Archaeometry 44, 4 (2002)

Maize613– and
624. Printed
bone: in Great Britain
residues of grinding in northwestern Argentina 613

MAIZE AND BONE: RESIDUES OF GRINDING IN

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NORTHWESTERN ARGENTINA*

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M. DEL PILAR BABOT
Instituto de Arqueología y Museo (IAM), Universidad Nacional de Tucumán,
San Martín 1545, (4000) San Miguel de Tucumán, Argentina

and M. C. APELLA

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Centro de Investigaciones y Transferencia en Química Aplicada (CIQ), Universidad
Nacional de Tucumán, Miguel Lillo 205, (4000) San Miguel de Tucumán, Argentina

Archaeometric and archaeobotanical analyses of grinding residues inside an archaeological

milling stone tool from the Cueva de los Corrales 1 site in northwestern Argentina are
shown. Multiple analytical techniques are used to identify ground substances, and their
results are compared and complemented. They give direct and reliable evidence of maize
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(Zea mays L.) and burned bone grinding in the pre-hispanic Argentine north-west, although
the latter is mainly related to milling tasks.
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KEYWORDS: ARCHAEOMETRY, PALAEOETHNOBOTANY, MAIZE STARCH, ZEA MAYS L.,
GROUND BONE, HYDROXYAPATITE, NORTHWESTERN ARGENTINA, MILLING STONE TOOLS
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INTRODUCTION

Physicochemical and archaeobotanical analyses yield important data on the technologies and
natural resources used in the past when studying residues in archaeological grinding tools. Such
analyses not only give direct and reliable clues as to what substances were really ground, but
they may also modify erroneous beliefs and assumptions concerning the function of tools. In
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this framework, it appears essential to determine to what extent grinding tools—traditionally

thought to be employed in food processing—were also used to process a variety of plant
materials and even non-edible substances. Through ethnoarchaeological, residue and use-wear
analyses, several studies have demonstrated the multiple functions that archaeological grinding
tools could have had (Hayden 1987; Adams 1988, 1997; Loy et al. 1992; Fullagar and Field
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1997; Piperno and Holst 1998; Babot 1999a,b; Checa et al. 1999; Babot and Würschmidt 2000;
Piperno et al. 2000; Babot and Apella 2001).
In this respect, we present the results of multiple tests carried out on the powder residues
found on the surface of a milling stone tool from the Cueva de los Corrales 1 site in northwest-
ern Argentina. Maize (Zea mays L.) and burned bone were detected, providing a good example
of the diversity of materials that could be related to milling tasks.
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To yield reliable evidence, we have integrated a suite of analytical techniques: microbotanical

remains analysis by petrographic microscopy and the I2-KI solution test, and compositional and
structural analyses (through X-ray fluorescence, gas chromatography—mass spectrometry, X-
ray energy-dispersive analyses, Fourier transform infrared spectroscopy, X-ray diffraction and

* Received 20 May 2001; accepted 21 February 2002.

© University of Oxford, 2002

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Figure 1 The location of the Cueva de Los Corrales 1 (CC1) site.

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scanning electron microscopy, respectively). As a result, we can point out that we can get more
complete data by using multiple lines of analysis.

MATERIALS AND METHODS

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The archaeological material studied came from the Cueva de los Corrales 1 site (CC1), a rock
shelter 3000 m above sea level at El Infiernillo, Tucumán, in northwestern Argentina (Caria
et al. l999) (Fig. 1). Several multiple-activity occupations took place at site CC1, which was
remarkable for its well-preserved contexts and for the occurrence of several bedrock mortars
used to make clayey pigment mixtures (Babot and Apella 2001). The occupations may be
attributed to farmer-ceramic groups who inhabited the Sierras Pampeanas area, including
Sierras del Aconquija, after c. 2000–1500 years bp (Scattolín and Gero 1999).

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 Maize and bone: residues of grinding in northwestern Argentina 615

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Figure 2 The milling stone tool analysed, showing the whitish-grey residues on its active surface.

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The artefact studied is a migmatite milling stone tool that was found covering a bedrock
mortar at the sloped entrance of the cave, with its active face down, in a ‘stored’ position that
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protected residues from posterior contamination (Fig. 2). Residues appeared as a layer of
abundant, whitish-grey powder, distributed only over the pecked active surface of the tool.
They were clearly different in colour and texture from the inorganic surrounding sedimentary
matrix, which was compounded by the eroded sediments of sandstones and pelites from Corral
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Quemado Formation at Los Corrales River (Bossi and Palma 1982).

Several compositional and structural analyses described below were carried out to identify
the residues, which were sampled by means of gentle brushing.

Petrographic microscopy: the I2-KI solution test

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In order to get a general view of the residues, a sample—mounted in a glycerine and Canada
balsam medium—was observed in a Zeiss Axioskop petrographic microscope at magnifications
of 400× maximum, with polarized and non-polarized light. The I2-KI solution test was used for
starch grains. Residues were compared with modern and archaeological reference collections.
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X-ray diffraction analysis (XRD)

A powder diagram was obtained with a Siemens D5000 diffractometer, using a copper
anode (λCu = 1.5406 Å). The diffraction lines obtained were assigned to hydroxyapatite
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(Ca10(PO4)6(OH)2) on the basis of the Inorganic index to the powder diffraction file (1968), card
number 9-432.

Fourier-transform infrared spectroscopy (FTIR)

The infrared spectrum in the range 4000–400 cm−1 was obtained with a Perkin–Elmer 983G
FTIR, using the KBr discs technique. The spectrum was assigned by comparison to that of pure
hydroxyapatite (Fowler 1974).

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X-ray fluorescence (XRF)

A multi-element analysis of the residues was performed with a Phillips 1540 XRF instrument.

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The compositional characterization was expressed in percentages of main and trace elements.

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Gas chromatography—mass spectrometry (GC–MS)
Solid–liquid extractions of the sample were carried out with chloroform. Extracts were sub-
mitted to gas chromatography—mass spectrometry analyses to identify the lipidic content.
A Hewlett Packard HP 6890 Series GC System coupled to a Hewlett Packard 5973 Mass
Selective Detector was used.

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(a)
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(b)

Figure 3 A micrograph of archaeological maize starch granules and burned bone particles without (a) and with
(b) polarized light. Starch grains show their characteristic extinction cross, and bone particles look semi-opaque
(magnification 400×).

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 Maize and bone: residues of grinding in northwestern Argentina 617

Scanning electron microscopy (SEM): X-ray energy-dispersive analysis (EDAX)

Samples were coated with Ag in a Balzers SCD 040 metallizer, and a Philips 515 SEM was
used to carry out the morphological characterization of their surfaces. EDAX semi-quantitative

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compositional analysis was expressed in weight percentage, element mapping and energy spectra,
using an EDAX 9100.

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RESULTS
Residues were identified as heterogeneous mixtures of burned bone and maize starch. Macro-
scopically they looked whitish-grey, according to the hues of burned bone (Gejvall 1980).
Under the petrographic microscope they appeared as a yellowish mixture of semi-opaque bone

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particles due to the optic anisotropy of bone metaplasm (Ascenzi 1980). They were together
with starch grains, silica phytoliths and microcharcoals that attest burning (Checa et al. l999)
(Fig. 3). Figure 4 shows a SEM image of bone particles and starch grains.
Bone was identified by the presence of hydroxyapatite, the main inorganic component that
constitutes a rigid matrix (Fowler 1974). EDAX semi-quantitative analysis on bone particles
showed phosphorus and calcium in a ratio corresponding to hydroxyapatite (Figs 5 and 6). The
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1.93 Ca/P ratio, calculated from XRF values (Table 1), was also comparable to the ideal 1.667
ratio for the stoichiometric material. Hydroxyapatite was clearly indicated in the X-ray
diffractogram (Fig. 7) and revealed through the presence of characteristic bands in the FTIR
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spectrum (at 3600 cm−1, 1060 cm−1, 1050 cm−1, 960 cm−1, 630 cm−1, 600 cm−1, 570 cm−1 and
480 cm−1) (Fowler 1974; and see Fig. 8). The occurrence of carbonate group bands at 1460–
1410 cm−1 and 875 cm−1 (Smith 1999) revealed partial carbonate for phosphate substitution.
The absence of displacements of the hydroxyapatite diagnostic bands in the spectrum indicates
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that there were no post-depositional calcium replacements due to chemical exchange with the
medium in the buried conditions (Sandford 1993). This situation would imply the possibility of
good preservation of residues.
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Figure 4 A scanning electron microscope micrograph of a large bone particle with an irregular surface, and
several starch granules at the sides distinguished with an arrow (bar: 50 µ m).

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(b)

Figure 5 EDAX mapping of calcium (a) and phosphorus (b) of hydroxyapatite on the bone particle of Figure 4
(bar: 50 µ m).
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Table 1 X-ray fluorescence multi-elemental analysis. Main and trace element contents in hydroxyapatite and sediments
are expressed as mass percentages

Main elements O Al S Ca Na Si Cl Fe Mg P K Sr
Percentage (%) 23.43 0.20 0.07 23.96 0.33 0.77 0.75 0.24 0.31 9.58 0.25 0.01
Trace elements Ti Mn Ni Cu Zn Ge Zr Cs Hg

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 Maize and bone: residues of grinding in northwestern Argentina 619

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Figure 6 The EDAX spectrum corresponding to Figure 4. Calcium and phosphorous of hydroxyapatite and
siliceous sediments are the main elements detected. The bands not labelled are due to the Ag coating of the sample.

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Figure 7 A diffractogram of the residue sample (λCu = 1.5406 Å) between 2θ = 5° and 2θ = 60°. The diffraction
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lines of bone hydroxyapatite are marked ‘HA’, and the lines of calcium silicate from the sedimentary matrix of site
are marked ‘CS’.

Several lipids of animal origin were detected by GC–MS that might largely be due to the fact
that bone was charred at low temperatures (Sánchez Vizcaíno and Cañabate Guerrero 1998).
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Lauric (C12), miristic (C14:0), cethilic (C16:0), oleic (C18:1) and stearic (C18:0) acids can
be found in animal fat in closer percentages to the ones obtained from the sample analysed
(Fig. 9). Pentadecilic acid (C15), cholesterol and oleamide or 9-octadecenamide are also import-
ant markers of animal lipids (Bisogno et al. 1997; Hanus et al. 1999; Boger et al. 1998; Sánchez
Vizcaíno and Cañabate Guerrero 1998; Lambert and Di Marzo 1999).
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Microscopic observations of samples and the positive reaction to I2-KI solution test showed
that the plant material was mainly constituted by simple and compound starch granules that
looked like fine bone powder, ranging in size from 1 to 20 µm, and having a symmetric
extinction cross, a central hilum with star fissures and rounded and polygonal shapes (Figs 3
and 4). These criteria determined that they came from maize kernels (Zea mays L.) (sensu
Wolf et al. 1950; Piperno and Holst 1998; Piperno et al. 2000). Cracked and broken granules
showed that the substance was submitted to a hard process of milling (Juan-Tresserras 1998;
Checa et al. 1999).

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Figure 8 The infrared spectrum of the sample in the range 4000– 400 cm−1. The band at 3600 cm−1 is attributed to
the stretching of the hydroxide (OH) group in hydroxyapatite. The two bands centred at 1050 cm−1 and 1060 cm−1
correspond to the antisymmetric P–O stretching mode of the phosphate (PO43−) group. The doublet at approximately
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600 cm−1 is assigned to the antisymmetric O–P–O bending. At 960 cm−1 there is a band that is attributed to the
symmetric P–O stretching mode. The band at 480 cm−1 corresponds to the symmetric O–P–O bending. The band
at 630 cm−1 is assigned to the OH librational mode. The bands between 1460 cm−1 and 1410 cm−1 and at 875 cm−1,
respectively, correspond to the antisymmetric C–O stretching and the out-of-plane O–C–O bending of the carbonate
(CO32−) group. The band centred at 3400 cm−1 is attributed to the stretching of the OH group of absorbed water.
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Figure 9 GC–MS spectrum of the sample. Points indicate the peaks due to lipids and appear labelled as follows:
1, cholesterol; 2, lauric acid; 3, miristic acid; 4, pentadecilic acid; 5, cethilic acid; 6, oleic acid; 7, oleamide;
8, stearic acid.
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Bilobed, trilobed and tetralobed silica phytoliths, characteristic of maize bran, were rarely
observed (Pearsall and Dinan 1992; Piperno and Pearsall 1993; Würschmidt and Korstanje
1998–9; Piperno 1998). This would reveal that kernel peeling took place before grinding, and
that it was performed in another artefact that until now has not been found at site CC1.
Phytoliths indicate that some kernels would have partially kept their bran when ground (Juan-
Tresserras 1998; Checa et al. 1999).
Bands of maize carbohydrates and fatty acids could not be ascertained though FTIR. This
fact could be attributed to the low proportion of maize components in the sample, and to the

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 Maize and bone: residues of grinding in northwestern Argentina 621

fact that some of their absorption bands overlap with those of the principal polifunctional
groups of hydroxyapatite. Nevertheless, miristic, cethilic, oleic and stearic fatty acids detected
through GC-ME (Fig. 9) could, to some extent, be also related to the presence of maize. A

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minimum amount of calcium and aluminum silicates from the sedimentary matrix of site CC1
were the only substances of mineral origin detected with XRD, XRF and MEB-EDAX (Figs 6

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and 7; Table 1).

DISCUSSION

The low amounts of starch and maize lipids suggest that these residues may be due to poor
cleaning of the tool prior to bone grinding. Maize residues would be related to a previous flour

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production episode, not linked to that of burned bone grinding. If maize had been burnt with
bone material, starch would have left no traces (Pochettino and Cortella 1989). Burned bone
grinding would have been a different and last episode of application of the tool, before dis-
carding it without cleaning. This event could have involved a search of the tool among the
discarded materials of previous occupations (a reclamation process sensu Schiffer 1987).
The ashy appearance of the sample and the presence of microcharcoals show bone burning.
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This process could have eliminated a part of the bone organic components before being finely
ground. However, the lipids of animal origin that were identified show that burning must have
been incomplete, and that the osseous material must have been submitted to different ranges of
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temperature that would have preserved organic substances in places that were more protected
from heat.
Ground bone appears in several pre-hispanic South American contexts related to subsistence
(Williams 1980, Holden 1991), metallurgical processes (González 1992; Tarragó and González
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1995–6) and pottery production (L. González 2000, personal communication). Nevertheless,
the context in site CC1 so far has not yielded any evidence of metallurgical activity. However,
this fact should not invalidate the possibility of transportation of bone powder to nearby sites
where such activity might have been carried out, as it has occurred in several places within the
Sierras Pampeanas area in northwestern Argentina. On the other hand, since dietary clues are
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not available, it is not possible to confirm or reject the ingestion of ground bone as a food
complement.
At Cueva de los Corrales, at least four mortars have been found with residues of black
pigment mixtures made of a clayish base coloured with manganese and ferrous oxides, com-
parable with the coatings of several ceramic fragments at the site. This would indicate the in
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situ carrying out of some of the stages of pottery making (Babot and Apella 2001), but until
now there has been no strong evidence to link ground bone with such kinds of activities.
According to our results, prior to milling, maize kernels were imperfectly peeled and winnowed
to partially eliminate bran remnants. This was confirmed by the scarce bran silica phytoliths
identified in the millstone. Peeling must have been carried out in a grinding tool different from
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the one studied. Then, the peeled kernels were ground to fine flour in the millstone at site CC1,
a fact shown by the fragmentary state of several starch grains. In several places in northwestern
Argentina, grinding takes place in a similar way and two different grinding tools are used, a
mortar to peel the grains and a millstone—called a conana or pecana—to mill them (Babot
1999a).
Due to its easy storage and high carbohydrate content in the form of starch, maize was used
in the Americas to make bread, cakes, porridge and succedaneums by baking, roasting or
boiling different flour mixtures obtained after peeling and grinding the dehydrated kernels

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 622 M. del Pilar Babot and M. C. Apella

(Babot 1999a). However, since our work only deals with the analysis of a single grinding tool
at site CC1, the final use of the maize flour identified cannot be ascertained.

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CONCLUSIONS

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Chemical residue and microbotanical remains analyses of archaeological grinding tools have
yielded reliable data about the many materials ground in the past, and direct evidence obtained
from tools has contributed to a better understanding of the grinding tasks. In this respect, we
have shown the grinding of two different resources, maize and burned bone, in the same
millstone.
This kind of evidence not only shows what natural resources were selected to be ground, but

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it also demonstrates the multiple-purpose use of grinding tools for processing both food and
non-food materials in the region. This suggests that closer scrutiny of the functional inferences
from the morphological characteristics of the artefacts will be necessary, since they are only based
on comparisons with historical, ethnoarchaeological and macrobotanical data (Babot 1999b).
Misidentified tool functionality may cause inappropriate assumptions about food-processing
activities, and even about agriculture—specifically maize agriculture—although other aspects
of prehistoric life could have been involved. D
We suggest that multiple and complementary analytical tests are indispensable to achieve
reliable data on the function of archaeological tools to obtain a better understanding of the
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diversity of roles and purposes of grinding technology in the past. Furthermore, we think that
the analyses that we have applied to a single millstone can profitably be used, even on a broader
scale than to grinding tools, to understand fully food and non-food production processes through
the examination of the different tools used. The main limitation to this approach is the fact that
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residue analysis is not possible in all cases, due to the scarcity of archaeological samples and
their inadequate degree of preservation.
Finally, we think that further contextual analysis is needed when the actual function of tools
is unknown. As far as our own study is concerned, the research at site CC1 is just beginning
and, to achieve a better understanding of the actual purpose for which maize and bone were
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ground, analyses of bone and ceramic assemblages, hearts and maize macroremains will be
necessary.

ACKNOWLEDGEMENTS
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This work was supported in part by research projects of Consejo de Investigaciones de la

Universidad Nacional de Tucumán (CIUNT) and by Consejo Nacional de Investigaciones
Científicas y Técnicas (CONICET) directed by C. Aschero. We would like to thank archaeo-
logists J. Martínez, N. Oliszewski and M. Caria for giving us free access to the materials at
the Cueva de los Corrales site. We are also very grateful for the technical assistance provided
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by the staff of the UAQ, CAC, CNEA. M.P.B. is grateful to CONICET and CIUNT for her
fellowships. M.C.A. is a member of the Research Career of CONICET.

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ARCH4C08 624 9/17/02, 9:26 AM