Current research on smoking pipe residues

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Journal of Archaeological Science 39 (2012) 1951e1959

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Journal of Archaeological Science

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Current research on smoking pipe residues

Sean M. Rafferty*, Igor Lednev, Kelly Virkler, Zuzana ChovanecUniversity at Albany, Department of Anthropology, 1400 Washington Ave., Albany, NY 12222, USA

a r t i c l e i n f o

Article history:Received 1 February 2011Received in revised form30 January 2012Accepted 2 February 2012

Keywords:Residue analysisRaman microscopyGCeMSTobacco

* Corresponding author. Tel.: þ1 518 442 4713.E-mail address: [email protected] (S.M. Rafferty

0305-4403/$ e see front matter � 2012 Published bydoi:10.1016/j.jas.2012.02.001

a b s t r a c t

This paper presents research into the identification of tobacco residues in ancient smoking pipes. Twotechniques have been used so far: gas chromatography/mass spectroscopy (GC/MS), and Ramanmicroscopy. GC/MS has been used successful in the past by the author to identify ancient tobaccoresidues, and the results of this round of analysis support prior research. Raman microscopy, which hasthe advantage of working on dry samples without solvents, was not successful. It appears thatcombustion products overwhelm any useful signal that would identify the substance smoked. We arepursuing the use of Raman in non-combusted samples.

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1. Introduction

This paper presents recent research results on smoking piperesidues using two analytical techniques: Raman microscopy andgas chromatography/mass spectroscopy (GCeMS). This focus of theresearch represents is the application of residue analysis to thedetection of intoxicant compounds. These two analytical methodsare applied to both experimental preparations of smoking piperesidues as well as to a sample of archaeological residues. Researchresult so far indicate that, while Raman microscopy has significantlong term potential for archaeology, additional methodologicaldevelopment is needed for its widespread application to organicresidues. GCeMS continues to be a viable technique for the analysisof smoking pipes, and current results are presented.

2. Research questions

Previous research on this topic used gas chromatographyemassspectroscopy (GCeMS) to identify nicotine degradation products inthree archaeological pipe specimens: a nineteenth-century pipefrom Ghana, and two Early Woodland Period pipes from EasternNorth American sites dating to between 2300 and 2500 B.P.(Rafferty, 2002, 2006).

The current stage of research investigates two research ques-tions. The first is the potential for using Raman microscopy onsmoking pipe residues. Raman microscopy is a highly accuratetechnique that requires minimal preparation of samples. Raman

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can detect the presence of compounds of interest directly from thesolid phase, in situ on an artifact’s surface. Growing interest inapplication of Raman spectroscopy in art and archaeology duringthe last decade is well described in a recent review (Vandenabeeleet al., 2007).

Current developments of Raman spectroscopy at the Universityat Albany department of chemistry (Lednev et al., 2005, 2006) havefurther improved the technique by allowing the analysis ofheterogeneous samples through statistical analysis (Shashilov et al.,2006) of multiple observations of a single sample. This is ideal forarchaeological samples, which are rarely homogenous.

Ramanmicroscopy has been applied in recent years to a numberof archaeological case studies, rock art and tomb paintings (Smithand Barbet, 1999), ceramic pastes and glazes (Bruno et al., 1997;Clark and Curri, 1998), ancient glass (Bouchard and Smith, 2002),stone tools and ancient metals (Gendron et al., 2002; McCann et al.,1999; Smith and Gendron, 1997), ancient textiles and pigments(Edwards et al., 1997; Wiedemann et al., 2002), and ancient organicresidues (Edwards et al., 1998), including residues associated withopium (Schultz et al., 2004). Results of the research presented hereinindicate that,while Ramanmicroscopy is a powerful technique, thereare some unique challenges posed in analyzing organic residues.

The second research question was does additional researchsupport previous research on smoking pipes. Previous GCeMSresearch (Rafferty, 2002, 2006) indicated an early adoption oftobacco in the Eastern Woodlands. That assessment was based ona small sample, and it was important to see if additional specimenswould corroborate earlier results. Results of this research showcorroboration for one pipe sample, but more equivocal results fortwo others.

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3. Current research

Initial use of Raman microscopy was promising. Standards ofpure nicotine were prepared on foil targets. Three samples wereprepared; two were subjected to artificial aging by heating andultraviolet light exposure. Clear spectra were recovered for theunmodified and aged samples, with slight differences betweenthem (Fig. 1). This showed that Raman can identify nicotine, andthat it may be useable to determine between “fresh” and agedsamples of nicotine.

The next step was to prepare samples of tobacco residuethrough controlled combustion of samples of Nicotiana rustica“Native Tobacco” and analyze the residue via Raman to ascertain ifnicotine was detectable. It was here that we ran into seriousproblems. At first it seemed that we had a clear spectrum fortobacco residue. However, we checked this spectrum against onederived from burned paper and found the two spectra to be iden-tical. This indicated that either general combustion products oforganic material, or the fluorescence of the residue, or both, over-whelm any nicotine present in the sample. In hindsight this is notsurprising as nicotine is present in minute abundance even in freshtobacco leaf. I will note in brief that the opium aspect of theresearch also met similar problems using Raman. These negativeresults raise concern about the suitability for Raman for the analysisof organic residues. Consultation with the co-Principal Investigatorfor the NSF research concluded that fluorescence is a seriousproblem for darker colored substances. Given that most organicresidues are by nature dark in color, this could prove a seriousliability for the technique.

As we were at an impasse with regards to Raman microscopy,we turned to “conventional” residue analysis techniques usingGCeMS, which had proven successful in the analysis of NorthAmerican artifacts in recent analyses (Reber et al., 2010;Tushingham et al., 2010). This research took the same approach asthe Raman analysis, in that the technique was first applied toexperimentally produced residues to verify efficacy, and then toarchaeological contexts.

GCeMS analysis followed a modified version of previouslysuccessful protocols (Rafferty, 2002, 2006), themselves adaptedfrom Gager (Gager, 1991) and by Zahlsen and Nilsen (Zahlsen andNilsen, 1994). Alkaloids were extracted from residues through the

Fig. 1. Raman spectrum of nicotine.

elution of methylene chloride. The resultant solution was thenconcentrated via evaporation under nitrogen flow. The concen-trated solution was then injected into the GC/MS instrument (HP6890 GC, 5972AMass Selective Detector, 1 ml auto-injector, HP-5MS30m� 0.25mm� 250 mm column). GC settings started at 150 �C for2 min, then ramped up at 10 �C/mine180 �C, for a total run time of5 min. Due to the small abundances of the compound beinganalyzed, MS proceeded using select ion monitoring for four ions(m/z of 84, 133, 161 and 162 respectively). While this is somewhatdifferent equipment than had been used in past analyses (mostsignificantly an HP-5 column as opposed to an HP-1 column), it isshown below that the instrumentation was effective in detectingnicotine in organic residues of varying ages.

First, standard solutions of pure nicotine were analyzed; in allcases the instrumentation was able to identify nicotine at a reten-tion time of 2.7min (Fig. 2). This shows that the instrumental set upis effective at detecting nicotine in organic residues. It should benoted that this is a significantly shorter retention time than hasbeen identified in previous research. This was not intentional onthe part of the researchers, as a measure to allow more rapidanalysis for example. Rather, it was an unavoidable side effect ofusing different instrumentation. Regrettably we were limited toinstrumentation available in the University at Albany Departmentof Chemistry.

Second, artificially prepared N. rustica residues were analyzed.Residues were prepared by reverse airflow combustion in a lab-produced ceramic pipe with paste and temper characteristicscongruent with prehistoric Native American examples (i.e., air wasblown through the bowl of the pipe, with the smoke being directedinto a fume hood). This created a viable pipe residue without thenecessity of smoking the tobacco directly or exposing researchersto “second hand” smoke. Nicotine was again identified in thisspecimen (Fig. 3).

These initial steps ensured that the extraction and detectionprotocols were appropriate for the detection of nicotine from burntorganic residues. Once the extraction and detection protocols wereknown to be functioning as expected, the technique was applied toarchaeological samples. The first of these was a mid-18th centuryspecimen from New Jersey. Nicotine was again detected in thisarchaeological sample (Fig. 3). Given the relatively recent date ofthe specimen and the clear Euroamerican manufacture, it wasexpected that this pipe was used for tobacco, and the successfuldetection of nicotine shows that tobacco residue remains detect-able in archaeological contexts over relatively short periods of time.

Finally, three pipe specimens of considerably greater age wereanalyzed. These pipes were recovered from the Mathies Moundsite, the Quaker State Rockshelter, and the Glenshaw Rockshelter,all located in Western Pennsylvania (Fig. 4). Residue samples fromthese pipes were generously donated by the Carnegie Museum ofNatural History where all three specimens are curated. All three arestylistically similar to specimens dated to the Early WoodlandPeriod, from approximately 2,000 to 3000 B.P. (Fig. 5).

A radiocarbon date of 2541 � 51 B.P. was derived for the QuakerState Rockshelter pipe (AA89866). This date yields a calibrated twosigma range of between 809 and 510 B.C.; the Adena affiliation ofthe site would indicate an origin towards the recent end of thatrange, most likely during the 6th century B.C. Therewas not enoughresidue for a date for MathiesMound, and regrettably a radiocarbonsample taken for the Glenshaw Rockshelter was lost in transit tothe lab.

All three of these residue samples tested positive for the pres-ence of nicotine, though the quality of the results varies among thesamples. The Mathies Mine site had the clearest chromatographicpeak (Fig. 6). While the abundance for this peak is relatively low,presumably due to the extreme age and small size of the sample,

Fig. 2. GCeMS spectrum of nicotine.

S.M. Rafferty et al. / Journal of Archaeological Science 39 (2012) 1951e1959 1953

the peak is discrete and is located at the right retention time fornicotine. The Glenshaw Rockshelter and Quaker State Rockshelterhad less clear chromatographic peaks, with the nicotine peakblending into a “plateau” on the chromatogram (Figs. 7 and 8). Thisfeature does begin at 2.7 min, the retention time for nicotine, and

does produce a positive mass spectrum identification for nicotineas well. While it is plausible that tobacco was smoked in these twopipes, the data is supportive, but not conclusive.

A caveat must be included at this point that the chromato-graphic peak that showed a mass spectrum of nicotine was of

Fig. 3. GCeMS spectrum for an 18th century smoking pipe.


extremely low abundance in all three cases, and that other, non-nicotine compounds that also include the four target ions couldgive false positives. However, the GC peak is at the same retentiontime (2.7 min) for nicotine derived from our control samples ofpure nicotine, and the MS identifications were at confidence levelsof over 80%; false positives are generally of much lower confidencefor this instrument. We are therefore reasonably confident thattobacco was smoked in each of these pipes. Regrettably the avail-able samples were all very small, less than 0.1 g each, and all weretotally expended in the residue analysis and AMS dating describedin this article.

4. Discussion

Raman microscopy is a powerful analytical technique, withgreat potential for archaeological analysis. However, based on ourcurrent results the technique is not yet able to detect low-abundance compounds in heterogeneous organic residues. Weare currently pursuing research on other substances, such as honeyor blood, where we expect a lower chance of sample fluorescence.

Our research shows that current GCeMS instrumentation andexisting analytical protocols are appropriate for the detection ofnicotine, and by extension, of tobacco, in prehistoric residues. Thiswas demonstrated by the detection of nicotine experimentalstandards and artificial residues, as well as a relatively recentarchaeological sample. When applied to a sample of much older

archaeological samples, the technique provided results whichsupport previous research indicating an Early Woodland intro-duction of tobacco into the Eastern Woodlands, between 2500 and3000 B.P.

This is significant as the current state of ethnobotanical datafor tobacco dates to the first century A.D., centuries after thedates of the smoking pipes analyzed in this research program sofar. The earliest archaeobotanical evidence of the use of tobaccoin eastern North America comes from the central MississippiValley between A.D. 100 and 200 (uncalibrated) (Asch, 1991;Asch, 1994; Haberman, 1984; Wagner, 2000; Winter, 2000a), withdates for the rest of Eastern North America falling severalcenturies later (Haberman, 1984; Von Gernet, 1992). Recentlyderived dates from the Southwest are earlier, with specimensfrom New Mexico dated to 1040 B.C. (Bohrer, 2004; Winter,2004). This indicates that tobacco was introduced into theSouthwest through Mexico along the same route as cultigenssuch as maize, and reached the Eastern Woodlands through theGreat Plains, most likely sometime in the mid-first millenniumB.C. based on our residue analysis data.

Documenting the early origin and spread of tobacco use is morethan a botanical curiosity. N. rustica was used by Native Americansin eastern North America at the time of contact, and has the highestnicotine content of any tobacco species. Nicotine causes tachy-cardia, vasoconstriction, and increased alertness. In large dosesnicotine has hallucinogenic effects (Joniger and Dobkin de Rios,

Fig. 4. Location of prehistoric smoking pipes analyzed.


1973; Joniger and Dobkin de Rios, 1976). Tobacco is safer than otherEastern North American psychoactive plants such as Datura, andmay have been adopted as a foreign alternative to potentiallydangerous local intoxicants (Goodman, 1993; Von Gernet, 1992;Winter, 2000b). Tobacco’s allure to prehistoric peoples was likelyexacerbated by the lack of any significant indigenous history of

Fig. 5. Images of smoki

fermentation of alcoholic beverages, which is the most commontype of intoxicant across most of world cultures today.

While there has been significant research on the prehistory oftobacco use in North America, there are still questions regardingthe chronology and geographic patterning of tobacco’s adoption.Ethnohistoric evidence indicates that the use of tobacco was

ng pipes analyzed.

Fig. 6. GCeMS spectrum of Mathies Mine pipe.


ubiquitous to Native American cultures at the time of contact(Springer, 1981). A practice with such a wide geographic distri-bution should have deep prehistoric roots, but the chronology ofits origin and spread is still poorly understood due to a lack ofbotanical data.

The effects of a particular intoxicant compound have a majoreffect on the sociocultural aspects of its use (Dobkin de Rios, 1975;Dobkin de Rios, 1984). The effects of high doses of nicotine, such as“out of body” or flying sensations, presumably affected ritualpractices in prehistoric Eastern North America, especially birdrepresentations exhibited found I a range of artistic media (Dobkinde Rios, 1976).

Our research into the prehistory of tobacco use through residueanalysis evidence shows that the early history of tobacco may be

longer than previously supposed. Some researchers have proposedthat tobacco was recently introduced into Eastern North America(Ford, 1981; Knight, 1975; Watson, 1989; Yarnell, 1964). Were thisthe case, it would imply that smoking pipes predating predate thesecond century A.D. would have been used to smoke somethingother than tobacco. The results of our research show that suchassumptions need further evaluation.

Limitations in the research program remain, and will providedirections for future investigations. We have not yet tackled theproblem of correlating abundance of nicotine in experimental orarchaeological residues, with the concentration of nicotine in theoriginal plant smoked. While it may be possible to make thiscorrelation for experimental residues, where the startingconcentration of nicotine in the tobacco plant tissue can be

Fig. 7. GCeMS spectrum of Quaker State Rockshelter pipe.


known in advance, the lack of this starting point datum, as wellas a wide variety of taphonomic processes that would degradethe abundance of nicotine over time, may make it very difficult ifnot impossible to determine this relationship for archaeologicalsamples. This is significant, in that it will likely limit our ability todetermine empirically the actual species smoked in prehistoricpipes based on residue analysis. While ethnobotanical evidenceindicates N. rustica was used in the Eastern Woodlands in the

early First Millennium A.D., we will likely have to wait foradditional botanical samples to extend this date earlier to meetthe date for a general species of tobacco based on residue anal-ysis. In short, we know prehistoric Native Americans weresmoking tobacco, we just can’t yet confirm that the species wasN. rustica.

We have also not determined what plants other than tobacco,if any, may have been smoked in prehistoric Native American

Fig. 8. GCeMS spectrum of Glenshaw Rockshelter pipe.


pipes. Ethnohistoric accounts indicate a variety of plants thatwere smoked in addition to tobacco, including Cornus sp.(Dogwood), Juniperus species (Juniper), Rhus glabra (Sumac) andArctostaphylus uva-ursi (Bearberry) (Brown, 1989; Hall, 1977;Springer, 1981; Yarnell, 1964). The limitation is that the use ofselect ion monitoring for GCeMS requires the researcher to lookfor the presence/absence of compounds, rather than scan for allcompounds. Active compounds must be determined in advance,and then compared to compounds in a sample, to make

comprehensive determinations of all plants smoked. Research toidentify biomarkers of the above listed tobacco alternatives iscurrently ongoing.

5. Conclusions

Residue analysis of intoxicants such as alkaloids is a profitable, ifunder-investigated, topic of research (Wink,1998). There have beenrecent examples of intoxicant research, on substances as varied as


cacao (Hurst et al., 2002, 1989), opium (Bisset et al., 1996; Koschel,1996), as well as other researchers looking at tobacco (Tushinghamet al., 2010). Intoxicants play roles in a variety of significant culturalfunctions, such as religious rituals or social feasting (Bourguignon,1973; Merlin, 2003; Rudgley, 1993; Winter, 2000b). Residue anal-ysis can provide data on such practices (Rafferty, 2007). Additionalresearch will seek to further corroborate and add detail to theseresults.

Acknowledgements

This research was funded in part by the National ScienceFoundation (BCS-0822493). Radiocarbon assays were performed atthe University of Arizona AMS Radiocarbon lab. Special thanks toWilliam Tippens and the curatorial staff of the Carnegie Museum ofNatural History for access to collections and photographs of spec-imens. Thanks to Colin Henck of the University at Albany’sdepartment of chemistry for assistance in modifying the GCeMSprotocols.

References

Asch, D.L., 1991. Tobacco Seeds in the Archaeobotanical Collections of the Center forAmerican Archaeology. Center for American Archaeology, Kampsville.

Asch, D.L., 1994. Aboriginal specialty-plant cultivation in eastern North America:Illinois prehistory and a post-contact perspective. In: Green, W. (Ed.), Agricul-tural Origins and Development in the Midcontinent. University of Iowa Press,Iowa City, pp. 25e86.

Bisset, N.G., Bruhn, J.G., Zenk, M.H., 1996. The presence of opium in a 3,500 year oldCypriote Base-Ring Juglet. Ägypten und Levante 6, 203e204.

Bohrer, V., 2004. Flotation analysis from High Rolls Cave (LA 114103) Otero CountyNew Mexico, Southwest Ethnobotanical Enterprises Report 39.

Bouchard, M., Smith, D.C., 2002. Archaeological and Experimental Stained Glass: ANon-destructive Raman Microscopic (RM) Study. In: ART 2002: Seventh Inter-national Conference on Non-destructive Testing and Microanalysis for theDiagnostics and Conservation of Cultural and Environmental Heritage.

Bourguignon, E., 1973. Religion, Altered States of Consciousness, and Social Change.Ohio University Press.

Brown, I.W., 1989. The calumet ceremony in the southeast and its archaeologicalmanifestations. American Antiquity 54 (2), 311e331.

Bruno, P., Caselli, M., Curri, M.L., Favia, P., Laganara, C., Traini, A., 1997. Surfaceexamination of red painting on Medieval pottery from the South of Italy. Annalidi Chimica e Roma 87, 539e553.

Clark, R.J.H., Curri, M.L., 1998. The identification by Raman microscopy and X-raydiffraction of Iron-oxide pigments and of the Red pigments found on Italianpottery fragments. Journal of Molecular Structure 440, 105e111.

Dobkin de Rios, M., 1975. Man, culture, and hallucinogens: an overview. In:Rubin, V. (Ed.), Cannabis and Culture. Mouton Press, The Hague, pp. 401e416.

Dobkin de Rios, M., 1976. Suggested hallucinogenic motifs in new world massiveearthworks. In: du Toit, B. (Ed.), Drugs, Rituals and Altered States ofConsciousness. Balkema Press, Rotterdam, pp. 237e249.

Dobkin de Rios, M., 1984. Hallucinogens: Cross Cultural Perspectives. University ofNew Mexico Press, Albuquerque.

Edwards, H.G.M., Farwell, D.W., Webster, D., 1997. FT Raman microscopy ofuntreated natural plant fibres. Spectrochimica Acta A 53, 2383e2392.

Edwards, H.G.M., Sibley, M.G., Heron, C., 1998. FT-Raman spectroscopic study oforganic residues from 2300-year-old Vietnamese Burial Jars. SpectrochimicaActa A 53, 2373e2382.

Ford, R.I., 1981. Gardening and farming before A.D. 1000: patterns of prehistoriccultivation North of Mexico. Journal of Ethnobiology 1, 6e27.

Gager, F., 1991. Studies of the History of Tobacco Use: Nicotine as a Chemical Marker,Paper presented at the Society of American Archaeology Annual Meetings,New Orleans.

Gendron, F., Smith, D.C., Gendron-Badou, A., 2002. Discovery of Jadite-Jade inGuatemala confirmed by non-destructive Raman microscopy. Journal ofArchaeological Science 29, 837e851.

Goodman, J., 1993. Tobacco in History: The Cultures of Dependence. Routledge,London.

Haberman, T.W., 1984. Evidence of aboriginal tobaccos in eastern North America.American Antiquity 49 (2), 268e287.

Hall, R.L., 1977. An Anthropocentric perspective for eastern United states prehistory.American Antiquity 42 (4), 499e518.

Hurst, J., Tarka Jr., S.M., Powis, T.G., Valdez Jr., F., Hester, T., 2002. Cacao usage by theearliest Maya civilization. Nature 418 (6895), 289.

Hurst, J., Martin, R.A., Tarka Jr., S.M., Hall, G.D., 1989. Authentication of cocoa inMaya vessels using high-performance liquid chromatographic techniques.Journal of Chromatography 466, 279e289.

Joniger, O., Dobkin de Rios, M., 1973. Suggestive hallucinogenic properties oftobacco. Medical Anthropology Newsletter 4 (4), 6e11.

Joniger, O., Dobkin de Rios, M., 1976. Nicotiana an hallucinogen? Economic Botany30, 149e151.

Knight, V.J., 1975. Some observations concerning plant materials and aboriginalsmoking in easternNorth America. Journal of Alabama Archaeology 21,120e144.

Koschel, K., 1996. Opium alkaloids in a Cypriote Base Ring I vessel (Bilbil) of theMiddle Bronze Age from Europe. Ägypten und Levante 6, 159e166.

Lednev, K., Ermolenkov, V.V., He, W., Xu, M., 2005. Deep-UV Raman spectrometertunable between 193 and 205 nm for structural characterization of proteins.Annals of Bioanalytical Chemistry 381, 431e437.

Lednev, K., Ermolenkov, V.V., He, W., Xu, M., 2006. Vibrational spectroscopy: bio-logical applications of ultraviolet Raman spectroscopy. In: Uversky, V.N.,Permyakov, Eu.A. (Eds.), Protein Structures, Methods in Protein Structures andStability Analysis. Nova Science Publishers, Inc.

Merlin, R.S., 2003. Archaeological evidence for the tradition of psychoactive plantuse in the old world. Economic Botany 57 (3), 295e323.

McCann, L.I., Trentelman, K., Possley, T., Golding, B., 1999. Corrosion of ancientChinese bronze money trees studied by Raman microscopy. Journal of RamanSpectroscopy 30, 121e132.

Rafferty, S.M., 2002. Chemical analysis of early Woodland period smoking piperesidue. Journal of Archaeological Science 29 (8), 897e907.

Rafferty, S.M., 2006. Evidence of early tobacco in Northeastern North America?Journal of Archaeological Science 33 (4), 453e458.

Rafferty, S.M., 2007. The archaeology of alkaloids. In: Barndard, H., Eerkens, J.W.(Eds.), Theory and Practice of Archaeological Residue Analysis. British Archae-ological Reports International Series 1650, pp. 179e188.

Reber, E.A., Blitz, J.H., Thompson, C.E., 2010. Direct determination of the contents ofa ceramic Bottle from the Moundville site, Alabama. Midcontinental Journal ofArchaeology 35 (1), 37e56.

Rudgley, R., 1993. The Alchemy of Culture: Intoxicants in Society. British MuseumPress.

Schultz, H., Baranska, M., Quiltzsch, R., Schütze, W., 2004. Determination of alka-loids in capsuls, milk, and ethnolic extracts of poppy. Analyst 129 (10), 917e920.

Shashilov, V.A., Ermolenkov, V.V., Lednev, I.K., 2006. Multiple bicyclic diamide-lutetium complexes in solution: chemometric analysis of deep-UV Ramanspectroscopic data. Inorganic Chemistry 45, 3606e3612.

Smith, D.C., Barbet, A., 1999. A preliminary Raman microscopic exploration ofpigments in wall paintings in the Roman tomb discovered at Kertch, Ukraine, in1891. Journal of Raman Spectroscopy 30, 319e324.

Smith, D.C., Gendron, F., 1997. Archaeometric application of the Raman microprobeto the non-destructive identification of two pre-Columbian ceremonial pol-ished ‘Greenstone’ axe-heads from Mesoamerica. Journal of Raman Spectros-copy 28, 731e738.

Springer, J.W., 1981. An ethnohistoric study of the smoking complex in easternNorth America. Ethnohistory 28 (3), 217e235.

Tushingham, S., Eerkens, J., Feihn, O., Nguyen, J., Nguyen, D. GCMS Analysis ofAlkaloid Residues in Ancient and Experimental Pipes. Paper presented at theSociety for American Annual Meetings, April 15, 2010.

Vandenabeele, P., Edwards, H.G.M., Moens, L., 2007. A decade of Raman spectros-copy in art and archaeology. Chemical Reviews 107, 675e686.

Von Gernet, A., 1992. Hallucinogens and the origins of the Iroquoian pipe/tobacco/smoking complex. In: Hays III, C.F. (Ed.), Proceedings of the 1988 Smoking PipeConference. Rochester Museum and Science Service, Rochester, pp. 171e185.

Wagner, G.E., 2000. Tobacco in prehistoric eastern North America. In: Winter, J.C.(Ed.), Tobacco Use by Native Americans: Sacred Smoke and Silent Killer.University of Oklahoma Press, Norman, pp. 185e204.

Watson, P.J., 1989. Early plant cultivation in the eastern Woodlands of NorthAmerica. In: Harris, D.R., Hillman, G.C. (Eds.), Foraging and Farming: TheEvolution of Plant Exploitation. Unwin Hyman, London, pp. 550e570.

Wiedemann, H.G., Arpagaus, E., Müller, D., Marcolli, C., Weigel, S., Reller, A., 2002.Pigments of the bust of Nefertete compared with those of the Karnak Talatats.Thermochimica Acta 382, 239e247.

Wink, M., 1998. A short history of alkaloids. In: Roberts, M.F., Wink, M. (Eds.),Alkaloids: Biochemistry, Ecology and Medicinal Applications. Plenum Press,pp. 11e44.

Winter, J.C., 2000a. Introduction to the North American tobacco species. In:Winter, J.C. (Ed.), Tobacco Use by Native North Americans: Sacred Smoke andSilent Killer. University of Oklahoma Press, Norman, pp. 3e8.

Winter, J.C., 2000b. Traditional uses of tobacco. In: Winter, J.C. (Ed.), Tobacco Use byNative North Americans: Sacred Smoke and Silent Killer. University of Okla-homa Press, Norman, pp. 9e58.

Winter, J.C., Creating Tobacco: Native American Origins, Beliefs and Uses, Paperpresented at Beloit College, Wisconsin, 2004.

Yarnell, R.A., 1964. Aboriginal Relationships between Culture and Plant Life in theUpper Great Lakes Region. University of Michigan, Ann Arbor.

Zahlsen, K., Nilsen, O.G., 1994. Nicotine in hair of smokers and non-smokers:sampling procedure and gas chromatographic/mass spectrometric analysis.Pharmacology and Toxicology 75, 143e149.

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