Lead isotope ratios of Pueblo I lead-glazed ceramics and galena from Colorado and Pueblo II galena from Chaco Canyon, New Mexico

Lead isotope ratios of Pueblo I lead-glazed ceramics and galena from Colorado and Pueblo II galena from Chaco Canyon, New Mexico

Journal of Archaeological Science: Reports 23 (2019) 634–645 Contents lists available at ScienceDirect Journal of Archaeological Science: Reports jo...

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Journal of Archaeological Science: Reports 23 (2019) 634–645

Contents lists available at ScienceDirect

Journal of Archaeological Science: Reports journal homepage: www.elsevier.com/locate/jasrep

Lead isotope ratios of Pueblo I lead-glazed ceramics and galena from Colorado and Pueblo II galena from Chaco Canyon, New Mexico

T



Brunella Santarellia, , Sheila Goffb, David Killickc, Kari Schleherd, David Gonzalese a

Department of Materials Science and Engineering, University of Arizona, Tucson, AZ, USA History Colorado, Denver, CO, USA c School of Anthropology, University of Arizona, Tucson, AZ, USA d Crow Canyon Archaeological Center, Cortez, CO, USA e Deparrtment of Geosciences, Fort Lewis College, Durango, CO, USA b

A R T I C LE I N FO

A B S T R A C T

Keywords: Lead isotope analysis Galena Sourcing Rosa black-on-white ceramics Pueblo Bonito

The earliest glazes in the American Southwest were produced during the early Pueblo I period (ca. 750–850 CE) in the Upper San Juan region of Colorado. Petrographic and isotopic techniques were used to study these early glaze-painted pots and to address questions of production locales and procurement strategies. The results of this study identify the preferred source of lead utilized by the potters as originating in the Galena District, in the Lake City and Uncompahgre calderas, in the western San Juan Mountains of Colorado. Glaze paints from three locations in the Mesa Verde region were produced with galena from these deposits, indicating that even when potters were choosing to use different clays and temper, the source of lead remained the same. Galena ores from these deposits have additionally been identified at other locations, including Dillard, a Basketmaker III site in southwest Colorado and in Pueblo II contexts in Pueblo Bonito, Chaco Canyon in New Mexico, indicating continuity in knowledge of distant lead sources.

1. Introduction The earliest independent invention of lead glaze technology in North America occurred during the early Pueblo I period (ca. 750–850 CE) in the Upper San Juan Basin in Colorado, the region identified as the eastern portion of the Mesa Verde region and geographically defined by the upper drainages of the Animas, La Plata and Piedra Rivers (Fig. 1). These glazes were produced nearly 500 years before the better-known glaze paints of eastern Arizona and New Mexico of the Pueblo IV tradition (1275–1400 CE). The unique aspect of Southwestern lead glazes is that they were developed as paints, thus serving solely as decorative elements. These technologies represent two separate, independent instances of invention of glaze technology in the prehistoric Southwest. No glaze paints were produced in the Southwest in the interim period 850–1275 CE, but lead continued to be used and galena specimens have been recovered in burial or ritual contexts at sites such as Aztec Ruins and Chaco Canyon, in New Mexico. The study of lead glazes has been a significant component of the ceramic literature of the Southwest, and archaeologists have been interested in this technology since the 1930s. Significant efforts have been dedicated to the study of the Pueblo IV glazes (DeAtley, 1986;



Duwe and Neff, 2007; Fenn et al., 2006; Habicht-Mauche et al., 2000; Huntley et al., 2007; Van Keuren et al., 2013), and researchers have successfully used chemical “recipes” of glaze paints as tools to study social dynamics (Cordell and Habicht-Mauche, 2012; Eckert, 2006; Habicht-Mauche, 2006; Huntley et al., 2012; Schleher et al., 2012; Stark, 2006). The Pueblo I glaze paints of the Upper San Juan have received comparatively little attention. In this paper we enhance the knowledge of these early glaze paints by providing new results of petrographic and isotopic studies of glaze-painted sherds to address questions of production areas and procurement strategies. A study of galena samples recovered from sites throughout the region demonstrates that there was continuity in knowledge of lead sources over time and space and suggest cultural transmission of this knowledge over more than 300 years. There is however no evidence for use of these sources in the production of Pueblo IV lead glazes. 2. Archaeological context Researchers have recognized eastern, central, and western cultural areas in the Mesa Verde region as early as the Pueblo I period (Schachner et al., 2012; Wilshusen and Glowacki, 2017). Differences in

Corresponding author at: The Cyprus Institute, 20 Konstantinou Kavafi St., 2121 Aglantzia, Nicosia, Cyprus. E-mail address: [email protected] (B. Santarelli).

https://doi.org/10.1016/j.jasrep.2018.11.027 Received 27 August 2018; Received in revised form 15 November 2018; Accepted 26 November 2018 Available online 06 December 2018 2352-409X/ © 2018 Elsevier Ltd. All rights reserved.

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Fig. 1. Map of southwestern Colorado and northwestern New Mexico with locations of interest.

(Bellorado, 2013; Bellorado and Anderson, 2013). In addition, there is substantial evidence for higher than expected intrinsic population growth in this area from the late eighth to early ninth centuries (Wilshusen and Perry, 2008). These immigrants previously lived in small, dispersed hamlets of extended families or kin groups, but as population rapidly increased, the majority moved into settlement clusters or villages (Bellorado, 2013; Bellorado and Anderson, 2013). This settlement change appears to have brought with it new organizations and structures to reinforce the social solidarity between people of different households and kin groups, giving them the means to deal with claims regarding land and resource use, while still allowing them to retain and signal their identities (Wilshusen and Potter, 2010). Throughout the Pueblo I period in the Upper San Juan people moved about four areas: the La Plata River drainage; Ridges Basin near present day Durango; the Piedra, Los Pinos and upper San Juan River drainages; and the Navajo/Fruitland area near Aztec, New Mexico.

site layout and architecture (Allison et al., 2012; Potter et al., 2012; Wilshusen et al., 2012), ceramics (Allison, 2008; Wilson and Blinman, 1995), agricultural practices (Bellorado and Anderson, 2013; Burrillo, 2017) and sandal construction (Webster, 2009) indicate each region had its own particular culture history and mix of social identities or ethnicities. By the mid-ninth century there was a rich mix of cultural identities in the villages of central Mesa Verde (Wilshusen and Ortman, 1999). The population of the Mesa Verde region increased rapidly beginning in the early 600 s, when there was an unprecedented migration of farmers into the central Mesa Verde region. Over the next century both the eastern and western portions of the region also filled with farmers seeking new opportunities. In the Upper San Juan, the population increase in the eighth century can be originally attributed to farmers moving from lower elevation settings along the San Juan River to higher elevations to the north due to climatic fluctuations that allowed for greater precipitation and moderate temperatures in this area 635

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found in all clusters. One cluster, Sacred Ridge (dendrochronological dates from 729 to 803 CE), was large enough and sufficiently aggregated to be considered a small village (Potter and Perry, 2011; Wilshusen et al., 2012). Sacred Ridge held a central role in the cultural landscape of Ridges Basin (Chuipka, 2009a; Potter, 2010b; Wilshusen, 2009). Located on a knoll at the west end of Ridges Basin, the residents of Sacred Ridge displayed their status by building larger homes, enclosures or stockages to delineate households (Potter and Chuipka, 2007), four oversized pit structures likely used for rituals and a tower that would have been visible to all residents of Ridges Basin. The form of organization developed by Sacred Ridge residents ultimately failed as many residents, likely members of a genetic subgroup unrelated to the larger Ridges Basin community (Potter et al., 2012), were victims of an episode of violence followed by the burning and depopulation of the village. Ridges Basin was not occupied again until historic times. Another cluster, Blue Mesa, was located east of Ridges Basin and, while certainly aware of and likely interacting with some Ridges Basin residents, developed a different strategy for integration (Bellorado and Anderson, 2013). The primary occupation of Blue Mesa ceased around 820 CE, with complete depopulation in the 840 s, likely due to lack of integration within the community and environmental issues (Chuipka, 2009b; Potter and Yoder, 2008). Glaze-painted Rosa ceramics represent 20% of the total white ware assemblage from the ALP project (Potter, 2010a). Results of temper and clay analyses suggest that ceramics recovered from the ALP project area were made with a variety of clays found in or near Ridges Basin, and tempered with rocks or sand available in the Animas River drainage, therefore indicating local production (Allison and Hagopian, 2010). Glaze-painted Rosa ceramics were recovered in much lower numbers during the DAP, a project from 1978 to 1985 near the town of Cortez, 65 km northwest of Durango, in the central Mesa Verde region. Approximately 0.4% of the white wares recovered by the DAP were glaze-painted, and occur in greater frequency in contexts dated 720–840 CE, although some were recovered in contexts determined to be as late as 840–880 CE (Blinman and Wilson, 1988; Waterworth, 1988). Results of temper and clay analyses identify glaze-painted sherds as nonlocal to the Dolores area, and suggest that they were produced in the La Plata River valley rather than the Durango area (Waterworth, 1988). These results support Shepard's hypothesis and confirm that there are at least two geographical areas of glaze manufacture during the Pueblo I period: one in the Durango area, and a concurrent or slightly later episode of production likely in the La Plata River valley. The occurrence of glaze paints in Dolores parallels the occupation of the La Plata valley, and it is probable that the ceramics were moved into the DAP area through down-the-line mechanisms of exchange (Waterworth, 1988). We selected a sample of materials from this collection as a representative case study of glaze paint production outside of the Animas River valley.

Glaze paints were developed in the Upper San Juan during this period of dynamic social changes and population movements. The choice by potters to use a glaze paint instead of the more common mineral or organic paints used in the rest of the Mesa Verde region was a way of forming and signaling the unique identities of a cultural group. The preference for making and acquiring glaze-painted pottery is a common trait at sites in the Animas River valley, and can be thought of as a community of practice (Wenger, 1998) based on the use of lead ores to decorate ceramics. Through transmission of the knowledge of how to make a lead glaze, including material procurement and processing strategies as well as details such as firing techniques, potters were able to differentiate themselves from people in other areas of the Mesa Verde region. Glaze-painted ceramics from the Upper San Juan are designated as Rosa black-on-white, a fairly distinctive ceramic type with limited temporal and spatial distribution. Rosa black-on-white ceramics differ from other types of the Mesa Verde region by temper and decorative style, but their defining characteristic is the presence of a lead-based glaze paint (Wilson and Blinman, 1993). The glaze paints range from fully vitrified, thick, transparent yellow glazes, to matte black paints showing minimal to no vitrification. These paints were often applied over an underpaint with washy edges indicative of an organic component, possibly bee-weed (Cleome serrulata), which was the preferred black organic pigment in the Southwest (Adams et al., 2002). Temper of the Rosa ceramics was dominated by quartz and feldspar grains, and likely originated from sand or crushed quartzite (Allison and Hagopian, 2010: Wilson and Blinman, 1993). These ceramics are found in higher frequencies in early Pueblo I contexts at sites in the Animas River valley, near the modern town of Durango, Colorado, where they were likely produced. Glaze paints have been found at other locations in the Mesa Verde region where they occur in lower abundances, including in the Dolores area and the La Plata valley west of Durango (Shepard, 1939; Waterworth, 1988), and the Navajo Reservoir district and the Piedra district to the east of Durango (Dittert, 1966; Roberts Jr., 1930). Glaze-painted ceramics found outside of the Animas River valley are generally tempered with a crushed igneous rock temper, identified as originating from andesite or diorite porphyries. This was first noted by Anna Shepard, who put forth the hypothesis that there were multiple production centers of glaze paints in the region during the early Pueblo I period (O'Bryan, 1950; Shepard, 1939). By the early 800 s Rosa style ceramics become less prominent, and glaze production technology disappears entirely by about 850 CE. For this study we chose to work with two collections from largescale and fully published archaeological projects in the Mesa Verde region: the Animas-La Plata (ALP) project and the Dolores Archaeological Program (DAP) (Fig. 2), to investigate material procurement strategies at the multiple centers of glaze paint production. The ALP project excavated over 70 sites between 2002 and 2005 in the area around Durango, in advance of the construction of a large reservoir (now Lake Nighthorse). The two main regions surveyed were Ridges Basin and Blue Mesa; in both areas excavations found a very short and intensive occupation. One of the earliest villages in the American Southwest, Sacred Ridge, was located in Ridges Basin. The ceramic assemblage is comparable to contemporary collections from other projects in the Durango region, and can be used as a representative case study for glaze paint production in the Animas River valley. This study area is also representative of the diversity and aggregation that occurred during the Pueblo I period. Immigrants from several locations, including the central and western Mesa Verde regions, northern New Mexico and local upper San Juan populations (Wilshusen, 2009), moved into Ridges Basin and occupied it between 750 and 815 CE (Bellorado and Anderson, 2013). Five settlement clusters in Ridges Basin varying in size and degree of aggregation were identified. Among these clusters, there are both similarities and differences in site layout, architecture, burial practices, access to agricultural land and other resources. Rosa black-on-white ceramics were

3. Materials and methods 3.1. Archaeological materials: glaze paints and galena For this study we sampled Pueblo I glaze-painted sherds from the collections described in the previous section. We selected 91 glazepainted sherds from the ALP collection (from nine sites) and 15 glazepainted sherds from the DAP collection (from three sites) (Table 1). Additionally, we selected five glaze-painted whole vessels from the Flora collection at the Arizona State Museum; this collection consists of materials that were excavated by the amateur archaeologist Isaiah “Zeke” Flora between 1933 and 1940 around Durango. Most of the Flora samples were collected on Blue Mesa, but one was collected 50 km east of Durango, near Stollsteimer Mesa in the Piedra District. To supplement the data from lead glazes, we also sampled galena from Pueblo I archaeological contexts in the Upper San Juan (Table 1). 636

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Fig. 2. Location of archaeological sites from which lead-glazed pottery originated and galena-bearing mineralized deposits in Colorado discussed in this study.

with other sulfide ores such as pyrite and sphalerite, occur in massive intergrowths in veins and replacement deposits in limestone beds of Paleozoic units (Leadville Limestone and Hermosa Group) (McKnight, 1974). Near-surface deposits of silver-rich ore have been recorded in the Rico district, so it is likely that there was galena associated with surface exposures of these deposits. We obtained eight samples of galena from three separate locations in the Rico district for analysis. The greatest concentration of galena sources in southwest Colorado is in the San Juan Mountains, where there is a cluster of more than a hundred historic mines in the San Juan, San Miguel and Ouray counties. The western San Juan Mountains consist of a complex of calderas that have massive ore deposits of gold, silver, copper, lead and zinc, generally found in fracture-filling veins that formed during periods of caldera formation (Sanford, 1992). These sources are located between 80 and 150 km northeast of Durango. The geology and geochemistry of the San Juan Mountains has been extensively characterized in the geological literature (Bove et al., 2001; Casadevall and Ohmoto, 1977; Doe, 1976; Doe et al., 1979; Foley and Ayuso, 1994; Hon et al., 1985; Lipman et al., 1978; Sanford, 1992; Steven and Lipman, 1975). We supplemented the published isotopic data from the region with new measurements on galena samples from nine mineral deposits in the western San Juan Mountains, coupled with the Rico and La Plata samples, all obtained from museum collections and through field collection by two of the authors (SG and DG) (Table 2, Fig. 2). We selected samples mostly from deposits located within the Red Mountain district,

Seven samples were selected from the ALP collections, and one from the Flora collection. One sample was selected from the Dillard site, a Basketmaker III site dated to 550–750 CE near Cortez, 65 km west of Durango (Fig. 2). The last sample set for this study comes from Pueblo Bonito, in Chaco Canyon, where galena was often found in ritual contexts dated between 850 and 1150 CE. We selected 9 samples that were excavated by the Hyde Expedition between 1896 and 1899 (Pepper, 1920) (Supplementary Table S1). 3.2. Geological samples of galena There are no recorded deposits of lead minerals in southeastern Utah, northwestern New Mexico or northeastern Arizona. The closest primary sources of galena to Durango are 15–25 km northwest in the La Plata Mountains; however, galena is generally rare in this area and occurs abundantly in only a few deposits (Eckel, 1949; Gonzales, 2015). The primary ore deposits in this district consist of telluride ores of gold and silver, which account for 95% of modern production (Van Loenen et al., 1997). Instances of galena have been recorded at the Gold King, Jumbo-Morovoratz and Puzzle deposits (Eckel, 1949), and as part of a lead-silver ore vein in the Black Rock claim of Bedrock Gulch (Lonsdale, 1921). We were able to obtain samples of galena from the Gold King Mine and Bedrock Gulch. Galena is a common mineral in the Rico district, 50 km north of Durango, where it accounts for approximately 30% of modern production (Van Loenen et al., 1997). Galena, along Table 1 Archaeological samples. Source Animas-La Plata Project (5LP#s) Dolores Archaeological Program (5MT#s) Flora Collection (GP#s) Dillard Site Pueblo Bonito, Chaco Canyon

No. of samples 91 7 16 5 1 1 9

Type

Curatorial institution

Glaze-painted sherds Galena Glaze-painted sherds Glaze-painted pots Galena Galena Galena

Canyons of the Ancients Visitor Center and Museum, Dolores, CO

637

Arizona State Museum, Tucson, AZ Crow Canyon Archaeological Center, Cortez, CO American Museum of Natural History, New York, NY

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Table 2 Mineralogical reference samples. Sample ID

No. of samples

MIN 015305 MIN 010981 88-1019 2011-1127-008 BM HMM RM GKM GM BWM RD CBM

1 1 1 1 2 3 1 1 2 2 8 1

Location/mining area

Curatorial institution/ Collection info

Bedrock Gulch, La Plata County Belle Mine, Montezuma/San Juan County Tomboy Mine, San Miguel County Idarado Mill, Ouray County Bonita Mine, San Juan County Highland Mary's Mine, San Juan County Revenue Mine, Ouray County Gold King Mine, La Plata County Guston Mine, Ouray County Barstow Mine, Ouray County Rico, Dolores County Camp Bird Mine, Ouray County

Peabody Museum of Natural History, Yale University, New Haven, CT Telluride Historical Museum, Telluride, CO Collected by David Gonzales, Sheila Goff and Lori Reed

Petrography was used to identify the temper of the ALP glazepainted sherds. Surface-polished thin sections were prepared, and were analyzed using an Olympus BX51 petrographic microscope using both transmitted and reflected light, at low to high magnifications (50× to 400×) to identify rock and mineral fragments. The temper data from the DAP glaze-painted sherds are reproduced from their ceramic dataset available online through tDAR (Dolores Archaeological Program, Ceramics: Temporal-Spatial Dataset. 1988 (tDAR id: 6039); doi:10.6067/XCV8TD9WNB). It is significant to note here that the DAP temper identification was made using a binocular microscope on break edges, not through petrographic analyses. The glaze-painted ceramics from the Flora collection are whole vessels and could not be sampled for petrography, so it was not possible to accurately identify the temper used.

following digestion and separation protocols (Thibodeau et al., 2013). Previous work done by the first author further confirms the validity of this method for analysis of lead glazes. The Pb isotopic ratios of swabbed glazes generally plot within the error margin of ratios from the same glaze prepared following the digestion and separation procedure, and any slight differences observed did not affect the interpretation of the data (Santarelli, 2015). The samples were analyzed using a GV-Instruments Isoprobe multicollector inductively coupled mass spectrometer (MC-ICP-MS) located in the Department of Geosciences at the University of Arizona. Results were corrected and normalized to reported values of the National Bureau of Standards NBS-981 lead standard (Galer and Abouchami, 1998). Prior to analysis all samples and standards were spiked with thallium (Tl) to achieve a Pb:Tl ratio of 10:1, and all results were corrected for mercury interference and normalized to Tl using an exponential law correction (Rehkämper and Mezger, 2000). The 2σ error associated with the NBS-981 standard over all analytical sessions ranges from 0.0011–0.0067 for 206Pb/204Pb, 0.0012–0.0070 for 207Pb/204Pb, and 0.0028–0.0190 for 208Pb/204Pb. Procedural blanks were measured periodically to determine background levels. In these blanks the amount of lead averaged between 100 and 300 pg (lead concentration 0.01–0.03 ppb).

3.4. Lead isotope analysis

4. Results

Two methods of sampling and preparation for isotopic analysis were used - the standard digestion and separation procedure, and a faster, less destructive surface swabbing method. All of the ALP glazes were processed by digestion and separation for analysis. A small sample of the glaze (approximately 5 mg) was removed and dissolved in 9:1 HF:HNO3, after which the solution was evaporated and refluxed subsequently with HCl, dried down again, and then taken up in HNO3 (all acids were doubled-distilled in Teflon stills in the Class 1 clean rooms in the Department of Geosciences, University of Arizona). The lead was separated using anion exchange columns with Eichrom Sr-spec resin following protocols established at the University of Arizona (Fenn et al., 2010). All samples were diluted to a concentration of 50 ppb prior to measurement. The remaining materials (DAP and Flora glazes, and all galena samples) were sampled using the swabbing method detailed in Thibodeau et al. (2013). The area to be sampled was first cleaned with a polyester-tipped swab dipped in twice-distilled 2% nitric acid. A small amount of lead was removed by rubbing a second acid-dipped swab on the cleaned area. The lead was removed from the swab by soaking it in twice-distilled 2% nitric acid, and the solute was diluted to a lead concentration of 50 ppb for analysis. This method has been successfully used in the analysis of lead minerals, with results showing that the isotopic ratios of samples prepared using the swabbing technique fall within the range of values obtained from the same materials prepared

4.1. Inferences from temper identification

between Ouray and Silverton, as these include galena ores with significant surface exposures that were likely available during the Pueblo I period. Samples were collected from numerous fragments at each location when possible, to ensure a thorough characterization of isotopic compositions from a single deposit. 3.3. Temper identification in potsherds

Petrographic analysis of 86 selected glaze-painted sherds from the ALP project identified two temper groups: (1) a temper dominated by single grains of quartz and feldspar (q-f) and a crushed rock (andesite/ diorite) temper (a/d) (Supplementary Table S2). These groups are consistent with previous studies of temper used in Upper San Juan ceramics (Allison, 1995; Wilson and Blinman, 1993). The most common temper found in the sample set, accounting for 98% of the sherds, is a quartz-feldspar temper. This temper is composed predominantly of single grains of angular to sub-angular quartz and feldspars (microcline and plagioclase), the latter often heavily altered to sericite or epidote, with minor mafic accessory minerals, mostly micas (both muscovite and biotite). Rock fragments in these sherds are rare, and are mostly from granite or granodiorite and sandstone; volcanic fragments are absent. The angularity and sorting of the minerals observed suggests that the temper was derived from crushed rocks. These observations are broadly consistent with the geology around Durango (Steven et al., 1974). Tertiary and Cretaceous sandstones and shales form Ridges Basin and Blue Mesa south of the town, while the Animas River drainage north of Durango cuts through Permian and Pennsylvanian arkose and sandstone, and winds around the West Needle massif of gneiss. This type of temper is consistent with the temper previously noted in Rosa ceramics in the Upper San Juan and 638

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suggests production in the Durango area. Two of the analyzed glaze-painted sherds are tempered with crushed intermediate igneous rocks. To maintain consistency with previous ceramic temper studies in the Upper San Juan, these are identified here as andesite/diorite, even though none are obviously of volcanic origin – they would be more accurately described as diorite. The lithic fragments are composed predominantly of angular to sub-angular plagioclase feldspars, and mafic minerals (mostly magnetite and clinopyroxene) occur in higher proportions than in the sherds tempered with quartz and feldspar. Quartz and alkali feldspars are scarce. This temper is consistent with the one commonly used in the Mesa Verde region, west of Durango, and these sherds therefore represent nonlocal products in the ALP ceramic assemblage. Potential sources of these tempers are the large plutons of Tertiary/Cretaceous (Laramide) intermediate igneous rocks in Sleeping Ute Mountain south of Cortez, and in the core of the La Plata Mountains. All of the fifteen DAP Rosa glaze sherds selected for this study are tempered with a crushed igneous rock temper, which is mineralogically and texturally consistent with our diorite temper class (Ceramics: Temporal-Spatial Dataset. 1988 (tDAR id: 6039); doi:10.6067/ XCV8TD9WNB). This temper accounts for 92% of the total glazepainted sherds from DAP (Waterworth, 1988). Significant differences in the abundance of the andesite/diorite temper between the ALP assemblage (2%) and the DAP assemblage (92%) confirm that this temper represents production outside of the Animas River valley. 4.2. Data summary and interpretations of Lead isotope ratios of upper San Juan glazes and galena The majority of the ALP glaze paints analyzed form a distinct cluster with ranges of 18.75–18.85 206Pb/204Pb, 15.61–15.64 207Pb/204Pb and 38.25–38.35 208Pb/204Pb (Fig. 3, Supplementary Table S2) with two tails towards more radiogenic values. The entire ALP glaze sample set, with the exception of one sherd, plot in the range of 18.75–19.15 206 Pb/204Pb. The data from the glazes of the Flora collection is consistent with the ALP data; this is expected as four of these bowls were collected from Blue Mesa in the ALP project area. The one bowl recovered east of Durango at Stollsteimer Mesa, near the Piedra River, also matches the major cluster of data points. The Pb isotopic ratios of glazes from the DAP collections all plot within, or very close, to the major cluster of points formed by the ALP data. The data from the DAP glazes, and the one specimen from Stollsteimer Mesa, indicate that the same source(s) of lead was used to produce the majority of lead glaze paints throughout the region, even though the temper data indicate at least two different loci of production. If there was a second source of lead glaze production in the Upper San Juan during the Pueblo I period, and the temper data certainly supports this, the potters were using the same lead ore source(s) as the potters in the Ridges Basin/Blue Mesa cluster. The Pb isotopic ratios of galena sampled from the ALP archaeological collections show similar distribution to that noted in the glazes, with four of the seven samples matching the major cluster of glaze paints (Fig. 3, Supplementary Table S3). This indicates that this cluster is not the result of mixing from multiple galena sources, but represents instead the preferred source of material of the potters. The one galena from the Dillard site, representing an earlier Basketmaker III occupation, also matches the major source of lead as the glaze paints. Lead glaze paints were not used, to present knowledge, during the Basketmaker III period, and the use(s) of galena at Dillard are unknown.

Fig. 3. Lead isotope ratios of Upper San Juan glaze paints and galena samples from archaeological sites.

to Durango, this is not surprising since galena is quite sparse in this district. Galena samples from the Rico district are quite distinct from La Plata and other western San Juan ores on the 208Pb/204Pb axis. One of the ALP glaze samples plots with galena from Rico; this particular glaze also demonstrated anomalous chemistry, with much higher zinc contents than other samples, thus further confirming a different source of ore (Santarelli, 2015). One ALP galena sample and the Flora galena sample are also consistent with the Pb isotopic signatures from the Rico district. These data suggest that the Durango inhabitants were obtaining some galena from Rico, although it was a minor source. This is likely due to the fact that galena tends to be intimately associated with other ore or gangue minerals in the Rico district, making it difficult to extract (Gonzales, 2015). The closest of the new samples that we analyzed to the glaze paint data are from Highland Mary's Mine (east of Silverton) and Tomboy Mine (east of Telluride). These deposits are associated with the Silverton volcanic caldera and are among the closest of the western San Juan Mountain sources to Durango (about 80 km away) (Fig. 4, Supplementary Table S4). The archaeological glaze paint data were also compared to published isotopic ratios of lead ores from the western San Juan Mountains

4.3. Identifying the sources of lead ore used in the production of glaze paints We can exclude the La Plata Mountains as a source of lead ore, as the reference samples from the Gold King and Bedrock Gulch mines have more radiogenic values than any of the archaeological samples. Even though the La Plata Mountains are the closest sources of lead ore 639

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Fig. 4. Lead isotope ratios of Upper San Juan glaze paints and galena samples from archaeological sites (grey circles), galena samples collected at various geologic sites (circles), and published Pb isotopic ratios for deposits in the Silverton, Lake City and Uncompahgre calderas (squares). *Data from Doe et al., 1979; **Data from Doe et al., 1979 and Sanford, 1992. Analytical errors are smaller than displayed symbols.

Deadman's Black-on-red (880–1100 CE) were recorded at site 5HN547. Ute Uncompahgre Brownware sherds, dating after 1000 CE were recovered from 5MN546 (Reed, 2008; Washburn and Reed, 2011). Our data suggests the same sources of galena were also used to produce the DAP glaze paints, and reinforces the strong preference for lead ores from this source. The location of a second area of production is still unconfirmed, but it is widely thought to be in the La Plata River valley (Fig. 1) where Morris (1939) reported finding glaze-painted pottery. As noted above, the lithic inclusions in the DAP sherds are of intermediate igneous rocks. We have followed the earlier literature in reporting these as “andesite/diorite,” an identification first made by Shepard; her exemplary description of the igneous inclusions in these pots from all periods (Shepard, 1939) makes then sound very similar to those observed in the ALP and DAP rock-tempered sherds. Shepard notes that the microstructures of these inclusions match those of cobbles in the bed of the La Plata River “carried down from the mountains to the north during an age of torrential conditions” (Shepard, 1939: 252). Although we have not yet had the opportunity to re-examine Shepard's thin sections, we provisionally accept that the “andesite/ diorite” is likely the same as that observed in the ALP and DAP sherds described above. Exploration of the high country must have begun before the manufacture of glaze paints in Pueblo I, as a galena sample with isotopic ratios matching the Galena District deposits was found at the Basketmaker III Dillard site west of Cortez, which is 130 km in a straight line away from them (Fig. 2). It is very likely that some of the lead deposits associated with the Silverton caldera were also exploited, as is suggested by the similarity of the isotopic ratios of a few of the glaze paints to galena samples from the Idarado-Black Bear vein. The southern half of the Western San Juan Mountains drains into the Animas River north of Silverton, which flows south through Durango into northwest New Mexico. At the peak of the last (Pleistocene) glaciation, the Animas valley was filled by a glacier that extended as far south as Durango. It is possible that galena-bearing rocks from mineral deposits in the Silverton caldera were pushed down the Animas River by this glacier, forming terminal moraines that may have included galena closer to the center of production of glaze paints in the Animas River valley. At least one of the galena ore specimens from the ALP archaeological collections is clearly a rolled cobble, which would support this possibility (unfortunately the swabs used to sample this galena did not yield enough lead for analysis, so we do not have isotopic ratios

(Doe et al., 1979; Foley and Ayuso, 1994; Hon et al., 1985; Sanford, 1992) (Fig. 4). Using the combined database of new analyses and published literature we are able to unequivocally identify the major source of the lead used in the production of Pueblo I glaze paints as originating in veins in the post-eruption fillings of the Lake City and Uncompahgre calderas, located between Ouray and Lake City (Doe et al., 1979; Sanford, 1992). The isotopic ratios of lead ores from the major cluster of glaze paints are a tight match to the Pb isotope ratios measured by Sanford (1992) for the former Galena District, which forms three groups of mines (the WG, CC and EG groups in Sanford, 1992, Table 1) above the north rim of the Lake City caldera, with the abandoned historic mining town of Capitol City (CC) at their center (Fig. 2). Almost all of the isotopic ratios in the tails to either side of this central cluster of archaeological glazes and galena samples fall within the distribution of Pb isotopic ratios of ore samples from the Uncompahgre, Silverton and Lake City calderas in the western San Juan Mountains. The Galena District deposits are located at altitudes from 2700 to 2850 m above sea level (asl), and in historic time have typically been covered by snow for at least five months each year. Although the straight-line distance from Durango (altitude: 2000 m asl) to Capitol City is about 100 km, human traffic would need to skirt around the rugged Needle Mountains by following the Animas River north to Silverton, then striking east along the north rim of the Lake City caldera. This increases the effective walking distance from Durango to the Galena District to around 150 km. Procuring ore from these San Juan deposits would clearly have required significant effort. All of the ore sources used in Pueblo I, except for Rico, lie above the altitude limit for growing corn, so there could have been no permanent settlement of Pueblo I agriculturalists there. Hinsdale County, Colorado, where the Lake City and Uncompahgre calderas are located has 171 recorded sites with prehistoric components. Only a small number of archaeological sites have been recorded close to the source used by most potters making Pueblo I glaze paint. Yet the area has not been widely surveyed so there is the possibility that there may be additional as yet unrecorded sites. There is also the possibility that sites have been erased due to the extensive mining that took place in the area in the late 1800s/early 1900s. Most of these sites are identified as open lithic scatters and campsites, with one (5HN510) yielding a Paleoindian spear point (Pitblado et al., 2007). “Black-onred” ceramic sherds, possibly Bluff Black-on-red (780–1000 CE) or 640

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(used from 1275 to ca.1700 CE) are all adjacent to the Rio Grande Valley of central New Mexico. The best known of these is Cerrillos Hills, located 30 km southwest of Santa Fe, which was a source for both galena and turquoise in the Pueblo IV period. The Cerrillos Hills are located 180 km from Pueblo Bonito and 250 km from Durango. Other galena sources that were exploited during the Pueblo IV period are Magdalena and Hansonburg, near modern Socorro in central New Mexico. These are about 240 km from Pueblo Bonito, and about 360 km from Durango (straight-line). The Pb isotopic signatures of galena from these sources are extensively characterized and matched to Pb isotopic ratios of Pueblo IV glaze paints (Habicht-Mauche et al., 2002, 2000; Huntley, 2008; Huntley et al., 2007; Thibodeau et al., 2013). The majority of the Pueblo Bonito galena (six of the nine samples) have very radiogenic 206Pb/204Pb values that match published isotopic ratios for lead ores from Hansonburg (Huntley et al., 2007; Stacey and Hedlund, 1983; Thibodeau et al., 2013). The source of one galena from Pueblo Bonito could not be positively identified, but its Pb isotope ratios are similar to published values from deposits in Box Canyon and Joyita Hills (Ewing, 1979; Thibodeau et al., 2013), located 70 km northwest of the Hansonburg deposits, suggesting a likely origin near Socorro. Interestingly, none of the Pueblo Bonito samples can be attributed to Cerrillos Hills, which was the most frequent source for galena used in lead paints in the Pueblo IV period. The Pb isotopic ratios of two of the galena samples from Pueblo Bonito match those of the lead used during the Pueblo I period, from deposits in the Lake City and Uncompahgre calderas in the Galena District, approximately 220 km away. One (H2835) comes from an early room in Pueblo Bonito (Room 6A), which is consistent with the idea that some people from the Durango area moved to Chaco Canyon (Wilshusen and Potter, 2010; Wilshusen and Van Dyke, 2006). The other (H4607A) comes from Room 32, adjacent to one with high status Northern Cluster burials. This particular galena was swabbed twice, and the swabs were processed and analyzed on two different days to ensure reproducibility in the data. 5. Discussion Shepard (1939) first brought to light the intentional production of lead glaze-painted pottery in the Upper San Juan, noting that lead ore was an ingredient in the paint. She suspected that the ore mineral was galena, which she said “is certainly the one to attract attention” (Shepard, 1939: 282). Our study is the first to investigate the provenance of the lead used in the production of Pueblo I glaze paints. Our results demonstrate that galena from the Lake City and Uncompahgre calderas, both in its mineral form and when incorporated into paint, had particular significance to Ancestral Pueblo people. The cultural significance of galena appears to have been established before the production of Pueblo I glaze-painted pottery, as evidenced by its recovery from the Dillard site. This site is an exceptional Basketmaker III village in the central Mesa Verde region with a great kiva that was built early in the history of the site, sometime between 600 and 650 CE (Ortman et al., 2016). The great kiva would have served as a focal point for incorporating new settlers into a new community and means of reinforcing community identity (Diederichs, 2016). The site survey results from around the Dillard site suggest that surrounding hamlets were established later and that over time this community center became more of a seasonal settlement than a fulltime village (Ortman et al., 2016). We cannot know how a piece of galena from the Galena District came to Dillard, or what significance was attributed to it, but its presence shows that at least some of these galena deposits were already known as pottery first began to be produced on the Colorado Plateau. In the Upper San Juan region, the Ridges Basin potters who made the earliest glaze-painted pottery in the Pueblo I period also showed a preference for the use of galena from this same source (150 km away), even though there were other sources of suitable galena closer to Ridges

Fig. 5. Comparison of lead isotope ratios of Upper San Juan glaze paints and archaeological galena samples and Pueblo Bonito galena samples. Analytical errors are smaller than displayed symbols.

for this particular sample). There is also a USGS record of an alluvial deposit (now underneath the town of Durango) listed as a minor historic producer of lead, under the name of Miller Mountain (https:// mrdata.usgs.gov/mrds/map). We have tried to find archived sources of lead from the Miller Mountain mine, so far without success. But no galena specimens from the Galena District – with which the major cluster of lead glazes is securely identified – could possibly have been pushed into the Animas River valley by glaciers; these galena samples could only have been procured by humans directly from the sources. 4.4. Sourcing of Pueblo Bonito galena The final aspect of this study was concerned with identifying the sources of galena found at Pueblo Bonito, in Chaco Canyon, New Mexico. All of these samples are attributed to the Pueblo II period, after the production of lead glaze paints had ceased. We compared the Pueblo Bonito data to our Pueblo I data from the Upper San Juan and to published Pb isotopic ratios of galena from ore deposits in New Mexico (Fig. 5, Supplementary Table S3). The deposits that were used during the Pueblo IV and Pueblo V periods in the production of glaze paints 641

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prehistoric use of this mining area although stone hammers found in adits provide undated evidence of exploitation (Eveleth, 2002). The presence of galena from the Hansonburg mining district in Pueblo Bonito suggests that some immigrants to Pueblo Bonito had ties to areas southeast of Chaco Canyon, and may have been ancestors of the potters who eventually began to make glaze-painted pottery at Zuni and elsewhere in the Northern Rio Grande area. They likely were bringing galena with them to Chaco Canyon that referenced a point on the landscape important to them even before the invention of Pueblo IV glazepainted pottery. More striking, however, are the two samples of galena whose Pb isotope ratios indicate that they originated from the same source of galena used in Pueblo I glaze-painted pottery made in the Upper San Juan. They came from initial construction at Pueblo Bonito, including Room 32 adjacent to the Northern Burial Cluster which represents an elite matriline that persisted between 800 and 1130 CE (Kennett et al., 2017). The earliest members of this matriline are likely the founders of Pueblo Bonito, considering the early dates for Burials 13 and 14 (Plog and Heitman, 2010). Room 32 has been described as a place of ritual retirement of collectively owned ritual goods likely used by Room 33 individuals (Mills and Walker, 2008). Could this powerful matriline have originated from the Upper San Juan? At the very least, the presence of galena from the Lake City and Uncompahgre calderas in Room 32 suggests that a group of immigrants from the Mesa Verde region, while not bringing much with them (Wilshusen, 2017), did bring ideas about how what worked and did not work to bring people into large villages and early great house communities. They also brought memories and mementos from a distant place on the landscape significant to their identity and their history, and which they wanted to reference in Chaco. A final factor to consider is that the sourced galena from Pueblo Bonito was derived from locations both north and south of Chaco Canyon. Core Puebloan ideas include (among other things) directionality. North/south and up/down were referenced in Chacoan architecture (Van Dyke, 2007) and these particular points on the landscape may be referencing the same. Bringing descendant communities into the conversation regarding the importance of the use and sources of the galena can shed additional light as to why Lake City and Uncompahgre calderas galena source in particular was so important.

Basin (Rico and Silverton calderas). It appears that potters with different cultural histories who formed these early aggregated settlements created a common community of practice around 750 CE by using galena to create transparent lead glazes, which were generally applied over black organic paints. They may have shared information about how to prepare, apply and melt these glaze paints with neighboring potters in the La Plata Valley, a possible second glaze paint pottery production area where a different temper source was used. Glazepainted ceramics produced using the same galena sources, but apparently made in the La Plata River valley based on temper identification, appear in the Dolores area in post 800 CE contexts when settlements on Ridges Basin were depopulated. Based on architectural, organizational and ceramic evidence, Wilshusen and Ortman (1999) and Wilshusen and Potter (2010) propose that at least some Upper San Juan inhabitants moved west and settled in the central Mesa Verde region. The large Pueblo I villages of the central Mesa Verde region flourished between 830 and 875 CE, but broke up between 875 and 910 CE. Population in the Mesa Verde region dropped dramatically in the tenth century, and most likely populations moved south and east towards or across the San Juan River, as there is a significant increase in residential sites and site densities in the Navajo Reservoir/Fruitland area and in the Piedra district between 875 and 925 CE. The presence of Rosa Black-onwhite ceramics in these areas, and the identification of a glaze-painted bowl with the same isotopic signature as the paints from Durango, lends support to cultural continuity (Chuipka, 2009b; Potter, 2010a). The descendants of these immigrant populations later appear to have contributed to the formation of the early great house communities centered around Chaco Canyon (Wilshusen, 2017; Wilshusen and Van Dyke, 2006). Galena from sources in the San Juan Mountains continued to appear into the Pueblo II period in Chaco Canyon, at Pueblo Bonito in particular, but the practice of decorating ceramics with lead glaze ceased by the mid-800s. Chaco Canyon gradually emerged as the social, political, economic and ritual center for ancestral Puebloans following the collapse of the early villages in the Mesa Verde region in the late ninth century and the resulting regional depopulation. It developed into the center of the Chaco regional system until about 1150 CE. Pueblo Bonito is thought to have dominated the Chacoan world at the time (Neitzel, 2003). The Chaco system has been extensively studied (Cordell et al., 2001; Heitman and Plog, 2015; Judge et al., 1989; Lekson, 2008, 2006; Mills, 2002; Van Dyke, 2009; Wilshusen, 2017). Our Pueblo Bonito galena results add to that existing large body of data. While the Pueblo Bonito galena sample is small (17 instances reported in the Chaco Research Archive) and their actual contexts are unclear (Pepper largely reported them to be in debris; Judd did not provide contexts), they are worthy of reflection and suggest additional avenues of research. The Pueblo Bonito galena in our sample set was mostly recovered in artifact rich rooms, suggesting that it (or the place it originated from) was possibly ritually significant to the people who used those rooms. The majority of the galena recovered from Pueblo Bonito originated in the north-central or western part of this great house in rooms constructed early in the history of the structure and where the two large burial clusters were found (Akins, 2003; Windes, 2003). Our sample included 9 of the 10 samples recovered from rooms in the north-central section (Supplementary Table S1). The samples from Pueblo Bonito with Pb isotopic signatures consistent with the Hansonburg mining district came from rooms constructed between 800 and 1100 CE. These samples are the earliest evidence yet found of exploitation of the Hansonburg source. With the second invention of lead glaze paints, around 1275 CE in the Silver Creek area of central Arizona (Fenn et al., 2006), lead minerals were imported from deposits adjacent to the Rio Grande valley in New Mexico, of which the Cerrillos Hills and the Hansonburg and Magdalena were the most favored. Galena from Hansonburg became the source of lead used in Zuni glazed pottery in the 1300s after the Cerrillos Hills source fell from favor (Huntley, 2008). Little is known about the

6. Conclusion This study traces the uses and sources of the galena from archaeological sites in southwestern Colorado and northwestern New Mexico between about 600 CE and 1150 CE. Using Pb isotopic ratios as tracers, we have shown that a single piece of galena from the Dillard site (ca. 600–650 CE, within the Basketmaker III period) derived from a set of lead sources at high altitudes (the former Galena District) near the modern town of Lake City in the San Juan Mountains of Colorado. We know from the reported find of a Paleoindian spear point near this lead ore source that humans had explored the high country long before the Basketmaker III period, but the galena sample from Dillard is, to our present knowledge, the earliest reported find of this mineral in the archaeological record of this region. Some of the earliest pottery in the entire southwestern USA was made in the Basketmaker III period, and within 150 years (at most) potters in two adjacent river valleys in southwestern Colorado were using galena (and perhaps other lead minerals) to decorate their pots, usually by melting a colorless lead-silicaalumina glaze over a dark organic underpaint (Santarelli, 2015). We have concentrated here upon the provenance of lead on the lead-glaze painted ceramics (Rosa black-on-white type) from sites in the Ridges Basin and Blue Mesa, near the modern town of Durango, and which are dated between 750 and 820 CE, within the Pueblo I period. Lead isotope ratios are consistent with the hypothesis that the main cluster of lead glazes correspond to the same set of sources – the Galena District near Lake City – as the Dillard galena. A small number of lead glazes appear 642

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References

to match other sources (Rico, Idarado), and it is very likely that other deposits in the western San Juan Mountains were exploited as well. Petrographic analysis of the bodies of almost all of these glazed sherds indicates that the temper is consistent with manufacture somewhere within the catchment of the Animas River near Durango, very likely within the Ridges Basin/Blue Mesa region itself. A second region of manufacture of Pueblo I lead-glazed Rosa pottery is indicated by two sherds from Ridges Basin, and by fifteen sherds from archaeological sites in the Dolores River valley, 60 km northwest of Ridges Basin. The lead in these glazes also came from the Galena District near Lake City, but the mineral temper in these potsherds is crushed diorite, the sources of which - as argued by Shepard some eighty years ago - are probably cobbles in the bed of the La Plata river, which runs south from the laccolithic intrusive complex of the La Plata Mountains and drains into the San Juan River in New Mexico. Her work suggests that this second region of manufacture is somewhere in the upper La Plata drainage, but this should be confirmed by comparing our thin sections from the Animas-La Plata and Dolores Archaeological Projects with Shepard's thin sections from sites excavated by Morris in the La Plata valley. In the ninth century CE the Upper San Juan was depopulated (Bellorado, 2013) and the use of lead glazes ceased. Our finding that two samples of galena in Pueblo Bonito, Chaco Canyon, also derive from the Galena District ore deposits near Lake City shows that these sources were still known in the tenth and eleventh centuries CE. When lead glaze paints were reinvented in the Pueblo IV period, the sources of lead in the western San Juan Mountains appear to have been forgotten. This is supported by the fact that none of the hundreds of lead glazed Pueblo IV sherds for which Pb isotopic ratios have been reported match those of galena from these Colorado sources (Fenn et al., 2010; HabichtMauche et al., 2000; Huntley et al., 2007). This study provides a robust beginning to understand Pueblo I glazepaint pottery and the cultural significance of galena to some Ancestral Pueblo people. Additional areas of study are important to an even greater understanding: sourcing the lead in other glaze paint production areas in the Upper San Juan, particularly the Navajo Reservoir/ Fruitland, Chimney Rock and Gallina areas, and conducting Pb isotopic studies on the remaining galena from Pueblo Bonito and that recovered at Aztec Ruin, established after the demise of Chaco.

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Acknowledgements This work was supported by grants from the National Science Foundation (grant number BCS-1419233) and the University of Arizona (Graduate and Professional Student Council, grant number R-206) awarded to the first author, and from a State Historical Fund Grant (grant number 2015-01-011) through History Colorado awarded to Crow Canyon Archaeological Center. We thank Bridget Ambler at the Canyons of the Ancients Visitor Center and Museum, Mike Jacobs at the Arizona State Museum, Kristen Mable at the American Museum of Natural History, Lori Reed at Aztec Ruins National Monument, Susan Ryan at Crow Canyon Archaeological Center, Stefan Nicolescu at the Yale Peabody Museum of Natural History, and K.D. Rohrer at the Telluride Historical Museum for providing the samples analyzed as part of this research. Thank you to Stephanie Martin for her help with Fig. 1. We thank Joaquin Ruiz for granting access to his laboratory facilities at the University of Arizona and Mark Baker and Tom Fenn for training and technical assistance during the isotopic analysis. We are grateful to Richard Wilshusen and Ben Bellorado for providing editorial comments on earlier drafts, and thank the two anonymous reviewers for their helpful comments, which helped to improve the manuscript. Appendix A. Supplementary data Supplementary data to this article can be found online at https:// doi.org/10.1016/j.jasrep.2018.11.027. 643

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