Archaeometry 51, 1 (2009) 125

doi: 10.1111/j.1475-4754.2008.00386.x

A. Seelenfreund the Vitreous Publishing Ltd ORIGINAL XXX University 0003-813X ARTICLES Archaeometry ARCH rocks in et al. 2008 Oxford, UK of Oxford, Atacama region, northern Chile Blackwell

GEOCHEMICAL ANALYSIS OF VITREOUS ROCKS EXPLOITED DURING THE FORMATIVE PERIOD IN THE ATACAMA REGION, NORTHERN CHILE*
A. SEELENFREUND
Escuela de Antropologa, Universidad Academia de Humanismo Cristiano, Condell 343, Providencia, Santiago de Chile

E. FONSECA and F. LLONA

Servicio Nacional de Geologa y Minera, Santiago de Chile

L. LERA
Unidad de Estadstica, Instituto de Nutricin y Tecnologa de Alimentos, Universidad de Chile, Santiago de Chile

C. SINCLAIRE
Museo Chileno de Arte Precolombino, Santiago de Chile

and C. REES
Santiago de Chile

Petrographic analysis and geochemical characterization studies were carried out on vitreous dacite and/or rhyodacite artefacts from Formative period archaeological sites in the upper Salado River Basin in the Atacama Desert, northern Chile. These were compared with samples taken from two source areas located within the subregion, named Linzor and Paniri. Source samples and archaeological specimens were analysed by inductively coupled plasma mass spectrometry (ICPMS) combined with optical emission plasma mass spectrometry (ICPOES) and atomic absorption spectroscopy (AAS). Results from the limited number of samples analysed indicate that the Linzor source seems to have been the primary source exploited during the Early and Late Formative periods in the Salado River Basin.
KEYWORDS: VITREOUS DACITE SOURCES, INDUCTIVELY COUPLED PLASMA MASS SPECTROMETRY, OPTICAL EMISSION PLASMA MASS SPECTROMETRY, ATOMIC ABSORPTION SPECTROSCOPY, FORMATIVE PERIOD, ATACAMA ARCHAEOLOGY, NORTHERN CHILE
8 University March 2007; accepted 30 September 2007 *Received 2 of Oxford, 2008

INTRODUCTION

Source provenance analysis of lithic artefacts has become increasingly abundant in South American archaeology for the elucidation of patterns of exchange and technological organization, among other issues. Most of these studies have been centred on the analysis of obsidian,
*Received 2 March 2007; accepted 30 September 2007 Corresponding author: email aseelenfreund@academia.cl University of Oxford, 2008

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using several instrumental techniques, primarily instrumental neutron activation analysis (INAA) (Braswell and Glascock 1998; Glascock et al. 1998; Burger and Glascock 2000; Yacobaccio et al. 2004), to a limited extent proton-induced X-ray emission (PIXE) (Seelenfreund et al. 1996; Bellot-Gurlet et al. 2005), energy-dispersive X-ray uorescence (EDXRF) and wavelengthdispersive X-ray uorescence (WXRF) (Shackley 1998; Ponomarenko 2004). A few studies have employed other methods (Pereira et al. 2001; Vsquez et al. 2001). By comparison with obsidian, other types of lithic material are far less well studied, not only in the Andean region but also elsewhere. Even in areas where obsidian is rare, analyses of other toolstone groups are seldom undertaken, and this is particularly the case for vitreous dacites or andesites. In the Americas, general studies on andesite artefacts are few, and have been carried out by Latham et al. (1992), Bostwick and Burton (1993) and Jones et al. (1997). The only such study that we are aware of centres on the provenance of andesite building blocks during the Inca Empire (Ogburn 2004). That such studies have not been conducted in South American archaeology primarily relates to the fact that equipment is expensive and not often available to the researchers. In this paper, we describe provenance analyses conducted over the past three years on vitreous dacite or rhyodacite, aimed at pinpointing the location of the sources of this rock, which was exploited during the Early and Late Formative periods in the Atacama region in northern Chile, particularly in the subregion of the Salado River (Fig. 1). Since sourcing studies in the Andes have mainly been applied to obsidian, we so far have little basis for evaluating other materials and for addressing questions such as regional versus interregional exchange networks, the importance of local versus non-local resources and topics relating to the acquisition of raw materials. The present research focuses on the potential of inductively coupled mass spectrometry (ICPMS) to effectively distinguish between the geological sources of these vitreous rocks and to ascertain the geological source of origin of archaeological artefacts, in order to assess Rees and De Souzas (2004) argument relating to the use of local versus non-local raw materials in the study area. On the basis of quantitative analyses of lithic debitage assemblages and the visual characteristics of the rocks, the above authors proposed that during the Early Formative period of the local chronology of the Salado River subregion (1400 bc ad 100) (sensu Sinclaire 2004), lithic resources were exploited from local and distantly located sources. The local sources, mainly basalts, andesites and quartz, were used for the manufacture of dart points and cutting and scraping tools. These resources are considered local since the raw materials can be found abundantly in local river beds and gullies. The authors dened the local resources on the basis of the presence/absence of the lithic tool manufacturing remains that represent the different stages of the reduction sequence of lithic production. According to Rees and De Souza (2004), the degree of segmentation of the chane opratoire determines whether a rock is considered local or non-local. In this sense, geographical distance is not the relevant factor. For a rock to be classied as local, the complete reduction sequence ought to be present at the sites or in the immediate surroundings. A non-local rock will be used in a different manner: the reduction sequence is only partially represented at the sites and will vary according to the distance to the source of origin. Therefore at the sites closer to the source, bifaces and preforms will be present; while at more distant sites the rock is represented by a few small occasional akes. For example, in the study area, an extensive black basalt workshop is found near the conuence of the Toconce and Salado Rivers, very close to the Alero Toconce site, which was sampled for the present study. Tools manufactured with the local raw materials, according to Rees and De Souza (2004, 549), show consistently less time and labour investment.
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Figure 1 The study area. AC, Vitreous rock sources: A, Linzor source; B, Paniri lower source; C, Paniri upper source. 110, Archaeological sites: 1, Punta Tetragonal; 2, Alero Derrumbado; 3, Alero Toconce; 4, Marilyn Manson; 5, Conuencia; 6, Los Morros 3; 7, El Otro Sitio; 8, Doa Marta; 9, La Mrula; 10, Incahuasi Aldea.

There are three types of non-local raw materials used for the production of stone tools: obsidian, with the nearest known sources over 60 km from the Salado River area; siliceous sedimentary rocks, where the closest documented source area is approximately 40 km away; and vitreous dacite, the sources of which are unknown (Rees and De Souza 2004). The tools manufactured with the vitreous rock, which the authors refer to as vitreous basalt, correspond to almost 11% of the raw materials used during the Early Formative period, most of them being large bifacial tools and dart points (De Souza 2004).
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Rees and De Souza (2004, 463) argue that during the Late Formative period (ad 100900) vitreous basalt or dacite represented less than 2% of lithic materials, and the size of both nished tools and debitage decreased. They believe that in general the acquisition of foreign lithic raw materials during this time mirrors the behaviour of other culture materials, suggesting close ties between the Atacama region and the high puna (altiplano), as has been observed by others (Castro et al. 1994; Dillehay and Nez 1988; Nez 1994). Preliminary petrographic analysis on the above vitreous rocks indicated that we were dealing with vitreous dacite or rhyodacites (Seelenfreund et al. 2004). At the beginning of our study, only one possible source of this raw material was known (Seelenfreund et al. 2004), the Linzor source, which showed clear evidence of having been used by prehistoric occupants, based on occurrences of quarrying debris. In that initial study we performed preliminary characterization analysis, using PIXE in combination with energy-dispersive X-ray uorescence (EDXRF), on a few archaeological samples and one sample from the source. We concluded that some of the archaeological samples analysed could have come from this source, but clearly some did not (cf., Seelenfreund et al. 2004). We therefore needed to initiate an extensive survey for alternative sources of vitreous rock exploited during the Formative period. For each new source found, we needed to dene the type of rock and its geochemical ngerprint. We could then investigate which of the sources were represented in the archaeological record and in what manner. Since very little research has been done anywhere in the world on the characterization of non-obsidian archaeological vitreous stone materials (see, e.g., Newman and Nielsen 1987), we therefore chose to use ICPMS combined with inductively coupled optical emission spectrometry (ICPOES) and atomic absorption spectrometry (AAS) for its high sensitivity, and since the use of these combined methods allows for the detection of a larger number of elements, including the rare earth elements, which have often been shown to be crucial for group discrimination (Franco and Aragn 2004). In order to locate potential vitreous dacite sources, geological maps for the region were analysed. On the basis of the cartographic analysis, certain localities were then explored in the eld. Only some of these surveys gave positive results, especially when looking for vitreous dacite outcrops. The only two further potential sources were both located on the slopes of the Paniri volcano in the Salado River Basin. In the present paper, we are therefore reporting the results for these two new sources in addition to the analyses performed on rock samples from Linzor, the source already reported previously (Seelenfreund et al. 2004).
THE STUDY AREA

The foothills of the Salado River in the north of Chile are the entrance way to the southern altiplano, or high Andean plateau. An extensive volcanic slope descends from the high mountains of the altiplano at 4000 m above sea level down to the pampas of the Atacama Desert. Several small rivers, located between 3000 and 4000 m altitude, ow along deep tectonic gullies feeding the Salado River Basin, which is the main tributary of the Loa River. Along the middle section of these gullies, between 3200 and 3000 m altitude, we nd a wetland environment (the vega de Turi), which continues to the represent the most important area for human settlement (see Fig. 1). Above 4000 m is the high puna, with extensive tussocky grasslands, while the area below 3000 m is characterized by the dry plains and hills of the Atacama Desert, with a sprinkling of oases along the Loa River, like Chiu Chiu village or the city of Calama.
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Since around 10 000 bc, huntergatherer communities have exploited the abundant resources of this environment. From 1400 bc up to ad 900, these communities of huntergatherers slowly began to develop camelid herding and a pastoralist economy, supplemented with the cultivation of a few crops, giving rise to the Formative period. This period was characterized by sedentary villages, domestication of llamas, technological innovations such as pottery, textiles and metalworking, and a diversication of economic networks, marking the beginning of more complex social structures (cf., Sinclaire 2004). The geological sources The Linzor source is a small distinctive outcrop located on the slope of the Toconce volcano at 4300 m altitude. It shows extensive quarrying and mainly primary reduction at the quarry in order to obtain standardized bifacial preforms or tool blanks. There is little evidence of secondary reduction of the preforms (Baeza 2008). Two separate areas or ows can be distinguished, separated by a small ravine. Samples were taken at several points along the ows and outcrop, in order to control for intra-source chemical variability (see Fig. 1, source A). The Paniri source was rst identied from a working oor located on the lower slopes on the southern side of the volcano. The source of the raw material seemed to come from a higher altitude along the volcanic slopes. However, during a subsequent survey we found that the raw material appeared in the form of small st-sized nodules dispersed on the lower slopes of the volcano, in and around the modern Paniri village. Samples were taken from several nodules from this area, which we designated as the Paniri lower source (see Fig. 1, source B). At 4700 m altitude on the eastern slope of the Paniri volcano, the raw material appears in the form of small boulders (of about 5080 cm in diameter) on a shoulder of the volcanic slope. Some primary reduction work can be observed around the boulders, but it seems that most of the later reduction was performed at somewhat lower altitudes. Samples for analysis were taken here from several different boulders. This sampling location was designated as the Paniri upper source (see Fig. 1, source C). Individual sample locations from each source are shown in Table 1. Geologically, these vitreous rock sources are associated with the late Pleistocene or Quaternary volcanism of the Central Puna Altiplano Volcanic Complex, located on the Chilean/Bolivian border of the Central Andean Cordillera volcanism (De Silva et al. 1994). In our study area this volcanic complex is represented, for example, by the Toconce and Paniri volcanoes, among others. The archaeological samples The comparative archaeological samples were selected from 10 different sites located in the vicinity of the vega de Turi or along the gullies of the upper course of the Salado River Basin. The samples are mainly, but not exclusively, from Early Formative period contexts; that is, dated between 1400 bc and ad 100. The samples analysed are presented in Table 2. A total of 30 samples from nine archaeological contexts dated to the Formative period were chosen for analysis. The samples were chosen following two criteria, rst to cover all locations of the study area, and second to span the chronological range of the Formative period; that is, both the Early and Late Formative. However, as can be seen in Table 2, we included an additional four samples that are ascribed to the Late Archaic period (10 0001400 bc), due to stratigraphy or associated typological cultural material (sensu De Souza 2003).
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Table 1 The source samples analysed

UTM datum (SAM 56) Provenance Sample code General sampling location and altitude East Linzor Linzor Linzor Linzor Linzor Linzor Linzor Linzor Linzor Linzor Paniri lower Paniri lower Paniri lower Paniri lower Paniri lower Paniri lower Paniri lower Paniri upper Paniri upper Paniri upper Paniri upper Z04 Z05 Z06 Z07 Z08 Z09 Z10 Z11 Z44 Z45 Z27 Z46 Z47 Z48 Z49 Z50 Z51 Z40 Z41 Z42 Z43 Outcrop on slope of the Toconce volcano, 4248 m Outcrop on slope of the Toconce volcano, 4248 m Outcrop on slope of the Toconce volcano, 4248 m Outcrop on slope of the Toconce volcano, 4248 m Outcrop on slope of the Toconce volcano, 4248 m Outcrop on slope of the Toconce volcano, 4248 m Outcrop on slope of the Toconce volcano, 4248 m Outcrop on slope of the Toconce volcano, 4248 m Outcrop on slope of the Toconce volcano, 4248 m Outcrop on slope of the Toconce volcano, 4248 m Lower slope of the Paniri volcano, 3300 m a.s.l. Lower slope of the Paniri volcano, 3297 m a.s.l. Lower slope of the Paniri volcano, 3297 m a.s.l. Lower slope of the Paniri volcano, 3297 m a.s.l. Lower slope of the Paniri volcano, 3297 m a.s.l. Lower slope of the Paniri volcano, 3297 m a.s.l. Lower slope of the Paniri volcano, 3297 m a.s.l. Upper slope of the Paniri volcano, 4700 m a.s.l. Upper slope of the Paniri volcano, 4700 m a.s.l. Upper slope of the Paniri volcano, 4700 m a.s.l. Upper slope of the Paniri volcano, 4700 m a.s.l. a.s.l. a.s.l. a.s.l. a.s.l. a.s.l. a.s.l. a.s.l. a.s.l. a.s.l. a.s.l. 599002 599128 598897 598897 599165 599172 598897 599134 599165 599165 575531 575531 575531 575531 575863 575863 575863 582878 582878 582878 582878 North 7542816 7543077 7543081 7543081 7543010 7543011 7543081 7543070 7543010 7543010 7551302 7551302 7551302 7551302 7551603 7551603 7551603 7557149 7557149 7557149 7557149

The sites from which the samples were chosen cluster basically in four discrete areas from west to east and north to south: the Toconce River Basin, the Turi wetland (vega de Turi), the lower course of the Caspana River and the upper Incahuasi River Basin. The Punta Tetragonal and Alero Derrumbado sites are both located close to the source of the Toconce River and in the vicinity of the Linzor source. The rst of these sites lies about 5 km east of the source, on the Toconce River bank on the southern edge of the Inacaliri wetland. It is an open site with a few round stone structures and abundant aking debris. Raw materials include rhyodacite and basalt. Pottery is of the Los Morros type, typical of the Early Formative (Sinclaire 2004). The Alero Derrumbado site is a rockshelter located about 1 km south of the Linzor quarry. It is located at a somewhat lower altitude just across the conuence of the Toconce River, with a gully that comes from the Linzor quarry area. The shelter is formed under a calcareous cornice. On the hill slope below the rockshelter are abundant vitreous dacite aking debitage, akes and bifaces characteristic of the Archaic. The Alero Toconce site is another rockshelter, with deep and dense stratigraphic deposits dating from the Middle Archaic (c. 6000 bc) to the Late Intermediate period (ad 1470) (Aldunate et al. 1986; De Souza 2003). It is located on the Salado River, just at the conuence with the Toconce River. Lithic cultural materials are dominated by black basalt tools. This basalt is available in the local river beds. The vitreous dacite is the second most popular rock type for the manufacture of tools during the early occupational history of the site. The samples analysed from this site are from Mid-Archaic and Early Formative contexts. About 100 m north of the Toconce rockshelter is a lithic workshop. This site (Marilyn Manson) boasts a
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Table 2

The archaeological samples analysed

Archaeological provenance Site name Sample number Site code Alero Derrumbado Alero Derrumbado Alero Derrumbado Alero Toconce Alero Toconce Alero Toconce Alero Toconce Conuencia Conuencia Doa Marta El Otro Sitio El Otro Sitio El Otro Sitio El Otro Sitio El Otro Sitio El Otro Sitio Incahuasi Aldea Incahuasi Aldea Incahuasi Aldea La Mrula Los Morros 3 Los Morros 3 Los Morros 3 Los Morros 3 Los Morros 3 Los Morros 3 Los Morros 3 Los Morros 3 Los Morros 3 Los Morros 3 Los Morros 3 Los Morros 3 Marilyn Manson Punta Tetragonal A62 A63 A64 A51 A52 A53 A54 A46 A61 A44 A55 A56 A57 A58 A59 A60 A45 A66 A67 A42 A40 A41 A47 A48 A50 A68 A69 A70 A71 A72 A73 A74 A43 A65 02Lz02 02Lz02 02Lz02 02To21 02To21 02To21 02To21 02Loa15 02Loa15 02Loa61 02Tu04 02Tu04 02Tu04 02Tu04 02Tu04 02Tu04 02CasInc63 02Cas Inc 63 02Cas Inc 63 02CasCas53b 02 Tu 07 02 Tu 07 02 Tu 07 02 Tu 07 02 Tu 07 02 Tu 07 02 Tu 07 02 Tu 07 02 Tu 07 02 Tu 07 02 Tu 07 02 Tu 07 02To22 02Lz01 Excavation unit Surface rec. Surface rec. Surface rec. Area M Area M Area M Area M Cuad B Cuad B Cuad B Unit A13 Unit AD16 Unit AD17 Cuadr 2 Cuadr 2 Unit BI4 Structure 2, spit 1 Structure 2, cuadr 2 Structure 2, unit R-B, spit 1 Cuadr 2E Structure 3, cuadr B2 Structure 3, cuadr B2 Structure 3, cuadr B1 Structure 3, cuadr B1 Structure rec. Structure 3, cuadr B2 Structure 3, cuadr B1 Structure 3, cuadr B2 Outside structure 3 Structure 3, cuadr A2 Structure 3, cuadr A2 Structure 3, cuadr A2 Cuadr A Surface rec. Level Surface Surface Surface Level E4 Level F5 Level F5 Level F5 + F6a Level 2 Level 6 Level 3 Surface Surface Surface Level 2 Level 1 Surface Level 2 Level 1 Level 2 Hearth Level 1 Level 1 Level 2 Level 2 Surface Level 1 Level 2 Level 1 Surface Level 1 Level 1 Level 2 Level 0 Surface Archaic Archaic Archaic Early Formative Early Formative Early Formative Archaic Late Formative Late Formative Late Formative Early Formative Early Formative Early Formative Early Formative Early Formative Early Formative Late Formative Late Formative Late Formative Early Formative Early Formative Early Formative Early Formative Early Formative Early Formative Early Formative Early Formative Early Formative Early Formative Early Formative Early Formative Early Formative Early Formative Early Formative Linzor Linzor Linzor Linzor Linzor Linzor Paniri upper Linzor Paniri upper Linzor Paniri lower Paniri lower Paniri lower Paniri lower Paniri lower Paniri lower Linzor NN1 Linzor Linzor NN2 or Paniri upper NN2 or Paniri upper Paniri lower Paniri lower Paniri lower Linzor Linzor Paniri lower Linzor Paniri lower Linzor NN2 or Paniri upper NN3 or Linzor Linzor Cultural period Source

Vitreous rocks in the Atacama region, northern Chile

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platform made of stones and soil, built against the same rock formation that hosts the Alero Toconce site. Both of these sites are located approximately 20 km to the south-west of the Linzor quarry and about 20 km south from the Paniri volcano. Three further sites are located in or around the vega de Turi. The Conuencia site is located on the southeastern periphery of this wetland environment and near the conuence of the Caspana and Salado Rivers. This is an open habitation site, primarily occupied since the Early Formative and up to the Late Intermediate periods. The rock walls of both the Salado and the Caspana Rivers in this area are covered in a profusion of rock art of all styles, techniques and dates (Gallardo et al. 1999). In addition, during the Formative period, the Conuencia site played an important role in a network of malachite bead production and exchange (Rees 1999). At this site, vitreous dacite represents less than 1% of the total lithic debitage. The site is located approximately 25 km to the south-west of Linzor and 15 km south of Paniri. The Los Morros 3 site, dated to the Early Formative, is located on the southern edge of the vega de Turi. It is an open habitation site with circular stone structures, and where its population exploited the rich wetland resources. Stone tool manufacture was another important activity at the site; large numbers of bifacial tool blanks and preforms are found at the site. Vitreous dacite is by far the most abundant rock used for tool manufacture, representing about 40% of all aking debitage. At this site we also have the highest frequency of use of this material for the whole region, as either debitage or nished tools. The Los Morros 3 site is about 25 km south-west of the Linzor source and about 15 km south of the Paniri lower source. Lastly, one further site is located at the western edge of the vega de Turi. This is the El Otro Sitio site, which corresponds to an open settlement site with sand-covered possible housing structures; it was occupied both during the Early Formative and Late Intermediate periods. At this site, surface lithic remains comprise an ample assortment of raw materials, in which vitreous dacite is the most popular for aking and tool manufacture, with relative frequencies similar to those of the Los Morros 3 site. The site is about 30 km to the west of the Linzor source and about 15 km distant from Paniri. On the lower course of the Caspana River we sampled two sites: Doa Marta and La Mrula. The rst site, located about 20 km south-west of the Linzor source and about 25 km from the Paniri volcano, comprises a number of circular habitation structures built against a rock wall and is associated with rock art. It is dated to the Late Formative period. Vitreous dacite represents about 7% of all lithics of the site. The La Mrula site is a small open settlement site, dated to the Early Formative, with circular adjacent stone structures. Vitreous dacite represents close to 2% of the lithic remains; it is also located about 20 km from Linzor and around 30 km from Paniri. Finally, on the extreme southern edge of our study area and near the head of the Incahuasi River Basin is the Incahuasi Aldea site. This site comprises a group of at least 50 different adjoining circular and oval house structures dated to both the Early and Late Formative periods: vitreous dacite represents 15% of the lithic debitage found at the site. The Incahuasi Aldea site is the furthest site from the Linzor and Paniri sourcesabout 30 km to the south-west of Linzor and 40 km south of Paniri. The samples analysed are from Late Formative contexts.
ANALYTICAL PROCEDURES

All samples analysed were examined in petrographic thin sections (see Figs 25). These thin sections were ground to 0.08 mm, thicker than normal, so that they could be used later for comparative non-destructive geochemical analysis with proton-induced X-ray emission (PIXE)
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Figure 2 Thin sections of two varieties of dacite rock (samples A45 and A40). (A) Rock containing plagioclase, biotite and amphibole and very few pyroxene phenocrysts: the spaces between the crystals are taken up by glass and tiny plagioclase microliths. (B) Rock containing plagioclase and biotite phenocrysts: the proportions of both minerals are very variable.

Figure 3 Vitreous dacite characterized by 2030% of short tabular and occasional long plagioclase crystals, generally fresh, with 10% of prismatic short or long biotite crystals, in a very fresh glass matrix, with a few plagioclase and/or biotite microlites. Opaque minerals are present at the 0.5% level. Both samples are from the Linzor source.

and energy-dispersive X-ray uorescence (EDXRF), which is part of a separate study (Morales et al. 2007). Part or all of the remnant rock of each sample was then used for further chemical analysis. Samples were pulverized and homogenized before grinding to mesh 200 in an agate mill. A solution of 50 ml in 10% nitric acid was prepared with 0.26 g of the powdered sample, and dissolved at 800C by alkaline fusion in a platinum crucible. ICPMS analysis was performed on all samples. For the procedure, pure water (18.22 M) was used to increase 5 ml of the previous solution to 25 ml. The equipment used for analysis was an Agilent model 7500a, calibrated using eight multi-elemental solutions, traceable to NIST patterns, with a linear response. Indium and rhenium were used as internal standards to correct for possible sensibility or matrix effects of the instrument. Instrumental parameters were adjusted according to factory specications. After calibration, samples were analysed routinely and the software (ChemStation-1834B) incorporated in the equipment calculated the element concentrations.
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Figure 4 Vitreous dacite. These samples are characterized by the presence of plagioclase phenocrystals of oligoclase composition. Some small pyroxene phenocrystals can be observed clustered as glomerocrystals. The matrix is glassy, with small plagioclase needles. Fine magnetite disseminations can be observed. The samples are from the Paniri upper source.

Figure 5 Thin sections of a dacite rock from the Paniri lower source (sample Z27). The dacite is formed by multiple plagioclase phenocrystals of varied sizes, generally short and tabular. There are also biotite phenocrystals, all in a glass matrix. (Left image, crossed nichols; right image, parallel nichols).

Thirty elements were analysed using this method (Sc, V, Cr, Co, Cu, Sr, Y, Zr, Nb, Cs, Ba, La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, Hf, Ta, Pb, Th and U). Additionally, ICPOES was performed using Jobin Yvon Model 70+ equipment. The analysis was performed in its sequential mode. The previously prepared solution was not further diluted for analyses. The equipment was calibrated using ve multi-elemental solutions, traceable to NIST patterns, within its linear response. Instrumental parameters were adjusted according to standard parameters for this equipment. After calibration, samples were analysed routinely and element concentrations were calculated by the software incorporated in the equipment (Jobin Yvon Version 4.01). The major elements expressed as oxides identied by this technique were as follows: SiO2, Al2O3, Fe2O3, CaO, TiO, MgO, K2O, MnO and P2O5. Further analysis was performed using AAS. For this, the equipment used was a Perkin Elmer Model 7000 analyst in its ame spectrophotometer mode. The equipment was calibrated using four mono-elemental solutions, traceable to NIST patterns, with concentrations in the linear range of the instrument. Whenever sample concentrations fell outside the instrument range,
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11

the solution was diluted. Instrumental parameters were adjusted according to standard parameters for this equipment. The elements identied by this method were Ni, Zn and Rb. Statistical methods The archaeological samples were analysed by standard multivariate statistical methods, such as principal component analysis (PCA), cluster analysis and discriminate analysis. The results were obtained using the Stata 9.1 package (Stata Corporation, College Station, Texas, 2005).
RESULTS

Petrographic thin sections performed on the source as well as on archaeological samples indicated that we were dealing with three different types of rocks, classed as andesite, dacite and rhyodacite. The petrographic characteristics of these rocks are as follows. Vitreous dacite is present in three distinct varieties. Variety 1 is characterized by 2030% of short tabular and occasional long plagioclase crystals, generally fresh, with 10% of prismatic short or long biotite crystals, in a very fresh glass matrix, with a few plagioclase and/or biotite microlites. There are some (0.5%) opaque minerals present. Some samples have a few pyroxene xenocrystals. The ow texture can be clearly identied. This rock is found at the Linzor source. Variety 2 is represented by a few samplesall from archaeological contextsthat show the presence of short tabular plagioclase crystals of oligoclaseandesine composition, somewhat less acid than the previous group. The ferromagnesian crystals are biotite, amphibole and pyroxenes. According to PCA analysis, samples A40 and A41, from the Los Morros 3 site, belong to an unknown source, and sample A45, from the Incahuasi Aldea, is ascribed to the Linzor source. Variety 3 is a dacite formed by multiple plagioclase phenocrystals of varied sizes, generally short and tabular. There are also biotite phenocrystals, all in a glass matrix (sample Z27 from the Paniri lower slopes). With regard to rhyodacite, these samples are characterized by the presence of plagioclase phenocrystals of oligoclase composition. Some small pyroxene phenocrystals can be observed, clustered as glomerocrystals. The matrix is glassy with small plagioclase needles. Fine magnetite disseminations can be observed (samples Z40Z43 from the Paniri upper slopes). One sample, A43, although petrographically classed as glassy andesite due to its high silica content, falls within the dacite group. In thin section it shows a few plagioclase and pyroxene crystals in a glass matrix, with ne needle-like plagioclase microlites and some chlorite. This sample in the cluster analysis was assigned to the Linzor group, but with PCA analysis it falls outside both the Linzor and Paniri sources, although it is closer to the Paniri source group (see Figs 6 and 7). Source adscription of this sample is therefore tentative. The chemical composition of the samples The analysis allowed for identication of 33 elements (Sc, V, Cr, Co, Ni, Cu, Zn, Rb, Sr, Y, Zr, Nb, Cs, Ba, La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, Hf, Ta, Pb, Th and U) and nine major elements found as oxides (SiO2, Al2O3, Fe2O3, CaO, TiO, MgO, K2O, MnO and P2O5). The petrological classication of the rocks using a Peccerillo and Taylor (1976) diagram groups most of the samples as dacite or rhyolite (Fig. 8). Two samples from the Linzor quarry
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A. Seelenfreund et al.

Figure 6 The principal component analysis for all source and archaeological samples. The elements and compounds used are K2O, CaO, TiO2, MnO, Fe2O3, Rb, Sr, Y, Zr, Ba, La, Ce and Nd.

Figure 7 A cluster analysis using average linkage for all source and archaeological samples. The elements and compounds used for the cluster analysis are TiO, MnO, Sc, Fe2O3, Cu, Zr, Rb, Zr, Dy, Y, Ba, La, Ce and Nd.
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Vitreous rocks in the Atacama region, northern Chile

13

Figure 8 The chemical composition, according to Pearce et al. (1977), for both archaeological and source samples. Samples Z74, Z10 and Z11 fall in the range of high-K andesite rock. All others can be classed as vitreous dacite or rhyodacite.

clearly fall outside this range due to their lower SiO2 contents, and some of the archaeological samples fall also outside the range due to their lower K2O contents. However, since K2O is a fairly mobile element, this does not change the major classication of the rock. Hence, in the present paper, when referring in a general way to the vitreous dacites, rhyolites or andesites, we will indistinctly use the term vitreous dacite for all samples. Concentrations were calculated to parts per million (ppm). The Paniri upper source, due to the higher iron (Fe) contents inside the pyroxene crystals, is well-separated from the Linzor samples, while the Paniri lower source falls somewhere in between. Comparison of the archaeological sample composition with the source samples The results of analysis of the source samples as well as of the archaeological pieces are listed in Tables 35. We analysed more than one sample from each source in order to check for internal source variability. The Linzor source is formed by two outcrops, separated by a small gully, both of which show evidence of extensive prehistoric quarrying. Samples were taken from both areas. At Paniri, at the Paniri upper source, we chose several samples from places where some evidence of prehistoric activity can be found. Samples from the Paniri lower area were taken within 1 km2 within and around the village of Paniri, located at the foot of the volcano. Principal component analysis on all source samples (Fig. 9) indicated that the Linzor source can be clearly distinguished from the Paniri source. The Paniri upper samples also cluster closely together in a single group; however, the samples from the Paniri lower source area show much more chemical variation, as indicated by samples Z27 and Z48, which do not cluster closely with the other samples, and are also distinct from samples from the Paniri
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Table 3

Concentrations of major elements for samples analysed by ICPOES. All elements expressed in per cent

Site name Alero Derrumbado Alero Derrumbado Alero Derrumbado Alero Toconce Alero Toconce Alero Toconce Alero Toconce Conuencia Conuencia Doa Marta El Otro Sitio El Otro Sitio El Otro Sitio El Otro Sitio El Otro Sitio El Otro Sitio Incahuasi Aldea Incahuasi Aldea Incahuasi Aldea La Mrula Linzor Linzor Linzor Linzor Linzor Linzor Linzor

Sample number A62 A63 A64 A51 A52 A53 A54 A46 A61 A44 A55 A56 A57 A58 A59 A60 A45 A66 A67 A42 Z04 Z05 Z06 Z07 Z08 Z09 Z10

SiO2 73.10 71.90 70.80 73.61 72.70 74.80 65.26 74.39 68.20 74.70 67.78 69.23 67.74 68.54 68.27 68.64 72.43 74.30 70.80 77.43 74.50 73.91 73.87 75.58 71.11 75.25 58.64

Al2O3 14.60 14.50 14.20 14.62 14.15 15.04 15.05 14.65 16.20 14.48 15.25 15.59 15.46 15.67 15.60 15.64 12.71 15.50 14.90 14.42 14.17 14.36 14.36 14.28 14.02 14.18 12.51

Fe2O3 1.30 1.30 1.20 1.28 1.24 1.24 3.45 1.21 3.20 1.27 2.23 2.28 2.42 2.40 2.42 2.52 1.21 0.70 1.30 1.09 1.40 1.29 1.18 1.35 1.34 1.42 0.94

CaO 1.40 1.40 1.40 1.40 1.36 1.46 3.37 1.25 3.10 1.26 2.18 2.25 2.31 2.20 2.25 2.30 0.43 0.40 1.40 1.34 1.24 1.28 1.28 1.24 1.21 1.24 0.73

TiO 0.18 0.17 0.16 0.17 0.17 0.18 0.57 0.19 0.47 0.18 0.41 0.42 0.43 0.42 0.43 0.44 0.17 0.07 0.17 0.16 0.18 0.19 0.19 0.18 0.17 0.18 0.18

MgO 4.40 4.80 4.60 4.58 5.90 6.10 5.79 3.29 3.70 1.74 6.66 5.87 5.86 5.72 5.48 4.43 8.65 4.70 6.10 4.34 4.07 3.95 3.82 4.23 3.16 3.38 3.20

K 2O 0.24 0.23 0.22 0.24 0.22 0.24 1.64 0.24 1.13 0.21 0.68 0.69 0.70 0.69 0.70 0.74 <0.2 0.11 0.23 0.22 0.23 0.23 0.24 0.23 0.22 0.22 0.16

MnO 0.07 0.07 0.07 0.07 0.07 0.07 0.05 0.07 0.05 0.08 0.03 0.03 0.03 0.03 0.03 0.03 0.07 0.17 0.07 0.07 0.08 0.08 0.08 0.08 0.07 0.08 0.06

P 2O 5 0.04 0.04 0.03 0.04 0.03 0.05 0.13 0.11 0.15 0.01 0.12 0.12 0.14 0.12 0.13 0.13 0.02 0.18 0.04 0.06 0.11 0.09 0.05 0.08 0.02 0.09 0.02

A. Seelenfreund et al.

Site name Linzor Linzor Linzor Los Morros 3 Los Morros 3 Los Morros 3 Los Morros 3 Los Morros 3 Los Morros 3 Los Morros 3 Los Morros 3 Los Morros 3 Los Morros 3 Los Morros 3 Los Morros 3 Marilyn Manson Paniri lower Paniri lower Paniri lower Paniri lower Paniri lower Paniri lower Paniri lower Paniri upper Paniri upper Paniri upper Paniri upper Punta Tetragonal

Sample number Z11 Z44 Z45 A40 A41 A47 A48 A68 A69 A70 A71 A72 A73 A74 A50 A43 Z27 Z46 Z47 Z48 Z49 Z50 Z51 Z40 Z41 Z42 Z43 A65

SiO2 59.92 71.90 74.47 67.75 72.22 72.02 70.46 71.50 74.40 69.30 73.00 69.60 71.50 60.50 70.99 72.01 68.31 69.97 69.40 68.34 69.76 69.59 69.78 70.38 70.88 66.77 67.80 72.20

Al2O3 13.19 12.24 12.85 13.58 15.11 15.35 15.52 14.20 15.20 15.70 14.80 15.70 14.60 16.40 15.82 16.07 13.03 0.41 0.43 0.43 0.41 0.42 0.41 14.47 13.30 13.60 13.07 14.40

Fe2O3 0.99 1.50 1.26 2.23 2.18 2.26 2.31 1.20 1.40 2.30 1.30 2.30 1.20 5.30 2.21 3.01 2.29 0.96 0.92 1.06 0.84 0.77 0.69 3.20 2.48 2.92 2.77 1.20

CaO 1.21 1.24 1.27 1.92 1.97 2.16 2.33 1.40 1.50 2.20 1.40 2.20 1.40 5.40 2.29 2.61 1.93 2.24 2.25 2.95 2.20 2.24 2.24 2.91 2.33 2.62 2.43 1.40

TiO 0.15 0.16 0.16 0.38 0.41 0.47 0.44 0.18 0.20 0.41 0.25 0.41 0.22 0.73 0.42 0.48 0.34 15.17 15.13 15.44 15.11 15.12 15.26 0.44 0.34 0.42 0.38 0.17

MgO 3.08 3.45 3.25 3.92 3.55 5.87 6.75 4.80 3.90 4.50 3.70 5.70 3.20 2.20 6.59 4.34 3.93 4.56 4.47 3.67 4.58 4.48 4.55 3.57 3.93 3.52 3.21 3.80

K 2O 0.22 0.24 0.25 0.45 0.62 0.68 0.69 0.23 0.24 0.68 0.24 0.66 0.22 3.30 0.69 0.82 0.69 0.71 0.71 1.03 0.68 0.70 0.74 1.18 0.95 1.05 1.02 0.24

MnO 0.06 0.06 0.06 0.03 0.03 0.03 0.03 0.07 0.07 0.03 0.07 0.03 0.07 0.08 0.03 0.06 0.03 0.03 0.03 0.06 0.03 0.03 0.04 0.05 0.04 0.04 0.04 0.07

P 2O 5 0.03 0.03 0.03 0.57 0.41 0.11 0.13 0.04 0.04 0.12 0.03 0.13 0.04 0.13 0.12 0.48 0.09 0.14 0.14 0.14 0.13 0.14 0.14 0.14 0.10 0.12 0.11 0.04

Vitreous rocks in the Atacama region, northern Chile

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Table 4

Concentrations of trace elements for samples analysed by ICPMS (V to Pr). All elements expressed in ppm

Site name Alero Derrumbado Alero Derrumbado Alero Derrumbado Alero Toconce Alero Toconce Alero Toconce Alero Toconce Conuencia Conuencia Doa Marta El Otro Sitio El Otro Sitio El Otro Sitio El Otro Sitio El Otro Sitio El Otro Sitio Incahuasi Aldea Incahuasi Aldea Incahuasi Aldea La Mrula Linzor Linzor Linzor Linzor Linzor Linzor Linzor

Sample number A62 A63 A64 A51 A52 A53 A54 A46 A61 A44 A55 A56 A57 A58 A59 A60 A45 A66 A67 A42 Z04 Z05 Z06 Z07 Z08 Z09 Z10

V 7.00 7.00 7.00 7.00 7.00 7.00 74.00 4.58 57.00 4.23 39.00 46.00 49.00 46.00 47.00 50.00 3.00 6.00 8.00 5.23 4.71 4.86 4.66 4.33 5.82 6.65 4.52

Cr <5 <5 <5 <5 <5 <5 27.00 3.00 43.00 3.00 9.00 14.00 127.00 13.00 13.00 108.00 3.00 <5 <5 3.00 73.58 80.21 83.92 60.18 9.71 9.48 72.50

Zr 134.00 142.00 133.00 137.00 149.00 138.00 213.00 104.75 193.00 108.41 205.00 220.00 221.00 214.00 216.00 219.00 95.56 43.00 137.00 108.03 104.59 105.95 103.79 101.24 175.00 142.00 102.47

Sr 206.00 209.00 204.00 212.00 215.00 219.00 304.00 145.99 341.00 149.79 358.00 350.00 375.00 336.00 367.00 380.00 92.73 26.00 209.00 151.54 148.01 148.47 144.43 144.61 115.00 203.00 145.42

Ba 979.00 969.00 954.00 970.00 976.00 1010.00 773.00 803.02 718.00 818.62 751.00 760.00 778.00 760.00 773.00 766.00 799.08 81.00 1010.00 805.46 803.17 811.43 783.52 796.57 759.00 962.00 794.27

Rb 141.00 141.00 135.00 140.00 142.00 145.00 188.00 116.75 141.00 110.23 223.00 230.00 219.00 229.00 218.00 221.00 111.89 265.00 142.00 120.54 115.44 116.51 113.15 113.83 159.00 157.00 113.97

Y 21.30 21.40 21.40 21.35 20.39 21.58 23.93 14.53 18.50 14.24 9.62 10.11 9.72 9.86 10.04 9.70 12.65 17.00 21.30 15.24 14.57 14.71 14.20 14.27 21.11 21.98 14.19

La 44.70 46.80 42.60 44.07 44.46 44.32 55.98 28.24 44.20 28.87 56.28 58.67 57.21 58.28 58.01 57.60 27.24 5.80 45.70 28.79 29.27 28.10 27.81 27.76 36.53 40.80 27.24

Ce 80.90 81.00 80.20 81.24 78.59 82.93 102.60 54.67 71.60 55.10 98.17 103.70 99.97 99.79 99.90 98.40 55.67 11.70 78.90 56.42 55.83 55.08 53.69 53.33 70.10 78.25 53.23

Pr 8.27 8.18 8.20 8.11 7.80 8.18 10.30 5.66 7.20 5.52 8.89 9.31 9.19 9.11 9.14 9.11 5.66 1.33 7.96 5.57 5.47 5.52 5.40 5.46 7.76 8.49 5.44

A. Seelenfreund et al.

Site name Linzor Linzor Linzor Los Morros 3 Los Morros 3 Los Morros 3 Los Morros 3 Los Morros 3 Los Morros 3 Los Morros 3 Los Morros 3 Los Morros 3 Los Morros 3 Los Morros 3 Los Morros 3 Marilyn Manson Paniri lower Paniri lower Paniri lower Paniri lower Paniri lower Paniri lower Paniri lower Paniri upper Paniri upper Paniri upper Paniri upper Punta Tetragonal

Sample number Z11 Z44 Z45 A40 A41 A47 A48 A68 A69 A70 A71 A72 A73 A74 A50 A43 Z27 Z46 Z47 Z48 Z49 Z50 Z51 Z40 Z41 Z42 Z43 A65

V 4.79 7.90 7.60 20.40 35.82 44.00 43.00 7.00 8.00 43.00 8.00 45.00 7.00 127.00 42.00 48.98 43.60 48.06 45.13 54.07 44.66 40.93 47.06 61.10 49.30 62.20 58.70 7.00

Cr 111.67 84.00 79.00 3.00 6.38 13.00 12.00 <5 <5 12.00 <5 17.00 6.00 67.00 10.00 3.00 155.00 116.30 171.50 246.80 241.70 178.70 182.35 157.00 129.00 153.00 264.00 <5

Zr 104.28 130.00 136.00 130.08 161.55 218.00 210.00 135.00 142.00 220.00 137.00 222.00 135.00 165.00 215.00 184.00 215.00 200.00 200.00 186.00 206.00 208.00 205.00 201.00 196.00 196.00 199.00 135.00

Sr 149.78 210.00 214.00 127.37 256.80 314.00 356.00 210.00 218.00 350.00 215.00 345.00 213.00 354.00 350.00 243.36 301.00 344.00 358.00 322.00 344.00 364.00 354.00 337.00 303.00 345.00 325.00 203.00

Ba 806.16 994.00 1030.00 539.94 619.80 773.00 761.00 996.00 1040.00 783.00 1020.00 748.00 959.00 631.00 759.00 818.25 777.00 825.60 827.90 798.70 859.00 822.10 907.06 766.00 753.00 758.00 754.00 989.00

Rb 116.65 155.00 155.00 185.65 199.30 240.00 226.00 138.00 146.00 238.00 144.00 237.00 138.00 116.00 236.00 126.68 261.00 226.00 213.00 143.00 227.00 220.00 220.00 170.00 181.00 165.00 172.00 135.00

Y 14.61 19.73 19.79 3.23 6.16 10.49 9.82 20.50 21.30 10.50 21.20 10.40 21.20 22.20 10.05 14.33 10.70 11.12 10.56 19.33 10.98 10.25 10.30 16.85 15.99 16.45 16.18 21.20

La 28.92 38.80 38.50 40.00 38.64 57.37 57.56 41.80 42.20 60.60 42.90 59.20 42.90 40.50 60.35 26.85 53.90 60.96 58.90 42.14 61.29 58.17 57.74 35.40 35.96 35.46 35.65 43.20

Ce 55.43 73.60 72.76 67.06 70.90 100.20 98.79 77.00 79.70 103.00 80.60 102.00 80.40 72.10 99.83 51.05 89.80 106.60 103.50 74.19 107.10 101.10 100.30 64.20 64.84 64.67 64.23 79.20

Pr 5.52 8.07 8.05 6.85 6.46 9.15 9.05 7.77 7.99 9.93 8.12 9.53 8.03 7.75 9.14 5.15 9.30 10.50 10.40 7.50 10.60 10.20 10.20 6.80 6.78 6.89 6.84 8.15

Vitreous rocks in the Atacama region, northern Chile

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Table 5

Concentrations of trace elements for samples analysed by ICPMS (Nd to U). All elements expressed in ppm

Site name

Sample number A40 A62 A63 A64 A51 A52 A53 A54 A46 A61 A44 A55 A56 A57 A58 A59 A60 A45 A66 A67 A42 Z04 Z05 Z06 Z07 Z08 Z09 Z10

Nd

Sm

Eu

Gd

Tb

Dy

Ho

Er

Tm

Yb

Lu

Nb

Cs

Hf

Ta

Pb

Th

Los Morros 3 Alero Derrumbado Alero Derrumbado Alero Derrumbado Alero Toconce Alero Toconce Alero Toconce Alero Toconce Conuencia Conuencia Doa Marta El Otro Sitio El Otro Sitio El Otro Sitio El Otro Sitio El Otro Sitio El Otro Sitio Incahuasi Aldea Incahuasi Aldea Incahuasi Aldea La Mrula Linzor Linzor Linzor Linzor Linzor Linzor Linzor

22.73 34.10 33.80 33.00 32.96 31.62 33.48 42.52 22.42 28.40 22.53 34.55 35.66 35.39 34.97 35.14 35.30 22.42 5.60 32.70 22.85 22.60 22.67 21.93 22.20 31.25 34.80 22.24

3.00 5.24 5.04 4.96 4.67 4.47 4.79 6.34 3.65 4.31 3.80 4.35 4.42 4.34 4.27 4.14 4.13 3.65 1.69 4.85 3.87 3.86 3.91 3.74 3.79 4.56 5.06 3.78

0.60 1.03 1.02 0.96 0.90 0.85 0.90 0.95 0.73 0.98 0.78 0.77 0.77 0.80 0.77 0.77 0.75 0.73 0.13 0.92 0.76 0.76 0.76 0.74 0.74 0.90 1.07 0.75

1.95 4.20 4.06 3.95 3.66 3.55 3.66 4.81 2.87 3.70 2.97 2.75 2.75 2.71 2.70 2.65 2.63 2.87 1.89 3.82 3.01 3.00 3.02 2.90 2.97 3.81 4.39 2.89

0.24 0.61 0.59 0.56 0.52 0.50 0.52 0.65 0.47 0.57 0.47 0.31 0.32 0.31 0.32 0.31 0.31 0.47 0.38 0.55 0.48 0.48 0.48 0.46 0.46 0.58 0.63 0.47

1.08 3.56 3.45 3.31 3.07 2.93 2.99 3.67 2.59 3.12 2.66 1.55 1.60 1.55 1.65 1.47 1.43 2.54 2.42 3.24 2.49 2.54 2.60 2.49 2.49 3.41 3.53 2.50

0.21 0.74 0.74 0.71 0.66 0.62 0.65 0.74 0.54 0.68 0.50 0.30 0.31 0.30 0.30 0.28 0.29 0.50 0.51 0.68 0.51 0.50 0.52 0.50 0.50 0.71 0.71 0.50

0.53 1.98 1.97 1.90 1.76 1.70 1.79 1.93 1.50 1.78 1.41 0.80 0.83 0.80 0.80 0.76 0.75 1.46 1.41 1.86 1.36 1.43 1.43 1.39 1.40 2.05 2.04 1.40

0.08 0.30 0.30 0.28 0.26 0.24 0.26 0.27 0.22 0.28 0.23 0.12 0.12 0.11 0.11 0.11 0.11 0.22 0.24 0.27 0.21 0.23 0.22 0.22 0.21 0.32 0.31 0.21

0.53 1.95 1.98 1.88 1.76 1.69 1.73 1.73 1.53 1.77 1.58 0.78 0.79 0.78 0.76 0.73 0.74 1.53 1.72 1.83 1.49 1.51 1.51 1.50 1.48 2.25 2.05 1.52

0.08 0.30 0.31 0.28 0.27 0.25 0.26 0.26 0.23 0.29 0.23 0.12 0.12 0.12 0.12 0.11 0.12 0.23 0.25 0.28 0.23 0.24 0.24 0.23 0.24 0.33 0.30 0.23

30.95 13.40 13.30 13.10 12.70 12.30 12.90 13.30 16.47 12.00 16.32 11.90 12.50 12.30 12.10 11.90 12.20 19.97 34.00 13.40 16.88 16.26 16.48 15.83 16.66 16.73 17.97 16.20

14.37 8.19 8.29 7.18 8.01 8.98 8.58 14.30 8.92 6.20 7.54 12.10 12.40 9.32 11.60 11.60 12.50 9.49 14.40 7.25 9.24 8.90 9.34 8.80 8.95 5.09 8.21 9.01

4.25 1.00 29.76 30.38 4.20 4.33 4.26 18.60 14.20 4.18 4.44 4.08 18.20 14.00 4.30 4.16 4.05 19.30 14.00 4.14 3.98 3.67 21.30 15.00 4.39 3.99 3.56 20.30 14.90 4.36 4.00 3.79 20.40 15.40 4.54 5.51 4.31 18.10 22.10 5.90 4.62 2.23 25.45 15.78 4.47 5.72 4.37 12.90 19.10 4.78 4.67 2.28 25.48 15.32 4.28 5.10 4.52 22.00 39.80 6.25 5.24 4.65 22.90 41.00 6.48 5.19 4.43 21.90 39.80 6.34 5.11 4.45 21.80 40.80 6.43 4.87 4.31 22.40 33.10 6.18 4.89 4.27 23.50 32.90 6.23 4.32 1.23 29.10 15.29 3.94 2.33 15.61 11.80 5.20 13.64 4.15 3.93 20.10 14.30 4.26 4.41 2.20 27.32 15.22 4.28 4.58 2.20 24.27 15.56 4.38 4.60 2.20 25.98 15.72 4.47 4.53 2.15 25.08 15.45 4.36 4.47 2.22 23.36 15.65 4.42 5.02 1.59 18.84 13.35 4.98 4.35 1.65 21.65 11.39 3.93 4.51 2.17 27.10 15.26 4.38

A. Seelenfreund et al.

Site name

Sample number Z11 Z44 Z45 A41 A47 A48 A68 A69 A70 A71 A72 A73 A74 A50 A43 Z27 Z46 Z47 Z48 Z49 Z50 Z51 Z40 Z41 Z42 Z43 A65

Nd

Sm

Eu

Gd

Tb

Dy

Ho

Er

Tm

Yb

Lu

Nb

Cs

Hf

Ta

Pb

Th

Linzor Linzor Linzor Los Morros 3 Los Morros 3 Los Morros 3 Los Morros 3 Los Morros 3 Los Morros 3 Los Morros 3 Los Morros 3 Los Morros 3 Los Morros 3 Los Morros 3 Marilyn Manson Paniri lower Paniri lower Paniri lower Paniri lower Paniri lower Paniri lower Paniri lower Paniri upper Paniri upper Paniri upper Paniri upper Punta Tetragonal

22.60 32.01 31.46 24.63 35.01 35.38 31.40 32.90 37.40 33.00 36.50 33.00 32.10 35.94 21.49 33.79 40.70 39.61 29.96 40.58 38.30 38.17 26.05 25.45 26.34 25.98 33.10

3.89 5.10 5.04 3.56 4.44 4.51 4.76 4.96 4.65 4.75 4.64 4.79 5.08 4.45 3.72 4.63 5.08 5.06 4.38 5.07 4.91 4.88 4.26 3.96 4.30 4.12 5.03

0.76 0.99 0.98 0.66 0.78 0.85 0.90 0.94 0.83 0.94 0.84 0.95 1.03 0.82 0.71 0.85 0.97 0.97 0.97 0.98 0.94 0.98 0.92 0.81 0.89 0.87 0.96

2.94 3.89 3.85 2.23 2.84 2.98 3.67 3.82 2.95 3.81 2.91 3.68 4.25 2.79 2.92 3.03 3.36 3.25 3.54 3.32 3.16 3.15 3.38 3.10 3.35 3.20 3.84

0.47 0.56 0.56 0.29 0.34 0.34 0.53 0.56 0.35 0.54 0.34 0.54 0.62 0.33 0.45 0.39 0.41 0.41 0.54 0.42 0.39 0.39 0.47 0.44 0.46 0.46 0.56

2.54 3.17 3.23 1.29 1.76 1.68 3.15 3.17 1.72 3.22 1.75 3.16 3.55 1.66 2.38 1.99 1.98 1.91 3.09 2.04 1.85 1.86 2.77 2.51 2.69 2.59 3.27

0.50 0.65 0.64 0.23 0.34 0.33 0.66 0.69 0.33 0.68 0.34 0.68 0.74 0.33 0.49 0.37 0.39 0.38 0.67 0.39 0.36 0.35 0.57 0.54 0.55 0.55 0.69

1.44 1.80 1.80 0.62 0.92 0.86 1.78 1.87 0.90 1.84 0.88 1.84 1.91 0.86 1.35 1.00 1.01 0.99 1.81 1.05 0.95 0.94 1.62 1.52 1.55 1.54 1.86

0.23 0.27 0.27 0.10 0.13 0.12 0.26 0.27 0.13 0.27 0.13 0.27 0.27 0.12 0.22 0.14 0.15 0.14 0.27 0.15 0.13 0.14 0.25 0.23 0.23 0.23 0.28

1.53 1.82 1.81 0.66 0.87 0.82 1.77 1.81 0.85 1.81 0.89 1.83 1.68 0.81 1.47 0.98 0.99 0.95 1.76 0.96 0.89 0.90 1.66 1.65 1.61 1.65 1.82

0.24 0.27 0.27 0.10 0.13 0.12 0.27 0.28 0.13 0.28 0.13 0.28 0.25 0.13 0.23 0.14 0.16 0.14 0.29 0.16 0.13 0.14 0.25 0.25 0.24 0.25 0.27

17.01 17.10 17.02 16.72 12.80 12.10 13.00 13.20 12.90 12.90 12.90 12.80 10.00 12.70 13.88 17.74 14.34 13.89 12.63 14.36 13.60 13.65 15.19 15.30 14.62 14.94 13.00

9.03 5.21 8.05 13.96 12.50 12.00 7.47 8.35 12.10 7.91 12.80 8.26 4.30 12.60 6.28 11.70 12.34 10.47 5.90 9.70 11.10 10.63 6.94 7.68 6.75 7.02 7.89

4.51 3.88 3.89 5.74 5.47 5.39 4.05 4.12 5.61 4.11 5.64 4.02 4.34 5.42 6.75 5.41 6.38 6.25 6.01 6.47 6.03 6.02 5.07 5.01 4.97 5.07 4.60

2.18 1.01 1.02 2.13 4.98 4.73 3.93 3.84 4.99 3.84 4.92 3.85 3.05 4.72 2.03 1.39 3.04 2.94 2.33 3.07 2.84 2.84 1.07 1.16 1.05 1.09 3.86

23.78 21.60 20.59 36.39 23.10 20.80 19.00 18.90 22.60 18.20 21.10 19.20 10.60 22.60 19.02 27.28 24.00 24.05 16.25 24.17 23.42 37.77 16.08 16.36 16.32 16.39 18.80

15.63 12.22 12.06 32.96 40.30 37.20 13.80 14.40 39.90 14.60 38.60 14.40 13.00 38.90 17.70 33.09 34.38 31.92 20.18 33.15 31.59 32.07 17.34 19.89 17.52 18.63 14.00

4.38 3.85 3.83 5.88 6.52 6.10 4.13 4.20 6.38 4.27 6.27 4.14 3.47 6.35 4.24 5.77 6.33 6.01 5.01 6.33 6.03 6.18 4.86 5.61 4.82 5.10 4.10

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Figure 9 The principal component analysis for all source samples. The elements and compounds used are K 2O, CaO, TiO2, MnO, Fe2O3, Rb, Sr, Y, Zr, Ba, La, Ce and Nd.

Figure 10 A cluster analysis using average linkage for samples from the Linzor and combined Paniri sources. The elements and compounds used for the cluster analysis are K2O, CaO, TiO2, MnO, Fe2O3, Rb, Sr, Y, Zr, Ba, La, Ce and Nd.

upper source. Samples from the Paniri volcano show higher values of MnO, Zr, Rb, Sr, La, Ce and Nd than the Linzor samples, and these contribute substantially to group discrimination. Concentrations of compounds and trace elements, which according to the principal components analysis accounted for 78% of the variance, were combined in a non-parametric cluster analysis, using average linkage method as shown in Figure 10. Separate dendrograms were constructed, rst for the source samples only, using different groups of elements in order to assess their power to discriminate between the known groups, and the process was then repeated with the archaeological samples. The resulting dendrograms
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Figure 11 K/Ar dates for ve samples from the Linzor and Paniri sources. Samples Z06 and Z11 are from Linzor, samples Z27 and Z46 are from the Paniri lower source, while Z42 comes from the Paniri upper source.

for the source samples (Fig. 10) indicate that the two sources Linzor and Paniri can be separated into two major groups. Within the Paniri group, we can clearly observe in both cases that sample Z27, collected at the Paniri lower source, and sample Z48 group as units that are separate and distinct from each other. Sample Z48 groups closer to the upper source samples than to the lower source samples. During initial data inspection, within the Linzor source, samples Z08 and Z09 grouped distinctly from the other Linzor source samples. We therefore decided to run additional samples (samples Z44 and Z45) from the same sampling units in order to assess the reality of these subgroups. As seen in Figures 9 and 10, these samples grouped closely with Z09, while sample Z08 consistently grouped separately from all others, but always within the Linzor group. The subgroups within the Linzor group, identied in the principal component analysis, are not related to either visible geomorphological aspects or to the two outcrops observed in the eld; they may, however, be associated with stratigraphical events, which were not considered in the sampling strategy in the eld. We were able to date two samples by K/Ar, one for each subgroup from the Linzor source. Figure 11 reects the above results, indicating two eruptive histories at the Linzor source. Different moments of the formation of the lava ow may therefore explain the variation of these samples within the Linzor source group. The dates obtained for the different sampling areas for the Paniri group gave overlapping results; therefore chemical diversity within the Paniri source may or may not be related to different eruptive events. In order to assess which of the archaeological samples could be assigned to any of the sources sampled, we performed a principal components analysis and cluster analysis using all samples analysed for the study (i.e., both source samples and samples from archaeological sites) (Fig. 6). The resulting dendrogram from the cluster analysis is shown in Figure 7. Discriminate analysis was then performed in order to determine the variables that allow for the best discrimination between the two sources Linzor and Parini (obtained by PCA and cluster). The elements Rb, Sr, Y, Zr, Ba, La, Ce and Nd discriminated correctly between the two sources Linzor and Parini (correctly predicted: 100%). The discriminate function coefcients are not shown. Of all of the archaeological samples analysed, 16 can unquestionably be associated with the Linzor source (samples A42, A43, A44, A45, A46, A51, A52, A53, A62, A63, A64, A65, A67, A68, A69 and A73), while 13 come from the Paniri source area. Two of these samples are from the Paniri upper source (samples A61 and A54), and the remainder (samples A47, A48, A50, A55, A56, A57, A58, A59, A60, A70 and A72) come from the Paniri lower source.
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Four out of the total number of samples cannot be ascribed either to the Linzor or the Paniri source. Sample A66 is markedly distinct from all other samples. Samples A40, A41 and A74 show a distinct grouping within the dendrogram. However, with PCA analysis, samples A40 and A41 cluster closely with the other Paniri source group samples, while sample A74 remains distinctly different. These results indicate that we are dealing at least with two additional, as yet unidentied, sources, which we have named NN1 and NN2. On visual inspection, these samples do not show any marked differences to the others; however, petrographically, samples A40 and A41 correspond to a slightly more acid dacite, as previously mentioned.
DISCUSSION

Distinct chemical proles separate the Linzor from the Paniri rock; however, within the Linzor group there is a fairly wide internal variation that could result in erroneous allocations of archaeological samples in the event of inadequate sampling. These differences can be attributed to different incidents of the formation of the lava ow, and to the superposition of distinct lavas from different eruptive events. The Linzor outcrop is the product of two different volcanic events, each separated by about 0.4 Ma. In the case of the Paniri vitreous dacite, this can be attributed to a single volcanic eruption that occurred during the mid-Holocene (0.4 Ma). Volcanic events from the same volcano or different volcanoes and similar magma show distinct mineralogical compositions that are reected in the geochemistry of the rocks. Sources must be extremely well sampled, both horizontally and vertically, since major compositional changes can occur within a single source. Dating should be considered whenever possible, since it can provide important additional information or explanation for internal rock variability. Petrographic thin sections allow for a preliminary classication of the samples, but are not sensitive enough to be used by themselves for source allocation or discrimination. Petrographic analysis and identication of mineral crystals in the rocks is of fundamental importance in order to understand variations in element concentrations. Crystallization, secondary melting and contamination of the original magma by the continental crust can occur during eruption in this continental subduction zone. The combination of analytical methods used (ICPMS, ICPOES and AAS) allowed for the identication of 33 trace elements, rare earth elements and major elements expressed as oxides. The rare earth elements were believed to be suitable for source discrimination due to their stability and low mobility during and after magmatic events. However, trace elements gave clearer and more accurate groupings, and are therefore reported here. However, since the method is a destructive one, its applicability to a large number of archaeological samples is a restrictive factor, and therefore we are investigating the potential and reliability of nondestructive analyses for these types of rock samples (Morales et al. 2007). From an archaeological point of view, the results shown allow us to address some issues concerning the prehistory of the Salado River subregion, related to the acquisition and use of non-local stone resources, and contribute to the general discussion on these issues within the south Andean area. First, the present results help to document the local temporal sequence for the exploitation of the vitreous rock sources analysed for this study. Second, the results allow us to understand, based on a case study, the dynamics of the exploitation of the three quarries analysed and the circulation of the raw material and/or the tools manufactured using that material. Finally, the results indicate the maintenance of the preferential exploitation over time of one of the studied sources.
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The results for a number of archaeological samples analysed for this study indicate that the Linzor quarry was the primary source exploited during the Early and Late Formative periods in the Salado River Basin, and that it was exploited during a longer time span than the other two sources at the Paniri volcano. The Linzor dacite has been found to be associated with archaeological contexts dating from at least the Archaic period, at the Alero Toconce and Alero Derrumbado sites. It is also linked with contexts dated to the Early Formative, such as at Alero Toconce, Los Morros 3, El Otro Sitio and La Mrula. During the Late Formative, the raw material from the Linzor source reaches sites as far away as Conuencia, Doa Marta and Incahuasi. In contrast, the Paniri upper source was exploited during both phases of the Formative. We nd vitreous dacite at Alero Toconce during the early phase of the Formative and at Conuencia during the Late Formative phase. Finally, the raw materials from the Paniri lower source were exploited solely during the Early Formative, at a time when the demand for this type of vitreous rock was at its highest, as evidenced from the Los Morros 3 and El Otro Sitio sites, located on the edge of the vega de Turi. The evidence for the Archaic indicated that the chain for the exploitation of the Linzor quarry and the manufacture of preforms and nished tools was carried out at sites in close proximity to the source: Alero Derrumbado and Alero Toconce. The results for a number of archaeological samples analysed for this study show, for the Early Formative period, the simultaneous exploitation of the three sources of raw material and complex strategies of production and distribution of the lithic materials. The material was extracted at the Linzor quarry and some initial stages of tool manufacture were performed at the quarry. Bifacial preforms were transported to other sites in the vicinity, such as Punta Tetragonal, an open site that combines lithic manufacturing activities with exploitation of the wetland resources. The operational reduction chain continues at other sites, such as Alero Toconce, Los Morros 3, El Otro Sitio and the La Mrula site at the Caspana River. On the other hand, the Paniri lower source was used exclusively at the Los Morros 3 and El Otro Sitio sites, both located at the edge of the vega de Turi. During this same period, at Alero Toconce we nd the presence of materials from the Paniri upper source, and at the Los Morros 3 site we nd raw materials from an as yet unidentied source. The samples from the Late Formative period indicate a restriction in the number of sources exploited, as observed in the distribution of the tool blanks in the study area. In fact, we only nd small-sized debitage from Linzor at the Conuencia, Doa Marta and Incahuasi sites, and some debitage from the Paniri upper source at the Conuencia site. Most signicantly, the present results indicate a preference over the complete time span covered by the analysed materials for the vitreous rock from the Linzor source. The explanation for the sustained use in time of this source, at least since the Archaic, may be attributed to three factors. In the rst place, we need to consider the aking quality of the raw material found at Linzor, something that has yet to be tested. The preference of the Linzor rock over others may be related to culturally constructed factors that may inuence the choice of the raw material used, but this question is beyond the scope of the present study. Additionally, we believe that the concentration of available good-quality aking raw materials at the Linzor source makes this a far more efcient location for the acquisition of raw materials than the sources at the Paniri volcano, where the rock is not readily available for extraction at one single point, but is highly dispersed and difcult to reach on the volcanic slope or at high altitude. Finally, the location of the Linzor source, at the drainage of the vega de Inacaliri, could be related to circuits of mobility that characterize the populations of the Early Formative period, whose subsistence strategy combined hunting and gathering with initial camelid herding.
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This pattern of mobility can be extended to places as far as 60 km to the south of our study area, as has been demonstrated by the presence of Linzor dacite at Formative period archaeological sites in Pelun, a locality on the northern edge of the Atacama saltplain (cf., Seelenfreund et al. 2004). Evidence of Linzor dacite also occurs at a site dated to the Middle Archaic huntergatherer era, called Huallajara, located in the highlands or puna of neighbouring Bolivia, at about 30 km from Linzor, indicating that this type of lithic material also circulated in that direction (Seelenfreund et al. 2004); the Linzor dacite disappears from the later Formative contexts of this site, to be replaced by obsidian (A. Nielsen, Instituto Interdisciplinario de Tilcara, Jujuy, Argentina, pers. comm. 2006).
ACKNOWLEDGEMENTS

The present research was funded by Fondecyt grant 1040633. We would like to thank Vernica Baeza, Patricio de Souza, Patricio Galarce, Gonzalo Pimentel, Carlos Carrasco and Denisse Pasten for their assistance in the eld. We also wish to thank Judith Hoffman for proofreading and editing our English, and nally the anonymous reviewers for their important and helpful suggestions.

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