of the previous one [21]. and check the reproducibility of their spectral patterns. The sam-
According to use-wear analysis, 8 flint tools and 13 obsidian ples housing was kept under continuous flow of dry nitrogen to
tools were used to process animal tissues [22]. eliminate atmospheric water and carbon dioxide.
The reference collection for FTIR analysis consists of 64 flint and
22 obsidian tools (Table 1) that were used to reproduce prehistoric
3. Results and discussion
activities as hunting, butchering, hide processing and production
of hard animal material implements and ornaments.
FTIR analysis singled out detectable residues on 49 flint repli-
cas out of 64 (77%) and 10 obsidian replicas out of 22 (45%)
2.2. Cleaning procedures (Table 1). Among the artefacts showing use-wear attributed to
animal material contact, the presence of residues was spectro-
Following the most diffused protocol carried out by use-wear scopically ascertained on 52 archaeological flint implements out
analysts, the archaeological tools were washed with water to of 79 (66%) and on 3 archaeological obsidian implements out of 13
remove the soil deposit from the surface. A further washing with (23%). This are collected in Table 2 where use-wear analysis sug-
de-ionised water in ultrasonic tank for 5–10 concluded the proce- gestions are compared to the proposed nature of micro-residues
dure. spectroscopically individuated. In the same table, 9 flint tools from
Before FTIR analysis, the second step of the washing proce- Masseria Candelaro showing use-wear interpreted as stone, min-
dure was repeated in order to eliminate all the residues not firmly erals, abrasive and not defined medium hard material are also
entrapped in the micro-cavities of the surface. reported since FTIR analysis detected residues of animal tissues in
Replicas expressly made for infrared observation were not contrast with use-wear suggestions.
washed at all. Conversely, experimental samples to be submitted to The higher percentage of residues observed on both prehistoric
use-wear study only, were washed in threes steps: water and soap, and experimental flint tools with respect to obsidian ones seems
chemical washing with a diluted acid followed by diluted base and compatible with the greater roughness of the former material. The
finally with de-mineralized water in ultrasonic tank, in order to stones, in fact, have identical chemical composition (mainly silicon
maximize the removal of residues while preserving the traces. oxide) but flint is microcrystalline while obsidian is a volcanic glass
S. Nunziante Cesaro, C. Lemorini / Spectrochimica Acta Part A 86 (2012) 299–304 301

Table 2 Table 3
List of archaeological tools from Masseria Candelaro and Sant’Anna di Oria with Infrared absorption frequencies (cm−1 ) of flint, obsidian and residues with the pro-
related use-wear interpretation and proposed attribution of micro-residues. posed assignment.

Archaeological site Use-wear Micro-residues Items Frequency (cm−1 ) Proposed assignment


analysis
2913 ␯C–H of proteins
Masseria Candelaro Fleshy tissues Adipocere 3 2845 ␯C–H of proteins
Fleshy tissues Adipocere, calcite 4 1735 ␯C O of lipids
Fleshy tissues Adipocere, bone, 1 1647 ␯C O of proteins (amide I)
proteins, calcite 1523 ␦N–H and ␯C–N of proteins (amide II)
Fleshy tissues Adipocere, bone, 1 1573 ␯C–O of fatty acid calcium salt carboxylate (adipocere)
proteins 1537 ␯C–O of fatty acid calcium salt carboxylate (adipocere)
Fleshy tissues Adipocere, proteins, 1 1392 ␦CH2 of proteins
calcite 1158 ␯Si–O (flint)
Fleshy tissues Adipocere, lipids, 1 790 ␦O–Si–O (flint)
proteins, calcite 1412 ␯as CO3 stretching of calcite
Fleshy tissues Bone, calcite 1 877 ␦as CO3 deformation of calcite
Fleshy tissues Proteins 1 912 ␯P–O (hydroxiapatite)
Fleshy tissues Calcite 1
Hide Adipocere, bone, 2
calcite
Hide Adipocere 3
Hide Adipocere, calcite 7 intensity peak approximately at 780 cm−1 readily assigned to the
Hide Adipocere, proteins, 2 Si–O stretching and to O–Si–O bending modes respectively [23–25].
calcite
The presence of the fundamental modes of SiO2 is an obvious
Hide Proteins, calcite 1
Hide Calcite 4
constraint to the detection of residues vibrations. However, ‘blank’
Hide and fleshy Adipocere, calcite 2 spectra of both materials did not present other features apart the
tissues mentioned ones even at high magnification. In addition, they were
Hide and fleshy Adipocere, bone, 1 absolutely reproducible and, as a consequence, the spectral changes
tissues lipids, calcite
observed were confidently attributed to the presence of different
Hide and fleshy Adipocere, proteins, 1
tissues calcite material.
Hide and fleshy Calcite 2 Table 3 summarizes the infrared vibrations assigned to residues
tissues and detected, separately or in different combination, both in
Hide, fleshy Adipocere, bone, 1
archaeological and experimental samples. As no diagnostic bands
tissues and bone lipids, calcite
Medium hard Adipocere, bone, 2
were detected in the 4000–3000 cm−1 range, the stack plots of the
material lipids, proteins, 3000–600 cm−1 interval only are reported in the following.
calcite The spectra of unused portions and ‘polished’ areas of flint repli-
Medium hard Bone, calcite 2 cas which worked hard tissues such as bone or teeth or antler
material
showed, in a high percentage of cases, appreciable differences with
Medium hard Bone, proteins, 1
material calcite respect to the blank. Analogous changes were observed in the spec-
Hard animal Adipocere, bone, 1 tra of several experimental flint tools used for hide processing.
material proteins, calcite Experimental obsidian tools appeared affected by the contact with
Hard animal Bone, calcite 1
antler only. The slope of the intense silicate stretching band, in fact,
material
Hard animal Bone, proteins, 1
appeared less steep towards the low frequency side and a shoulder
material calcite was detected at 912 cm−1 . A few samples showed additional peaks:
Hard animal Calcite 3 weak broad features at 1633, 1533, 1392 cm−1 and sharper peaks
material of low intensity at 2913 and 2845 cm−1 .
Abrasive Adipocere, bone, 1
It is known that hard animal tissues (teeth, bone, antler and
lipids, calcite
Abrasive Lipids, proteins 1 tusks) are a complex mixture of a phosphatic mineral phase (car-
Stone Bone, calcite 1 bonated hydroxiapatite) and an organic matrix, mainly constituted
Minerals Proteins, calcite 1 of a flexible protein (collagen). The vibrational behaviour of recent
Sant’Anna di Oria Hide Adipocere 1 and ancient samples of human or animal origin has been exten-
Hide Adipocere, bone, 1 sively investigated in the past. Literature data agree in assigning the
calcite most intense IR absorption lying in the 1170–900 cm−1 interval to
Hide Bone, proteins 1
the asymmetric stretching mode (␯3 ) of the PO4 3− of hydroxiapatite
Hide Lipids 2
Hide Lipids, calcite 1 [26–29] and the peaks around 1630, 1540 and 1390 to the amide
Hide Ipids, proteins, 1 I (␯C O ) and amide II (␦N–H and ␯C–N ) modes and CH2 deformation
calcite of the proteinaceous component (mainly collagen) respectively
Fleshy tissues Bone, calcite 1 [30–32]. Amide III absorption, normally weak and expected around
Fleshy tissues Lipids 1
1240 cm−1 was never detected because of its closeness to the SiO2
stretching intense mode. Bands appearing in the 2800–3000 were
assigned to C–H stretching cm−1 .
In recent samples the organic matrix/mineral phase ratio is
which presents a smoother surface. The lack of micro-cavities suit- about 0.5 [27,29] but it can decrease in fossil samples since col-
able for long-lasting trapping of residues should also explain the lagen can survive for millennia but it is very affected by the burial
lower amount of worked material found on prehistoric obsidian conditions [33,34].
tools with respect to the experimental ones. In this work a few samples of ancient and recent bones, teeth
All archaeological and experimental tools were firstly ana- and antler were examined in the same experimental conditions of
lyzed in unused parts. As expected, flint and obsidian showed stone items. In all cases an excellent agreement with literature data
two vibrations: an intense band around 1200 cm−1 and a medium was found. In Fig. 1 an archaeological bone is compared to a bovine
302 S. Nunziante Cesaro, C. Lemorini / Spectrochimica Acta Part A 86 (2012) 299–304

1.0

0.35 0.40

912
0.8

0.30
Reflectance
0.25
0.6
Reflectance

2913
2845
0.20
1633
1533

1392

1736

1574
1540
0.4

0.15
0.10
b c
0.2

0.00 0.05
b
a a
0.0

3000 2500 2000 1500 cm-1 1000 3000 2500 2000 1500 cm-1 1000

Fig. 1. Micro FTIR spectra of fossil (a) and recent (b) bone. Fig. 3. Micro FTIR spectra of: unused portion of flint tool (a), flint replica that worked
hide (b), working edge of flint tools n. 3405 and n. 2920 from Masseria Candelaro (c
and d).
fresh sample showing the expected lowering of intensity of peaks
attributed to collagen.
In Fig. 2 the spectra of flint replicas that worked bone and This evidence suggests a butchering activity with a consequent con-
fleshy tissues are compared to archaeological tools of different tact with bones. In this case, the FTIR investigation details traces
provenance: flint artefact n. 1066, 3105 and 3388 from Masse- analysis.
ria Candelaro showing traces attributed to stone, hard material Spectroscopic data add information also in case of the flint tools
of unknown nature and bone respectively and n. 222 and 1092 3105 and 1066 from Masseria Candelaro (Fig. 2f and g). In the for-
from Sant’Anna di Oria with polishes interpreted as hide and fleshy mer case, polish is interpreted as generic hard material contact
tissues contact. while the residues analysis evidences the presence of hard ani-
Unfortunately the strong SiO2 stretching mode of flint and mal material remains. In the latter case, the spectrum suggests the
obsidian partially hides the PO4 3− stretching mode. However, it existence of an analogous residue in contrast with the traces inter-
seems reasonable to attribute the spectral changes observed to the pretation. The spectroscopic investigation is therefore particularly
overlapping of the mentioned bands. The concurrent detection of valuable in detailing not well developed polishes due to stone or
absorption peaks attributable to the amide I, amide II and CH2 bend- bone or teeth which can appear quite similar.
ing bands of the organic component, in the proper intensity ratio, It is worth adding that hide worked with replicas (Fig. 2b) was
supports the hypothesis of hard animal material micro residues contemporary processed with osseous tools. Evidently, during the
entrapped in micro cavities of the edges of the archaeological arte- experiment bits of bone from osseous tools scattered on the worked
fact. As predicted, the intensity of peaks assigned to proteins vs the surface of hide and migrated on the edge of the stone tool. A similar
silica and apatite overlapped stretching modes appear less promi- procedure could be hypothesized in order to justify the presence of
nent in archaeological than in experimental tools. hard animal tissues on the archaeological stone tools showing use-
The identification of hard animal tissues residues in ancient arte- wear of hide processing such as the artefact n. 222 from Sant’Anna
facts showing traces of bone contact, e.g. the flint tool n. 3388 from di Oria (Fig. 2d).
Masseria Candelaro (Fig. 2h) and in the correspondent experimen- The stack-plots reported in Fig. 3 compares the spectrum of a
tal implements seems quite straightforward. flint replica used for hide processing to those of archaeological
More surprising, however, the presence of hard animal mate- flint items n. 2920 (Masseria Candelaro) with traces interpreted
rial residues on ancient artefacts with polishes suggesting only soft as hide working and n. 3405 (Masseria Candelaro) with polishes
animal tissues contact. As an example, the flint item n. 1092 from interpreted as contact with fleshy tissues, hide and bone.
Sant’Anna di Oria (Fig. 2e) shows use-wear of meat while spec- In the spectra of all specimens, excluding the artefact n. 2920
troscopic data reveals the presence of hard animal tissues residues. (Fig. 3d), the mentioned bands in the 1650–1400 cm−1 range are
still detectable and assigned to amide I and II modes of proteins
present in the biological tissues.
An additional peak is observed at 1736 cm−1 and attributed, for
0.7

912

its spectral position, to the carbonyl CO band of unsaturated tria-


0.6

cylglycerols constituting the subcutaneous fatty layer of the skin


2913
2845

[35–38].
1633

1533
1392
0.5

Some dissimilarities between recent and archaeological arte-


Reflectance

h
facts must be evidenced. In the spectra of the ancient tool n. 3405
0.4

g
f from Masseria Candelaro (Fig. 3c), e.g., the bands attributed to
0.3

proteinaceous tissues, that is the amide bands and CH stretching


e modes, loosen intensity with respect to the peak assigned to fat
0.2

d
tissue. Amide bands show also some coalescence indicating same
c degradation of the remain [39].
0.1

b The tool n. 3405 from Masseria Candelaro shows also the shoul-
a der at 912 cm−1 , discussed above and confidently attributed to hard
0.0

3000 2500 2000 1500 cm-1 1000 animal material working in agreement with use-wear analysis. In
addition, a doublet starts to appear at 1574/1540 cm−1 definitely
Fig. 2. Micro FTIR spectra of: unused portion of flint tool (a), flint replica that worked
indicating the presence of calcium palmitate which is an impor-
skin (b), flint replica that worked bone (c), working edge of flint tools n. 222 and n.
1092 from Sant’Anna di Oria (d and e), working edge of flint tools n. 1066, 3105 and tant constituent of adipocere [35–37]. The formation of adipocere
3388 from Masseria Candelaro (f–h). or grave wax is the result of a microbial activity converting body fat
S. Nunziante Cesaro, C. Lemorini / Spectrochimica Acta Part A 86 (2012) 299–304 303

4. Conclusions

This work emphasises the usefulness of combined use-wear


and residues analyses to interpret the function of prehistoric stone
tools. Flint or obsidian assemblages from the Masseria Candelaro
and Sant’Anna di Oria archaeological sites showing use-wear of
animal tissues processing have been investigated.
For the first time FTIR micro spectroscopy has been extensively
employed for the non destructive individuation of deposits without
pre treatment or manipulation of samples. The identification of the
remains has been based on comparison with residues present on a
suitable number of replicas.
In almost all cases spectroscopic data supported the use-wear
analyses adding some explicative details.
Organic and inorganic remains have been confidently individu-
Fig. 4. Micro FTIR spectra of a flint tools that worked calcite: unused portion of
ated indicating the presence of hard and soft animal tissues and/or
flint tool n. 169 from Masseria Candelaro (a), working edge of flint tool n. 169 from
Masseria Candelaro (b), flint replica that worked calcite (c). calcite. Moreover, the simultaneous presence of residues of differ-
ent nature detailed the work processing adopted in the prehistoric
times.
The percentage of residues on archaeological items itself indi-
into a mixture of fatty acids palmitic, stearic and myristic, and/or cates the existence of more or less favorable conditions to their
in their calcium salts [38]. The conversion is a long-lasting process survival through centuries which can be schematized in three
which requires the proper conditions of humidity. In the spec- factors: implements raw material, working time-span and post-
trum of sample n. 2920 from Masseria Candelaro (Fig. 3d), only depositional processes.
the adipocere fingerprint is present suggesting that residues of dif- A very high percentage of implements with micro remains on
ferent nature were too scarce to be spectroscopically observed. the working edges has been observed in the assemblage of Masseria
Alternatively, a complete conversion of fatty micro residues can be Candelaro.
considered due to a particularly favorable archaeological context The industry of Masseria Candelaro consists only of flint imple-
at least for some lapses of time. The latter hypothesis seems quite ments which, for their coarse surface, traps the worked material
probable since the doublet at 1574/1540 cm−1 was detected in a more efficiently than obsidian. All tools present very well devel-
great number of specimens coming from Masseria Candelaro exca- oped traces attributed to a very long lasting employment of the tool
vation (Table 2). As a further proof, several replicas used for process itself. Moreover, the archaeological site suffered, after is genesis, a
the inner part of hide were spectroscopically analyzed just after the desertification process which probably ensured the best conditions
contact and showed the band at 1736 cm−1 . This lost intensity after for the survival of the resides.
few month and the doublet started at 1574/1540 cm−1 to appear
reproducing the transformation hypothesized for archaeological Acknowledgments
items.
A broad absorption band centered about 1412 cm−1 was The authors acknowledge the Wenner Gren Foundation (NY)
observed in many prehistoric stone tools and when intense it was that supported this research with an International collaborative
paralleled by a weaker feature at 877 cm−1 . On grounds of com- Research Grant.
parison to experimental tools that worked calcareous stones, the The authors acknowledge Prof. A. Manfredini (University of
bands are assigned to ␯3 and ␯2 modes respectively of calcite Rome “Sapienza”) and Prof. E. Ingravallo (University of Lecce) who
residue [40]. For sake of example, the spectra of a flint replica gave the permission to analyze, respectively, Masseria Candelaro
which worked calcite and the flint item n. 169 from Masseria Can- and Sant’Anna di Oria lithic assemblages.
delaro, with traces suggesting a contact with hide, are compared in
Fig. 4.
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