k F LIBRARY "Wilson State I University J L ‘0 ‘1 —— fl PLACE IN RETURN BOX to remove this checkout from your record. TO AVOID FINES return on or before date due. DATE DUE DATE DUE DATE DUE fl i _______1 Lg; rim, MSU Is An Affirmative Action/Equal Opportunity Inmnmion cmma-oi Comp Composition Analysis of the O'Neil Site Ceramics: A Study of Raw Material Use in Northwestern Lower Michigan By Janet Stouffer Dunn A THESIS Submitted to Michigan State University in partial fulfillment of the requirements for the degree of MASTER OF ARTS Department of Anthropology 1992 Con JJl/_ '. I, 5 ’1' 0")" 0 ABSTRACT Composition Analysis of the O'Neil Site Ceramics: A Study of Raw Material Use in Northwestern Lower Michigan By Janet Stouffer Dunn In this study the chemical compositions of prehistoric ceramic vessels from the O'Neil Site of northwestern lower Michigan were determined by Instrumental Neutron Activation Analysis (INAA) in order to test whether the residential patterns noted during and after excavation were apparent in the pottery paste. A secondary purpose was to determine whether an intensive sampling and analysis of pottery from a single intermittently occupied site could provide meaningful information about the behavior of the prehistoric inhabitants of the Upper Great Lakes. The results of the analyses of pottery and clay samples from the O'Neil Site, as well as clay and temper samples from the nearby Skegemog Point Site, suggest that simple relationships between raw clays and prehistoric pottery in the Great Lakes do not exist. Several possible explanations for this are considered, and the need for additional information regarding the composition of geologic clays and archaeologically—derived clays is discussed. Copyright by JANET STOUFFER DUNN 1992 As with mos of many individu: chair, William A‘ m Cornplcu'on in When, Kcnne PM)» aft cvider iIISU'umcnm role at the Michigan 5 Ofcrifical i mm“ by Edv Memorial Phoer Mam“ for Res PYOjCCt, who C(x The may: Michigan Menu ACKNOWLEDGEMENTS As with most research projects, this one has benefitted from the input and assistance of many individuals. Foremost among these has been my advisor and thesis committee chair, William A. Lovis, Jr., Ph.D., who not only guided this research, but also facilitated its completion in many ways. In addition, the contributions of the other committee members, Kenneth E. Lewis, Ph.D., Helen P. Pollard, Ph.D., and Norman J. Sauer, Ph.D., are evident throughout this thesis. Michael Hambacher, Ph.D. also played an instrumental role by kindly re-typing all of the known vessels in the O'Neil Site collection at the Michigan State University Museum. Of critical importance to the completion of this study was the technical support provided by Edward A. Birdsall, Engineering Technician, Nuclear Reactor, Michigan Memorial Phoenix Project. His assistance was facilitated by Philip A. Simpson, Assistant Manager for Research Support Activities, Nuclear Reactor, Michigan Memorial Phoenix Project, who coordinated the analysis at the reactor. The analysis of the samples by INAA was performed with funds provided to the Michigan Memorial Phoenix Project, University of Michigan by the U.S. Department of Energy under a reactor sharing grant. Supplies used in the course of the analysis were purchased with funds made available by the Michigan State University Museum, Anthropology Division. Thomas A. Vogel, Ph.D., Department of Geological Sciences, Michigan State University, and Randall Schaetzl, Ph.D., Geography Department, Michigan State University, graciously reviewed the initial results of the analysis and made useful suggestions for further investigations. Kathy Welch, of the Center for Statistical Consultation and Research, University of Michigan, provided assistance with the use of the iv S YSTAT staistical Several frienc Michigan have hci; Minim-Davigv R program also mad: “13 presentation. My. and en“mgmlent of SYSTAT statistical program Several friends and colleagues at the Reproductive Sciences Program, University of Michigan have helped me with their expertise and advice. Among these are Holly Anderson-Davis, Ruth Lum, and Michael Muha. The administrative personnel of this program also made available to me their computers and software for statistical analysis and data presentation. Finally, and most importantly, this research was helped by the quiet support and encouragement of my husband, John David Dunn. For this support I am ever grateful. List of Tables List of Figures Introduction Background Dcscriptior Descfiptior Experimental EXperimel HYPOIhesc Sample Colleen, 33mph“! Method TABLE OF CONTENTS Page List of Tables . ........................................................................... viii List of Figures ........................................................................... ix Introduction ............................................................................... 1 Background . .............................................................................. 2 Description of Problem ............................................................. 2 Description of Site ................................................................... 7 Experimental Approach and Hypotheses ........................................ 15 Experimental Approach .............................................................. 15 Hypotheses and Assumptions ...................................................... 15 Sample ...................................................................................... 19 Collection . ............................................................................ 19 Sampling Procedure ................................................................. 28 Method . ..................................................................................... 38 Sample Preparation .................................................................. 38 Analytical Approach ................................................................. 44 Results ...................................................................................... 48 Data Evaluation ....................................................................... 48 Data Analysis . ........................................................................ 52 Summary of Data . .................................................................... 72 Validity of Hypotheses .............................................................. 79 Summary ................................................................................... 82 Errors in Original Assumptions .................................................... 82 Significance of Results .............................................................. 90 vi Future Dir Notes ............ Appendix A Concentratii Appendix B Concentrat Appendix C Concentrat Appendix D Centroid 1 Appendix E K‘means ADDendix F Elements TABLE OF CONTENTS (cont'd) Future Directions ..................................................................... Appendix A Concentration and Standard Deviation Results (All Elements) ................. Appendix B Concentration and Standard Deviation Results (11 Elements) .................. Appendix C Concentration Values for 11 Elements, in Increasing Order .................... Appendix D Centroid Linkage Dendrograms Using 10 of 11 Elements ...................... Appendix E K-means Clusters Using 11 Elements ............................................. Appendix F Elements Detected by INAA and Used in Pottery Paste Analyses .............. References eeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeee 93 95 98 130 138 144 155 172 177 Table l - Vessel. Table 2 . Vesse Table 3 - Sherd j Table 4 - INA} Table 5 - COHCer Table 6 - 51mg} Table 7 . Concem DUPIiC: Table 8 ‘ Multi; Table 9 . Mean LIST OF TABLES Page Table l - Vessels From the O'Neil Site (20CX18) ....................................... 20 Table 2 - Vessels and Sherd Information .................................................. 22-25 Table 3 - Sherd Provenience and Sampling Information ................................ 29—35 Table 4 - INAA Batch Information ......................................................... 39-41 Table 5 - Concentration of Elements in NBS Standard 1633a .......................... 43 Table 6 - Energy Lines and Half-Lives Used in Calculations ............................ 47 Table 7 - Concentration and Ratios of Selected Elements From Duplicate Samples ................................................................. 61 Table 8 - Multiple Samples Taken From Single Vessels ................................. 67 Table 9 - Mean Iron Concentrations, in Increasing Order ............................... 89 Figure 1 . Map HEW: Z - Ma; Figure 3 - O'Ne Figure 4 - Cenm Figurc 5 _ Sche Figure 6 _ Sch: am 7 _ le Figure 8 - pk“ HERE 9 . p10, Fig“ 10 - P14 LIST OF FIGURES Page Figure 1 - Map Showing Location of O'Neil Site ....................................... 8 Figure 2 - Map of O'Neil Site .............................................................. 9 Figure 3 - O'Neil Site Showing Areas A and B ......................................... 10 Figure 4 - Centroid Linkage Dendrogram Using 11 Elements ......................... 53 Figure 5 - Schematic Dendrogram of Groups 1-6 ....................................... 55 Figure 6 - Schematic Dendrogram of Group 1 ........................................... 57 Figure 7 - Plots of Ratios for Samples 8-10 .............................................. 62 Figure 8 - Plots of Ratios for Samples 53-54 ............................................. 63 Figure 9 - Plots of Ratios for Samples 23-25 ............................................. 64 Figure 10 - Plots of Ratios for Samples 33-36 ........................................... 66 INTRODUCTION For archaeologists the study of behavior involves extracting information from the remainsofmaterialculture. 'I'niscanbeaccomplishedbyexaminingpattemsofartifacts and land use at archaeological sites, or by intensively extracting information from individualartifactsa'groupsofartifacts. Inthisstudythelatterapproachismkeninan attempt to discern patterns of behavior relating to the manufacture, use, and discard of pottery vessels, and the relationship of this behavior to raw material (clay) acquisition in the early and late Late Woodland periods in northwestern lower Michigan. Clay and pottery samples from the O'Neil Site, a stratified Late Woodland through prouohistoric occupation site, as well as additional samples from a nearby site, were analyzed compositionally in an attempt to discern whether habitation patterns at the site could be seen in the concentrations of elements in the pottery samples. Intensive within- siteelemental analysesofpotteryfromsingle sitesintheUpperGreatLakes have notbeen previously performed. Hence this investigation was undertaken in part to determine whether such an intra-site analysis could provide information about the use of clay resources within a small region. The results ofthis study indicate that compositional analyses ofpottery are far more complex than originally believed. Not only do the individual components of pottery paste (clay and temper) each contribute to the analytical results, but the natural variability of the clay and tempering material also appear to affect the results. These factors may have little impact on the outcomes of larger regional studies where the variability of raw materials between regions may be far greater than that within the region. But for the analysis of pottery and clay collected from closely-spaced sites, the natural range of variation of the mwmatefialsusedmmanufacnnemepomerybccomesaucialmthemtapmmdonofme results. Likewise, the effects of mixing varying amounts of clay and temper to produce the final paste must be considered. These factors are detailed in the following sections with the hope that future analyses of pottery paste will address these concerns. 1 BACKGROUND Description of Problem The interaction of human populations and the environments in which they find themselves has recently been the subject of much anthropological study (e.g. Orlove 1980; Vayda and McCay 1975; Moran 1979). In the Great Lakes this interest in the ecological approach has often been reflected in archaeological studies dealing with food resources and the carrying capacity of certain environments (Cleland 1966; Yarnell 1964). The emphasis on food availability, procurement, preparation and storage is in large part a reflection of the importance of food procurement in prehistory. However, it also reflects the relative abundance of food-related artifacts in archaeological sites in the Upper Great Lakes region, where projectile points, animal bone, floral remains, and in later sites, ceramic materials dominate the prehistoric artifact assemblages of this region (Fitting 1975; Griffin 1983). Non-food resources utilized by prehistoric hunter-gatherer groups have also been the focus of research in the Great Lakes area. Predominant among these are studies of the availability, acquisition and use of chert (e.g. Ellis 1969; Luedtke 197 6; Wahla 1981) which was fashioned into projectile points, knives, scrapers and other tools (Frtting 1975). Others have addressed the role of exotic materials in the material culture of the Great Lakes Indians, and the importance of trade in the social and economic networks in prehistory (e.g. Griffin 1983; Brose, er al. 1985). Only recently have the "everyday" utilitarian items such as clay cooking and storage vessels been examined in terms of resource utilization. Although the prehistoric pottery of the Great Lakes has long been examined on stylistic grounds in an attempt to establish regional chronologies, to define cultural groups, and to identify spheres of social interaction, only in recent years has the chemical composition of the pottery vessels been the subject of serious inquiry (Trigger, er al. 1980; Clark 1991). In part, this stems from the inability, until recently, to analyze clays for minute traces of elements which might 2 individual occupa whenever vessels COiflCidcnt Howe allliyses of pom in the analysis of The study fittest Pottery: 3 distinguish one clay source from another. It also results from the unstated assumption that where clayisubiquitous —-asitisinMichiganandotherareaswithan abundanceof glacial deposits (Dorr and Eschman 1977: 134) -- pottery-making took place in siru at individualoccupation locales. Ithasbeen assumedthatpottersmanufactmed theirwares whenever vessels were mded, and in areas where habitation sites and clay sources were coincident. However, recent interest in regional studies, as well as successful elemental analyses of pottery and other artifacts throughout the world. have have spin-red an interest intheanalysisofdreseculturalmaterials. The study of pottery floor the standpoint of resource utilization is of particular interest. Pottery first made its appearance in the Upper Great Lakes region in the Early Woodland period, or around 600 BC. (Fitting 1973; Griffin 1983), and is found in nearly all Woodland sites in Michigan (Fitting 1975). Therefore, the presence of prehistoric pottery in Michigan spans a period of at least 2,000 years. Together these factors permit pottery sherds to be studied extensively over time and space, or intensively at a single location or for a single period in prehistory. In addition pottery vessels can have fairly short use-lives. It is assumed that since the prehistoric pottery of the Upper Great Lakes was heavy and prone to breakage, it was probably used for short periods of time before being discarded. In fact, the pottery sherds found in archaeological sites are likely to reflect relatively short periods in the lifetimes of the potters who manufactured them. As such, the study of pottery paste composition can provide a snapshot of time, preserving in the ceramic matrix evidence of behaviors relating to raw material acquisition and its modification into domestic implements. Although pottery vessels were used extensively in the Great Lakes region throughout prehistory, in the seventeenth and eighteenth centuries European metal kettles began to replace pottery vessels in most Native American communities of this region (Kinietz 1965), largely because the metal kettles were more durable and better able to withstand the direct heat of cooking fires (Holman and Egan 1985: 63). Because metal kettles so quick sought for prom. manuacmnng 0 Which each vessr Indians. Howeve as from analog south wesrcm U is made from cl Without m: be of the South“ 4 kettles so quickly replaced pottery vessels, little is known about the types of raw material sought for pottery-making. the people who took part in the procurement, preparation, or manufacturing of the vessels, the method of pottery manufacture, the specific use(s) to whicheachvesselwasputorthesignificanceofpotteryintheculnneoftheGreatLakes Indians. However, some information can be gleaned from the artifacts themselves, as well as from analogy with the pottery-making processes of the native porters of the southwestern United States. We know, for example, that pottery in the Upper Great Lakes ismadefromclayandatcmperingmaterialsuchasgrit. Itwasfiredatlowtemperatures, without the benefit of kilns, resulting in a somewhat hard but brittle ware. Like the pottery of the Southwest (Bunzel 1972), Great Lakes pottery is believed to have been made by women. A unique 17th Century description of pottery making among the Huron by the French explorer Sagard supports this assertion: But as for our Huron and other peoples and sedentary nations, they had (and they still have) the usage and the skill of making earthen pots, that they bake on their hearth; these are very good and never break in the fire, even though there is no water in them; but yet they cannot withstand humidity or cold water for long without softening and breaking at the least blow that is given them, otherwise they last a very long time. The Indian women make them, taking suitable earth, which they clean and knead very well, mixing in it a little sandstone [as a tempering material], then the mass being reduced to a ball, they make a hole in it with the fist, which they enlarge continuously while heating it inside with a little wooden paddle, as much and as long as is necessary to complete them; these pots are made without feet and without handles and are entirely round like a ball, except the mouth which projects out a little (Kinietz 1965: 47). However, the prehistoric pottery of the Upper Great Lakes differs from that of the Southwest in its construction and decoration. Prehistoric pottery of the Southwest was made by the coiling technique, and was frequently decorated with painted designs (Bunzel 1965). The late prehistoric pottery of the Great Lakes, on the other hand, was prepared with a paddle-and-anvil technique (Kinietz 1965), and was decorated only with incisions and other markir other rrraterial to Althougl lakes region is r ”exchanged" bot Brashler 1981). adjacent and me The anal dealing with pot ComPOSiIiOn of } grounds. On at 31%, Which in . 5 and other markings which altered the surface of the pot, but which did not add pigment or othermaterialtothe surfaceofthevessel. AlthoughthemleofponeryintheprehistoricexchangenetworksoftheGreat Lakes region is not well understood, certain elements have been shown to have been "exchang " both within and between groups (see for example, Trigger, er a1. 1980; Brashler 1981). In this way pottery styles have served as markers of interaction between adjacent and more distant groups of people in prehistory. Theanalysisofponerypasteaddsanodra'dimensiontothelargebodyofdata dealing with pottery structure and decoration. The determination of the chemical composition of pottery matrices makes possible the comparison of vessels on non-stylistic grounds. On a regional scale, this permits the assessment of clay and pottery fiom various areas, which in turn can provide information about the movement of clay, pottery, or porters throughout the area of study. This process has been successfully used in the Near East (Bieber er al. 1976; Gunneweg and Mommsen 1990; Hancock, er a1. 1989) and in parts of Mesoamerica (Arnold, er al. 1991; Mine, er al. 1989; Olin and Blackman 1989), but its use in the Great Lakes area is rare. Trigger and colleagues (1980) used X-ray Fluorescence to compare the pottery of sixteen Iroquois village sites in Ontario. The data thus obtained suggest that the transporting of pets from one village to another may account for the presence of stylistically foreign vessels at certain sites. Further analysis indicated that intra-site patterning at the household level may reveal itself in the composition of ceramic vessels. More recently Clark (1991) examined the analytical results of Instrumental Neutron Activation Analysis (INAA) of pottery and clay samples fiom over 30 late Late Woodland sites in the Lake Superior region. His results imply two patterns of cultural interaction within the Lake Superior basin. One of these involves the transfer of finished pots throughout the region by exchange a importation. The other involves the local manufacture of pottery of a particular style in various regions of the study area, implying either the mover (Clark 1991). Work or Great Lakes re g within-site corn mm the inter northern Michig Whether popula Vessels locally 1 mt Vcssels mag mmfm vair Michigam as w populadons_ A Seco; cOultl be Used a hat/e SquSSt-u. 6 either the movement of potters or the transfer of information over large geographic areas (Clark 1991). Work on ceramic composition analysis on a more local level is nearly absent in the Great Lakes region. Although the analysis by Trigger, er al. (1980) consisted in part of within-sitecompafisonsnootherwa'kofthisnamreislmown forthisarea. Forthis reason, the intensive sampling and analysis of pottery fiom a single semi-stratified site in northernMichiganwastmdertaken. 'I‘hebroadgoalsoftheprojectweretodetermine whetherpopulationsresiding atthe siteon a seasonal basis manufacturedtheirpottery vessels locally fiom nearby clays, and whether these vessels could be differentiamd from the vessels made by short-term occupants of the site. The results of this analysis could therefore provide information regarding the nature of resource (clay) utilization in northern Michigan, as well as data related to the movement and settlement patterns of prehistoric populations. A secondary purpose of the project was to test whether this method of analysis could be used at the site level in the Upper Great Lakes area. Studies of paste composition have successfully been performed on materials derived fiom state level societies (for example in Mesoamerica and the Near East), whose populations are relatively sedentary and whose resource bases are well-defined. Paste composition has also provided information of a regional nature on artifacts fiom band-level societies. However, assays of pottery from a single site occupied by hunter-gatherers involved in seasonal migrations have not been performed in this region. The results of an intensive intra-site sampling and analysis program would therefore provide data regarding the variability in the paste composition of vessels found at a single site. It would also prove useful in determining whether, based on such variability, single vessels from one site could be considered representative of the pottery from that site in larger regional studies of paste composition. Description i The site ct site excavated by ; Afllhmpology in l I Called "Traverse C Southern pom tr PM from both t 551765 as an ldtal S} and its manufacmrg The O'Neil MW in Charlevo; archamlogieal invc mood Creek. Ex: Description of Site The site chosen for this analysis was the O'Neil Site (20CX18), a partially stratified site excavated by crews fiom the Michigan State University Museum, Division of Anthropology in 1969 and 1971. The site lies along the shore of Lake Michigan in the so- called "Traverse Corridor" (Levis 1973), midway between the loci of the Northern and Southern pottery auditions of northwestern Lower Michigan. Because the site contained pottery from both traditions, each of which spans the Late Woodland cultural sequence, it serves as an ideal site for posing questions of behavior centered around clay procurement anditsmanufacnrreintopotteryduringthelateWoodlandperiod. The O'Neil Site is located in the NE quarter of the SE quarter of Section 7, T 33 N, R 9 W in Charlevoix County, Michigan (Lovis 1973) (see Figure 1). At the time of the archaeological investigation, the site was located on an active beach dune near the mouth of Inwood Creek. Excavations at the site uncovered a partially-stratified Late Woodland village site which contained ceramics, lithic material, bone and charred wood from the early and late phases of the Late Woodland period, as well as some ceramics and European trade items dating to the early historic period (Lovis 1973, 1991). Preceding the initial excavation of the site, the area to be investigated was sectioned off into ten-foot by ten -foot excavation units designated by unique unit numbers (see Figures 2 and 3) which are retained in the catalogue numbers of the artifacts. Initial work at the site revealed that most of the human activity occurred in one region of the site, which was further subdivided into Areas A and B on the basis of the degree of stratification noted during the excavations (see Figures 2 and 3). Area A was the mac deeply-stratified area of the site and was overlain by a layer of loose, wind-blown sand up to 0.5 feet thick. Beneath this was a humic zone of deep grey loamy sands 0.3-1.0 feet thick, which was designated Occupation Zone 1. Aboriginal materials and European //// , // , / / (After Levis 1973: Figure 5) Figure l - Map Showing Location of O'Neil Site 35 .ezb .e .52 . N 2:3... W110 N330 “'90 Wu; \ 10 N360 W110 N330W90 W112 5 N430E0 El/2 E Z I AREAB N390W20 5’— E112 nssowzo ‘— E112 N370W20 5—— am Nsrsowzo <—E&Wl/2 N340 W20 E 1/2 Figure 3 - O'Neil Site Showing Areas A and B (After LOVE n.d.) 11 trade goods dating to the late Seventeenth and early Eighteenth Centtnies were recovered form this zone. In the eastern parts of Area A an additional level could be discerned. It was designated Occupation Zone 1b, and consisted of a light grey sand zone extending to 1.0 feet below the humus zone, with a sand lens separating the two zones. Immediately below the first occupation zone was a layer of sand devoid of cultural material, followed by alensofblackerganic material. Thisblacklenscontainedcultm'al materialandwas designated Occupation Zone II. Beneath this zone was a thick layer of water-lain sands containing black laminae. Carbon-14 analysis of carbonized organic materials incorporated into these sands provided a date of 905 i 115 B.P., corrected to AD. 1073-1155 (N- 1268). This date is not compatible with the dates obtained for the underlying occupation zone, and is thought to be caused by foreign materials introduced into the site during the deposition of the lacustrine sands (Levis 1973: 24—34, 1991: 196-7). The basal occupation level in Area A, which ranges in thickness from 0.05 to 0.3 feet, represents an intensive use of the site by Late Woodland period peoples. This level, designated as Occupation Zone III, consists of a series of thin, grey-black sand layers whose individual lenses were not possible to isolate. Two 14C dates, both of which were compatible with associated cultural materials, were obtained from charred wood remains collected from a hearth. These organic materials yielded dates of 740 :t: 100 B.P., corrected to AD. 1277 (M-2406) and 670 :l: 100 B.P., corrected to AD. 1283 (M-2405) (Levis 1973: 34, I991: 196). The stratigraphy of Area B is less complex, and is roughly the same as the upper portions of Area A. This area was overlain by tan, wind-blown sands, under which lay a dark grey loamy zone. Beneath the learn was an occupation zone consisting of black sands. This zone yielded a 14c date of 430 :l: 100 B.P., corrected to AD. 1441 (M- 2398), for carbon associawd with a hearth designated as Feature 8. Based on the refitting of sherds from this level and Occupation Zone 11 of Area A, it is thought that the occupation 12 zoneofAreaB maycorrespond totheintermediateoccupation zoneofAreaA (Lovis 1971: 35-39, 1991: 197). Underlying the occupation zone of Area B were basal yelow-tan sands. Material for a 14c analysis was obtained from Feature 3, a hearth which was intrusive into this level. The date obtained for this material was 1000 1:140 B.P.(M2401), corrected to AD. 1004-1019, which was compatible with the materials found nearby in the occupation zone of Area B (Lovis 1973: 35-39, 1991: 197). In addition to the excavations of Areas A and B, a series of test pits were also dug to the northeast and southwest of the major occupation area (Lovis 1973) (see Figure 2). The depositional and occupational history of the site is one of dune formation through wind-blown and water-lain sand, interspersed by depositions of cultural materials. It is thought (Lovis 1973, 1991) that by AD. 1000, parts of Area B were stable, and that afterthistimeoccupationstookplaceinAreaB andpartsofAreaA. Some timepriorto A.D. lZWfinthasmbflizafionofAmaAoccmredleadingtotheoccupationofthisareaas well as of Area B. This was followed by the inundation of Area A and the deposition of water-bome sands; during this phase no occupations took place in Area A. Subsequently there was a limited occupation of Area A, after which the area was covered by wind-blown sands. By the fifteenth century, Areas A and B had become somewhat stabilized, and were re-occupied. Further wind activity precluded the complete stabilization and formation of discrete layers of occupation. The later occupations of the site in the ensuing years, along with the deposition of sand and organic material, covered the site with a modern sand loam. The final stabilization of Area A occurred in the late seventeenth and early eighteenth centuries, when groups of historic Native Americans visited the site (Lovis 1973: 39-40, 1991: 197-9). Throughout its occupational history, the site was inhabited on a seasonal basis (probably dtu'ing the warm season) for varying lengths of time. No evidence of permanent, year-round habitations were recovered at the site (Lovis 197 3, 1991). 13 Theceramic assemblagefromthesiteoonsistsofpotteryfromtheearlyandlate LateWoodlandperiod. 'I'heearlylateWoodlandis characterized by Mackinac Ware vessels and by Skegemog Ware vessels; the late Late Woodland is represenwd by Juntunen Ware pottery as well as by Traverse Ware vessels (Lovis 1971). The Mackinac and Juntunen Wares represent wares whose styles reflect the Northern pottery tradition of upper Michigan. The type site for these wares is the Juntunen Site, located on Bois Blanc Island in the Straits of Mackinac (McPherron 1967). The Southern pottery tradition is illustrated at the O'Neil site by the Skegemog and Traverse Wares, both of which were named for pottery found at the Skegemog Point Site in Grand Traverse County, Michigan (Hambacher 1992). A recent re-analysis of the O'Neil Site artifacts from a spatial point of view (Lovis 1991) indicates that the site was occupied in two different ways. The occupations of the site by groups manufacturing Mackinac, Juntunen and Traverse Ware pottery consisted of residential, or long-term habitations containing areas related to domestic and/or core- reduction activities. The occupations of the site by groups using Skegemog Ware vessels, on the other hand, are characterized by "logistic," or extractive camps. Although all of groups are thought to have visited the site in part to collect chert from the nearby Pi-wan- go—ning Quarry, the groups responsible for the Skegemog Ware sherds at the O'Neil Site were thought to have stayed at this site only long enough to extract the chert and to perform some basic core-reduction activities. The other occupations of the site are believed to have been longer in duration and are thought to have encompassed more activities than the Skegemog occupations. Furthermore, it is presumed that dming the Mackinac, Juntunen and Traverse occupations, the site would have been utilized by more diverse groups of individuals, probably representing family groups rather than age- and gender-specific groups which most likely utilized the site during the logistic forays (Lovis 1991). Because the two difi‘erent forms of occupation correspond to different pottery types, this site is ideal for examining the relationship between residency and pottery mnufacnring lx'l potta'y traditiom cxamintd from it pmwidcs the motel rtlitivcly small n: Sampling of the pl set of Salnplcs for and Utilization 14 manufacturing behavior. In addition, the presence of four ceramic types representing two pottery traditions as well as two time periods permits the paste composition results to be examined from several points of reference. Also, the presence of raw clays at the site provides the necessary baseline against which to compare the pottery samples. Finally, the relatively small number of identifiable vessels found at the site permits the intensive sampling of the pottery vessels from this site. In short, the O'Neil Site provides an ideal set of samples for examining, within one site, the relationship between clay procurement and utilization. l EXPE Experiment The anal} Itsidcnce and the This method is ca 53mph mmix. It dim a large nut die identified ves Chm“ a“Elysis it Widens of Hypotheses PRVious two different wa Trims: and In Marion ( rtPitts flit Sit: {01, Stay EXPERIMENTAL APPROACH AND HYPOTHESES Experimental Approach The analytical method chosen for exploring the relationship between population residence and the use of resources was Instrumental Neutron Activation Analysis (INAA). 'I'hismethodiscapableofdetectingandquantifyingasmanyasSOdifi‘erentelementsinthe samplematrix. Italsocombineseaseofanalysiswith analyticalaccm'acyandtheabilityto detect a large number of elements nearly simultaneously. Using this method, a majority of the identified vessels from the O'Neil Site were analyzed and the data were subjected to cluster analysis in order to determine the statistical groupings based on the elemental compositions of the samples. Hypotheses and Assumptions Previous work at the O'Neil Site (Lovis 1991) suggested that the site was utilized in two difi'erent ways: as a seasonally-occupied residential site (represented by the Mackinac, Traverse and Juntunen pottery), and as a ”logistic" occupation of considerable shorter duration (represented by the Skegemog pottery). This suggests that the people who utilized thesiteforseasonalhabitationusedmostoralloftheresourcesavailabletothematornear the site, including local clays. During shorter "logistic" occupations, however, it is expected that a more selective use of resom‘ces would have occurred, and that any clay vessels used at the site would have been manufactured elsewhere and brought to the site as needed. Further, this pattern is expected to have remained the same for potters of different pottery traditions throughout the Late Woodland period. These suppositions can be re- stated as follows: Groups occupying the site for long periods of time (residential occupants) would have manufactured their pottery locally from locally-obtained clays 15 16 and temper, while short-term occupants (logistic occupants) would not have made their pottery locally, but would have brought them to the O'Neil Site fiom other locations. Residential occupants of the site at any point in the Late Woodland period would have made their pottery locally, while logistic occupants during any sub-phase of the Late Woodland would have made their pottery elsewhere. This difi‘erential pattern ofpottery-making based on the use ofthe site is discernible in the chemical composition of ceramic pastes. In addition, several assumptions about the nature of the materials to be analyzed, as well as presumptions about the behavior of the prehistoric potters are necessary. The first is that local and non-local clays are compositionally different fiom each other, permitting differentiation between local and non-local pottery. Although this assumption seems obvious, in fact it has not been tested for small areas (less than 100 mile radius) in the Upper Great Lakes area. For this reason, clays collected during archaeological excavations of the O'Neil Site and the nearby Skegemog Point Site, a Late Woodland occupation situated along Lake Skegemog about 40 miles to the southwest of the O'Neil Site (Hambacher 1992), were analyzed by INAA in order to determine the relative differences in the composition of clay fiom a nearby site. The second assumption is that the clays collected during the archaeological excavations are representative of the clays used to manufacture prehistoric pottery vessels. Thisassumesthat: 1)theclaysom'cesremainedthesametluoughouttheLateWoodland period, and were not exhausted during this time, and 2) the clay deposits within the procmementareaofaparticularsite wereusedin the samemannerandtothe sameextent throughout the Late Woodland period. It further assumes that the clays collected at the O'Neil Site and the Skegemog Point Site are native to these respective areas, and were not simply brought to the site and discarded there. In spite of these assumptions, it is believed that the use of archaeological clays from the sites more truly represents the actual composition of the clays used in the manufacture of Late Woodland pottery, since these clays would hit: manufacture. about the manufa waltriscomrnon the composition c Clements to the p: ”31- These assur 1973) was suffici ShOwn later. this : “it paste. and in , Wading imposs Occ“pardons iden. idmfi'y the atthe Wyn With sim- Gil/en [ht 338:1 l7 clays would have been obtained and prepared by the individuals involved in the pottery manufacture. Ancillary assumptions regarding the nature of the pottery paste include assumptions about the manufacturing processes and the final composition of the ceramics. Although wateriscommonlyaddedtotheplastic material, thisisassumednottosignificantly alter the composition of the clay. Similarly, the addition of temper was assumed not to add elements to the paste in significant amounts, and was thought to only minimally "dilute" the clay. These assumptions stemmed fiom the belief that the grit temper in the paste (Lovis 1973) was sufficiently large so as to permit sampling which avoided the temper. As will be shown later, this assumption was not correct; temper was very well dispersed throughout thepaste,andinmostcaseswas sofinelydividedastomakeavoidingitinthe sampling procedure impossible. Finally, it was also assumed that the logistic and residential occupations identified by Lovis (1991) were correct, and that the pottery sherds used to identify the archwological culture of the occupations could be re-identified by another analyst with similar outcomes. Given the foregoing, the following hypotheses were established for this study: 1: There are no significant differences between the chemical compositions of the pottery from each of the residential occupations (i.e. the Mackinac, Traverse and Juntunen pottery). 2: There are no significant differences between the chemical compositions of the local (O'Neil Site) clay and the pottery from the residential occupations (i.e. the Mackinac, Traverse and Juntunen ponery). 3: There is a significant difference between the chemical compositions of the non-local (Skegemog Point Site) clay and the pottery fiom the residential occupations (i.e. the Mackinac, Traverse and Juntunen pom). The validity of tl MMhm Site. 18 4: There is a significant difi’erence between the chemical compositions of the pottery from the logistic occupations (i.e. the Skegemog Ware pottery) and the pottery from the residential occupations (i.e. the ' , Traverse and Juntunen pottery) The validity of these hypotheses were examined using a total of 52 samples of pottery and clay m the O'Neil Site, and 7 samples of clay and temper from the nearby Skegemog Site. Collection The oer dttaii (Inns 1' researchers 91' which 777 had 50). Each 0ft and were subs “33°15 (Lovis is given in Ta] Site (Lovis 19' number 10 at l indWits vegs, however, lac} The q the Late Woo (See Table 1). SAMPLE Collection The ceramic assemblage form the O'Neil Site has been previously described in detail (Lovis 1973). During the excavation of the site by Michigan State University researchers 9194 Late Woodland and prom-historic pottery sherds were recovered, of which 777 had decoration or surface treatment enabling categorization (Lovis 1973: 41, 50). Each of these 777 sherds we identified with an MSU Museum catalogue number 1. and were subsequently sorted into groups representing a minimum of approximately 80 vessels (Lovis 197 3: 50). The distribution of identifiable vessels reported by Lovis (1973) is given in Table 1. Although a minimum of 79 vessels have been reported for the O'Neil site (Lovis 1973), it is believed that subsequent work on this collection expanded this number to at least 92 vessels, since the Minimum Vessel Sheets 2 for the O'Neil Site includes vessels with numbers ranging from 1 to 92 (Lovis n.d.). This same document, however, lacks information for vessel numbers 22, 27, 3, 45, 46, and 89. The ceramic vessels represented at the O'Neil site consist primarily of pottery fiom the Late Woodland period, with some additional pottery from a prom-historic occupation (see Table 1). Within the Late Woodland period, vessels were attributed to the early and the late phases of the Late Woodland period, as well as to both the Northern and Southern pottery making traditions in Michigan (Lovis 1973). The Mackinac Ware vessels, representing the Northern pottery tradition of the early Late Woodland period at the O'Neil Site, are believed to date to around AD. 800 - 1,000 (Lovis 1973: 59). The Skegemog Ware vessels hour this site are thought to be roughly contemporaneous with the Mackinac Ware, and represent the Southern tradition of pottery in the early Late Woodland (Lovis 1973: 63). The Juntunen Ware pottery at the O'Neil Site is a Northern pottery type. Its incidence at the site is dated to AD. 1,200 - 1,300 as well as to the fifteenth century AD. 19 [Ill iilil-llilli EFF Couture:— 7.3.x: : sated; CLUECOZ N . . 3: 29003 “364 CQNntCCMu Q ( ~ N 325 a: — 80:0t-050“ To a: \ Car-=39. — 5%) H e \ .2. . a N UG-LQL Khuuuauah an t: anvil-P lb . 5 WEEK. 0.3%; V i! . t Enoch. Aanuflnv @Nv 02.0 .3770 a... Ear-bu Evacntxv H O\ N 225 8. e223 mmEb F‘NF‘N n 25. a 25 m 25. A..§eaa..v a on»... coca 5;er .oaeé H 25. E3502: Anew ”m8" «fired .0 .2: has \ .u a: 22 32.550 :02.0 $860 ea a5 ease 82.82 .Q.< @5883 8a..— 8a— chasm Oswv—tv—tv-t .§< cage—h. 355m $3.5. eon—£30m 883$. 3383:: 823:. 85055 9.83%. mmmgé . Cbu "3% «30d .Q.< .U 52 d cam—8.3 .D.< 3683 23 a: 50582 t‘fl' n2. d wan cos—“5:. 382:5 .3054 5555—. 752322 So "at: ”sea Ba? 8582 8 08am .cnaofiefiaoo3 33 2.30 Eufizom MN 358 mmaomoam ae— znahm moaomoam 005on an £63 £66 oouToow .Q.< 3683 o3 :5 E0582 v m Bodega: 8582 33582: 8:282 375654 gut—0&0“ 825 02m .623 Etch 85.5... Ease.— £089» E 8ng as can =oz.o 2: sou..— 288> . _ can... on: 933 (lovis 1991'. 2C9 and spans the P- The abo archaeological ti compare the bet In order to Sim; Traverse or Jur SUI>gmup of tl genera] pone: 0“ Compositit 21 (Lovis 1991: 207). The Traverse Ware pottery, in turn, represents a Southern pottery type and spans the Period from AD. 1,200 - 1,500 (Lovis 1973: 85). The above four pottery types representing two cultural traditions as well as two archaeological time periods were used for the paste composition analysis in an attempt to compare the behavior involved in pottery making, use, and discard of these four groups. In order to simplify the data analysis, only the pottery type (Skegemog, Mackinac. Traverse or Juntunen) was recorded for each vessel number, the variety being considered a sub—group of the general pottery type. As will be shown in subsequent chapters, even this general pottery classification proved to be too fine a distinction for the classification based on composition alone. After completing an initial inventory of all of the O'Neil pottery available at the time of the project, a list of the vessel number and cultural designation was compiled. The original cultural designations for 33 of the 92 vessels was determined using the original Minimum Vessel Sheets (Iovis n.d.) along with photographs of sherds with type/variety designations (Lovis 1973). Because complete cultural designations for each of the original vessels was not available, the vessels were re-typed by Michael Hambacher, whose designations of the known vessels (Michael Hambacher, personal communication 1991) closely matched those proposed by Lovis (1973) in the original analysis. However, four early Late Woodland vessel (Vessel 17, corresponding to Sample 13; Vessel 28, corresponding to Sample 5; Vessel 32, corresponding to Sample 6; and Vessel 53, corresponding to Sample 14) were identified differently by Hambacher and Lovis. These dual designations are maintained throughout this study. A listing of the pottery type designations given by both Lovis and Hambacher can be found in Table 2. Pottery types were established by Hambacher for 54 of the 92 O'Neil vessels. Another 6 vessels could only be given tentative type designations, 6 could only be identified (or tentatively identified) within the early or late Late Woodland period, and 15 could not be identified at all (Michael Hambacher, personal communication 1991). ‘rl‘ultlL h new—QCEV. .3: _Umau> Dinosaur—L. ~ N 023: N N M Ca: .558 £th Eocene—:5: 3.9.: ..o.: erect! b 535:2 535:2 00.07. 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I! .. .. _ a..fl;lu~d=: ‘ \ 05‘s: \ 3 .5353. .3: .0mmu> — Mczawuxv‘ Azimoaw x \ 0.5: \ Mn 4 :oo— .EEe imam Coco-550:» at: :3... £39: Len—=32 L353? 332 09:. 003$ «EAR. 903$ 235$. 39%) 1‘. «ELIOUV N Q—Qfirfi 3388 00: ~800> :0::0::_. :0:::::~ 0:0: «0 00—980 .0: $0005 Baas—0:: AN 093 _.:0£m8_0::_. 0:0: 3 55:3. 5:85;. Vn - mm o0 28:08 8:88:85 02 0:0: 3 33:80 :0: ~0mmo> :0::82. 0:0: xx 5523. On 5 00—980 00: ~080> 5505:: 0:0: 8 00:025. mm - mm mm :0:::::~ :0::83 on SW @0383 00: ~800> 5505:: a mm @0183 00: _ommo> 058003 83 08— 3.3080 0:0: mm :0::83 \ ‘ mm 5 00—0080 .0: ~800> 220003 003 0:: >368: 0:0: aw 0fi0>flh mm 2. 0328; :0: _0000> 0:0: E. 00:025. 00:90:. an E. 0328.»: 00: ~00mo> 0:0: or 00—0880 00: ~0000> 5505?: 0:0: nh 003800 00: _0mmo> 565:: 0:0: E. 33:80 00: _0000> mofiowoxm 3:38: 0:0: 2. :03 .5500 .0000 £053.55 Ana“ 90.: 030‘: LEE—.2 :0:—.52 8.02 003. 95$ 09¢. 0.55 0.05—um .008> 8.253 N 0.8:. Undoubtedly (I ”other" catcgm and to the “um Emily, S VtSE been othmis shcnis and th Miami sugg “mbfi‘S, bu: Vessel" cour Bee: ‘0 sample an mm W6 dCK'Tmine x were 13mm 26 Undoubtedly many of these 27 difficult-to-identify vessels correspond to Lovis's (197 3) "other" category which contained 29 vessels represented by sherds too small to classify, and to the ”unclassified" category, which contained 7 vessels of 5 "types" (see Table 1). Finally, 5 vessels were not available for sampling due to either being on display, or having been otherwise removed from the collection. For an additional 6 vessels both the pottery sherds and the Minimum Vessel Sheets corresponding to these vessels could not be located, suggesting that these may have been "vessels" which were assigned vessel numbers, but which were later found to be subsumed by other pots in the ”minimum vesse " count. Because the collection represented a small number of vessels, an attempt was made to sample as many of the identified containers as possible. Of the 54 vessels with known pottery types, 37 were sampled at least once (see Tables 2 and 3). The criteria used to determine whether a vessel would be sampled was four-fold First, vessels from Area A were preferred over those from Area B, since the former was the stratified area of the site, andthe latterwas not. Likewisevessels fromareaAorB werepreferredoverthosefrom the test pit area, since little habitation information was available from these test pits. Second, where practical, a preference was given to vessel whose sherds had complete unit and level information recorded on the Minimum Vessel Sheets or on the Museum catalogue cards (Michigan State University Museum n.d.). Third, a representative number of samples from each of the four pottery types was required. For this reason, samples were taken from all of the Skegemog and all but one of the Mackinac vessels. (The Mackinac vessel designated as vessel 19 was not sampled simply because the single sherd representing this vessel was too small, and sampling would have destroyed the specimen.) Finally, as far as practicable, the number of vessels sampled from each of the four pottery types was kept relatively equal. Thus not all of the Traverse vessels were sampled, since the available vessels of other types was much lower than that available for the Traverse vessels. 27 The total number of vessels sampled is as follows: Skegemog 6 Skegemog/ "Problematic" 1 Mackinac / Skegemog 3 Mackinac 4 Traverse 12 Juntunen 1 1 For most of these vessels, samples were removed from only one sherd. However, in the case of Vessel 57 (Samples 8-10), Vessel 50 (Samples 19-20), Vessel 85 (Samples 23- 25), Vessel 90 (Samples 53-54) and Vessel 11(Samples 29-30), samples were taken from multiple sherds both to test for the reproducibility of the INAA results across a given vessel (e.g. Vessels 57, 50, 85, and 90) and to check for the effect of diagenesis in the case of vessels whose sherds were found in multiple locations (e.g. Vessels 50, 85, and 90). In addition, because the temper pieces were so large in one vessel (Vessel 11) it was possible to isolate some of the temper fragments and collect them as a separate sample (Sample 30) which could then be compared to the corresponding paste sample from the same vessel (Sample 29). Likewise, when vessel 52 was sampled, it was noted that most of the resulting sample consisted of untcmpered clay. This "pm-e" clay was collected as Sample 32. In addition, three clay nodules collected from the O'Neil Site during the 1969-71 excavations were also sampled in duplicate or triplicate (Samples 33-35, 37-40). These dried nodules proved to be very sandy and broke apart easily when slight pressure was applied. "Sand" collected from just beneath one of the nodules during the original O'Neil Site excavations was also sampled for this analysis (Sample 36). Four prepared clay nodules collected from the Skegemog Point Site during the this site's original excavations in the 1960's (Michigan State University Museum n.d.) were also sampled in singletons or duplical Sktgcrr 49 (Jur of 100 pmV'ldt the pot check each k We “limb Table 28 duplicates (Samples 41-43, 45-47, 60). Finally, one piece of presumed temper from the Skegemog Point Site was also sampled (Sample 44). A total of 60 pottery, temper, clay and sand samples were collected. Two of these samples (Sample 8 and Sample 53) were run in duplicate (hereafter designated as S8N1/2 and SS3N1/2, respectively) to test the homogeneity of ground samples and the reproducibility of the INAA results. Three other samples were not analyzed by INAA. Samples 19 and 20 (Traverse Ware) were not run due to suspected contamination of the sample by the adhesive and India ink used in the curation of the sampled sherds. Sample 49 (Juntunen ware) was not run due to insufficient material having been collected. (A total of 100 - 200 milligrams (mg) of sample was required for the INAA analysis. Sample 49 provided only 46 mg of material.) In addition to the pottery, clay and temper, each lot of dental bits used to remove the pottery and clay samples from the artifacts were also analyzed by INAA in order to check for possible contamination of the samples with filings from the bits. Two bits from each lot were sampled by breaking off the tips of the bits and running these in a separate INAA batch (see Chapter 5, Method). A complete listing of sample number, vessel number, pottery type, sherd provenience, INAA batch, and bit lot number can be found in Table 3. Sampling Procedure The artifacts used in this analysis were sampled by grinding off material from the inner surfaces of the sherds with Tungsten-Vanadium hardened steel dental bits (Pfingst & Company, Inc., South Plainfield, NJ). The dental bits, which were cleaned with disnlled water and powder-free tissues, were used in conjunction with a Dremel Tool for the sample collection. The sherds were prepared for sampling by first removing 1-2 millimeters (mm) of surface material in a 1-2 square centimeter area and discarding this material. The +5.... accz ~ “Qt-(q r um“. 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This was done in order to avoid collecting samples from areas which might have been contaminated by exposure to the soil in the archaeological context, or by handling during the curation of the artifact. In order to further avoid contaminating the samples during collection, powder-free polyvinyl chloride gloves were worn during the sampling procedure. The gloves were discarded after each sample was collected. Samples were collected on weighing paper and transferred to N algene high density polyethylene (HDPE) bottles (4 mL size with screw-top caps) which had been previously washed with dilute nitric acid, rinsed three times with distilled water, and allowed to air-dry at room temperature. The sampling technique utiliwd in this study permitted the collection of samples which were relatively free of soil and other potential contaminants. It also allowed the collection of relatively thin sections of the sherd, and affected an area of only 1-2 square centimeters. However, although it permitted large pieces of temper to be avoided, complete avoidance of temper was not possible, since in most cases the temper was thoroughly mixed with the clay. An exception to this was found in Vessel 52, which, as described above, contained apparently untempered clay on the surface of the vessel. The extent of the untempered clay was not determined, but it extended to at least three mm below the inner surface of the vessel. The presence of temper throughout the vessel matrix was apparent in two ways. First, the sherds were significantly harder and resistant to grinding than were the clay samples. Second, the ground pottery samples (except for Sample 32) contained both a powdery material (clay) and granular material of varying sizes (temper). The larger pieces of this temper were removed from the pottery samples, but grains less than 1-2 mm in diameter could not easily be removed. Therefore, except for Sample 32 the pottery samples are all considered to be mixtures of clay and srnall-grained temper. The effect of this admixture is discussed under Results (Chapter 6). 37 Two styles of dental bits were used for the sample collection. One was a "cone" shaped bit (size 023, lot number 555828), and the other a "bud" shaped bit (size 023, lot numbers 442988 and 625828). The best results were obtained from the "bud" shaped bits, and consequently this style was used for the majority of the samples. Initially each bit was used for the collection of two samples, with the bit being cleaned with distilled water and powder-free tissues between samples. However, this practice was soon abandoned, since the wear on the bits made the collection of the second samples difficult. Although the bits were made of a hardened steel, they became heavily abraded during use. Presumably the grit temper (consisting primarily of crushed granite [Lovis 1973]) had the effect of grinding ofl’ the sharp edges of the bits during the collection of the sample. Because of this contamination of the samples with the metal from the dental hits, the bits themselves were sampled for analysis. Two representative bits from each lot were cleaned, after which the tips of the bits were broken off with clean pliers. The tips were then weighed and analyzed in the same manner as the pottery and raw material samples. During the sampling, differences in the composition and hardness of the sampled sherds were noted. These are summarized in Table 3, which also provides a listing of the dental bit lot numbers used for each sample. Sample (Q oven. Vials prep: Inc., Bufo mmparab 0f sample amount 01 ‘0 PTBCluc' METHOD Sample Preparation All ofthepotteryandraw material samples were dried overnightin a90°Celcius (C) oven. Afterdryingthe sampleswereweighedonaMettlerAE 2(X)balanceintoglass vials prepared from high pmity quartz tubing (Supersil T/21, lot 22942, Herasil Amersil, Inc., Buford, GA). As much as possible, sample weights and standard weights were kept comparable (approximately 130-175 mg). In some cases, however, insufficient amounts of sample material forced the sample weights to be as low as 70-100 mg. In one case, the amount of sample material was so little (Sample 49, which consisted of a total of 46 mg) as to preclude it from being run by INAA. A listing of the weight of each of the samples and standards in each of the batches can be found in Table 4. Prior to weighing the samples, the one-meter long tubing sections were cut into sections, and one end of each section was sealed with a flame torch. The resulting vials were then cleaned by soaking them in a solution of Pierce RBS-pf cleaning agent (Pierce Chemical Co., Rockford, IL) and rinsing them five times with distilled water. All manual operations following the soaking of the vials was performed using clean sm'gical gloves. The tubes were subsequently dried ovemight in a 90° C oven and marked with a sample number using a glass-scribing tool. After filling the vials with the samples, the open ends of the vials were sealed using a flame torch and set aside for irradiation. All subsequent operations involving the samples were performed by Michigan Memorial Phoenix Project / Ford Nuclear Reactor personnel due to safety considerations in the handling of radioactive materials. The pottery and raw materials samples were prepared and analymd in three batches, each of which was run with a blank (empty) vial, and three vials containing standards whose elemental concentrations were subsequently averaged and used as the batch standard. Additionally, a vial containing a "check standard" was run. This "check 38 . A 7.1 22:22 2222:2222 2222222222222 22.. 39 Table 4 - INAA Batch Information Vessel Ware Type * INAA Number INAA Sample Number l 2 NBS Standard 1633a - 3 Sample 4 Skegemog 164.0 4 Sample 6 SkegemL 164.5 5 Sample 8 Mac / Skegi‘“ 111.4 6 Sample 15 Skegemog 70.0 7 Sample 28 Skegemog 142.4 8 Sample 32 Skefl Prob *** 150.1 9 Sample 51 Skegemog 1 13.3 10 Sample 8 N1 57 Skegemog 151.2 11 Sample 8 N2 57 Skegefl 132.9 12 Sample 9 57 Skegemog 133.5 13 Sample 10 57 Skegemog 153.0 14 Sample 1 1 16 Mackinac 164.6 15 NBS Standard 1633a NIA NIA N/A 156.6 16 Ck Std (NBS 1633a) NIA N/A NIA 157.3 17 Sample 12 21 Mackinac 158.9 18 Sample 13 17 Mac / Skeg ** 96.9 19 Sample 14 53 Mac / Skeg ** 151.6 20 Sample 15 69 Mackinac 93.5 21 Sample 16 26 Mackinac 163.8 22 Sample 17 44 Traverse 158.6 23 Sample 18 36 Traverse 161.8 NIA NIA 19 50 Traverse not run NIA N/A 20 50 Traverse not run 24 Sample 21 54 Traverse 155.4 25 Sample 22 77 Traverse 157.6 26 Sample 23 85 Traverse 150.8 27 Sample 24 85 Traverse 101.1 28 Sample 25 85 Traverse 154.2 29 Sample 26 3 Traverse 160.4 30 NBS Standard 1633a N/A N/A N/A 151.8 22L F2L INAA Number I Unit 222222222222 Table 4 (cont'd) Sample Vessel Ware Type * INAA Number Number Spl Wt "n... . . ......................................... (mg) ‘ 1 N/A 0.0 2 NBS Standard 1633a NIA NIA NIA 156.0 3 Sample 27 62 Traverse 172.0 4 Sample 28 79 Traverse 145.0 5 Sample 29 1 1 Traverse 149.7 6 Sample 30 11 Traverse 130.2 (temper) 7 Sample 31 2 Traverse 153.8 8 Sample 32 52 Traverse 151.7 (clay) 9 Sample 33 Clay O'Neil Site 163.0 10 Sample 34 Clay O'Neil Site 167.0 11 Sample 35 Clay O'Neil Site 154.6 12 Sample 36 . Sand O'Neil Site 173.3 13 Sample 37 Clay O'Neil Site 162.6 14 Sample 38 Clay O'Neil Site 163.7 15 NBS Standard 1633a NIA NIA NIA 153.0 16 Ck Std (NBS 1633a) NIA NIA NIA 164.0 17 Sample 39 Clay O'Neil Site 155.5 18 Sample 40 Clay O'Neil Site 158.1 19 Sample 41 Clay Skegemog Site 168.0 20 Sample 42 Clay Skegemog Site 154.4 21 Sample 43 Clay Skegemog Site 167.1 22 Sample 44 Temper Skegemog Site 154.5 23 Sample 45 Clay Skegemog Site 152.3 24 Sample 46 Clay Skegemog Site 156.1 25 Sample 47 Clay Skegemog Site 166.1 26 Sample 48 10 Juntunen 164.5 NIA N/A 49 30 Juntunen not run 27 Sample 50 87 Juntunen 1 13.2 28 NBS Standard 1633a NIA N/A N/A 166.2 0.1. 1 11234567009 01.123456 1111111 123456789 ‘0 41 Table 4 (cont'd) ____ males if“; if: ’ffzis._?_.i"'i':':‘j'f q'iii‘ifgliér 1 Blank 2 NBS Standard 1633a 3 Sample 4 Sample 5 Sample 53 N1 90 Juntunen 152.8 6 Sample 53 N2 90 Juntunen 164.3 7 Sample 54 90 J untunen 151.9 8 Sample 55 31 Juntunen 167.8 9 NBS Standard 1633a NIA NIA N/A 162.1 10 Ck Std (NBS 1633a) NIA N/A N/A 156.8 1 1 Sample 56 37 Juntunen 156.2 12 Sample 57 5 Juntunen 152.0 13 Sample 58 81 Juntunen 160.2 14 Sample 59 84 Juntunen 158.6 15 Sample 60 Clay Skegemog Site 158.3 16 NBS Standard 1633a NIA N/A NIA 159.8 1 N/A 0.0 2 NBS Standard 1633a NIA N/A 224.4 3 Sample Bl-l (for spls 1-12) 50.6 4 Sample B1-2 (for spls 1-12) 48.6 5 Sample BZ-l (for spls 13-17) 20.2 6 NBS Standard 1633a NIA N/A NIA 258.2 7 Ck Std (NBS 1633a) N/A N/A NIA 261.9 8 Sample B2-2 bit (for spls 13-17) 23.2 9 Sample B3-l bit (for spls 18-60) 48.4 10 Sample B3-2 bit (for spls 18.60) 50.8 11 NBS Standard 1633a NIA NIA NIA 252.6 ‘ New bit used (otherwise cleaned bit from previous sample used) " ' Mackinac per Lovis (1973); Skegemog per Hambacker (pers. comm. 1991) ' ‘ ' Skegemog pottery type per Lovis (1973); problematic per Hambacher (personal communication 1991) between standard 1633a, 'l oven for contain: 00ncent PRpara in placr the use Vial, 11‘ Mar Race of the Samp of flu clay POM h ”h! Q The De 3'9"; 42 standard" consisted of a stande run as an unknown sample to check for within- and between-batch reproducibility. The standard used for all the batch standards and check standards was the National Btueau of Standards's (NBS) Standard Reference Material 1633a, Trace Elements in Coal Fly Ash, lot 682306, which previously had been dried in an oven for one week by Phoenix Project personnel. A lisdng of the samples and standards contained in each batch can be found in Table 4, while Table 5 lists the known concentration of each element in the standard. Thebatchofdental bittips(Batch4)waspreparedinamannersimilartothe preparation of the first three batches, with the exception that plastic sample vials were used in place of glass vials since the lower irradiation time for this batch (see below) allowed for the use of plastic vials. As with the first three batches, this batch was run with one blank vial, three standards vials, and one check standard vial. The vials for this batch were prepared by personnel from the Michigan Memorial Phoenix Project / Ford Nuclear Reactor, who also weighed the samples and standards. During the weighing of the samples differences in the consistencies and densities 3 of the samples were noted. The clay samples from the O'Neil Site as well as two clay samples from the Skegemog Point Site (Samples 41 and 42) were very sandy. The density of this clay was similar to that of most of the pottery samples. However, the remaining clay samples from the Skegemog Point Site (Samples 43, 45, 46 and 47) were very powdery and were approximately half the density of the previous clay samples. For the most part the Skegemog Ware samples (including Samples 1-10) were very light and finely divided, and seemed slightly less dense than the following pottery samples. The Mackinac Ware samples (except for Samples 12 and 13, but including samples 11, 14, and 15) were more granular (possibly due to more grit temper in the samples) and less powdery than the Skegemog Ware samples. Samples 12 and 13 (Mackinac Ware) appeared more like the Skegemog Ware samples (Samples 1-10) than like the other Mackinac Ware samples. )Gv‘l‘flh h: nIN-fliltN" . Ill]! 4 I amnc- tea—052m. V572 5 3:05.030 .3 5.2.2.200209 t m. .0355 43 cm H Omm A: H 8.0. o H o. H “an 06 H Eva 06 H Wu Nd H QN on H 600 cd H 0.3 m H 00 N H 2mm 0 H R— 86 H 36 08% H ooofo 3.0 H 26 md H 02.2. 0 H on ad H hm m H 00 o H 03 he H m6. 5 H ms.— 06 H 06 EsmzoohN _.. ofiN 8S. ... 80:35. 0 83.8.5. HEP—oh. a. 833:5. 0. 808.000 8080.00 Bum—800$ ... 8.5033— .0322 5802 :9: 80:05 a. 8350m— 0 835—0006 0 8.38.0 .. 880 .. 8.3.25 83000 a. 83.00 0. 0008280. A803 00300800000 8.8.0 0.80 .c 9.8.5 m 80.. 8.080 288.0 2.0:: 2 .. . .08 808.33. 0.2 e. 8:82 a 82.... 880800 0.0 A... 00 .3 000008. 0030> 000800-002 .an> 00.00 02030.2. 00 300200000 <03. mmz .«0 2 030p. 80.a 20 0020> 009.000 N... a 3 83.2.3 .. .0 a N... 8.85 0.. a 2.. 8880 _. o. 0 2. 8.30.82 s m a 00 8823.32 .. 0.... u N... 82.2.... s 0 a a. 60858.. _. 0.... a 8.. 8.3.80 n... a «N 8.880 ... 8. a 0N... .880 .. 0003 808.8080 .88....— 2800 .c 825 . 80< 8.080 388.0 88. 888.0 002 2 28.8.0 3 02.8.8080 . m 030... 44 In contrast, the Traverse Ware samples tended to be very granular and contained a great deal of grit temper. An exception to this was Sample 32 which was believed to have consisted almost entirely of clay. This sample was very powdery and was half as dense as the pottery samples; essentially it behaved like the second group of Skegemog Point Site clay samples described above. The Juntunen Ware samples were grainy and very finely divided, but exhibited some variation in the consistency of the samples. Sample 50 had the consistency of the clay samples, but had the density of the other pottery samples. Likewise Samples 56-57 had a consistency resembling that of the lighter clay samples and, like these clay samples, had densities one half to two thirds that of the other pottery samples. Finally, Sample 58 was somewhat gritty and less finely divided, resembling the Traverse Ware samples more than the other Juntunen samples. Analytical Procedure Theconeentrationsoftheelementsin thepotterymatrixandtherawmaterials were determined using Instrumental Neutron Activation Analysis (INAA) which permits the fast and simultaneous detection of a variety of elements ranging in amounts from the percent (%) to the part-per-million (ppm) levels. With INAA the sample to be analynd is plawd in a radioactive flux where it is bombarded with neutrons. While situated in this flux the elements in the sample absorb one or more neutrons, transforming these elements into radioactive isotopes of the original elements . These isotopes then undergo radioactive decay, emitting energy in the form of gamma rays and other forms of radiation (Nuclear Reactor Laboratory 1988). Each radioactive isotope has a characteristic half-life and emission spectrum (Erdtman 1976, 1979; Brown, 1986) which is used to identify the element originally present in the sample. Quantitative information is obtained by a direct comparison of the intensity of the emission spectrum of the standards with those of the sample, since the quantity of a given element is direct]: 1988). thetw Univ: 3 $3: with the s detc‘ COD N u sut We inf fiv fiv 45 directly proportional to the intensity of a given spectral line (Nuclear Reactor Laboratory 1988). The pottery, clay and temper samples (Batches 1-3) were irradiated for six hours in the two mega-Watt Ford Nuclear Reactor of the Michigan Memorial Phoenix Project, University of Michigan, Ann Arbor, Michigan. The samples were irradiated in-core in a nominal flux of 1 x 1013 neutrons/cmzlsecond (Nuclear Reactor Laboratory 1988) within a sample holder which spins on its axis in order to ensure equal irradiation of the samples within each batch (Edward Birdsall, personal communication 1991). Following irradiation the samples were allowed to decay for approximately one week, and the gamma radiation emitted from the samples was counted on a Lithium-drifted Germanium (GeLi) gamma ray detector equipped with an automatic sample changer. Each sample and standard was counted for 40(1) seconds (live time), and the results were electronically transferred to a Nuclear Data 6700 computer system, which automatically background-corrects the data by subtracting the values obtained for the "blank" from the sample values. The samples and standards were allowed to decay for another four weeks (for a total of five weeks) and were counted in the same manner as the week-one counts. The week-one counts provide information on elements with half-lives of between one and twelve days, while the week- five counts provide information on elements with half-lives of between fifteen days and five years (Nuclear Reactor Laboratory n.d.) Due to the high metal content of the dental bits, these samples were irradiated separately for only one hour in batch number four. This change was necessary since samples with high metal concentrations activate very easily, and when they are irradiated for long periods of time produce is0topes with activity levels beyond the safe limits of this reactor (Edward Birdsall, personal communication 1991). The subsequent decay and counting of batch 4 was identical to the parameters utilized in batch numbers 1-3. Following irradiation and counting, data from the "peaks" (spectral emission lines as seen by the gamma counter) were collected through the computer interface. The energy of these p qualiadv intensity quarries ifiycfiu 3ch an intens'r‘ Ymes s indica analy infor Slam of A encr 45 of these peaks, which is measured in thousands of electron volts, or Kev, provides qualitative information about the identity of the element producing the emission. The intensity, (1' activity level of the peaks (measured in counts per second, or cpm) provides quantitative information about the amount of each element in the sample. The initial listing of peaks for the week one and week five counts was checked against tables of neutron activation (Erdtman 1976; Brown 1986) in order to select the peaks with the highest intensity and the least interference from other peaks for each element in the standard. The lines selected are listed in Table 6 by element. As a quick glance of the calculated results indicates(seeAppendixA),someofthelines selectedprovednottobeusefulinthefinal analysis of the data, since they were not found in all of the standards for each batch. Subsequent to the selection of the lines to be used in the analysis, the following information was entered into the computer for each batch: mass (mg) of each sample and standard, concentration (ppm) of each element in the standard (as reported on the Certificate of Analysis for the NBS standard), the half-er of each element in the standard, and the energy emission line(s) attributed to each element in the standard. This information, together with the peak intensity data (corrected for background) were run through the Nuclear Data "Gamma Spectroscopy" and "NAA" software packages. Using the afore- mentioned data, this software calculated the concentration of each of the specified elements in every sample 4. Subsequently, a report of the results obtained during the week-one and week-five counts was generated for each batch. These reports contained calculated concentration values for 31 elements in each of the samples analyzed, as well as "standard deviation" values (error estimates) associated with each concentration value. A digital version (on floppy-disk) of these reports is on file at the Michigan Memorial Phoenix Project / Ford Nuclear Reactor under file number R481, and a hard copy version is on file at the Michigan State University Museum, Anthropology Division. The concentration and standard deviation data from these reports are summarized in Appendix A. 47 Table 6 - Energy Lines and Half -Lives used in Calculations Line 1 (KeV) Line 2 (KeV) Line 3 (KeV) Barium 11.7 days 123.7 373.2 496.3 Bromine 35.4 hour 554.3 776.5 Lanthanum 40.23 hour 815.8 Lutetium 6.71 days 208.3 Molybdenum 66.02 hour 140.5 739.7 Neodynium 10.98 days 91.1 531 Samarium 46.5 hour 103.2 Uranium 2.35 days 99.5 106 277.6 Ytterbium 4.19 days 282.6 Element -'-‘. . C. ....................................... . ‘.‘.‘.‘.‘ r . t'. . . . '. ‘.’.'.‘¢'.:‘:-;.;. -:.;.’.:. -‘~ . .‘. . ........ ........ Half-Life Ener '.‘.'.‘ ._., ' ~ '2-I-I‘I‘Z'f-I-EPN'I'}I'I-Z'Z'i‘?I'I‘I'I'I‘W'I f I 3‘: f‘Z-I‘Z‘C'Z-Ii-i-N Enegg Line 1 (KeV) Line 2 (KeV) Line 3 (KeV) Antimony 60.2 days 1691.04 Cerium 32.38 days 145.45 Cesium 2.062 years 604.7 795.76 Chromium 27.70 days 320.01 Cobalt 5.27 years 1332.51 Europium 12.7 years 1085.8 1 112 1408.08 Gadolinium 241.6 days 103.2 Hafnium 42.5 days 482.16 Iron 45.1 days 1099.22 1291.6 Mercury 46.59 days 279.17 Nickel 70.78 days 810.75 Rubidium 18.6 days 1076.63 Scandium 83.85 days 889.26 Selenium 120.4 days 136.00 Strontium 64.73 days 513.99 Tantalum 115.0 days 1 189.00 1221.28 Terbium 72.1 days 879.37 1178.00 Thorium 27.4 days 311.9 Thulium 128.6 days 84.26 Tin 115.1 days 391.71 Zinc 243.8 days 115.52 Zirconium 64.4 days 756.72 than one ener; Standards (Set Clem“, hox Barium N60 each batch w COHCentmu'QI Check Stands RESULTS Data Evaluation AsseeninAppendixA,thepereentstandarddeviation associatedwiththe measm'ement of each element varies widely by element and even varies somewhat between samples for the same element. As will be shown below, these standard deviation values helped to determine which elements would be used in the final analysis of the INAA data. For some of the elements present in the NBS standard it was possible to use more than one energy line to calculate the concentrations of the elements in the samples and standards (see for example Ytterbium, Emopium and Terbium in Appendix A). For other elements, however, multiple lines gave different concentration values (see for example Barium, Neodymium and Cesium in Appendix A). In such cases, the check standard for each batch was examined to determine which line(s) provided the calculawd value of concentration corresponding most closely to the known concentration of that element in the check standard. Using this method the following multiple-line elements were eliminawd from further analysis: I Barium ( 373.2 KeV line) Uranium (99.5 KeV line) Gadolinium (103.3 KeV line) An additional review of the concentration of elements in the check standards revealed that the values for certain elements did not closely approximate the known concentrations of these elements in the standards. In addition, some of the elements could not be found in the batch standards by INAA, and therefore no accurate concentration values could be calculawd for the check standards. Finally, in a few cases the concentrations of elements in the check standards could only be reported as "less than" somevaluesincethebaselinelevelinthisareaofthespectrumwastoohightoyieldamore 48 accmattme further data Simil Values in exc fouowmg ad 49 accurate measurement. For these reasons, the following 10 elements were eliminated from fin'ther data analysis: Bromine ( 554.4 and 776.6 KeV lines) Molybdenum (793.7 KeV line) Mercury (297.2 Kev line) Nickel (810.8 Kev line) Selenium (136.5 Kev line) Strontium, 514.0 Kev line) Terbium (879.4 and 1178.0 KeV lines) Thulium (84.3 Kev line) Tin (391.7 KeV line) Zirconium (756.7 KeV line). Similarly, elements whose concentration values had percent standard deviation values in excess of 15% were not used in the analysis. This latter procedure eliminated the following additional elements from consideration : Molybdenum (140.5 KeV line) Neodymium (91.2 and 531.2 KeV lines) Uranium (106.1 and 277.7 Kev lines) Ytterbium (282.5 KeV line) Antimony (1690.5 Kev line) Europium (1085.6 and 1112.2 KeV lines) Tantalum (1189.1 and 1221.5 KeV line) In addition, the 604.4 and 795.5 KeV lines for Cesium had relatively low standard deviation values for most of the samples except for the O'Neil clay samples, which had standard deviation values on the order of 10-30%. However the Cesium concentration results for these clay samples were between one and two orders of magnitude smaller than the Cesium concentration values for the remaining samples. Therefore, even with a high contan ftpres, PrCSur his 211 Such l COne 50 percent standard deviation, the Cesium concentration values in the O'Neil clay samples was significantly difi'erent from that in the other samples. For this reason, this element was included in the final analysis of the INAA data. The 795.9 KeV line was chosen over the 604.7 KeV line because the concentration of Cesium in the check standards calculawd with the former energy line was closer to the known value than was the concentration calculated with the latter energy line. Finally, several elements were not used because they were thought to be possible contaminants from the drill bits used in collecting the samples. The elements which were represented in significantly greater proportions in the dental bits than in the samples were presumed to have been added to the in the pottery samples through contamination by the bits and were eliminated from further consideration. The following elements represent such potential contaminants: Chromium (320.2 Kev line) Cobalt (1332.5 KeV line) Iron (1099.3 and 1291.6 KeV lines) Since it was known that the drill hits were comprised in large part of Iron, the concentration of this element in the bits and in the samples provided a useful measure of the degree of contamination of the samples by the drill bits. As shown in Appendix A, Iron comprises 82.5% to 89.3 % (825,000 ppm and 893,000 ppm, respectively) of the matrix of the drill bits. In the pottery samples -- samples which were most contaminated by the drill bits due to the hardness of the sherds -- Iron is found in levels ranging from 2.58% to 7.10% (25,800 ppm to 71,000 ppm, respectively). Hence, taking into account the purity of the iron in the bits (as low as 82.5% pure iron) the greatest amount of contamination of the samples by the bits is 8.6% 5. Even with this low level of potential contamination, however, two other elements were eliminated from further data analysis: Rubidium (1076.8 KeV line) Althc bits, 1 tone pom: rhcs thcc COM 38C Ce] Val of 51 Zinc (115.6 Kev line). Although the exact concentrations of these elements could not be determined in the drill bits, their maximum concentration levels were as much as two to three times the concentrations of these elements in the pottery samples, thereby raising the question of potential contamination of the samples by the drill bits. In one instance, the concentrations of elements in the drill bits relative to those in the samples were used to select one calculated concentration value over another. In this manner, the calculated concentration of Barium using the 123.7 KeV line was selected over the concentration calculated using the 496.3 KeV line, since in the latter the maximum concentration of Barium in the drill bits exceeded the concentration of barium in the pottery samples, whereas with the 123.7 KeV line the concentrations of this element in the pottery samples and in the drill bits were approximately equal. The elimination of the foregoing elements from subsequent analysis yielded a list of eleven elements which could be used to further examine the pottery and clay samples. For each of these eleven elements - Barium, Lanthanum, Lutetium, Samarium, Ytterbium, Cerium, Cesium, Europium, Hafnium, Scandium, and Thorium --- the concentrations in each sample, along with the associated percent standard deviation of each concentration value, are listed in Appendix 2. These eleven elements represent the elements whose calculated concentrations in the check standards closely matched the known concentrations of these standards as reported on the Certificate of Analysis for the NBS Standard. They also represent only those elements whose concentrations were reported with relatively low percent standard deviation values. Finally, the patential contamination of these elements fiom the bits is considered to be negligible, since the concentration of these elements in the bits was, for the most part, lower than the concentrations in the pottery samples. For these reasons, the reported concentrations of these eleven elements in the samples are believed to accruately represent the concentration of these elements in the pottery and clay samples. 52 One exception to this are the reported concentrations for Sample 46, a Skegemog Point Site Clay sample which was collected from the same artifact box as Sample 47. As is shown in Appendix A, many of the percent standard deviation values for the elements in this sample exceeded 15% and several exceed 25%. When only the above-liswd eleven elements are considered, the percent standard deviations for this sample are higher than for any other single sample. It is presumed, therefore, that this sample represents a measuring outlier, and that the results reported are not accurate representations of the concentrations of these elements in the sample. No other such outliers were noted in the samples analymd. Data Analysis Following the selection of elements, the concentration of elements in each sample was analyzed. Due to the multivariate nature ofthe data, the logarithms ofthe concentrations were calculated and used in the analysis, since the log of concentration standardizes the data and "corrects” for differences in magnitudes between elements whose concentrations range from the percent level to the part-per-million level (Sayre 1977; Bishop and Neff 1989). A cluster diagram using centroid linkage of Euclidian distances was generated for all of the pottery, clay, and temper samples using the Systat 5.0 Statistical Package (Wilkinson 1989). As shown in Figure 4, this cluster diagram separated the O'Neil Site clays and the Skegemog Point Site clays from each other and from the majority of the pottery samples, but did not produce the expected clusters of "local" clay and pottery versus "non-local" clay and pottery. In order to determine whether only one or a few of the eleven elements used in the analysis were responsible for producing the cluster outcome, the samples were sorted by increasing order of concentration for each of the eleven elements. The resulting compilation of ranked concentration values, listed by element in Appendix C, indicates that 53 W.W-WmnanHHHHHHHHHHHHHHHHHHHHHHHHW W W-W-W-W . ....... . a. m . .-mmmwnmnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnunnnnunnnnm ....... W W-an W m n . . . W W-W W-W W- ”-unuunnnunnnuuunnun...”n"...“n.--- . W WNW .--um . . . W W W -HW--HW--nnnunnuW----H--W W . W W . W . W-W--HW . -W W . w- ---W _.._ W. .. .....-.W..W_W_ ' . ............n...._..._........a............a..... mmumuuaau Figure 4 - Centroid Linkage Dendrogram Using 11 Elements athc tide ckwer mtdu codd I989) OHkr numb Opfior 50th 0ftm ttoa dive joint” Celtic] @DUp must: 54 each of the eleven elements alone more or less reproduces the clusta' result obtained with all eleven elements. Similarly, a series of clusters diagrams produced using only ten of the eleven elements -- sequentially deleting each of the eleven elements in turn -- also produced results similar to the cluster diagram formed with all eleven elements (see Appendix D). Hence, since there was no reason to believe that any one element produwd a better clay or pottery "fingerprint" than any other element, or that any one element was adding unnecessary "noise" to the cluster diagram, the original eleven-element cluster diagram was used for subsequent interpretations. To determine the optimal number of groups into which the multivariate samples could be subdivided, a partitioning of the sample via K-means was performed (Wilkinson 1989). This method determines the best way in which to divide the collection of samples in order to maximally separate the groups (Wilkinson 1989: 25). Without specifying the number of groups into which the samples were to be divided, the K-means clustering option yielded only two groups, one containing all of the O'Neil Site clay samples and some of the Skegemog Point Site clay samples, and another group containing the remainder of the samples . By specifying the number of desired groups (i.e., by "forcing" the results into a given number of groups) the samples were subsequently divided into from three to eleven groups, respectively (see Appendix E). A further examination the eleven-element cluster diagram revealed that based on the joining distances -- a measme of the relative distances from the center of one cluster to the center of the next nearest cluster -- the cluster diagram could be subdivided into six major groups whose components are listed below. A schematic drawing of the six groups illustrating their relative joining distances is shown in Figure 5. Group 1: All pottery samples (Samples 1-29, 31-32, 48-59) + Skegemog Point Site clay samples (Samples 41 and 42) GROI Ska GROI 33C Tta‘ GROI 0.0 0. 1 GROUP 1 - (0.0 - 0.124) All pottery samples including S32 (”pure" clay, Traverse Ware) + S41 and 842 (Clay, Skegemog Pt. Site) 55 I Relative Joinling Distlances I 032 0.3 GROUP 5 - (0.149) S44 (Temper, Skegemog Point Site) GROUP 6 - (0.189) 830 (Temper. Traverse Ware) GROUP 3 - (0.106 - 0.113) S43, S45, 847, 360 (Clay. Skegemog Pt. Site) GROUP 2 - (0.102 - 0.110) S33, 834, 835, 836, S37. S38. 839. 840 (Clay, O'Neil Site) 0.4 0.5 0.6 0.7 Joining D'utances are shown in parentheses () following group number GROUP 4 - (0.361) 846 (Clay, Skegemog Pt. Site) Figure 5 - Schematic Dendrogram of Groups 1-6 0.8 The con the six-1 groups] in“) me. SUbSeq. Chalet ; Lite W by Sher, Group3: Group4: Group 5: Group 6: 56 : O'Neil Site Clay 8: Sand Samples (Samples 33-40) Skegemog Point Site Clay Samples (Samples 43, 45, 47, 60) Skegemog Point Site Clay Sample (Sample 46) - Probable Outlier Skegemog Point Site Temper Sample (Sample 44) Temper Sample from Traverse vessel (S30) The components of these six groups also correspond exactly to the group membership in the six-group K-means cluster, suggesting that the division of the samples into six major groups provides the best possible separation, while simultaneously dividing the samples into meaningful groups. Because Group 1 contains the majority of the samples analyzed, a schematic diagram of this group, showing joining distances within it, was produced (see Figure 6). Subsequent examination of the Group 1 cluster revealed that the pottery samples did not cluster by pottery tradition (Northern or Southern tradition), by time period (early or late Late Woodland time periods), by site provenience (Area A or B, or levels 1 through 4), or by sherd type (rim or body sherd). In fact, with the exception of one small cluster of five Juntunen samples representing three Juntunen Vessels (Samples 53Nl, 53N2, and 54, all representing Vessel 90; Sample 56 representing Vessel 37; and Sample 57 representing Vessel 5), few uruelawd samples of the same pottery type joined directly to another sample of the same type. This lack of pairing, however, is not due to an inability of the Neutron Activation Analysis to detect similar concentrations of elements in similar sherds. Nor is it due to an inability of the clustering program to match similar samples. Instead, the lack of W“. _..n 2m. Wm WWW—Wm. m 0 5 8 WWW 0.8.0. 852 328 57 Relative Joining Distances I I I I I I I . . I I I 0.00 ' 0.02 ' 0'04 ' obs ' 0.110 ' 0.10 0.12 0.14 "——353N1, 553m. s—54' . "sso. I ss7 (0.027 - 0.037) "_'so. sro—, 321, 351 In (0.035 - 0.038) 829 (0.040) ’ S9, 812 (0.030) fl Joining Distances are S8N 1, 88N2 (0.038) shown in parentheses () 816 (0.042) following sample numbers S50 (0.045) S7 (0.046) 7 Si, 817, 818, 823, 824, 831. S48. 851. 855 (0.026 - 0.037) 859 (0.047) 82 (0.053) 1 827 (0.057) 815 (0.057) 822 (0.064) 813 (0.069) S32 (0.073) 1 SS (0.072) 83', s' l'4',"s'25—, 826, S41, S42, sss * , .— (0.042 -0.066) I'— 34 (0.099) 852 (0.113) 811 (0.116) to Group 5 828 (0.124) Figure 6 - Schematic Dendrogram of Group 1 varia com; 53, ll duph' B as other pair; bting SW] and t 35 (c d0 nt Sam; “Tire elem (Mid 58 pairingofsherdsofthesamepotterytypesseemstobeduetothelargewithin-type variabilityinthe sherdmatrix, avariability which isgreaterthan thatbetweenpotterytypes. The ability ofthe INAA and clustering methods to pair samples ofsimilar composition is borne out by the results of the analysis of duplicate samples. Samples 8 and 53, representing a Skegemog and a Juntunen vessel, respectively, were analyzed in duplicate by INAA, and the results of these analyses are summarized in Appendixes A and B as Samples 8N1, 8N2, 53N1, and 53N2. When these results were clustered with the other samples in the eleven-element cluster, both pairs of samples joined with its corresponding duplicate sample (see Figlue 4). Furthermore, the duplicate samples in each pair join at very low joining distances, indicating that these duplicate samples are seen as being very similar in composition to one another, and that these pairs are closer in composition to each other than to any other samples. Although the method is capable of pairing duplicate samples of pottery, it is less successful in pairing samples taken from lumps of clay collected from the same location and curated together in the same storage bags or boxes. For example, Samples 33, 34, and 35 (collected from three lumps O'Neil Site clay from the same archaeological provenience) do not join together directly, but instead are part of a larger cluster (Group 2) including Samples 36, 37, and 38. In fact, none of the clay samples from the O'Neil Site which were collected from the same archaeological context joined together directly in the eleven- element cluster. On the other hand, Sample 36, described as ”fired sand found beneath clay" (Michigan State University Museum n.d.) appears to be compositionally very similar to the O'Neil Site clay samples. This, together with the sandy texture of the O'Neil Site clay samples suggests either that these clays were nannally rich in sand, or that sand was added to the clays during the preparation of the clays by prehistoric potters. Given the available data, preference cannot be given to either of these possibilities. ll collected container of this pa Samples joining d the clay I 6). The 1 A the other the densi some "te bomadc' 59 Within the Skegemog Point Site clay samples only two pairs of samples were collected from lumps of clay with the same archaeological provenience. One of these pairs contained Samples 46 and 47, but since Sample 46 appears to be an outlier, no comparison of this pair can be accomplished. However, the other pair of Skegemog clay samples - Samples 41 and 42 -- while they do not pair together, do appear in a small cluster with low joining distances. However, this small cluster appears within Group 1, and, in addition to the clay samples, also contains samples fiom every pottery type sampled (see Figures 4 and 6). The remaining Skegemog Point site clay samples are clustered in Group 2. As noted in the previous chapter, Samples 41 and 42 had a sandier consistency than the other Skegemog Point Site clay samples. Also, unlike any of the other clay samples, the densities of these samples were similar to the densities of the pottery samples. Since some "temper" was noted in the clay lumps during sampling, it suggests that temper had been added to this clay by the prehistoric potter who prepared the clay. However, it is also possible that these lumps of clay contained nannal inclusions which mimic temper in composition and cause these samples to fall in the pottery group. The joining pattern of the raw material samples indicates that the clay samples fiom the two sites are clearly distinguishable from each other. It also indicates that, with the exception of Samples 41 and 42 (Skegemog Point Site clay), the O'Neil Site clay samples and the Skegemog Site clay samples are more similar to themselves than to any of the pottery samples. What is not clear, however, is what is responsible for the differences between the clay samples and the pottery samples. If these differences are due only to the elements in the clays, one could then conclude that the the clays sampled are not the same clays used to manufacture the pottery from the O'Neil Site. However, because most of the Pottery samples analyzed contain temper, the contribution of this material to the elemental composition of the samples must also be considered. In order to address this question of added temper, a mathematical test of mixing Was conducwd according to the method described by Vogel, er al. (1989). Using this nthoh the elements a, rigorous ten dd. which i denotninntt do not yielt TCSponsiblt Onhttotx Since the : samples f. Skegcmo Ware ves VCSStl re necessar itscga elemem Citroen l . Lil/Sm ”006s: Pitsm MN the it: Subsn “Ugh 60 method, the mixing of two components can be evaluated by plotting the ratios of any four elements a, b, c, and (1 found in the samples. According to Vogel, er al. (1989: 17,948) a rigorous test is performed by plotting two pairs of ratios: the ratio of a/b versus the ratio old, which should form a hyperbola, and the ratio a/b or c/d versus the ratio of the original denominators (i.e. b/d or d/b) which should form a straight line. If the plots of these ratios do not yield the expected hyperbola and straight line, then more than one process must be responsible for the mixtures in the samples (Thomas Vogel, personal communication). In order to perform this test, related samples containing both clay and temper were needed. Since the relationship between the individual vessels was not known with certainty, only samples from the same vessel were plotted together. Three vessels -- Vessel 57, a Skegemog Ware pot represented by Samples 8N1, SN 2, 9 and 10; Vessel 90, a Juntunen Ware vessel represented by Samples 53Nl, 53N2 and 54; and Vessel 85, a Traverse Ware vessel represented by Samples 23 - 25 -- provided a sufficient number of samples necessary to determine whether the plots of the ratios produced the expected curves. For these samples, in order to achieve the greatest possible separation of plotted points, four elements with high within-vessel variability were selected for analysis. A list of the elements used as well as the numerical value of the ratios a/b. old and M appears in Table - 7 . The plots of the ratios a/b versus c/d (i.e. La/Sm vs. Ce/Eu) and Nb versus d/b (i.e. La/Sm vs. Eu/Sm) for vessels 57, 90 and 85 are shown in Figures 7-9. As shown in these figures, the plots of these ratios do not provide the necessary hyperbolas and straight lines necessary to confirm the simple mixing of two components. Therefore it must be presumed that even within individual vessels more than one mixing process was responsible for producing the resultant mixtme of clay and temper. One possibility is that the temper added to the clay in the pottery-making process was not a homogeneous substance, and therefore added elements in varying amounts to the clay substrate. The crushed granite temper used in these samples (Lovis 1973), if not thoroughly pulverized 61 80... ..00 00.0 00.... 00.0 :0... 00.0 2.0 .82... .080. 000 :0... 0.00 0.0. 0. .... 00.0 0.0... 00.0 2.0 82.0 00.0 000 0.0... 0.0 00.0 .0... 00.0 80... ...0 o..0l..oz.o .0... .00 00.... .0... .0. 0...... 0.... 0%.. 00.0 2.0 .82... 00.0 000 .00... ..0.. 000 3.0... 0.8. 00... 000 082.80 00 000 00.... 0.0.0l 00.0 0.... 3.0 000 0.00 082.80 00 000 0.0... 0.00 00.0 0... 0.0 00.0 0.00 08:8... 00 000 .00... .00 3.0 00.. 0.00 ..0.0 0.00 8888. 00 .00 80... .00 00.0 000... ....0 00... 0.00 8888. 00 02000 000... 0.00 00.0 08... 0.00 l8... 0.00 88.8.. 8 .2000 00.... 0.0.0 .00 0.... ....0 00.0 0.00 008008.0 00 ...0 0.0... 0.0 .00 00.. ....0 3.0 0.00 08.0000. 00 00 :0... 0.00 0.0 00.. 0.00 000 0.00 00808.0 00 0200 0.0... 0.00 ....0 00.. 0.00 00.0 0.00 880086 00 .200 W 900. 0...... _ $3. 0.... W 93. 0.... W 93. 0.0. 8030 :0:... 80:... =0 00 E0 0.. 8:5— 0:58 22.00.200.50 0:0:—0:0 090,—. 0.55 0.008.» #2..an 00.0.5.0 0.3:...5 5......— 00008200 0000200 0.. 02.3— 0.... 00.00.508.30 . b 030,—. 62 7.00 6.80 6.60 6.40 6.20 6.00 $5.80 ' \5.60 3 5.40 5.20 5.00 I 1' : i : 4 = 50.00 55.00 60.00 65.00 70.00 75.00 80.00 Ce/ Eu Figure 7 - Plots of Ratios for Samples 8-10 63 7.00 6.80 6.60 6.40 6.20 6.00 5 5.80 \ 5.60 5 5.40 5.20 5.00 . : I I I I T I I 50.00 55.00 60.00 65.00 70.00 75.00 80.00 6.90 -- 6.70 ~- 6.50 -- 6.30 -- W 6.10 -- \ 5 5.90 "" 5.70 -- 5.50 4. 0.18 0.19 Ce/ Eu 0.20 0.21 0.22 0.23 Eu / Sm Figure 8 - Plots of Ratios for Samples 53-54) 7.00 6.80 . 6.60 6.40 6.20 6.00 w5.80 \5.60 5 5.40 5.20 5.00 . : : é : i Q. 40.00 45.00 50.00 55.00 60.00 65.00 70.00 Ce/ Eu 6.90 .- 6.7o .- 6.50 ~- 6.30 -- - (,5, 6.10 .- ‘ 5.90 -- ' 5.70 ~- 5.50 : ; : = .1 0.19 0.2 0.21 0.22 0.23 0.24 Eu / Sm Figure 9 - Plots of Ratios for Samples 23-25 and 1 subs mica 31H Shem from 00111 65 and mixed by the potter prior to addition, could be considered such a non-homogeneous substance, since granite itself is made up of several minerals including quartz, feldspar, mica and/or hornblende (Dorr and Eschman 1977: 36). In addition, the clay itself may not be completely homogeneous. For example, when the test for mixing was performed on three lumps of clay collected together from the O'Neil Site (Samples 33-36), the plots did not yield the expected straight line and hyperbola for a simple mixing process (see Figme 10). In spite of the fact that these clay samples contain a great deal of sand, the mixing process (either natural or as a result of human activity) was apparently not a simple mixing process of sand and clay. Therefore, it appears that the components used to make pottery are themselves heterogeneous mixtures of several materials. Another possibility is that diagenesis within the site is not uniform, thereby causing sherds found in different areas to have some elements differentially added to or extracted from the individual sherds, and producing a reconstructed vessel whose component sherds contain widely different concentrations of one or more elements. However, this appears not to be the case for two of the three groups of samples taken from a single vessel. For both the Skegemog Ware Vessel 57 (Samples 8-10) and the Juntunen Ware Vessel 90 (Samples 53-54), the multiple samples taken from each pot cluster closely together with small joining distances, in spite of the fact that the sherds sampled from each vessels were found in different archaeological contexts (see Table 8). Such is not the case, however, for Traverse Ware Vessel 85 (Samples 23-25). Although the two sherds found in the same unit (Samples 23 and 24) pair together with very small joining distances (see Figures 4 and 6), the third sample from this vessel (Sample 25), which was taken from a sherd collected from Area B, has more similarity with other pottery and clay samples than with the two other samples from the same vessel (see Figures 4 and 6). These results preclude the complete dismissal of the role of diagenesis in the analytical results obtained. However, two other factors could also account for this lack of growing of the three samples taken from Vessel 85. The first is the previously-mentioned 17.00 -- 15.00 -- ' 13.00 -- E 11.00 “- tn \ 9.00 -~ 7.00 -- 5.00 l 1 i l l 50.00 60.00 70.00 80.00 90.00 100.00 Ce / Eu II I 536 ("Sand") 15.50 14.50 13.50 I 12.50 11.50 E 10.50 ‘2 9.50 8-50 -s36 ("Sand") - 7.50 6.50 5.50 . : i : : : 0.18 0.19 0.20 0.21 0.22 0.23 ll Figure 10 - Plots of Ratios for Samples 33-36 67 .. 250 .80 _ 003 0002 _ < _ .280. 0000 _ 00 _ .0 _ 02.280 0 _ 003 0002 _ m _ 0.80 _ 00 _ 00 _ 08.0.5. €058 mm 5 .0820 .. 250 .80 003 0002 < 0.80 00 00 .5: .00. 022,80 .. 260 .80 003 0002 < 8.. 00 0. .5... 80. 6228.0 08 0.0 .800 250 .80 SB 0002 m 0000 00 00 608220 .. 250 .80 02 00>» 0002 < a... 00 ..0 022,0... .. 250 .80 02 00>» 0002 < 8.. 00 00 ".0860... 0 003 0002 m a... 00 0. 00660020 0 003 0002 < 8.. 00 0 00882.0 0 00>» 0002 < 6.. 00 0 00682.0 _ _ _ .0008, :e _ 03:52 mi 03:52 _ .951— _ 0...: _ 09:... _ 0.2.8...— _ $08.» _ 2956 _ 25$ 0.0000.» 055m 595 50.5. 8.0.55 2.5.32 . a 0.0.5. hem will aSl dun' Gm (Sal C011 Vcs Silt 311C Par abc the Cor Cor. 68 heterogeneity within vessels, caused by the inclusion of varying proportions of clay and temper in the analytical samples, or by the heterogeneity of the raw materials themselves (i.e. clay and temper). The second possibility is that the classification of the vessels is not completely accurate, and that more than one vessel is represented by Samples 23-25. In addition to the groups of pottery and clay noted above, three other groups, each with a single member, were found by the cluster analysis. Group 4 consists of Sample 46, a Skegemog Site clay sample considered to be an outlier. Groups 5 and 6 are temper sarrrples collected during the excavation of the Skegemog Point Site (Sample 44) and timing the sampling of a Traverse Ware vessel (Sample 30, collected from Vessel 11). Group 5 (Sample 44) join most closely to Group 1 (pottery samples), while Group 6 (Sample 30) joins most closely to Group 3 (Skegemog Point Site clays), indicating that the composition of the temper collected at the Skegemog Point Site is most similar in composition to the pottery samples from the O'Neil site, and the temper collected from Vessel 11 has elemental concentrations most similar to the clay from the Skegemog Point Site. The latter result is surprising, since the temper was taken from a mixture of clay and temper (Sample 29, containing both clay and temper from Vessel 11) which, when analyzed, fell within Group 1 and showed little similarity to Sample 30. This suggests that both the clay and temper are contributing to the elements contained in the pottery samples, and that each component by itself will not necessarily detemrine the group to which a particular sample is assigned. However, given the results of the mixing test described above, it appears that not only is the temper itself adding to the elemental composition of the pottery samples, but individual fractions of the temper and/or clay are probably contributing elements differentially to the overall mixtme. Although the elemental concentrations of the majority of clay samples support the contention that both clay and temper are necessary for determining group membership, three samples of clay contradict this premise. First, the two previously-mentioned clay samples from the Skegemog Point Site (S41 and 42) are found within the pottery cluster (Gt 85; Wt ”0s; 69 (Group 1), and more specifically within a smaller cluster containing a Juntunen Ware sample (Sample 58, from Vessel 81), two Traverse Ware samples (Sample 25, from Vessel 85; and Sample 26, from Vessel 3), a Skegemog Ware sample (Sample 3, from Vessel 53) and a vessel attributed to both Mackinac and Skegemog Wares by different investigators (Sample 14, from Vessel 53). These clay samples, then, are compositionally similar to each of these wares. This is not surprising, since these clay specimens were observed dtn'lng sampling to have contained pieces of temper (see Table 3). Likewise, the "pure clay” sample collected from Vessel 52 (Sample 32), when evaluated by multivariate analysis, was also placed in Group 1. This sample's placement near the small cluster containing Samples 41 and 42 (Skegemog Point Site clay samples) suggests that each of these three clay samples are relatively similar to each other. Fmther, the placement of these clay samples inside Group 1 indicates that these clay samples have more similarities with the pottery (clay + temper) samples than with the other clay samples. This suggests that in certain cases the composition of the clay alone may be sufficient in determining the groups to which pottery samples belong. It also underscores the variability in the composition of archaeologically-obtained "raw" clays, particularly if they have been altered through the addition of temper. Clearly, several factors are at work within the samples analyzed for this study. The importance of temper, as well as the non-homogeneity of the temper and/or clay used is suggested by the difierences in elemental concentrations between samples from the same vessel. Differences in the composition of the clay samples from the same site are seen in the large joining distances within the O'Neil Site and Skegemog Point Site clay groups, and in the placement of a pair of Skegemog Point Site clay samples with the pottery samples. In addition, the potential use of a variety of temper and clay raw materials by the prehistoric potters may further complicate the analytical outcomes, resulting in a cluster diagram which does not replicate the known pottery groups in the samples. Such is indeed the case for the pottery samples found in Group 1 (see Figure 6). 70 Within Group 1, only six small sub-groups can be found, the remainder of the group being comprised of single stringers attaching sequentially to these sub-groups. Of the six sub—groups, only one is comprised exclusively of one ware type. This sub- group contains five Juntunen Ware samples, including three samples (Samples 53Nl, 53N2 and 54) from one vessel, and two samples (Samples 56 and 57) from two additional vessels. Given the many sources of variability described above, this sub-group stands out in its relative homogeneity, which is underscored by the small relative joining distance of 0.037 within this sub-group. The significance of the joining distances of this sub- group is apparent when compared to the relatively small joining distance of 0.038 for the duplicate samples SBNl and 88N2 (Mackinac Ware), which comprise a second sub-group within Group 1. Three other sub-groups of Group 1 also have relatively small joining distances, but none are comprised solely of samples atu'ibuted to the same ware, pottery tradition, time period, or provenience within the O'Neil Site. One sub- group consists of Sample 6 (Skegemog/'Problematic" Ware), Sample 10 (Skegemog Ware), Sample 21 (Traverse Ware), and Sample 51 (Juntunen Ware), . Another consists of Samples 9 and 10 (Mackinac Ware). A third sub-group is comprised of Sample 1 (Skegemog Ware), Samples 17, 18, 23, 24 and 31 (Traverse Ware), and Samples 48, 51 and 55 (Juntunen Ware). Finally, the last sub- group within Group 1 has larger joining distances than the previously-described sub-groups (from 0.042 to 0.066), and additionally contains both pottery and clay samples. This set consists of Sample 3 (Skegemog Ware), Sample 14 (Mackinac/Skegemog Ware), Sample 25 and 26 (Traverse Ware), Sample 58 (Juntunen Ware), and Samples 41 and 42 (Skegemog Point Site clay). The dearth of clusters within Group 1 representing single ware types suggests three possible explanations. The first is that the INAA and multivariate analytical methods are incapable of separating the samples into their proper groupings. This possibility is negated both by the ability of the methods to group duplicate samples, and by their ability to form a close is ill: with com mug H01 clus (tag Site Pm the C01] 71 closely-related cluster of Juntunen Ware samples within Group 1. The second possibility isthat thevarietyofrawmaterialsused by thepotters, aswell as the inherentvariability within each raw material, makes this type of composition analysis difficult for within-site comparisons of vessels. However, the between-sample variability of the pottery sherds is roughly the same as the variability within the clay samples from each site (see Figure 5), and is less than the difference between the pottery samples and the clay or temper samples. Ifthe raw materials sampled are analogous to those actually used to manufacture Late Woodland pottery vessels, this implies that the mixing of the ingredients obliterated the unique chemical compositions inherent in the clay and temper samples and produced pottery which closely resembles all of the other pottery from the site. Alternatively, the raw materials used to make the pottery may have been unlike those sampled for this study. However, the fact that two of the Skegemog Point Site clay samples (Samples 41 and 42) cluster with the pottery samples suggests that the sampling procedure was capable of capuningatleastsomeofthematerialsusedtomanufacmredteponeryfiomtheO'Neil Site. The third possible explanation of the lack of clustering by pottery type is that the pottery types are not generally congruent to behaviors which would cause the vessels to group together by type. That is, vessels of different types could be assembled by different groups of potters from local materials of similar composition. Conversely, vessels produced by the same group or individual could be manufactured from different materials procured at the site or elsewhere. In either case the style of the vessel, which determines the ware category to which it is assigned, would not necessarily be parallel to the chemical composition of the vessel's paste. Su 72 Summary of Data Since the Late Woodland ware categories are based largely on stylistic considerations (primarily vessel form and design) it should not be entirely surprising that the composition of these vessels does not conform to the same categories as the stylistic classification. In the upper Great Lakes region, archaeological sites frequently contain pottery samples representing a variety of styles and time periods. Occasionally, as in the case of the O'Neil Site, pottery vessels from separate pottery-making traditions within the sametimeperiods arefound. Thepresenceofthesedifl‘erentpotterytypes attire same site has frequently been interpreted as evidence for the occupation of the site by culturally distinct groups, each with unique pottery-making traditions. What the results of this study suggest, however, is that the technological and stylistic realms may function independently of one another, producing stylistic categories which do not match clusters based on composition analysis. However, it must also be recalled that the analysis indicated a high degree of variability in the composition of the raw materials. This variability undoubtedly accounts for a large proportion of the within-ware variability. One conspicuous exception is the cluster comprised of three Juntunen Ware vessels (Vessels 5, 37 and 90) which cluster very closely together, in spite of consisting of sherds found throughout the site at various levels. The similarity in the composition of these three vessel suggests that they were manufactured from identical or nearly-identical raw materials, possibly by the same person or group of people. The fact that sherds from these vessels were found across the site is somewhat surprising, but may simply be an indication of the amount of post-depositional churning which occurred at the site. Alternatively, it may represent different areas utilized by one individual or a single group at the site. If the latter is true, then further studies of paste composition may reveal that areas in a site used by a single potter or family may be discernible from the elemental composition of sherds found at the site. of tha (Q 73 Based on the results of the clustering algorithm, several conclusions regarding the nature ofthe pottery and raw material samples can be drawn. The first is that the O'Neil clay samples are unlike any of the pottery samples and unlike the clay samples fiom the Skegemog Point Site. Similarly, with the exception of Samples 41 and 42, the Skegemog Point Site clay samples are unlike any of the pottery samples. In order to test for the homogeneity of clay samples collected from the sarrre deposit at the site, multiple nodules of clay from the same storage box or bag were sampled and analyzed The results indicate that although these pairs frequently join together, their joining distances are large, indicating a relatively large degree of difference between these samples. These differences could be due to inherent differences in the distribution pattern of elements within geologic clays, especially sedimentary clays. It may also reflect a different pattern of diagenesis between adjacent nodules of clay. Fm'ther, due to the unfired nature of ”raw" clays, the absorption of elements from the soil, or conversely the leaching of elements from the individual clay nodules, may result in larger differences between nodules than between sherds of fired pottery. Finally, some of the differences between the clay sampl ~- especially within the O'Neil Site clay samples -- may simply be due to the effects of statistical counting errors, which are larger for smaller concentrations of elements such as were found in these samples, or to errors associated with the measurement of concentrations far smaller that those found in the standards. The two temper samples analyzed -- Sample 44 which consists of material collected at the Skegemog Site and identified as "temper," and Sample 30, which is comprised of relatively large pieces of temper from Vessel 11 -- are not grouped with either the pottery or the clay samples. However, the temper sample from the Skegemog Point Site (Sample 44) is more closely related to the pottery samples than it is to either the temper from Vessel 11 (Sample 30), or to the clay samples. This suggests that material similar to that collected as temper from the Skegemog Site was used as temper in at least 74 scmeofthepotteryanalyzed, sincethecompositionofthismaterialisnotunliketlratof some of the vessels found at the O'Neil Site. However, the fact tlrattlre tempertakerr from Vessel 11 clusters moreclosely tothe Skegemog Point Site clay group (Group 3) than to either the pottery samples (Group 1) or the Skegemog Point Site temper (Group 5) is intriguing. It is possible that the collection method precluded the possibility of obtaining a representative sample of temper from this vessel. Since only the larger pieces of temper were collected, this may have skewed the results in favor of elements incluad only in the larger-grained temper fragments. Alternatively, the larger pieces of temper in this vessel may represent only one of several tempering materials used in the vessel, one which adds a lower concentration of elements to thetctalpotterysampletlrandotlrectherpotential tempersin thepottery. Since the elemental concentrations of both temper samples lie between the higher pottery concentration values and the lower clay values, it appears that the temper has the effect of emiching the clay with most of the elements examined. However, this assumes that the clay samples analyzed were the same clays which were used to make the pottery vessels from the O'Neil Site. Such an assumption at this time may be unwarranted, possibly leading to incorrect conclusions regarding the use of clay at the O'Neil Site. An alternative view is that the temper collected from Vessel 11 (Sample 30) accurately represents the temper fiom this vessel. If this is the case, it would appear that the temper has the effect of "diluting" the pottery sample, since the elemental concentrations for the temper are lower than those of the pottery (clay + temper). If this is the case, then the concentrations of elements in the clay raw material should be greater than those found in the temper. This clearly is not the case for the clay samples collected fiom the O'Neil Site and the Skegemog Point Site. Two options are therefore possible. First, the assumption that the temper is diluting the clay may not be correct. The second possibility is that the assumption is correct, but that the clays analyzed (i.e. the O'Neil Site and Skegemog Point Shtcia meow Sand: the por b6 Cllht chfiv nfixuu day 53 Sample tkunr mum. (Skegr knpor Cathc “turn mesk Samp} event afthaf SUgge Of C13: 75 Site clays) are not the clays which were actually used to manufacture the pottery found at the O'Neil Site. The incorporation of Samples 41 and 42 (Skegemog Site clay samples) as well as Sample 32 ("pure" clay from Vessel 52, a Traverse Ware pot) in the group containing all of thepottery samples (Group 1) isalsoofinterest. Given thattlre temperinthepottery may be either enriching or diluting the clay used to make the pottery, the inclusion of these raw clays with samples of pottery suggests that these clay samples may have contained small grains of temper. Alternatively the clays themselves may be sufficiently similar to the mixtureofclayandtemperastomakethemmore sirrrilartothepotterysamplestlrantothe clay samples from either site. Unfortunately, neither tempering material nor a pottery sample with temper and clay was collected from Vessel 52, making impossible a determination of the effect of known tenrper inclusion on the chemical composition of the paste. In any case, the difference in the chemical composition between Samples 41 and 42 (Skegemog Point Site clay samples) and the other Skegemog Point clay samples is important tonote, sinceit suggests that the claysfiom this site arequite dissimilarfiom each other. (It also suggests that Sample 44, another Skegemog Point Site clay sample, may not be an outlier, but my represent the other extreme in the range of variation within the Skegemog Point Site clays.) Whether this dissimilarity is due to added temper in some samples, or to differences in the elemental content of various nodules of geologic clays, or even to the presence at one archaeological site of clays transported from other archaeological sites, the large difference in the cherrrical composition of these clays suggests that single clay samples fiom single sites do not adequately represent the variety of clay composition at any one site. Other conclusions can be drawn from the pattern of clustering within Group 1, the group consisting of all of the pottery samples analyzed. Unlike the small cluster of five Juntunen Ware samples noted above, no other cluster of this size is comprised of a single pottery type. Nor are any ccrnposed of samples from a single pottery tradition, time period, or Skegemog. Skcgcmo Figures 4 samples ( 76 period, or provenience on the site. Furthermore, except for Samples 8N1 and 8N2, no Skegemog Ware samples pair with each other. That is, at least compositionally, the Skegemog Ware samples appear more like other wares than like the Skegemog Ware (see Figures 4 and 6). For example, Skegemog Ware samples pair with Mackinac Ware samples (e.g. Sample 9 and Sample 12) and with Juntrrnen Ware samples (e.g. Sample 1 and Sample 55). Other Skegemog Ware samples are grouped with Juntunen-Traverse pairs (e.g. Sample 3 with Samples 58 and 26, and Samples 10 and 6 with Samples 21 and 51). In even larger clusters within Group 1 Skegemog Ware falls into clusters with all three of the other ware types. The pattern of grouping for the Mackinac Ware is not dissimilar to that of the Skegemog Ware. No Mackinac Ware samples pair with each other. This includes all of the samples designated "Mackinac" and "Mackinac/Skegemog." In one instance a Mackinac Ware vessel is paired with a Skegerrrog Ware vessel (Sample 12 with Sample 9). Also one Mackinac Ware sample is clustered with a Traverse Ware pot and a sample of clay from the Skegerrrog Point Site (Sample 14 with Samples 25 and 42). All other Mackinac Ware samples are grouped with larger clusters containing the three other pottery types. Traverse Ware samples, however, do pair with each other, as shown by Samples 17 and 18, and Samples 23 and 24. They also pair with Juntunen Ware samples, as exhibited by the pairing of Sample 26 with Sample 58, and the pairing of Sample 21 with Sample 51. Traverse Ware pottery also forms a small cluster of five Traverse Ware and one Juntunen Ware samples (i.e., Samples 17, 18, 23, 24, 31, and 48). This small cluster has joining distances of 0.026 - 0.031 -- the smallest joining distances for any cluster. In another instance Traverse Ware is found in a cluster of two Traverse Ware, two Skegemog Ware and one Juntunen Ware samples (Samples 6, 10, 21, 29, and 51). As noted above, the sample of "pure clay" from a Traverse Ware pot (Sample 32) lies within Group 1. It falls in a cluster containing samples from all four pottery types. The remaining Traverse Ware samples (Samples 22 and 27) group with large clusters containing all pottery types. Ex itself. H0} SS3N2, Sf within this Juntunen c Juntunen V In larger cl I POW WP In pairs and s manufac related p0 However, i for analys' Within the r In t is a great (it Vm&mWi in the pone Several P05 1. 77 Except for Samples 53N1 and 53N2, the Juntunen Ware pottery does not pair with itself. However, as noted above, it does form one distinct cluster of five samples (SSBNI, 853N2, SS7, 856, and SS4) representing three separate vessels. The joining distances within this cluster (0.027 - 0.037) is very small; only the above-mentioned Traverse / Juntunen cluster has smaller joining distances than this five-sample Juntunen cluster. Juntunen Ware samples also group with Traverse Ware samples, as previously described. In larger clusters, the Juntunen Ware samples are found in clusters containing all other pom WP“ Interestingly, the more recent Late Woodland pottery in this study tends to form pairsandsmallclusterswitlrthesamepotterytypes. Thismayindicatethatmorevessels manufactured with the same raw materials (perhaps at roughly the same time by the same or relawd potters) are more likely to be found at the O'Neil site in the later time period. However, it may also simply be a consequence of the larger number of samples available for analysis from the late Late Woodland period, resulting in a higher probability in pairing within the ware type. In general, the clustering pattern of the clay and pottery samples indicates that there is a great deal of variability in the clay and pottery samples. The fact that the within-pottery variability is similar to the within-clay variability is puzzling, since the inclusion of temper in the pottery samples is presumed to contribute additional variability to these samples. Several possible explanations for this phenomenon are possible. 1. The pottery was made from a more uniform clay (either a different O'Neil Site clay or clay fiom another location). 2. The clay fiom the O'Neil and Skegemog Sites is "prepared clay" with more or less material (temper) added to it. Because of the presence of this added material, the variability within the clays is as great as that within the pottery group. 3. The clay samples analyzed are "rejects" which were considered by the prehistoric potters to have been unsuitable for pottery-making. The 78 fact that these pieces of clay were apparently discarded may support this explanation. 4. The mixing of clay and temper results in a fortuitous mixture which is relatively similar for all pottery. The last possibility seems highly unlikely, since it would imply that each potter throughout time and space had similar mental "recipes" for pottery which resulted in similar paste composition regardless of the composition of the raw materials. This possibility also seems to be negated by the results reported by Trigger, et al. (1980) and Clark (1991) which indicate that variations in pottery composition occur over large regional areas. Therefore, it appears that the clay collected from the O'Neil Site and analyzed by INAA was not the clay used to manufactrue the pottery at the O'Neil site, or, if it was, the clay analyzed was so modified as to render a definitive conclusion impossible. In the case of the Skegemog Point Site clay it is tempting to suggest that the clay nodules which clustered with the pottery samples (Samples 41 and 42) represent the clay used to manufacture these vessels. However, the variability within the Skegerrrog Site clay samples is greater than that of the O'Neil Site clay samples, and therefore any conclusions regarding the nature of individual clay samples from the Skegemog Point Site are at best tenuous. With very few exceptions, the pottery samples grouped more fiequently with other pottery types (including types of a dissimilar pottery tradition or time period) than they did with the same pottery types. The duplicate samples (Samples 8N1 and 8N2, and Samples 53N1 and 53N2), however, join at the first level of joining. Therefore for a given portion of a given sherd, the results obtained by INAA are reproducible. For multiple samples taken from a Skegemog Ware vessel (Samples 8-10, representing Vessel 57) the analytical results were very similar to one another. Likewise, the samples taken fiom the same Juntunen Ware vessel (Samples 53-54, representing Vessel 90) gave very similar composition profiles. However, for the multiple samples collected from a Traverse Ware vessel (Samples 23-24, representing Vessel 85), only two of the three samples show close similarity the possit vessel T prehiston AltcmzuhI diagcncsi I 53316 VCSS Ofptoblcr Validit) Gi with Egan O'Neil Sit Obtained . 79 similarity in composition. The relative dissimilarity of the third sample (Sample 25) raises the possibility that one or more factors may be operating differentially within a single vessel. The results obtained may be due to the incomplete mixing ofclay and temper by the prehistoric potter, leading to differential sampling of clay and terrrper from the three sherds. Alternatively, the variability within these three samples may be due to differential diagenesis across the site, or even to the incorrect assignment of these three sherds to the same vessel. The analytical results from this single vessel, therefore, illustrates the range of problems associated with each of the vessels analyzed. Validity of Hypotheses Given the results obtained in this study, only tentative conclusions can be drawn with regardtothe behaviorofthepotters manufacturingtheLate Woodland pottery ofthe O'Neil Site. In fact, most of the hypotheses put forth are not supported by the results obtained. The first hypothesis states that: 1: There are no significant differences between the chemical compositions of the pottery from each of the residential occupations (i.e. the Mackinac, Traverse and J untunen pottery). Although it appears that each pottery vessel from the residential occupations is similar to every other vessel from residential occupations, the significance of this result is questionable, since all of the pottery samples «- both those from residential and those from logistic occupations - are chemically similar to each other. No clear differentiation between the presumably locally-made pottery from the residential occupations and the purported non-locally—made pottery associated with the logistic occupations was possible. This negates the validity of the fourth hypothesis which states that: GroUp ‘. FBI [3 reSu] 80 4: There is a significant difference between the chemical compositions of the pottery from the logistic occupations (i.e. the Skegemog Ware pottery) and the pottery from the residential occupations (i.e. the Mackinac, Traverse and Juntrmen pottery) As previously shown, all of the pottery samples analyzed are compositionally similar to one another, and the samples from residential occupations are intermixed with samples from logistic occupations in the cluster of Group 1. Likewise, the second hypothesis, which states that: 2: There are no significant differences between the chemical compositions of the local (O'Neil Site) clay and the pottery from the residential occupations (i.e. the Mackinac, Traverse and Juntunen pond?) is not supported, since the pottery from the residential occupations is grouped separately (in Group 1) from the O'Neil Site clay samples (Group 2). The final hypothesis to be considered (hypothesis 3) states that: 3: There is a significant difference between the chemical compositions of the non-local (Skegemog Point Site) clay and the pottery from the residential occupations (i.e. the Maclo'nac, Traverse and Juntunen POW)- For most of the Skegemog Point clay samples the hypothesis is supported. However, for two Skegemog Site clay samples (Samples 41 and 42) which are found in Group 1, the results do not support the hypothesis, since these non-local clay samples are chemically similar to the pottery from residential (as well as logistic) occupations. The inability to support the majority of the hypotheses indicates that the underlying assumptions about the nature of the clay and pottery samples may be invalid. That is, the homogeneity of the clay samples, as well as the relationship of the clay samples to the pottery samples may not be as clear-cut as expected The results also suggests that the assumptions about the regularity of past behaviors may not be correct. The pattern of clay procutm the come. . assumpti 81 procurement and manufacture into pottery containers may be highly variable, even within the context of a residential community occupying a site with clay resorn'ces. These assurrrptions will be dealt with in the following summary chapter. Errors h being an material: were batc assumpt the tesul 35$umpt extent 01 We: Wat f0 material Pithisto SUMMARY Errors in Original Assumptions Inundertakingthisprojecaseveralassumptions aboutthenatmeofthematerials being analyzed, as well as about the behaviors which produced the archaeological materials were necessary. Some of these assumptions were stated from the outset, and were based on the results obtained by previous investigators. Other underlying assumptions, however, were not obvious until after the analytical data were reviewed and the results were found not to be in accord with the expected results. Some of these assumptions are practical in nature and involve simply the choice of sampling tools or the extentofsampling witlrina site. Others aremoretheoreticalinnature andrequirea modification of the research design in order to control for them in future investigations. What follows is a list of the underlying assumptions regarding the nature of the raw materials and finished pottery, as well as assumptions relating to the behavior of the prehistoric potters and analytical procedtne. The local clays are compositionally difl'erent from the non-local clays. This assumption held true for the O'Neil Site clays versus the Skegemog Site clays. However, the O'Neil Site clays were extremely sandy and crumbly, while the Skegemog Site clays were more compact and firm. This raises the question of whether the O'Neil Site clays contain added sand (possibly as a tempering material) which would have the effect of diluting the clay substrate. The fact that the "fired sand found beneath [the] clay" at the O'Neil Site (Sample 36) falls in the middle of the O'Neil Site clay cluster supports the premise that the O'Neil Site clay samples may be showing more similarity to its sand components than to its clay components. Of course, it is also possible that the O'Neil Site clays are by nature very sandy, and the elemental composition obtained by INAA is representative of the composition of the geologic clays found in this area. In order to definitively resolve this issue, a systematic sampling and analytical program is required in 82 83 order to determine the elemental composition of geologic and archaeological clay samples within a small region such as the so-called Traverse Corridor. The clays from one site are similar to themselves (i .e. these clays are fairly homogeneous). Surprisingly, what this study revealed is a great deal of variability in the composition of the clays collected from these archaeological sites. Whether this heterogeneity in the clays from a particular site is due to the variability of the parent clay formation, to the addition of temper to the "raw" clays, or to the importation of clays from other sites cannot as yet be determined. Again, a systematic analysis of geologic and archaeological clays from a variety of sites would be helpful in ascertaining the cause of this variability. Unworlced clays were not transported long distances, but instead were mined near the area where the vessels were made. One of the major premises of this study was that locally-made pottery could be distinguished fiom non-locally-made pottery on the basis of the composition of the ceramic paste. In addition to assuming that local clays were similar to themselves and different fiom non-local clays, it was also assumed that the vessels made from non-local clays were not manufactured at the O'Neil Site, but instead were made at another site near the source of the clay raw material. While this may indwd be the case for the majority of vessels, it may not be true in all cases. In particular the large variability of the composition of the Skegemog Point Site clays suggests that some of these clay raw materials could have been brought to the Skegemog Point Site from another location. Whether this clay was then used to manufacture pottery is still an open question, but it suggests that clay (and temper) procurement behavior was probably more variable than once believed. The clays collected from the archaeological context are representative of clays used to manrfacture prehistoric pottery vessels. This assumption is related to the above two premises that clays found locally are in fact local clays and are homogeneous in composition. However, it also includes the assumption that potters were exploiting the 84 same sources of geologic clays throughout the prehistoric period, and that a sample of unused clay formd in an archaeological context is representative of all of the clays used to manufactrne pottery vessels at that site. At this point it is not clear whether the potters who occupied the O'Neil Site used the clay sources within their procurement area in the same marrnerandtothe sameextentthroughoutthelateWoodlandperiod. Norisitkrrown whether the clay som'ces available to Late Woodland potters remained the same throughout this period, or whether some clay deposits became exhausted during this time. Analyses of presently-available geologic clays as well as archaeologically—derived clays could shed some light on this question, provided that the archaeological clays have not been extensively modified by the addition of temper. The clays from the ONeil Site (and/or the Skegemog Point Site) are compositional- ly similar to some of the pottery samples. None of the pottery analyzed proved to be similar in composition to the clay from the O'Neil Site. Likewise, rrrost of the clay samples from the Skegemog Point Site were unlike any of the pottery samples. One simple explanation for this may be that the pottery was not manufactured fiom the O'Neil Site clays or from most of the clay found at the Skegemog Point Site. However, the complexities of the clusters discussed previously suggests that a such a facile explanation is not adequate. What is apparent, though, is that behaviors involved in the production of prehistoric pottery are far more complex than originally assumed, and that hypotheses dealing with the chemical composition of pottery sherds must be more carefully constructed. Temper added to the raw clays does not significantly alter the chemical composition of the resultant pottery. This assumption appears to be incorrect, although a definitive answer is not possible. The fact that the temper samples from the Skegemog Point Site lies closer to the pottery samples than do all of the clays from the O'Neil Site and most of the clays fiom the Skegemog Point Site suggests that the elerrrents contained in the temper may be adding constituent elements to the pottery samples. However, the inclusion of the 85 "pure" clay sample from Vessel 52 (Samples 32) as well as the inclusion of the Skegemog Point Site clay samples (Samples 41 and 42) with the pottery samples in Group 1, suggests thatinsomecasestempa'may notbenecessary fordeterminingthegroup membershipof the sample. Temper is evenly dispersed throughout the vessel, its composition is homogeneous. and it is constant between vessels. All of these assumptions are negated by the observations of the pottery paste made during the sample collection step. Both the size of the tempergranulesandtlre amountoftempercontained in the sherds was foundtovary between vessels, although there was a greater degree of similarity in the physical composition of the sherds within the same pottery types. Also noted visually were the individual light- and dark-colored grains which comprised the crushed- granite temper. The lack of temper homogeneity suggested by the light- and dark-colored fragments is also supported by the results of the mathematical test of mixing performed on samples of pottery. These results indicate that the pottery matrix (composed of clay and temper) is the result of more than one mixing process, that is, either more than two components were mixed together to produce the pottery, or the clay and temper themselves were made up of several components. Finally, as discussed previously, the inclusion of varying amounts of temper in the samples analyzed by INAA is suspected to have contributed, at least in part, to the large variability in the composition all four pottery wares. One extreme end of the spectrum of temper inclusion was seen in Sample 32 which contained no visible temper. Other samples (for example Sample 29) contained such large amounts of temper that the larger pieces in the original sample were removed prior to placing the material in the sample bottles. In both cases the remaining pottery sherds from these vessel were not examined to determine if the amount of temper in the samples were representative of the amount in the vessels, but it is suspected that the amount of temper does vary within each pottery vessel. That the relative amount of temper varies between vessels is undeniable. Therefore, if the inclusion of temper has either an additive or diluting effect on the final composition of the 86 sherd, then varying amounts of temper in the sample will yield varying results. Although Mommsen and others (Mommsen 1981; Mommsen, et al. 1988) have established means of mathematically sorting out temper from clay in INAA results, this method requires analyses of known temper and clay raw nurterials. Certainly, additional studies of both temper and clay composition would assist in eliminating this problem for future research. Temper can be avoided in the sampling process. Even with the use of a fine-tipped dental bit it was found that temper could not be completely avoided. By using these bits only the larger pieces of temper could be avoided and/or removed from the sample before placing the remainder in the collection bottle. But because even the small grains of temper are larger than the individual clay particles, it may be possible, in future investigations, to separate the clay from the temper with soil sieves, with a mechanical shaker, or by means of flotation using ultra-pure water. Although such procedures would add significantly to the sample collection time, the resulting clay and temper samples obtained could more easily be used to interpret past behaviors relating to the procurement of raw materials and their manufacture into pottery. The addition of water by potters during the preparation of the clay does not alter the chemical composition of the finished pottery vessel. This assumption was not tested in this study but reportedly (Thomas Vogel, personal communication 1991) the addition of flesh water would not add significant amounts of trace elements to the pottery matrix. This may be a factor, however, for pottery made at locations where sea water might have been used in the manufacturing process. The sampling procedure will not contaminate the samples. In an attempt to avoid temper as much as possible in the collection of the samples, hardened steel (Tungsten- Vanadium) dental bits were used to collect the samples. However, the bit material proved to be softer than the temper in the pottery sherds, and the bits became heavily abraded by the sherds. Therefore, although care was taken to avoid contarrrinating the samples with other materials, the samples became contaminawd with metal filings from the dental bits. 87 Forumately the extent of the corrtarrrination could be determined by analyzing representative bits, but the contamination ofthe samples precluded the use in this analysis ofcertain elements (notably Iron) which might have been useful in separating the samples into more meaningfulclusters. Onesolutiontothisproblemmightbetouseaharderdrillbit, suchas a carbide bit, but the brittleness of such materials may also lead to contamination of the samples. Anotheralternativeistouseanagatemortarandpestletobreakapartthepottery sherds. However, this method would not pernrit the removal of the surface material from the sherd prior to sampling -- material which could include soil and other potential contaminantsnotdesiredinthefinalsample. Also,carewou1dneedtobeexercisedin ordertoavoidbreakingupthegrainsoftemperto suchan extentastomake tlreirseparation from the clay particles impossible. All in all, where temper inclusion can affect the final analyticalresults,itappears thatthe bestaltemativeistouseadrill bitmadefromtlre hardest material available, to incorporate a method or removing small-grained temper fiom the clay, and to analyze the drill bit(s) used in order to determine the extent of possible contamination of the samples with the drill bit(s). The elements analyzed for and used in the clustering program are important in difl’erentiating between difl’erent types of pottery and between clays fi'om difi'erent sites. This assumption was found to be at least partially correct, since the analytical procedure was able to differentiate between the clays from the O'Neil Site and those fiom the Skegemog Point Site. However, the same analysis clustered all of the pottery into a single group, with only small sub-groups within it. Whether this was due to characteristics inherent in the pond? matrix, or to the choice of elerrrents used for the clustering program cannot be determined. Other investigators have used a variety of elements to specify groups within the sample population (see Appendix F for a listing of the elements used by these investigators). At present there is no consensus as to which elements provide the best differentiation between pottery types or clay sources, although for the Michigan clays the concentrations of Iron, Magnesium, Potassium, and Sodium are thought to be effective 88 markers for differentiating clays from different sources ( Randy Schaetzl, personal communication 1991). In this study Magnesium and Potassium were not determined, since their half-lifes were too short for the method used. Sodium is not detectable using the standardsattheMichiganMemorial PhoenixProject. Finally,Ironwas notusedin thedata analysis due to the contamination of the samples with rrretal filings fiom the drill bits. Although the concentration of Iron may be useful in differentiating one clay source from another, the addition of crushed granite temper (Lovis 1973) would significantly alter the concentration of Iron in the pottery since granite and other rocks of igneous origin are rich in Iron (Randy Schaetzl, personal communication 1991). The inability of Iron to difi‘erentiate the pottery from the O'Neil Site is borne out in Table 9, which lists the mean Iron concentration of each sample in increasing order. As this table illustrates, the concentration of Iron in the pottery samples cannot distinguish between pottery types, and is not helpful in determining whether or not the O'Neil Site clay or the Skegemog Point Site clay was used to manufactrne the pottery from the O'Neil Site. The usefulness of Magnesium, Potassium, or Sodium in differentiating clays from nearby sites or in distinguishing one group of pottery from another has yet to be determined. The pottery sherds analyzed belong to discrete ware types discernable on stylistic grounds. The validity of this last assumption is perhaps the most difficult to determine, since the analytical results of the pottery samples were inconclusive. Although it has been argued that much of the variability seen in the paste composition of the forn' pottery types is due in large part to methodological problems and variable behavior on the part of the potters, it could also be argued that some of the variability is due to the classification of the pottery itself. In many region in Michigan, the prehistoric pottery frequently exhibits structural and decorative attributes sirrrilar to those of adjacent areas (see for example Brashler 1981). Similarly, the evolution of pottery design from one style to another over time rarely proceeds with sharp breaks between pottery types. Instead, pottery styles, like other aspects of material culture, are often fluid and ever-changing. Because of this, there 89 Table 9 - Mean Iron Concentrations, in Increasing Order Spl Sample Site or Mee- Fe Grp Spl Sample Site or Mean Fe Grp Type Ware Type Cone. # Type Ware Type Cone. O'Neil O'Neil O'Neil O'Neil O'Neil O'Neil Pt 50 Juntunen 22 Juntunen 6 Prob 27 Traverse 51 Juntunen 15 Mackinac 4 BN2 1 l 7 22 56 9 32 2 333333..3 IdHHuhilflO-IMHHHt-It‘tdI-l—I—IHHI-IHHH CkStd CkStd CkStd CkStd >>>> Drill Bit Drill Bit Drill Bit Drill Bit Drill Bit Drill Bit >>>>>> 2 2 2 2 2 2 4 2 3 6 3 3 3 l l 2 l l l l l l l 1 l l l l 1 1 l 1 l l l l 90 is the risk of lumping "transitional" pottery types into earlier or later pottery styles, simply because the classificatory scheme is not sufficiently detailed to accommodate it. Likewise pottery vessels with design elements borrowed from adjacent areas have the potential of being misidentified and assigned to the wrong cultural group. Finally, and perhaps because of these problems, there is the potential of having classificatory schemes which are interpreted differently by different investigators. Some evidence of this was seen with this collection, as exemplified by the conflicting pottery types assigned to Vessel 17 (Sample 13), Vessel 28 (Sample 5), Vessel 32 (Sample 6), and Vessel 53 (Sample 14). The extent of these potential classificatory problems and their effect on matrix studies of this type is as yet undetermined. However, future studies may reveal that ceramic categorization by paste composition is not precise enough to separate the pottery discarded at a single site. Conversely, once the sources of variation in paste composition analysis are sufficiently well understood, this analytical method may prove useful in the classification of POW types. Significance of Results This study attempted to discern from the chemical composition of the O'Neil Site cerarrric assemblage the residency of the prehistoric potters in the hopes of shedding light on the question of resource utilization among the Late Woodland hunter-gatherers of northern Michigan. Instead, what was found was a ceramic collection which could not be easily differentiated into sub- groups on the basis of chemical composition. In addition, a high degree of variability was found in the samples of archaeologically-derived clays from the O'Neil and Skegemog Point Sites. Ftu'ther, little correspondence between these clays and the pottery samples from the O'Neil Site was apparan Although the expected results of this study were not forthcoming, some tentative conclusions about the behavior of the prehistoric potters can be suggested. 91 Although the O'Neil Site was re-occupied several times, it was never intensively occupied, and the re-occupations took place over a period of several centuries (Lovis 197 3, 1991). The site is known to have been occupied throughout the Late Woodland period by groups with different pottery u'aditions. In addition to having their own pottery making u'aditions, these groups may also have had different strategies for obtaining raw materials for pottery unnufacturing. In this light, the lack of large distinct clusters corresponding to one pottery type or even to one pottery u'adition or time period is not entirely unexpected. given the mobility of the groups in question and the access to a potentially large number of clay and temper resources. The lack of such clusters implies that the people making the O'Neil Site pottery were obtaining their raw materials from a variety of locations, most likely including the Skegemog Point Site, and possibly including the O'Neil Site itself. In addition, the occupants of the O'Neil Site may have brought finished vessels to the site, but the evidence for this is still inconclusive. What is evident, however, is that the potters manufacttuing the vessels found at the O'Neil Site were not limited to discreet somces of clay and temper which would manifest themselves in clear clusters of vessels and a tighter grouping of unfired clays. Instead, one sees pottery types whose ranges of variation are as great as the range of variation of all the pottery samples combined. This implies not only the use of a variety of raw materials, but potentially a mixing of pottery styles and populations, resulting in pottery whose stylistic attributes are not congruent to the elemental composition of its paste. The unexpectedly high variability in the clay samples, particularly those from the Skegemog Point Site, may simply be a reflection of the variability of the geologic clays available in the immediate vicinity. Alternatively, it may indicate that raw clays were transported to the site from other locations within the seasonally-traversed territory of the groups inhabiting the site. Two reasons for u'ansporting raw clays fiom one occupation to another can be envisioned. The first is that although clay is ubiquitous in Michigan, those 92 clays desired for pottery-making may not have been abundant in all areas. The second reason is that the difficulty in transporting clay may have been offset by the greater difiiculty in transporting finished pottery from one location to another. Fired pottery, particularly the pottery of the Upper Great Lakes which is fired at low temperatures, is relatively fragile. Raw clay, on the other hand, is also relatively fragile in its dried state, but with the addition ofwater it can easily be re-molded into a lump ofclay, or, with the Ma addition of temper and subsequent firing, it can be fashioned into a pottery vessel. Although it is not suggested that all pottery vessels were made from lumps of clay which were carried from one site to another, it is probable that some vessels were made from such imported raw material. A final possibility is simply that the clay samples obtained from the O'Neil Site and the Skegemog Point Site were representative of various stages of clay preparation. Thus samples 41 and 42, which were noted as having some temper in them, may represent the stage of clay preparation just prior to its being shaped into a vessel, whereas other clay samples might have been discarded or lost by the potter prior to the addition of temper. Further investigations into the range of variation of the natm'ally- occm'ring geologic clays are necessary before these premises can be considered more fully. Given the large variability in the analytical results of both the clay samples and the pottery samples, the small tightly-clustered group of three Juntunen Ware vessels, (represented by Samples 53Nl, 53N2, 54, 56 and S7) is quite unexpected. This small group of vessels represents the only cluster of pottery whose members are comprised of the same pottery type. Yet the similarity between the members of this group is greater than that between some lumps of clay collected together at the same site. This suggests that these vessels were manufactrned from identical or nearly-identical raw materials, and possibly by the same potter or group of potters during a single work episode. The question of where these vessels were manufactrned still cannot be not resolved, but a close temporal and spatial relationship between these vessels is suggested. A novel application of this method of analysis thus emerges from these results. Although the analysis of ceramics for gross 93 similarities between pottery types has proven to be difficult due to the potential variability of the clay and temper, this technique may be useful in determining whether any vessels at a given site were made with the same raw materials, and presumably by the same potter(s) atroughly the same time period. Finally, the near absence of clusters of the same p0ttery typemaybeafrn'therindicationofthe wide availability ofraw materials forpottery making, as well as a potential marker of the relatively mobility of the groups manufacturing thepottery. Future Directions Previous investigations of paste composition have shown that INAA is useful in helping to identify somces of clays used for pottery making among settled populations. It has also been used with some success on a regional level for more mobile hunter-gatherer populations. However, more work is needed to determine whether this method is useful in the intra-site analysis of hunter-gatherer behavior. Of primary importance for futru'e work on paste composition in the Great Lakes area is a determination of the name] range of variation in the chemical composition of geologic clays collected from particular regions. This would require an intensive and systematic sampling program of geologic clays tluoughout Michigan and other areas. Additionally, it would be useful to include samples of archaeologicallysderived clays in order to determine whether these clays are representative of nann'al clays from the region. The analysis of archaeological clays alongside natm'al clays could also help establish whether the archaeological clays had been modified in prehistory by the addition of other materials. It may also help determine whether the clays found in archaeological contexts are native to the region of study. In addition to analyzing the clays fiom various regions, it would also be useful to analyze Late Woodland pottery collections fiom nearby sites in order to establish the 94 relationship between the pottery from the O'Neil Site and similar pottery from neighboring sites. This would help determine whether or not the pottery collected from within small geographic areas in Michigan can be differentiated on the basis of paste composition. It would also help establish the general relationship between raw clay samples and pottery samples recovered from various archaeological sites. Finally, any ftu'ther work on the analysis of pottery composition within small regions should take into account the effect of temper on the final concentration of elements in the pottery samples. If temper cannot be avoi®d in the sampling process, care should be taken to analyze enough temper samples to enable the effects of this material to be "subtracted" from the communion values of the whole pottery samples. Alternatively, methods for separating ground temper from powdered clay could be explored. If such separations are possible, this would enable the individual components of pottery to be analyzed separately, and would permit the comparison of pottery clays to geologic clays. The use of Instrumental Neutron Activation Analysis for the determination of pottery paste composition is relatively rare in the Upper Great Lakes. Research has indicated that this method can be useful in large-scale regional studies relating the composition of pottery paste with past human behavior. This study has shown that archaeologically-derived clays from closely-spaced sites can be differentiated by INAA. However, the determination of the relationship between these clays and archaeologically- related pottery sherds is difficult to establish, presumably due to the effect of temper which is incorporated into the pottery samples, and possibly also because of the natural variation between clay samples collected from the same site. It is hoped that future work in the area of paste composition analysis can resolve some of the methodological problems identified in this study. NOTES The MSU Museum, Anthropology Division catalogue number consists of a unique . accession number which identifies the site, as well as a series of decimal suffixes whrch identify the provenience of the artifact within the site. The Minimum Vessel Sheets (Lovis n.d.) are internal worldng documents originally used to assist in the analysis of the O'Neil Site pottery. The vessel numbers assigned to each vessel are recorded only on these Minimum Vessel Sheets and in the storage boxes where each individual vessel is stored. The original Minimum Vessel Sheets do not indicate the type/variety designation of each vessel. In fact, no listing correlating vessel numberstopotterytypescouldbeobtained. Densities were not measured, but were noted visually as gross difi‘erences in volume (height of sample in the sample tube) relative to the weight of the samples in the tubes. This process is performed in two steps. First the K, or constant (in cps/mg/ppm) for each element in each standard is calculated according to the equation: [(Peak area std " BaCkgrOund area std) / live counting time std] e (0-693)(l / T) K std = (Mass std) (Concenuation std) where t= decay time in seconds for each element (relative to the time of irradiation, t o) and T = half-life in seconds for each element In addition, the counting error associated with each peak in the standard is calculated according to the formula: 95 96 l ErrorofPeakstd = [2(backgroundareastd)-t-areaofpeakstd]I2 This error value for the peak is then plugged into the formula for the constant K std in order to yield an error associated with K std. or Error ofK std. An additional error associated with the concentration of the standard (i.e. the "error" of the concenu'ation value) is not used in this analysis because the current software package is incapable of handling this variable. Other potential sources of error which affect the calculated values of K include variations in the neutron flux received by each sample due to the sample's position in the reactor, errors in weighing the samples and standards, errors related to the determination of the concentration of elements in the standards (leading to later calculation errors), and errors due to non-homogeneous standards (Meyers and Denies 1972: 21). Due to the many sources of error, Birdsall (personnel communication 1991) estimates that the final concentration values obtained from INAA at this facility are within t 10% of the true values for these concentrations. OncetheK stdvalues and associatedenorvalues foreach elementin the standardare calculated, the mean K std ( or K std "bar") is calculated using the equation: Estd = (E: Kstdi) / n i=1 where n= numberofstandardsin each batch and the error of K std (error K std "bar" ) is calculated according to the equation: Errorof I-(std = {(5 [ErrorosttdiPN/z} /n 1:! (Edward Birdsall, personal communication 1991). The second part of the computer calculation involves the calculation of the concenuations of elements in each sample. This is done according to the following equation: [(Peak area spl - Background area spl) / live counting time SP1] e (0693th T) (Mass spl) Cone 3p] = Kstd 97 where K std , t and T are as defined above. (Edward Birdsall, personal communication 1991). Likewise, the calculation of the counting error associated with each peak in the sample is analogous to the calculation performed for the standards. Thus 1 ErrorofPeakspl = [2(backgroundareasp1)+areaofpeaksp1] ,2 The concentration represented by this enor estimate is obtained by plugging this value into the formula for determining the concenu'ation of each element in the sample, or Cone 3131- Once the concentration errors related to each peak in the standards and samples are established, a "standard deviation" (or error estimate for each concentration measm'ement) can be determined for each concentration determination according to the equation: Std. Deviation = {(21,1 [Error of {($412 + [Error of sample]2 )1/2} / n 1 The concentration values for each of the elements, as well as the associated standard deviation values for each sample are reported in Appendix A. 5 Ifthe greatest amount oflron in the samples is 7.1%, and the least amount of Iron in the bits is 82.5%, then the greatest level of contamination of the samples by the bits is [ (7.1% Fe in samples) / (82.5% Fe in bits) ] x 100% = 8.6% APPENDICES APPENDIX A 98 APPENDIX A Concentration and Standard Deviation Results (All Elements) COUNTED AFTER 1 WEEK OF DECAY Barium Barium Barium Barium Barium Barium 7 7 496.3 Cone % Std Dev Cone ‘5 Std Dev Cone % Std Dev 1 99 APPENDIX A (cont'd) Concentration and Standard Deviation Results (All Elements) COUNTED AFTER 1 WEEK OF DECAY Barium Barium Barium Barium Barium Barium 7 7 496.3 496.3 Cone % Std Dev Cone it Std Dev Cone % Std Dev not not not not not not not not not not not not §§§§§§ 100 APPENDIX A (cont'd) Concentration and Standard Deviation Results (All Elements) COUNTED AFTER 1 WEEK OF DECAY Bromine Bromine Bromine Bromine Lanthanum Lanthanum .4 4 15 15 Cone ‘5: Std Dev Cone ‘5 Std Dev Cone % Std Dev < not not not BO! 00! 101 APPENDIX A (cont'd) Concentration and Standard Deviation Results (All Elements) COUNTED AFTER 1 WEEK OF DECAY Bromine Bromine Bromine Bromine Lanthanum Lanthanum .4 .4 15 15 Cone 5 Std Dev Cone % Std Dev Cone % Std Dev §§§§§§§§§§§§§§§§ not not not not not not not not not not not not not not not not not not not not not not not not not not not not §§§§§§§§§§§§§ 3 5 § 5 5 5 E 5 5 § § § 5 5 § § 5 102 APPENDIX A (cont'd) Concentration and Standard Deviation Results (All Elements) COUNTED AFTER 1 WEEK OF DECAY Lutetium Lutetium .7 .7 Cone ‘1» Std Dev Cone ‘5 Std Dev Cone % Std Dev 5 AAAAA < < < < < < < < < AAA 103 APPENDIX A (cont'd) Concentration and Standard Deviation Results (All Elements) COUNTED AFTER 1 WEEK OF DECAY Lutetium Lutetium 140.5 40.5 .7 .7 Cone ‘5 Std Dev Cone ‘5 Std Dev Cone ‘5 Std Dev < not not stds not not not < not not not not not not not not not not not not not not not not not not not not not not not not not not not not 5 555555 3 i 104 APPENDIX A (cont'd) Concentration and Standard Deviation Results (All Elements) COUNTED AFTER 1 WEEK OF DECAY Samarium Samarium 1.2 1.2 1.2 03.2 03.2 ‘5 Std Dev Cone ‘5 Std Dev Cone “lb Std Dev 105 APPENDIX A (cont'd) Concentration and Standard Deviation Results (All Elements) COUNTED AFTER 1 WEEK OF DECAY Samarium Samarium 1.2 1.2 1.2 03.2 03.2 it Std Dev Cone % Std Dev Cone % Std Dev 1 1 not not not not not not not not not not not not not not not not not not not 106 APPENDIX A (cont'd) Concentration and Standard Deviation Results (All Elements) COUNTED AFTER 1 WEEK OF DECAY Urani- Uranium Uranium Uranium Uranium Uranium .5 .5 06.1 06.1 .7 7 Cone % Std Dev Cone ‘5 Std Dev Cone ‘5 Std Dev 1 5. not not not not not not not not not not not not 107 APPENDIX A (cont'd) Concentration and Standard Deviation Results (All Elements) COUNTED AFTER 1 WEEK OF DECAY Uranium Uranium Uranium Uranium Uranium Uranium SPL Q .5 .5 06.1 06.1 .7 .7 Cone ‘5 Std Dev Cone % Std Dev Cone ‘5 Std Dev 1 not not not not not not not not not not not not not not not not not 108 APPENDIX A (cont'd) Concentration and Standard Deviation Results (All Elements) COUNTED AFTER 1 WEEK OF DECAY Ytterbium Ytterbium Ytterbium Ytterbium Cone 9b Std Dev Cone % Std Dev 1 109 APPENDIX A (cont'd) Concentration and Standard Deviation Results (All Elements) COUNTED AFTER 1 WEEK OF DECAY Ytterbium Ytterbium Ytterbium Ytterbium SPL # Cone it Std Dev Cone ‘5 Std Dev not not not not not not 353533 l 10 APPENDIX A (cont'd) Concentration and Standard Deviation Results (All Elements) COUNTED AFTER 5 WEEKS OF DECAY Cerium Cerium Cesium Cesium 690.7 45.5 45.5 % Std Dev Com: ‘5 Std Dev Cone l ll 1 APPENDIX A (cont'd) Concentration and Standard Deviation Results (All Elements) COUNTED AFTER 5 WEEKS OF DECAY Cerium Cerium Cesium Cesium 690.7 45.5 45.5 ‘5 Std Dev Cone ‘5 Std Dev Cone not not not not not not not not not not not not 1 12 APPENDIX A (cont'd) Concentration and Standard Deviation Results (All Elements) COUNTED AFTER 5 WEEKS OF DECAY Cesium Cesium Chromium Chromium Cobalt .7 .7 1332.5 Cone ‘5 Std Dev Cone '5 Std Dev Cone 1 13 APPENDIX A (cont'd) Concentration and Standard Deviation Results (All Elements) COUNTED AFTER 5 WEEKS OF DECAY Cesium Cesium Chromium Chromium Cobalt Cobalt .7 7 Cone ‘5 Std Dev Cone ‘5 Std Dev Cone % Std Dev 1 not not not not not not l 14 APPENDIX A (cont'd) Concentration and Standard Deviation Results (All Elements) COUNTED AFTER 5 WEEKS OF DECAY 085.6 112.2 1112.2 1408.1 ‘5 Std Dev Cone ‘5 Std Dev Cone 1 15 APPENDIX A (cont'd) Concentration and Standard Deviation Results (All Elements) COUNTED AFTER 5 WEEKS OF DECAY SPL # 1085.6 1085.6 1112.2 1112.2 1408.1 Couc 96 Std Dev Cone ‘5 Std Dev Cone 1 1 not not not not not not not not not not 1101. not not 110! not 1 16 APPENDIX A (cont'd) Concentration and Standard Deviation Results (All Elements) COUNTED AFTER 5 WEEKS OF DECAY Gadolinium Gadolinium Hafuium Hafnium Iron SPL 6 103.3 103.3 482.3 482.3 099.3 Cone it Std Dev Cone ‘5 Std Dev Cone not l 17 APPENDIX A (cont'd) Concentration and Standard Deviation Results (All Elements) COUNTED AFTER 5 WEEKS OF DECAY Gadolinium Gadolinium Hafnium Hafnium Iron SPL # 03.3 03.3 482.3 482.3 099.3 Cone ‘5 Std Dev Cone % Std Dev Cone < 1 <1 < l. §§§§§§§§ not not not not not not l 18 APPENDIX A (cont'd) Concentration and Standard Deviation Results (All Elements) COUNTED AFTER 5 WEEKS OF DECAY Iron Nickel 1.6 .2 .2 10.8 ‘5 Std Dev Cone ‘5 Std Dev Cone not not not 110! not not not not not not not not not not not not not not not iii 119 APPENDIX A (cont'd) Concentration and Standard Deviation Results (All Elements) COUNTED AFTER 5 WEEKS OF DECAY Iron Nickel 1291.6 .2 .2 10.8 5 Std Dev Corn: 5 Std Dev Cone not not not not not not not not not not not not not not not not not not not not not not not not not not not not not not not not not not 5 § § 5 5 §§§§§§§§§§§§§ §§§§§§§§§§§§§§§§ 120 APPENDIX A (cont'd) Concentration and Standard Deviation Results (All Elements) COUNTED AFTER 5 WEEKS OF DECAY Rubidium Rubidium Scandium Scandium Selenium Selenium SPL # 076.8 076.8 .3 .3 Cone 5 Std Dev Cone 5 Std Dev Cone 5 Std Dev 121 APPENDIX A (cont'd) Concentration and Standard Deviation Results (All Elements) COUNTED AFTER 5 WEEKS OF DECAY Rubidium Rubidium Scandium Scandium Selenium Selenium SPL 0 1076.8 1076.8 .3 .3 136.5 Cone 5 Std Dev Cone 5 Std Dev Cone 5 Std Dev not not not not not not 1'10! not not not not not not 122 APPENDIX A (cont'd) Concentration and Standard Deviation Results (All Elements) COUNTED AFTER 5 WEEKS OF DECAY Strontium Strontium Tantalum Tantalum Tantalum Tantalum SPL I 14.0 14.0 1189.1 189.1 1221.5 1221.5 Couc 5 Std Dev Cone 5 Std Dev Conc 5 Std Dev 5 3333 not not not not not not not not 123 APPENDIX A (cont'd) Concentration and Standard Deviation Results (All Elements) COUNTED AFTER 5 WEEKS OF DECAY Strontium Tantalum Tantalum Tantalum Tantalum 14.0 189.1 189.1 1.5 1.5 5 Std Dev Conc 5 Std Dev Cone 5 Std Dev 1 not not not not not not not not not not not not not not not not not not 555555 5555555 555555 555555 124 APPENDIX A (cont'd) Concentration and Standard Deviation Results (All Elements) COUNTED AFTER 5 WEEKS OF DECAY Terbium Terbium Terbium Terbium Thorium Thorium .4 .4 178.0 178.0 12.0 12.0 Cone 5 Std Dev Cone 5 Std Dev Cone 5 Std Dev not 125 APPENDIX A (cont'd) Concentration and Standard Deviation Results (All Elements) COUNTED AFTER 5 WEEKS OF DECAY Terbium Terbium Terbium Terbium Thorium Thorium .4 .4 1178.0 178.0 12.0 12.0 Conc 5 Std Dev Cone 5 Std Dev Com 5 Std Dev not not not not not not not not not not not not not 126 APPENDIX A (cont'd) Concentration and Standard Deviation Results (All Elements) COUNTED AFTER 5 WEEKS OF DECAY Thulium Tin Tin Zinc Zinc 3 1.7 1.7 15.6 115.6 5 Std Dev Cone 5 Std Dev Conc 5 Std Dev not not not ll)! 5555555555555555 a 5555555555555555555 5 5 not 1'10! not not not not 1101 not not not 1101 not not not not not not not not not 5555555555555555555 5 55 555555 5555555555 555555 127 APPENDIX A (cont'd) Concentration and Standard Deviation Results (All Elements) COUNTED AFTER 5 WEEKS OF DECAY Thulium Tin Tin Zinc .3 1.7 1.7 15.6 5 Std Dev Conc 5 Std Dev Conc < 5555555555 55555555555 5 9. 5 5 not not not not not 555 5555 555555 55 5 5 5 5 5 5555 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 128 APPENDIX A (cont'd) Concentration and Standard Deviation Results (All Elements) UNTED AFTER 5 WEEKS OF DECAY Zirconium Zirconium 7 7 Cone 5 Std Dev 129 APPENDIX A (cont'd) Concentration and Standard Deviation Results (All Elements) UNTED AFTER 5 WEEKS OF DECAY Zirconium Zirconium 7 7 Conc 5 Std Dev not not not not not 1101 not APPENDIX B 130 APPENDIX B Concentration and Standard Deviation Results (11 Elements) SAMPLE ELEMENT CONCENTRATION (PPM) Barium Barium Cerium Cerium Cesium Cesium SPL # 123.7 123.7 145.5 145.5 .9 .9 Cone 5 Std Dev Conc 5 Std Dev Cone 5 Std Dev 131 APPENDIX B (cont'd) Concentration and Standard Deviation Results (11 Elements) SAMPLE ELEMENT CONCENTRATION Barium Barium Cerium Cerium Cesium Cesium SPL # 7 7 45.5 45.5 Cone 5 Std Dev Cone 5 Std Dev Conc not not not not not not not not not not not not 132 APPENDIX B (cont'd) Concentration and Standard Deviation Results (11 Elements) SAMPLE ELEMENT CONCENTRATION Hafnium Hafnium Lanthanum Lanthanum 408.1 482.3 482.3 15 15 5 Std Dev Cone 5 Std Dev Conc 5 Std Dev 133 APPENDIX B (cont'd) Concentration and Standard Deviation Results (11 Elements) SAMPLE ELEMENT CONCENTRATION Hafnium Hafnium Lanthanum Lanthanum 1 15 15 5 Std Dev Cone 5 Std Dev Conc 5 Std Dev not not 1101 not not not not not not not not not 134 APPENDIX B (cont'd) Concentration and Standard Deviation Results (11 Elements) SAMPLE ELEMENT CONCENTRATION Lutetium Lutetium Samarium Samarium Scandium SPL # 03.2 03.2 .3 Cone 5 Std Dev Cone 5 Std Dev Conc 135 APPENDIX B (cont'd) Concentration and Standard Deviation Results (11 Elements) SAMPLE ELEMENT CONCENTRATION (PPM) Lutetium Lutetium Samarium Samarium Scandium Scandium SPL S 03.2 03.2 .3 .3 Cone 5 Std Dev Cone 5 Std Dev Cone 5 Std Dev 1101 not not not not 110i 110! 1101 not not not not 555555 136 APPENDIX B (cont'd) Concentration and Standard Deviation Results (11 Elements) SAMPLE ELEMENT CONCENTRATION Thorium Thorium Ytterbium Ytterbium SPL O 12.0 12.0 Cone 5 Std Dev Conc 5 Std Dev 137 APPENDIX B (cont'd) Concentration and Standard Deviation Results (11 Elements) SAMPLE ELEMENT CONCENTRATION Thorium Thorium Ytterbium Ytterbium SPL # 12.0 12.0 Cone 5 Std Dev Conc 5 Std Dev 1 not not not not not not not not not not not not APPENDIX C 138 APPENDIX C Concentration Values for 11 Elements, in Increasing Order mm mm Sample Cone. Sample Cone. Sample Cone. Sample Cone. Number (ppm) Number (ppm) Number (ppm) Number (ppm) 46 35.8 5 620 39 6.92 53N2 64.1 40 120 2 625 40 7.02 48 64.5 45 149 53N2 625 46 7.36 51 66.5 39 156 11 633 36 7.89 29 66.8 36 198 53N1 639 35 7.93 12 66.9 37 219 51 648 34 8.05 2 67.2 38 225 26 654 37 8.49 55 67.4 28 228 56 654 38 9.78 31 68.1 47 229 27 660 33 10.6 21 70.2 35 248 1 665 60 25.3 9 71.4 43 249 23 678 45 28.3 59 73.4 60 267 30 679 30 31.8 6 73.6 33 326 57 705 43 35.8 1 73.8 34 402 12 715 47 40.9 57 75 13 415 59 726 3 41.7 56 76.7 42 451 9 727 25 44.5 28 78.1 14 464 54 730 14 46.9 54 78.2 41 470 44 736 26 47.3 27 79.3 3 528 24 741 41 51 16 81.6 48 528 6 748 42 51.5 8N2 82.9 25 542 29 750 58 54.1 50 84.8 15 548 55 751 11 55.1 7 85.9 18 570 22 758 18 55.1 5 87.9 16 571 32 770 17 58.1 8N1 92.6 17 575 10 833 13 58.5 32 97.7 21 580 52 836 22 58.6 4 102 31 588 7 861 10 60.1 15 106 58 595 8N2 881 23 61.7 44 106 50 603 SN] 913 53N1 62.7 52 123 4 619 24 64.1 139 APPENDIX C (cont'd) Concentration Values for 11 Elements, in Increasing Order Caum i795 Kev; ‘ ‘ Europr'um Hm Kev; Sample Cone. Sample Cone. Sample Cone. Sample Cone. Number (ppm) Number (ppm Number (ppm) Number (ppm) 40 0.125 2 3.95 46 0.0501 29 1.01 35 0.127 55 4.15 33 0.108 48 1.02 33 0.183 50 4.16 35 0.115 59 1.02 36 0.191 12 4.26 39 0.121 10 1.03 34 0.193 7 4.32 36 0.125 17 1.03 37 0.242 5 4.47 34 0.131 21 1.06 38 0.256 52 4.65 40 0.134 56 1.06 39 0.348 13 4.81 38 0.147 6 1.07 46 1.08 21 4.89 37 0.156 24 1.07 60 1.8 9 4.96 47 0.182 18 1.09 11 1.83 8N2 4.97 60 0.219 15 1.1 45 2.08 3 4.98 43 0.286 50 1.1 47 2.24 10 5.06 45 0.333 31 1.11 43 2.28 16 5.1 30 0.491 55 1.11 4 2.37 58 5.18 3 0.605 52 1.14 25 2.45 54 5.42 58 0.757 1 1.15 41 2.65 51 5.43 11 0.767 23 1.15 42 2.74 26 5.5 41 0.775 51 1.17 31 2.91 8N1 5.73 26 0.799 7 1.19 27 3.02 53N2 5.76 13 0.826 4 1.2 48 3.13 57 5.8 14 0.863 32 1.2 24 3.26 6 5.98 2 0.898 27 1.22 30 3.44 53N1 6.03 22 0.902 8N2 1.23 18 3.45 28 6.16 44 0.925 16 1.26 1 3.47 29 6.84 28 0.933 54 1.26 59 3.61 56 6.89 25 0.944 5 1.33 15 3.71 32 7.02 53N2 0.97 8N1 1.33 23 3.74 22 7.7 57 0.971 12 1.33 14 3.75 44 13.4 53N1 0.992 9 1.38 17 3.77 42 1 140 APPENDIX C (cont'd) Concentration Values for 11 Elements, in Increasing Order um e Lanthanum iSIS KeWi Sample Cone. Sample Cone. Sample Cone. Sample Cone. Number (ppm) Number (ppm) Number (ppm) Number (ppm) 46 0.535 58 5.31 46 2.78 29 32.7 33 0.695 31 5.42 40 4.73 51 32.7 35 0.919 22 5.43 34 5.01 59 33.3 36 0.943 51 5.57 36 5.02 1 33.6 38 0.994 57 5.58 37 5.35 55 33.6 39 1.02 4 5.63 39 5.84 18 33.7 34 1.18 8N2 5.7 38 5.88 31 33.9 37 1.26 3 5.79 35 7.33 24 34.5 40 1.26 10 5.79 47 7.64 6 34.7 47 1.36 15 5.9 33 8.78 57 35.2 60 1.48 1 5.93 60 9.42 50 35.5 45 1.52 55 5.93 43 12.7 8N2 35.6 43 2 25 5.99 45 12.8 12 35.8 30 2.9 53111 6.08 30 17.2 32 36 41 3.53 32 6.13 3 19.1 48 36.3 14 4.25 7 6.27 41 22.5 7 36.4 18 4.51 8N1 6.27 14 23.3 56 36.5 44 4.58 54 6.35 26 23.6 54 36.7 50 4.62 56 6.4 25 25.2 5 36.8 42 4.65 5 6.46 58 25.3 9 36.8 23 4.68 9 6.53 42 26 23 36.9 29 4.7 16 6.64 11 26.8 8N1 37 24 4.73 11 6.65 2 30.2 16 37.6 6 4.77 12 6.77 10 30.9 21 37.6 17 4.89 59 6.81 17 31.9 27 38.7 26 4.91 53N2 7 22 31.9 15 44.3 48 4.95 27 7.52 13 32 4 44.9 13 5 2 7.58 53N1 32.2 44 45.9 21 5.21 28 7.98 53N2 32.2 52 61 52 5.29 28 32.7 Concentration Values for 11 Elements, in Increasing Order 141 APPENDIX C (cont'd) utetrurn e Sample Cone. Sample Cone. Number (ppm) Number (ppm) 46 0.0324 48 0.308 39 0.0334 23 0.312 35 0.036 18 0.314 34 0.04 59 0.315 38 0.0462 50 0.318 0.0481 15 0.319 33 0.0696 57 0.324 60 0.078 51 0.33 37 0.083 1 0.331 47 0.0918 21 0.333 36 0.105 53N2 0.336 30 0.132 53N1 0.339 43 0.148 6 0.342 45 0.154 10 0.347 58 0.231 56 0.35 14 0.237 8N2 0.352 41 0.245 54 0.355 26 0.254 52 0.356 11 0.257 27 0.358 3 0.261 22 0.361 25 0.267 28 0.363 13 0.269 8N1 0.364 24 0.278 4 0.395 17 0.29 12 0.396 2 0.291 9 0.397 42 0.295 16 0.397 31 0.297 7 0.399 55 0.299 32 0.445 29 0.301 5 0.457 44 0.301 armrrurn e , Sample Cone. Sample Cone. Number (ppm Number (ppm) 46 0.355 21 5.22 39 0.517 10 5.23 35 0.545 13 5.26 33 0.582 18 5.26 34 0.609 29 5.28 36 0.611 28 5.3 40 0.635 31 5.36 37 0.733 15 5.38 38 0.751 55 5.38 47 1.1 6 5.39 60 1.46 23 5.42 43 1.82 50 5.42 45 1.93 24 5.46 30 2.16 56 5.48 3 3.14 51 5.49 11 3.65 1 5.67 58 3.65 54 5.7 41 3.81 8N2 5.82 26 3.93 32 5.88 14 3.95 8N1 6.07 25 4.25 44 6.12 2 4.37 27 6.33 42 4.65 7 6.4 53N2 4.65 16 6.42 22 4.78 9 6.44 53N1 4.79 12 6.52 57 4.82 4 6.97 48 5.03 5 7.69 17 5.1 52 7.99 59 5.15 142 APPENDIX C (cont'd) Concentration Values for 11 Elements, in Increasing Order Sal-Iaium 1889 KEV) N onum e Sample Cone. Sample Cone. Sample Conc. Sample Cone. umber (PPIII) Number (ppm) Number (ppm) Number (ppm) ' 35 0.258 4 9.68 35 0.623 10 10.1 33 0.261 1 9.76 39 0.68 21 10.1 39 0.307 23 9.95 37 0.691 55 10.2 37 0.36 13 10.2 36 0.732 8N2 10.7 40 0.381 5 10.4 40 0.762 6 10.9 34 0.4% 21 10.5 34 0.78 29 1 1 36 0.4% 28 10.6 38 1.04 9 1 1.7 38 0.477 51 10.7 46 I.“ 50 12 46 0.914 50 10.9 33 1.08 8N1 12.4 47 3.04 52 10.9 45 2.83 27 12.9 45 3.22 27 11.1 47 3.38 12 13 60 3.6 2 11.2 60 3.95 22 13.1 43 4.34 10 1 1.3 43 4.94 57 13.2 30 4.59 15 1 1.7 30 5.32 2 13.3 25 6.74 16 11.8 41 6.35 1 1 13.3 41 6.83 8N2 11.9 42 6.7 13 13.5 42 7.49 7 12 14 7.16 7 13.6 14 7.78 6 12.1 26 7.63 59 13.9 58 7.96 12 12.3 48 7.75 32 14.2 31 8.56 56 12.7 25 7.98 44 14.4 26 8.59 22 13 31 8.02 16 14.5 18 8.67 8N1 13.2 58 8.13 53Nl 15.5 59 8.75 53N1 13.4 17 8.2 53N2 15.5 17 8.83 9 13.5 18 8.2 4 15.7 48 8.94 53N2 13.6 3 8.63 28 15.8 55 9.12 57 13.8 23 8.7 54 15.8 3 9.45 54 14 24 9.09 5 16.7 29 9.52 32 16.4 51 9.75 56 16.7 1 1 9.53 44 20.1 1 9.99 52 18.9 24 9.65 15 10 143 APPENDIX C (cont'd) Concentration Values for 11 Elements, in Increasing Order tte turn , Sample Cone. Sample Cone. Number (ppm) Number (ppm) 46 0.163 6 2.36 39 0.247 10 2.37 35 0.271 59 2.37 40 0.282 1 2.38 34 0.31 48 2.39 38 0.34 55 2.4 37 0.42 8N1 2.41 47 0.48 21 2.41 33 0.499 22 2.41 60 0.738 53N2 2.41 43 0.757 56 2.42 36 0.766 51 2.44 45 0.822 29 2.46 30 0.984 50 2.46 41. 1.61 8N2 2.51 58 1.67 15 2.54 11 1.7 57 2.54 14 1.87 28 2.6 25 1.94 54 2.61 26 1.95 53N1 2.7 44 2.02 32 2.71 42 2.03 9 2.74 13 2.04 12 2.82 24 2.12 27 2.83 23 2.16 16 2.9 3 2.21 52 2.93 17 2.22 4 3 2 2.25 7 3.21 18 2.3 5 3.5 31 2.31 APPENDIX D 144 APPENDIX D Barium (123.7 KeV) Deleted I I I I I I I I I I I I I I I I I I II II II I 9-I II I I I I I I I I I I I I I I I I l I I I I l I I I I I I I I I I I I .- __ E O O D, 1. 6 R ‘ mmumumunummumnmmuuumnnoummmmumu 811 I) II. ms I‘M I“ It! 823 a m 81! an an I! mmmumumuttnasm u. a. Centroid Linkage Dendrograms Using 10 of 11 Elements .1. m m m D m m 145 APPENDIX D (cont'd) - -2 _ ................................................................................. .uwmeum-uta — . _ Cert. (145.5 KeV) Deleted I I I I I I I I I I I I I I I I I 1 _ ‘7 ’5 8843 3 6 I I 0.8 7.. 0 6 m.m.m.mm............m.am..mn.»...uums.mamauaamaaam.mmms.m.. Centroid Linkage Dendrograms Using 10 of 11 Elements 146 APPENDIX D (cont'd) Cesium (795.9 KeV) Deleted Centroid Linkage Dendrograms Using 10 of 11 Elements d ..... _ _ __ ____-.__ __ ‘ T 3 : ‘Oa‘ at, D. .1 ‘ ' gammamummum-mumumuuuunnuumunummmnummnnmmmmmmmmnmmu-mnmm ummeramurmwunmm 147 APPENDIX D (cont'd) Europlum (1408.1 KeV) Deleted Centroid Linkage Dendrograms Using 10 of 11 Elements mmmmmamnum __ a»: 8 1 numuunun-m 1 G 3 41 uunmmaumummn I .. m m m m u m m 148 APPENDIX D (cont'd) Hamlum (482.3 KeV) Deleted I 0'- I II I II I II I II I II I II I II I II I II I II I II I II I II I II I II I II I II I “II I II I 9—II I II I I I I I I I I I ’ D .1 O 1 0 an t : Cal 21 s, 1‘ womanmumnumunnmmnmnnuuumumnumm—uuammmnmnnumuamuumuummmmmmmm m ......... ...--.- M m m n m m Centroid Linkage Dendrograms Using 10 of 11 Elements 149 APPENDIX D (cont'd) 11111111 Lanthanum (815 KeV) Deleted 'T I I i I i E i I I I I I I i i l I I I I I :- O .7 O: T o D a o 1 mnunmumunmmmoummamnunun—mummmummuommnnmmmu «magnum Centroid Linkage Dendrograms Using 10 of 11 Elements D!“ “C 18 marma- urea-n. me In!“ turn ISII APPENDIX D (cont‘d) L: kmuuhl __.r_: Ianeflunr(2085ilhwn Defined m m ---_- -.--wawwwwwmmwwwwmwwumuflwna m tit—t _ t—tetct _ .. m m m s O . T o T O a ) r C 1 1a 3 i 1 O o u.m...m..m”sameness..m...u.a..s..nmm.am..m.u.m..a...mmam.mm Centroid Linkage Dendrograms Using 10 of 11 Elements 151 APPENDIX D (cont'd) Samarium (103.2 KeV) Deleted ..... _H-- _ no} _a_ s .‘T . .3 1. 0", 3.1.... ,, mmuummmmmunnmmnmnuanceuuummuummmunumnommmununmuumm ::ummm Centroid Linkage Dendrograms Using 10 of 11 Elements arm ”16 I. mama- arm. me In!" turn 152 APPENDIX D (cont'd) O .- “WU _ _ .3 _ Scandium (889.3 KeV) Deleted I I I I I I I I ., 3 O s 7. s, O s ‘11 ,3 7 ‘7 m....mmauu.smammasam..msma.mmaammnma.asmanauau.amumaammm Centroid Linkage Dendrograms Using 10 of 11 Elements mam-stunt: IIMDIM moms-nun 153 APPENDIX D (cont'd) Centroid Linkage Dendrograms Using 10 of 11 Elements Thorium (312.0 KeV) Deleted euttttet :i. __ s o 1 I. a ‘ 5’ .‘T 3 3 m...m.am.aum.mams...ua"an.a.m.aam.mmaammu a m m m m m m m m m m m m m m m m m m m m 154 APPENDIX D (cont'd) Centroid Linkage Dendrograms Using 10 of 11 Elements Ytterbium (396.5 KeV) Deleted .- II II II II II O-I I 9.. i Q- I mumnmmmmttmasm an an II m 111111111111111111111111111111111111111111111111111111111111111111111111111111111 ’ m 1111111111 cram-m mare ll mama: arm. we in!" m APPENDIX E 155 00.0 00.0 00.0 00.01 00080 . 00.0 000 00.0 00.0 00.01 00.01 0080 . 00.0 000 00.0 00.0 00.0 00.0.. .380 . 00.0 000 00.0 00.01 00.01 00.01 :3 _ 00.0 000 00.0 00.0 00.01 00.01 0980 . 00.0 000 00.0 00.0 00.0 00.0 0080 . 00.0 000 00.0 00.01 00.01 00.01 0.80 . 00.0 000 00.0 00.0 00.01 00.01 $080 _ 00.0 000 00.0 00.01 00.01 00.01 380 . 00.0 000 00.0 00.0 00.0 00.0 (.080 _ 00.0 00.0 00.0 00.0 00.0 00.0 g _ 00.0 000 408.0. g; It! 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