2008-shackley-archeometry.pdf

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Archaeometry 50, 2 (2008) 194215 doi: 10.1111/j.1475-4754.2008.00390.x

*Received 10 September 2007; accepted 5 December 2007

University of Oxford, 2008

BlackwellPublishingLtdOxford,UKARCHArchaeometry0003-813X0003-813XUniversityofOxford,2008XXXOriginalA rticlesArchaeological petrology and the archaeometry of lithic materialsM. S. Shackley*Received10 September2007;accepted5December2007UniversityofOxford,2008

ARCHAEOLOGICAL PETROLOGY AND THE

ARCHAEOMETRY OF LITHIC MATERIALS*

M. S. SHACKLEY

Geoarchaeological XRF Laboratory, Department of Anthropology, University of California, Berkeley,

CA 94720, USA

For 50 years, archaeologists and physical scientists have been dating, determining the

composition of and measuring stone tools, and reporting them in Archaeometry

and many

other journals. In Archaeometry

specifically, the number of papers devoted to the analysis

of lithic material has increased at least 30 times since 1958 and volume 1. This is a reflection

not only of an increase in the number of scholars devoting their time to the archaeometry

of stone, but also of increases in the quality and quantity of instrumental technologyavailable to researchers in the field.

KEYWORDS:

ARCHAEOLOGICAL PETROLOGY, LITHICS, OBSIDIAN, CHERT, MARBLE,

INSTRUMENTAL TECHNIQUES, SAMPLING

INTRODUCTION

In 1983, D. R. C. Kempe and Anthony Harvey published an edited volume entitled The petrology

of archaeological artefacts

. This was the first attempt to compile the ever-increasing work on

the geoarchaeological analysis of stone in all its forms from chipped to sculptural stone, and

it included chapters on ceramics and metals. The latter two data sets are not part of this paper;they are covered very well by others in this set of special review papers. This was a landmark

study that received very little attention by lithic technologists, particularly in the Americas.

The purpose here in the space allotted is to examine a bit of the history and advances made

in the archaeometry of stone, with special emphasis on the direction that a 21st-century

archaeometry is currently making towards an understanding of the composition of stone artefacts.

From chipped stone to sculptural stone, by both optical methods (petrography) and analytical

chemistry, the quantity and quality of research has increased exponentially. This is, to a limited

extent, an expanded view of a similar review about 10 years ago (Shackley 1998a). There is

no attempt to cover dating stone, or lithic technology, in this case defined as the metric and

technological analysis of stone as an artefact produced by humans through time (debitageanalysis, use-wear studies etc.), except where archaeometric techniques are beginning to shed

light on technological issues (cf., Grace 1996). This is a huge literature, and beyond the focus

of archaeometry in my estimation (for chert, see Delage 2003). However, as I will note

throughout, lithic technologists have much to gain from those of us who are focused on the

archaeometry of stone. Many lithic technologists have learned this in the past decade or so, and

all of us are better for it (Shackley 1998a; Odell 2003). Unfortunately, most lithic technologists,

particularly those in the Americas, have not even heard of Kempe and Harveys (1983) volume.

To this, as a geoarchaeological scientist and a lithic technologist, I devote this paper.


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Disclaimer

As with many of the subjects covered in these relatively short summaries, the entirety of

archaeological petrology and stone is impossible to cover. The goal here is to address some of

what I consider to be the important recent advances, as well as some of the continuing problems

that affect archaeological geochemical studies of stone, with the archaeologist in mind rather

than the trained geochemist. There are a number of important new and experimental techniques

in archaeometry, both in the field and laboratory, that are being applied to stone tools and structural

stone studies in archaeology, and some will wonder why their favourite technique or perspective

was not covered (such as the exciting new possibilities of isotope studies through ICPMS;

see Speakman and Neff 2005). I want to emphasize that this is my particular view, and not

necessarily that of other archaeologists or archaeometrists. I find the new techniques and subject

areas discussed here to be of primary importance to the shifts in archaeological thought in the

past decade, and the set of problems in chert, marble and obsidian characterization, one that

simply will not and should not go away.

A SHORT HISTORY IN THE JOURNAL ARCHAEOMETRY

As suggested earlier, papers on analyses of lithics inArchaeometry

are indicative of the trajectory

of research on this subject in archaeology in general (see the Appendix and Fig. 1). The

Appendix is a bibliography of all the 117 papers devoted to lithic material analysis from and

including volume 1 (1958) through to volume 49 (November 2007). Again, this does not

include those papers devoted solely to lithic technology as I defined it above; there are very

few of these. The Journal of Archaeological Science (

JAS

), published first in 1974, seems to

accept more purely technological papers on lithics than Archaeometry

has by comparison. As

first an associate, then the Society of Archaeological Science Managing Editor atArchaeometry

between 1999 and 2006, I would say that this is not due to editorial fervour or preference, but

a perception by archaeologists thatJAS

is more accepting of technological studies.

Figure 1 exhibits the frequency of papers devoted to archaeometric analyses of lithic material,

arbitrarily divided into decades. The earliest class is only from 1958 to 1959, and the latest

class only runs from 2000 to 2007 for obvious reasons. The near exponential rise in this research

is not due to editorial preference or the increase in page numbers (from two to four issues per

year), but is a real reflection of the increases in lithic material research similarly reflected in

other subject areas reported in this volume (see Delage 2003). However, it is noticeable that

Archaeometry

was dominated by ceramic and metals studies in the early days, still a prevalent

ratio in many parts of the world and lamented by some (Williams-Thorpe 1995; Shackley1998a, 2005).

THE CHEMICAL CHARACTERIZATION OF STONE:

BEYOND FISHING EXPEDITIONS

Define the problem. A good source analysis is usually complex and expensive, and should

not be initiated merely as a fishing expedition in the vague hope that you might find some-

thing interesting. (Luedtke 1992, 117)

Since a good part of my own research is involved in the wavelength and energy-dispersive X-rayfluorescence (EDXRF) analysis of obsidian artefacts, it seems odd that I would continually

discuss what I call the sourcing myth in archaeometry (Shackley 1998a, 2005). As many of


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M. S. Shackley

the archaeometrists who are involved in chemical characterization know, few archaeologists

understand the physics and geochemistry of XRF, neutron activation analysis (NAA), proton-induced X-ray emission proton-induced gamma ray emission spectrometry (PIXEPIGME),

mass spectrometry (MS), inductively coupled plasma mass spectrometry (ICPMS) or any

of the other techniques used to characterize stone materials. Even more worrisome is that few

explore the issue of statistical probability and its role in assigning an artefact to source (see

Baxter 1994; Neff and Glascock 1995; Shackley 1998b). This would all be fine if archaeometrists

were all absolutely honest (and most are, most of the time), and there was a better line of com-

munication between the scientist and the archaeologistwhich there is not, or at least there has

not been good communication. There are, of course, good reasons for this lack of communication.

Due to heavy workloads and the sheer size of the printed world in archaeology, it is necessary

that the archaeologist trusts the archaeometrist to be honest and that the source assignmentsare right.

In this review, the problems in the chemical characterization of three very important

substances used throughout prehistory and the focus of much archaeometric research in the

past three decadesmarble, secondary siliceous sediments, called chert here, and volcanic

glass, both silicic and maficare the focus. The issues raised are typical of the analysis of any

stone material, particularly those that are heterogeneous.

One of the most misused terms in archaeometry is the word sourcing. Archaeologists most

often use it, and unfortunately archaeometrists do too. Besides the grammatical problems with

the word, it implies that whatever is submitted to the archaeometrist will return with a bona

fide and certified source provenance that is not probabilistic at all, but confidently determined.I am certainly not the first to say this, but I will reiterate that nothing is ever really sourced.

The best we can do is provide a chemical characterization and a probable fit to known source

Figure 1 The frequency of papers devoted to the archaeometric analysis of lithic material in Archaeometryin 10-year

increments (the earliest and latest classes are truncated).


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data. The key words here, of course, are characterization

and known

. So many regions have

poor source standard data that we can never really be sure, even beyond the scientific process

of orderly refutation of alternatives (Ward 1977; Luedtke 1992; Hughes and Smith 1993;

Williams-Thorpe 1995; Cauvin and Balkan-Atl 1996; Gratuze 1999; Kuzmin et al.

2002;

Shackley 2005; Maniatis 2007).

Chert and characterization

Attempts to determine the source provenance of chert through chemical characterization have

vexed archaeologists and archaeometrists for decades (Luedtke and Myers 1984; Matiskainen

et al.

1989; Luedtke 1992; Warashina 1992; Church 1995; Hoard et al.

1995; Roll et al.

2005).

This is mainly due to the processes of the formation of chert through precipitation from a

parent material at ambient temperatures, where only certain elements and compounds can be

removed from the original matrix. Additionally, sources of chert, particularly Phanerozoic

marine cherts, by their nature often cover large geographical expanses, which decreases theirutility as a means to derive inferences for exchange, interaction or procurement processes.

Most of the techniques that have proven helpful in deriving useful chemical data for cherts are

destructive and expensive, further limiting its utility, at least where conservation of objects is an

issue (see Roll et al.

2005). Barbara Luedtkes (1992) treatment of the subject for archaeologists

is an excellent step towards generating an understanding of chert among archaeologists. Among

the many useful ideas, Luedtke suggests a four-step process for determining the probable

source of cherts (1992, Appendix A). I have modified these steps and added a few more based on

my own experience, and indeed, in general, these steps are appropriate for most stone provenance

studies:

(1) A number of similar unknown sources may be detected from various archaeological contexts.Often, these will cluster in various geological regions.

(2) Consult the regional geological literature to ascertain the location of the nearest and most

likely rock bodies. In the case of obsidian, glass is rarely mentioned in association with

mapped rhyolite bodies in the geological literature.

(3) Frequently, local residents, archaeologists, rock hounds, rock hound guides and generally

word-of-mouth have been found to be excellent sources for locating obsidian and chert. Nearly

all of the obsidian and chert sources discovered in the North American Southwest were first

found by non-scientists (Shackley 2005).

(4) Most often, it has been found necessary, after determining the general location of a source,

to begin the search downstream from the probable source area. Many of the Tertiary and earliersources are highly eroded, and many nodules and fragments of rock can be released into the

sediment load and carried many kilometres downstream from the source (Shackley 1998c, 2005).

(5) In the field, when the source or source area is discovered, the extent and density, general

geological setting and variability of lithic production should be recorded. Pedestrian transects

across the source area are sampled and form strata from which probability samples are selected

for optical and/or instrumental analysis, ensuring as representative a sample as possible.

(6) Determine which techniques or procedures are worth pursuing. For museum specimens,

it is often unacceptable to thin section the material for petrographic analysis or subject it to

destructive NAA, while non-destructive methods such as XRF may be acceptable. Keep in

mind that each method has its advantages and limitations, and the results of a given techniquemay not be specifically valid (see Goffer 1980; Neff and Glascock 1995; Green 1998; Shackley

1998a; Roll et al.

2005; Speakman and Neff 2005).


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(7) Finally, match artefacts to sources. The uses and abuses of performing this step are

astronomical in the literature. Multivariate techniques are often sought after with the ease of

PC-level software now available, but archaeologists often do not have the statistical background

to evaluate these results. Starting with simple bivariate plots and central tendency statistics

comparing the artefact and geological data is often sufficient to assign artefacts to sources(Hughes 1984a; Shackley 1988, 2005; Baxter 1992, 1994; Neff and Glascock 1995; Glascock

et al.

1998).

(8) The source descriptions should include exact locations; preferably Universal Transverse

Mercator international grid system (UTMs), a description of the geological context,

megascopic attributes of the raw stone (cortical and interior variation, nodule size, colour, fabric

and opacity), the distribution of secondary deposits, the density and character of lithic reduction

at the source, and relevant published sources.

Due mainly to these issues, archaeometrists and archaeologists have in the past decade or so

begun to focus on the very real problems of chert characterization and source assignment

(Church 1995; Hoard et al.

1995; Roll et al.

2005). As archaeologists begin to gain an under-standing of the instrumental techniques involved and the assumptions that archaeometrists

often must make, they are beginning to require that archaeologists who employ archaeometric

techniques for characterization pay heed to sampling design and presentation of results. Much

of the wrangling apparent in two of the articles cited above revolved around issues of sampling

at the source. Church rightfully questioned whether sampling reduction debris at the source

was sufficient and necessary to deal with source variability. Hoard et al.

noted that while some

geological samples were gathered, much of the characterization project was based on second-

hand collections. In this case the potential for committing Type I or

Type II errors, mainly due

to retooling at the source, can be great, and the archaeologist or the archaeometrist may not

even be aware (Thomas 1986, 21317; Bernard 2006). Without a firm knowledge of potentialchert sources in a region, errors of misassignment will occur. Even with this knowledge, the

level of macroscopic and chemical variability inherent in secondary siliceous sediments,

confident characterization and source assignment can be hazardous. Given all these caveats,

however, chert characterization and source assignment are just beginning to be a real tool in

archaeology, using confocal microscopy tied to optical petrography, as well as the instrumental

techniques mentioned here. While fraught with the difficulties of source heterogeneity and the

general need to use destructive or partially destructive techniques, hope is in the air for the

relationship between archaeometry and one of the most commonly used flaked stone raw

materials in prehistory.

Obsidian characterization and the sourcing myth

Many of the points briefly outlined for chert studies are equally relevant for obsidian studies

in archaeology, but because these homogeneous, disordered, silicic glasses can be so precisely

characterized, the potential abuses are much greater. Since it is a common aspect of archaeo-

logical practice and a good example for other data sets, a few words will be directed towards

some of the problems in the chemical characterization of silicic glasses that directly impact

the resolution of archaeological problems.

Obsidian studies in archaeology are a relatively recent aspect of archaeological research

(Boyer and Robinson 1956; Green 1962, 1998; Cann and Renfrew 1964; Jack and Heizer1968; Jack and Carmichael 1969; Williams-Thorpe 1995; Shackley 2005). Early on,

megascopic (macroscopic) observation, density measures and mass spectrometry were all used


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in an attempt to define source groups and correlate artefacts to sources, with mixed results. In

the late 1960s and early 1970s, with the evolution of relatively inexpensive X-ray fluorescence

spectrometers and the increasing use of NAA, obsidian studies in archaeology began to be

used in an effort to deal with issues of exchange and interaction (Glascock 1994; Shackley

1998b, 2005; Glascock et al.

2007). Archaeologists working in the Mediterranean, the New Worldand Oceania were particularly keen to use these new methods, mainly since the instruments

were available at most university campuses (Hughes 1984b; Nelson 1984; Shackley 1988,

1995, 2005; Tykot 1992; Williams-Thorpe 1995; Green 1998). By the 1980s, archaeologists in

every part of the world where obsidian occurred were engaged in obsidian provenance studies.

Now, thousandsif not tens of thousandsof pieces of archaeological obsidian are analysed

yearly by X-ray fluorescence spectrometry (XRF), neutron activation analysis (NAA or

INAA), inductively coupled plasma mass spectrometry (ICPMS) and proton-induced X-ray

emission proton induced gamma ray emission (PIXEPIGME), and much of the analysis is

performed by archaeologists now rather than by physical scientists (Shackley 2002). This is

the hope for the future, but there are limitations. As discussed above, while most archaeologistsinherently know that a chemical signature is only as good as the instrument and, more importantly,

the available source data, too few seem to worry about this. Many of the source assignment

problems inherent in earlier semi-quantitative analyses, however, are simply gone now, with

the emphasis on easily derived quantitative estimates.

The obsidian hydration controversy

Archaeometry

has played a role in the issues surrounding obsidian hydration dating nearly

since the beginning (Layton 1973; Ericson and Kimberlin 1977; Michels et al.

1983; Stevenson

et al.

1987, 1989; Liritzis 2006). Obsidian hydration dating, however, has not played a majorrole in Old World chronology building for a number of reasons, and European scholars have

not dealt with the controversy in a major way. For this and the controversy surrounding the

method, I will not spend much time on the subject. It is most popular in the New World, and

mainly restricted to parts of North America (California, the Great Basin) and Oceania, particularly

New Zealand. There are historical reasons for thisprimarily, of course, a dominance of

obsidian raw materials in those regions, and the absence of other datable materials. For many

of us in the field, it has been fraught with too many issues to function as a reliable member of

the chronometric toolkit (Shackley 2005).

Beginning with Friedman and Smiths (1960) paper on dating using obsidian hydration,

scholars have moved into two camps; those who believe fervently in the utility and validity ofthe method (Jackson 1984; Hall and Jackson 1989; Hull 2001, 2002) and those who find the

recurring problems simply too much (Riddings 1996; Anovitz et al.

1999; Loyd 2002cf.,

Stevenson et al.

1998). Even those, as above, who have found issues regarding the use of

obsidian hydration as a direct dating method still work towards resolution of the issues.

Factors such as variances in atmospheric heat and humidity through time, the inability to

control the burial history of the artefact, resetting the hydration rim after post-depositional

burning, seemingly exponential, non-linear shifts in the absorption of water over time and

inter-observer measurement error all frustrate attempts to use hydration as an absolute method.

More recently, Hull (2001) has argued that these critiques are simply because researchers

focus on the method as a direct rather than relative technique, although Hull seems to use it asthe former in her own work (Hull 2002). The recent symposium on the effects of fire on obsidian

hydration in California found, through empirical observation and experimentation, that hydration


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rims can be reset when subject to forest fire conditions, dealing a lethal blow, at least for the

non-believers (Deal 2002; Loyd 2002; Loyd et al.

2002; Skinner 2002). Some western North

American federal archaeologists will no longer pay for obsidian hydration analyses through

federal funds (Skinner 2002, and pers. comm.). Parenthetically, through experimentation and

in-field studies, it has been found that there is no statistically significant change in traceelement chemistry when heated to high temperatures (Skinner et al.

1996; Shackley and Dillian

2002; Steffen 2002).

So, what should archaeologists do? Hull suggests that obsidian hydration should not be seen

as an absolute dating method like dendrochronology, but as a relative dating tool for application

in, for example, site contexts where the depositional history is similar from one area to another

(Hull 2001, 1026). In recent Historic-period sites, Hull has been able to derive some interesting

relative dates in a chronological context where 14

C dating is useless, given the inherent

uncertainty of the calibration curve in near modern periods (Hull 2002; see also Ambrose

1998). Even so, these dates have yielded error rates due to the vagaries of hydration. Riddings

(1996) and Anovitz et al.

(1999) seem to be willing to claim obsidian hydration a failure. I amglad to see, however, that some, including Anovitz, are willing to continue experimentation in

the hope that the issues will be resolved (Friedman et al.

1997; Stevenson et al.

1998).

Fun with marbles

Aside from obsidian provenance studies, marble is one of the success stories in lithic provenance

work in archaeology, or at least scholars are intensively focused on resolving the issues (Herz

and Waelkens 1988; Polikreti and Maniatis 2002; Luke et al.

2006; Maniatis 2007). Archaeo-

logically, marble is one of the most important metamorphic rocksif not the most important.

Fine-grained varieties have been used for sculptural and architectural stone throughout history,in both the Old and New Worlds (Garrison 2003). In the classical Greco-Roman tradition, marble

became the

preferred building stone, and it continues to be an important interior and exterior

stone.

Marble, as a granular, heterogeneous rock primarily composed of calcite or dolomite,

derived from limestone, is subject to many of the same heterogeneity issues as chert. The colour

and texture, which are sometimes quite variable, are the result of precursor minerals and

metamorphism. The lower the concentration of accessory minerals, the whiter is the marble

(Maniatis 2004). As in many early studies, NAA was seen as the saviour of marble analysis,

and would simply solve all the issues. However, as discussed above, NAA, like XRF, is a mass

analysis technique, and all elements for all the constituents are included in the analysis. Again,as in chert studies, it is now accepted that multiple analyses are necessary to confidently

characterize marbles (Polikreti and Maniatis 2002; Maniatis 2004; Luke et al.

2006). Other

techniques that are frequently usedor at least were used in the pastinclude: stable isotope

analysis by mass spectrometry, focused on 13

C/

12

C and 18

O/

16

O ratios; cathodoluminescence

(CL); optical petrography; and most recently electron paramagnetic resonance spectroscopy

(EPR), also known as ESR. Polikreti and Maniatis (2002) note that EPR is very effective at

detecting manganese (Mn

2

+

) and iron (Fe

3

+

) ions, which exist in various amounts in every

marble crystal, replacing calcium (Ca

2

+

). The proportions of these ions follow the conditions

present during metamorphism, and therefore are very locally source specific (see also Maniatis

2007). This resolves some of the stable isotope difficulties where source overlap problems arenot solved. While EPR has been shown to be quite successful in separating many marble

sources in the Old World, it still relies on an extensive source database, and does not solve all


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source overlap. However, it does look as thoughin the Old World at leasta comprehensive

and usable database for marble is nearly here. If chert were not so widespread, as marble, this

would be the case for that stone too.

Sampling: how much is enough?

Sampling issues in archaeology are, of course, not new. In the 1980s, the US Department of

the Interior spent a considerable sum investigating the issue, both for confidence in predictive

modelling and for regional and intra-site sampling (Judge and Sebastian 1988). Running

throughout this work, and many others, and a basis for probability theory, is the necessity for

adherence to the simple law of large numbers: as the sample size increases, the probability of

attaining a representative sample increases, diversity issues aside. Given the funding con-

straints on archaeology in all forms, the law of large numbers is an ever-present demon. The

sampling issue deserves some thought at all levels of archaeometric analysis, both in the field

and the laboratory, and while we may not always be able to fund projects based on theseprecepts, we at least need to be familiar with the risks inherent in our decisions. In both source

sampling and sampling artefacts for analysis from an archaeological assemblage, there appears

to be a minimum number necessary to derive a confident conclusion. Again, a couple of examples

at both the source and artefact assemblage level from my own work in the North American

Southwest are offered.

The Mule Creek regional source: real chemical source variability

In a 1988 study of the Mule Creek source in western New Mexico, sampling 15 source standards

from a population of 200 gathered at five localities, two chemical outliers were noted,collected with significantly higher rubidium concentration values (Shackley 1988a, 767).

These outliers have now been identified as a distinct chemical group, often mixed in the

regional Gila Conglomerate with three other chemical groups (see Shackley 1995, 2005). The

eruptive geology in the area is complex, and has been studied by Ratt and others for some

time (for a summary of this work, see Ratt 2004). Primary in situ

perlite localities with remnant

marekanites for three of the chemical groups have thus far been located.

At least four distinct chemical groups are evident, distinguished by the incompatible

elements Rb, Y, Nb and Ba, and to a lesser extent Sr and Zr, and are named after the localities

where marekanites have been found in perlitic lava: Antelope Creek, Mule Mountains and

Mule Creek/North Sawmill Creek, all in New Mexico. Additionally, during the 1994 fieldseason, a fourth subgroup was discovered in the San Francisco River alluvium near Clifton,

Arizona, and in older alluvium between Highway 191 and Eagle Creek in western Arizona,

north of Clifton. While in situ

nodules have not yet been found, they are certainly located

somewhere west of Blue River and north and west of the San Francisco River, since none of

this low zirconium subgroup was discovered in alluvium upstream from the juncture of the

Blue and San Francisco Rivers. The genetic relationship is apparent in the bivariate and trivariate

data plots (Shackley 2005, 51, figure 3.6), and signifies the very complex nature of the Mule

Creek silicic geology, with subsequent depositional mixing in the Gila Conglomerate. The

original simple random sample of 15 nodules merely indicated that some variability existed,

and only after extensive transect survey and sampling, and locating three localities with in situ

marekanites did it become apparent that there was significant chemical variability inherent in

the source. Perhaps most importantly, without the knowledge of these other subsources,


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analysis of archaeological obsidian in the region could posit a new and unknown source. This

process has been repeated throughout the world, and has really changed the way in which we

view sources of archaeological stone (Hughes and Smith 1993; Williams-Thorpe 1995; Cauvin

et al.

1998; Glascock et al.

1998; Summerhayes et al.

1998; Tykot 1998; Gratuze et al. 2005;

Poupeau et al. 2005; Shackley 2005).So, how much should be sampled? As usual, the answer depends on many factors. Often,

the archaeometrist has detected variability in the source from archaeological analyses even

though source standards have not indicated that variability (Hughes and Smith 1993; Glascock

et al. 1998; Kuzmin et al. 2002; Gratuze et al. 2005; Poupeau et al. 2005; Carter et al. 2006;

Carter and Shackley 2007). No longer are 10 samples sent to an archaeometrist sufficient to

confidently define the elemental variability of a source. The following source sampling

strategy is a guide [composed of our own work in the American Southwest; the work of Glascock

and others (Glascock et al. 1998) in Mesoamerica; Skinners (1983) work in the American

Northwest; Jacksons (1986, 1989) and Hughes (1988, 1994; see also Hughes and Smith

1993) work in California and the Great Basin; the work of Torrence and others (Torrence1992; see also Summerhayes et al.1998) and Green (1998) in Oceania; and the work of Carter

et al.(2006), Gratuze et al.(2005), Poupeau et al.(2005), Williams-Thorpe (1995) and Tykot

(1998) in the Mediterranean and the Near East]:

(1) On the ground, sample surveys must include the entire primary and secondary extent of the

source. This often requires days or weeks of field reconnaissance, and extensive discussions

with geologists and the local populace.

(2) Often, in order to determine the probable location of primary sources, extensive sampling

of the secondary distribution can isolate probable areas for further studythe San Francisco

River Alluvial samples were delimited in this way (see above).

(3) All samples should be located at least to the section, square kilometre, UTM or globalpositioning system (GPS) coordinates, depending on the country of origin.

(4) Stratified subsamples should be derived in the laboratory by the sublocalities collected in

the field (preferably analysing at least five or more samples from each localitybut note that

this is not a magic number). This could mean taking thousands of samples in the field.

The above is only an outline for research. In some instances, particularly with Quaternary

sources, secondary deposition may not be an issue, since there has been little geological time

for the glass to erode into the environment and/or large-scale pyroclastic eruptive events may

not have occurred (see Shackley 2005). While this eliminates the problems of secondary

deposition, it does not allay the problems of possible intra-source chemical variability. While

this strategy is focused on obsidian sources, most of the steps are equally valid for any otherstone material, including marble, other volcanics and secondary siliceous sediments.

INSTRUMENTATION: WHICH INSTRUMENT IS BEST?

Just about the most frequently asked question by archaeology students is: Which instrument

is best to analyse my stone objects? The answer, unfortunately, is: It depends . . . Again, the

problem design and the level of precision needed to address that design will determine which

instrument is the best for a given project. Ten years ago, this question was a bit easier to

answer (Shackley 1998b).

With the general improvements in technology, instrumental techniques in archaeologicalgeochemistry have similarly improved. Almost all instrumental and empirical techniques have

been used, including density, magnetism, atomic absorption, PIXEPIGME, ICP (for obsidian,


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Archaeological petrology and the archaeometry of lithic materials 203

see Tykot and Young 1995; Shackley 2005; Speakman and Neff 2005), megascopic criteria

and others. Today, three major instrumental methods dominate the field: neutron activation

analysis (NAA or INAA), wavelength- and energy-dispersive X-ray fluorescence (XRF),

including portable XRF (PXRF), and increasingly LAICPMS (Neff and Glascock 1995;

Glascock et al.2005; Shackley 2005; Speakman and Neff 2005). All of these methods havebenefited from the revolution in microprocessors and the attendant software industry, and are

easier to use, and hence misuse, today. In this summary, there is not the space to detail the

intricacies of each method. For archaeologists, Goffer (1980) and, to a certain extent, Harbottle

(1982) do this quite well for the earlier period. Glascock (1991) presents a good, though

technical, treatment of NAA (see also Neff and Glascock 1995, and see Speakman and Glascocks

2007 special issue on NAA in Archaeometry), and XRF and PIXEPIGME are explained in

some detail in Shackley (1998b) (see also http://www.swxrflab.net/xrfinstrument.htm). The goal

here is to address the relative merits of the three most commonly used analytical techniques,

NAA, EDXRF and PIXEPIGME, given the very real situations encountered by archaeologists.

Marble analyses have gone through even more experimentation with regard to instrumentation,as briefly discussed above.

There has been a certain level of mythology regarding the optimal analytical instrument for

geochemical studies of stone. The prevailing ideal seems to be that NAA is the best way to

go if funding is not a problem. NAA for most elements is certainly precise and it simply can

detect more elements than the other two methods (Glascock 1991; Neff and Glascock 1995;

Speakman and Glascock 2007). Neutron activation analysis, however, has two primary short-

comings. It is in essence a destructive technique, and while the material is not technically

destroyed, depending on original size, it may be broken into relatively small pieces and remain

radioactive for many years. Additionally, partly due to cost and partly due to the public fear of

nuclear energy, NAA is not readily available. Also, for obsidian characterization, NAA cannotanalyse for Ba, Sr and Zr as accurately as the other two methods (see Shackley 2005; Craig

2007). These three elements are important incompatibles in silicic melts and can be extremely

important in separating sources or dealing with intra-source issues (Hildreth 1981; Mahood and

Hildreth 1983; Macdonald et al.1987; Hughes and Smith 1993). Neutron activation can, however,

analyse for a number of other incompatibles quite accurately that are outside the range of XRF.

For museum specimens and artefacts that are subject to repatriation, NAA is not a feasible

choice. If precision and accuracy are necessary, which can be an issue in intra-source studies

and where the possibility of long-distance exchange is probable, then NAA will always

provide the most efficient alternative. Additionally, if the sample is extremely small (


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204 M. S. Shackley

What this all means for an archaeologist is that any laboratory employing EDXRF,

WDXRF, NAA, PIXEPIGME or ICPMS will provide valid and comparable results, given a

sufficient sample size, particularly for obsidian. The particular project constraints are now the

main criteria for the selection of analytical methods. What is probably more important now is

the accuracy of the source standard data, given the caveats throughout this paper. If the regionof interest has not received the level of geoprospection necessary for accurate source assignment,

it really does not matter how precise the instrument employed is known to be.

ARCHAEOMETRY AND THE INFERENCE OF TOOL USE

For most of its intellectual history, the understanding of prehistoric lithic technology has been

dominated by direct observation, experiment and, fortunately or unfortunately, opinion; and

just as dominated by polarized dialectic as to which particular paradigm was correct, or even

politically correct (Grace 1996). Many of these arguments have been based on opinions

about the method and the validity of the assumed analogy between modern experiments andprehistoric knappers and tool users (Keeley 1980; Odell and Odell-Vereecken 1980; Gendel

and Pirnay 1982; Unrath et al.1986; Lewenstein 1987; Bamforth et al.1990; Young and Bamforth

1990). The problems of inferring use from marginal damage on stone tools, particularly

utilized flakes, has produced a rather high level of consternation among lithic technologists,

and paramount frustration among contract archaeologists who are most pressed for time in

concluding site function, and therefore site significance, in management decisions (see Graces

1996 review of the literature inArchaeometry).

One of the most commonly practised techniques, and one of the most empirically frustrating,

is inferring use-wear and therefore function on unmodified flakes. Studies that rely on readily

available microscopic techniques are exceptions rather than the rule. Most archaeologists relyon macroscopic examination of flake margins, deriving inferences concerning use on the basis

of these gross morphological indications. Frighteningly, blind tests of various researchers

examining experimental specimens macroscopically have indicated that few archaeologists

agree on the character of the damage and hence the implied function of the tool (Bamforth

et al.1990; Young and Bamforth 1990; Christensen and Walter 1992; Christensen et al.1992).

It is true that the more experienced observers more often correctly identified the use-wear;

some did not. This is considerably disturbing, since themost common flaked lithic tool found

in prehistoric contexts is often the utilized flake. Young and Bamforth argue that some degree

of experimental experience should be required of all archaeologists who intend to include such

tools in their research, simply to ensure that they observe their collections accurately (1990,408). Gaining some experience with archaeometric methods should carry equal importance

(see Burroni et al.2002). Young and Bamforth may be over-optimistic and the error rate using

macroscopic criteria is probably too high.

So what can archaeometry and analytical chemistry offer to solve the dilemma? Some studies

by Marianne Cristensen, Phillipe Walter and others in France using environmental scanning

electron microscopy (ESEM) may have far-reaching implications for use-wear research, and

more recent studies using a variety of techniques have refined their effort (Christensen et al.

1998; Evans and Donahue 2005). Generally, even if you can determine the scraping, cutting,

rotary-wear utilization with some degree of confidence, it is rarely possible to determine the

actual material that the tool was used on beyond hard or soft material. Bone and wood areoften lumped together under one material, but it is obvious that there are often important

behavioural differences between stone tool use on either of these two materials.


12/23


Christensen et al. (1992see also Christensen and Walter 1992; Menu and Walter 1992)

have focused on margin polish on various stone tools by replicating tools and employing

ESEM with an EDXRF probe to yield qualitative elemental data that can be paired with various

substances. The results were cross-checked using RBS (Rutherford backscattering spectrometry)

and PIXE (proton-induced X-ray emission spectrometry). Another aspect of their research thatwill not be treated in depth here is the empirical evidence for melting silica where the polish

is essentially a combination of loss of lepispheric quartz from the chalcedony matrix in chert

andan accumulation of material, in this case bone (Fig. 1; Christensen et al.1992, 491; see

also Witthof 1967).

What is apparently important from this work is that the material that the tool was actually

used on can be empirically defined. Quite similar and reliable data were also obtained

with ESEMEDXRF. Christensen et al.s (1992) pilot study was applied to 13 000-year-old

Magdelenian burins recovered from the important Paris Basin site of Etiolles, which was

thought to be a lithic production area. Their study indicated that some of the burins were used

to modify chalky matter, suggesting that they used the burins to remove the chalk cortexbefore early stages of reduction (Christensen et al.1992, 4923). Perhaps more illuminating

was the analysis of Pre-dynastic Egyptian fishtail knives and ripple-flaked knives, which have

often thought to have been used only for ritual purposes and not household or other utilitarian

functions. Christensen et al.concluded, using this technique, that the fishtail knife was used to

cut meat and the ripple-flaked knife was used in plant cutting (1992; Menu pers. comm. 1993). Most

importantly, these tools were museum pieces that were thousands of years old, and that had

been handled by many different people throughout their over one hundred years of museum life,

and the technique is completely non-destructive when using the ESEM. This technique, while

still experimental, is readily available to most archaeologists worldwide, and promises to solve

some important issues that macroscopic and low-power microscopic techniques cannot.This study has been replicated and refined more recently using LAICPMS by Evans and

Donahue (2005). The authors not only used LAICPMS to great effect, but used even harsher

cleaning techniques than the Christensen group a decade earlier and found that there was still

not significant removal of the organic material (cf., Burroni et al. 2002). While ESEM and

RBS are useful in determining the material targeted by the tool users in prehistory, LAICP

MS is more efficient, and given that the instrumentation is becoming readily available at many

universities, promises to revolutionize lithic use-wear studies in the 21st century.

AND NOW FOR THE FUTURE . . .

There is always a risk of hoisting oneself on ones own petard when forecasting the future, but

there are a few comments that can be made with regard to the future of archaeological petrology

and lithic studies. First, it is apparent that we are on the right track. Few people think that a

single analytical method is sufficient to characterize any stone materialthis is a good thing.

Even obsidian, which is by definition completely disordered, with no crystalline structure, has

been shown to often exhibit source heterogeneity. While XRF is a good non-destructive tool

for characterizing obsidian sources and artefacts, it may not always include enough elements

to solve all the problems. There are many regions in the world (northern Mexico, Eurasia, and

even parts of the United States and Canada) where unknown sources are still evident in the

archaeological record.Chert is another story. Many chert sources, particularly the Phanerozoic marine sediments,

cover very large regions (i.e., the Ouachita Transition of the Edwards Plateau of Texas, and the


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206 M. S. Shackley

region of central France), and the consequent elemental and isotopic variability is so great that

it may be a long time until chert characterization studies approach those of obsidian or even

marble. As for marble, given that the sources are much more localized than for chert, and

archaeometrists have been working with marble for decades now, the future looks very bright

(Y. Maniatis pers. comm. 2007).There is one point that bears repeating: megascopic characterization and source assignment

on any rock is hazardous at best, and in many cases simply does not work (Shackley 2005,

1015). We are long past the need for megascopic source characterization, and good riddance.

Many of the techniques used to characterize rocks that have been discussed most here are relatively

inexpensive, and in most cases there is no excuse to resort to megascopic speculation.

The Old versus the New World

I have not really spent much time discussing the very real differences between archaeometric

practice and pedagogy in the Old World versus the New with regard to lithic material. I havetalked to many on both sides of the Atlantic about this over the years, and especially Dave Killick

at the University of Arizona, who is British but gained his Ph.D. at an American university.

Now in press, Killick has a paper (2008) that every archaeologist on both sides of the Atlantic

should read. In the United States and Canada, there are virtually no dedicated archaeological

science programmes at any public or private university. There are those of us, such as Dave

and I, who teach archaeological science as undergraduate and graduate method courses and

have developed dedicated laboratories, but Americanist archaeology has fallen well behind

Europe in dedicating courses of instruction and conferring degrees in the field (Calgary does

have a graduate programme in geoarchaeology). Just as Europe cannot rely on the United

States to supply brainpower, and should not, the lack of archaeological science programmes isa weakness of North American anthropological archaeology programmes, which seemingly

rely on Europe to lead in this area. There are a number of social and structural reasons for this

lack in US institutions; dominance of social anthropologists in anthropology departments, a

continuing lack of rigorous science instruction in US K-12 schools; the religious rights and

postmodern philosophys attacks on science in the US; and very real funding issues. There

really is not space to deal with these points here (see Killick 2008). These are some of the reasons

why I suggest to my undergraduate students who are interested in archaeological science that

they should look towards Europe for their graduate schools. The unfortunate outcome, however,

for these students, is that US universities will not be interested in hiring archaeological scientists

in anthropology departments. Still, many of us carry on, and very much look to the Old Worldas far as models for archaeological science programmes are concerned.

At 50 years old,Archaeometryis still the premier journal for archaeometry and archaeological

science. With the proposed shift to nearly monthly publication of Archaeometry, the completion

of digitization of all articles since 1958 and the journals great editing staff, lithic material

studies and archaeological petrology in archaeology are in good hands. We still have many

unanswered questions in the lithic realm, but I am confident that in time all of them will be

addressed.

ACKNOWLEDGEMENTS

Reviews like this are not the work of one scholar. I benefited immensely from advice on marbles

and stone archaeometry generally from Yannis Maniatis. Obsidian, chert and marble geochemistry


14/23


have suffered through many of the same obstacles, and I value our discussions about stone and

archaeometry. The undergraduate and graduate students in my lithic technology, archaeological

science and archaeological petrology summer field school classes have taught me as much

about geoarchaeological science as I have ever learned on my own. I want to thank Mike Tite

for having the foresight to make the first grand changes at Archaeometry, instituting ManagingEditors from the major archaeological science organizations worldwide, and Mark Pollard for

continuing that trendall the issues of Archaeometry are now digitized. Archaeometry has

joined the 21st century!

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tative analysis,American Antiquity, 60, 53151.

Shackley, M. S., 1998a, Gamma rays, X-rays and stone tools: some current advances in archaeological geochemistry,

Journal of Archaeological Science, 25, 25970.

Shackley, M. S. (ed.), 1998b, Archaeological obsidian studies: method and theory, Advances in Archaeological and

Museum Science 3, Springer/Plenum Press, New York.

Shackley, M. S., 1998c, Intrasource chemical variability and secondary depositional processes: lessons from theAmerican southwest, in Archaeological obsidian studies: method and theory (ed. M. S. Shackley), 83102,

Advances in Archaeological and Museum Science 3, Springer/Plenum Press, New York.

Shackley, M. S., 2002, Precision versus accuracy in the XRF analysis of archaeological obsidian: some lessons for

archaeometry and archaeology, inArchaeometry 98: proceedings of the 31st Symposium, Budapest, April 26May

3 1998 (eds. E. Jerem and T. K. Bir), 80510, British Archaeological Reports International Series 1043 (II), Oxford.

Shackley, M. S., 2005, Obsidian: geology and archaeology in the North American Southwest, University of Arizona

Press, Tucson.

Shackley, M. S., and Dillian, C., 2002, Thermal and environmental effects on obsidian geochemistry: experimental

and archaeological evidence, in The effects of fire and heat on obsidian (eds. J. M. Loyd, T. M. Origer and D. A.

Fredrickson), 11734, Cultural Resources Publication, US Department of the Interior, Bureau of Land Management,

Washington, DC.

Skinner, C. E., 1983, Obsidian studies in Oregon: an introduction to obsidian and investigations of selected methodsof obsidian characterization utilizing obsidian collected at prehistoric quarry sites in Oregon , Masters project,

Interdisciplinary Studies, University of Oregon.


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Skinner, C. E., Thatcher, J., and Davis, K., 1996, X-ray fluorescence and obsidian hydration rim measurement of arti-

fact obsidian from 35-DS-193 and 35-DS-201, Surveyor Fire Rehabilitation Project, Deschutes National Forest,

Oregon, Northwest Research Obsidian Studies Laboratory Report 96-33, Corvallis, OR.

Skinner, C. N., 2002, Fire regimes and fire history: implications for obsidian hydration dating, in The effects of fire

and heat on obsidian(eds. J. M. Loyd, T. M. Origer and D. A. Fredrickson), 14752, Cultural Resources Publi-

cation, US Department of the Interior, Bureau of Land Management, Washington, DC.Speakman, R. J., and Glascock, M. D. (eds.), 2007, Special issue; acknowledging fifty years of neutron activation

analysis in archaeology,Archaeometry, 49, 179420.

Speakman, R. J., and Neff, H. (eds.), 2005, Laser ablation ICPMS in archaeological research, University of New

Mexico Press, Albuquerque.

Steffen, A., 2002, The Dome Fire pilot project: extreme obsidian fire effects in the Jemez Mountains, in The effects

of fire and heat on obsidian(eds. J. M. Loyd, T. M. Origer and D. A. Fredrickson), 159202, Cultural Resources

Publication, US Department of the Interior, Bureau of Land Management, Washington, DC.

Stevenson, C. M., Carpenter, J., and Scheetz, B. E., 1989, Obsidian dating: recent advances in the experimental deter-

mination and application of hydration rates, Archaeometry, 31, 193206.

Stevenson, C. M., Freeborn, W. P., and Scheetz, B. E., 1987, Obsidian hydration dating: an improved optical tech-

nique for measuring the width of the hydration rim, Archaeometry, 29, 1204.

Stevenson, C. M., Mazer, J. J., and Sheetz, B. E., 1998, Laboratory obsidian hydration rates: theory, method, andapplication, in Archaeological obsidian studies: method and theory(ed. M. S. Shackley), 181204, Advances in

Archaeological and Museum Science 3, Springer/Plenum Press, New York.

Summerhayes, G. R., Bird, J. R., Fullagar, R., Gosden, C., Specht, J., and Torrence, R., 1998, Applications of PIXE

PIGME to archaeological analysis of changing patterns of obsidian use in west New Britain, Papua New Guinea,

inArchaeological obsidian studies: method and theory(ed. M. S. Shackley), 12958, Advances in Archaeological

and Museum Science 3, Springer/Plenum Press, New York.

Thomas, D. H., 1986, Refiguring anthropology, Waveland Press, Prospect Heights, IL.

Torrence, R., 1992, What is Lapita about obsidian? A view from the Talasea sources, in Poterie Lapita et peuplement:

actes du Colloque Lapita, Nouma, Nouvelle-Caldonie, Janvier 1992, (ed. J. C. Galipaud), 11126, ORSTOM,

Nouma.

Tykot, R. H., 1992, The sources and distribution of Sardinian obsidian, in Sardinia in the Mediterranean: a footprint

in the sea(eds. R. H. Tykot and T. K. Andrews), 5770, Sheffield Academic Press, Sheffield.Tykot, R. H., 1998, Mediterranean islands and multiple flows: the sources and exploitation of Sardinian obsidian, in

Archaeological obsidian studies: method and theory(ed. M. S. Shackley), 6782, Advances in Archaeological and

Museum Science 3, Springer/Plenum Press, New York.

Tykot, R. H., and Young, S. M. M., 1995, Archaeological applications of inductively coupled plasma-mass spectrometry,

inArchaeological chemistry V(ed. M. V. Orna), 11630, American Chemical Society, Washington, DC.

Unrath, G., Owen, L., Van Gijn, A., Moss, E., Plisson, H., and Vaughn, P., 1986, An evaluation of microwear studies:

a multi-analyst approach, Early Man News, 911, 11776.

Warashina, T., 1992, Allocations of jasper archaeological implements by means of ESR and XRF, Journal of Archaeological

Science, 19, 35773.

Ward, G., 1977, On the ease of sourcing artefacts and the difficulty of knowing prehistory, New Zealand Archae-

ological Association, 20, 18894.

Williams-Thorpe, O., 1995, Obsidian in the Mediterranean and the Near East: a provenancing success story,Archaeometry, 37, 217248.

Witthof, J., 1967, Glazed polish on flint tools, American Antiquity, 32, 38388.

Young, D., and Bamforth, D. B., 1990, On the macroscopic identification of used flakes, American Antiquity, 55, 4039.

APPENDIX

Archaeological petrology/lithic (stone) papers in Archaeometry, 19582007

This compilation of 117 papers that have appeared in Archaeometry over the past 50 years

concerns the analysis of stone, but does not include any papers that cover purely lithic tech-nology, and there are not many that cover the technology of stone tools. The list includes all

stone analyses from the first issue in 1958 through to November 2007. The citations do not


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212 M. S. Shackley

include the journal title Archaeometry. If the stone material is not mentioned in the title, it is

noted in square brackets.

Adan-Bayewitz, D., Asaro, F., and Giauque, R. D., 1999, Determining pottery provenance: application of a new high-

precision X-ray fluorescence method and comparison with instrumental neutron activation analysis, 41, 124

[obsidian].

Aitken, M. J., and Wintle, A. G., 1977, Thermoluminescence dating of calcite and burnt flint: the age relation for

slices, 19, 10010.

Allen, R. O., Luckenbach, A. H., and Holland, C. G., 1975, An application of instrumental neutron activation analysis

to a study of prehistoric steatite artifacts and source materials, 17, 6984.

Anovitz, L. M., Elam, J. M., Riciputi, L. R., and Cole, D. R., 2004, Isothermal time-series determination of the rate

of diffusion of water in Pachuca obsidian, 46, 30126.

Antonelli, F., Nappi, G., and Lazzarini, L., 2001, Roman millstones from Orvieto (Italy): petrographic and geochemical

data for a new archaeometric contribution, 43, 16789.

Antonelli, F., Bernardini, F., Capedri, S., Lazzarini, L., and Montagnari Kokelj, E., 2004, Archaeometric study of pro-

tohistoric grinding tools of volcanic rocks found in the Karst (ItalySlovenia) and Istria (Croatia), 46, 53752.

Armiento, G., Attanasio, D., and Platania, R., 1997, Electron spin resonance study of white marbles from Tharros

(Sardinia): a reappraisal of the technique, possibilities, and limitations, 39, 30920.

Aspinall, A., Warren, S. E., Crummett, J. G., and Newton, R. G., 1972, Neutron activation analysis of prehistoric flint

mine products, 14, 4154.

Attanasio, D., de Marinis, G., Pallecchi, P., Platania, R., and Rocchi, P., 2003, An EPR and isotopic study of the marbles

of the Trajans Arch at Ancona: an example of alleged Hymettian provenance, 45, 55368.

Attanasio, D., Armiento, G., Brilli, M., Emanuele, M. C., Platania, R., and Turi, B., 2000, Multi-method marble

provenance determinations: the Carrara marbles as a case study for the combined use of isotopic, electron spin

resonance and petrographic data, 42, 25772.

Banks, M., and Hall, E. T., 1963, X-ray fluorescent analysis in archaeology: the Milli-probe, 6, 3126 [general technique].

Beck, C. W., Wilbur, E., Meret, S., Kossove, M., and Kermani, K., 1965, The infrared spectra of amber and the

identification of Basaltic amber, 8, 96109.

Bello, M. A., and Martin, A., 1992, Microchemical characterization of building stone from Seville Cathedral, Spain,

34, 2130.

Bimson, M., 1982, The characterisation of mounted garnets, 24, 518.

Bowman, H. R., Asaro, F., and Perlman, I., 1973, Composition variations in obsidian sources and the archaeological

implications, 15, 1238.

Byrne, L., Oll, A., and Vergs, J. M., 2006, Under the hammer: residues resulting from production and microwear

on experimental stone tools, 48, 54964.

Capedri, S., and Venturelli, G., 2004, Accessory minerals as tracers in the provenancing of archaeological marbles,

used in combination with isotopic and petrographic data, 46, 51736.

Carter, T., and Shackley, M. S., 2007, Sourcing obsidian from Neolithic atalhyk (Turkey) using energy-dispersive

X-ray fluorescence, 49, 43754.

Conforto, L., Felici, M., Monna, D., Serva, L., and Taddeucci, A., 1975, A preliminary study of chemical data (trace

element) from classical marble quarries, in the Mediterranean, 17, 20114.Corazza, M., Pratesi, G., Cipriani, C., Lo Giudice, A., Rossi, P., Vittone, E., Manfredotti, C., Pecchioni, E., Man-

ganelli Del F, C., and Fratini, F., 2001, Ionoluminescence and cathodoluminescence in marbles of historic and

architectural interest, 43, 43946.

Cordischi, D., Monna, D., and Segre, A. L., 1983, ESR analysis of marble samples from Mediterranean quarries of

archaeological interest, 25, 6876.

Craddock, P. T., Cowell, M. R., Leese, M. N., and Hughes, M. J., 1983, The trace element composition of polished

flint axes as an indicator of source, 25, 13564.

Croudace, I. W., and Williams-Thorpe, O., 1988, A low dilution wavelength-dispersive X-ray fluorescence procedure

for the analysis of archaeological rock artefacts, 30, 22736.

DAmico, C., 2005, Neolithic greenstone axe blades from northwestern Italy across Europe: a first petrographic

comparison, 47, 23552.

Debenham, N. C., and Aitken, M. J., 1984, Thermoluminescence dating of stalagmitic calcite, 26, 15570.de Bruin, M., Korthoven, P. J. M., Bakels, C. C., and Groen, F. C. A., 1972, The use of non-destructive activation

analysis and pattern recognition in the study of flint artefacts, 14, 5564.


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Decrouez, D., Burns, S. J., Chamay, J., and Maier, J. L., 1992, Cathodoluminescence of white marbles: an overview,

34, 17584.

Della Casa, Ph., 2005, Lithic resources in the early prehistory of the Alps, 47, 22134.

Domanski, M., Webb, J. A., and Boland, J., 1994, Mechanical properties of stone artifact materials and the effect of

heat treatment, 36, 177208.

Ericson, J. E., and Kimberlin, J., 1977, Obsidian sources, chemical characterization, and hydration rates in west Mexico,19, 15766.

Flamini, A., Graziani, G., and Grubessi, O., 1975, Inorganic inclusions in amber, 17, 11011.

Fornaseri, M., Malpieri, L., and Tolomeo, L., 1975, Provenance of pumices in the north coast of Cyprus, 17, 112

15.

Gale, N. H., 1981, Mediterranean obsidian source characterization by strontium isotope analysis, 23, 4152.

Germann, K., Holzmann, G., and Winkler, F. J., 1980, Determination of marble provenance: limits of isotopic analysis,

22, 99106.

Glascock, M. D., Speakman, R. J., and Neff, H., 2007, Archaeometry at the University of Missouri Research Reactor

and the provenance of obsidian artefacts in North America, 49, 34357.

Gksu, H. Y., and Fremlin, J. H., 1972, Thermoluminescence from unirradiated flints: regeneration thermoluminescence,

14, 12732.

Gordus, A. A., Fink, W. C., Hill, M. E., Purdy, J. C., and Wilcox, T. R., 1967, Identification of the geologic originsof archaeological artifacts: an automated method of Na and Mn neutron activation analysis, 10, 8796 [early

North American obsidian study].

Grace, R., 1996, Use-wear analysis: the state of the art, 38, 20930.

Gratuze, B., Barrandon, J. N., Al Isa, K., and Cauvin, M. C., 1993, Non-destructive analysis of obsidian artefacts

using nuclear techniques: investigation of provenance of Near Eastern artifacts, 35, 1122.

Greilich, S., Glasmacher, U. A., and Wagner, G. A., 2005, Optical dating of granitic stone surfaces, 47, 64565.

Hall, E. T., 1960, X-ray fluorescent analysis applied to archaeology, 3, 2937 [general technique].

Hall, E. T., Banks, M. S., and Stern, J. M., 1964, Uses of X-ray fluorescent analysis in archaeology, 7, 849 [jade

analyses].

Harrell, J. A., 1992, Ancient Egyptian limestone quarries: a petrological study, 34, 195212.

Hassan, A. A., and Hassan, F. A., 1981, Source of galena in Predynastic Egypt at Nagada, 23, 7782.

Hay, R. L., Asaro, F., Bowman, H. R., and Michel, H. V., 1988, Sources of the quartzite of some ancient Egyptiansculptures, 30, 12031.

Herz, N., 1992, Provenance determination of Neolithic to Classical Mediterranean marbles by stable isotopes, 34,

18594.

Herz, N., Grimantis, A. P., Robinson, H. S., Wenner, D. B., and Vassilaki-Grimani, M., 1989, Science versus art

history: the Cleveland Museum head of Pan and the Miltiades Marathon victory monument, 31, 1618.

Holmes, L. L., and Harbottle, G., 2003, In the steps of William the Conqueror: neutron activation analysis of Caen

stone, 45, 199220.

Holmes, L. L., Harbottle, G., and Blanc, A., 1994, Compositional characterization of French limestone: a new tool for

art historians, 36, 2540.

Hunter, F. J., McDonnell, J. G., Pollard, A. M., Morris, C. R., and Rowlands, C. C., 1993, The scientific identification

of archaeological jet-like artefacts, 35, 6990.

Huxtable, J., and Jacobi, R. M., 1982, Thermoluminescence dating of burned flints from a British Mesolithic site:Longmoor Inclosure, East Hampshire, 24, 1649.

Jackson, M. D., Marra, F., Hay, R. L., Cawood, C., and Winkler, E. M., 2005, The judicious selection and preserva-

tion of tuff and travertine building stone in ancient Rome, 47, 485510.

James, W. D., Raulerson, M. R., and Johnson, P. R., 2007, Archaeometry at Texas A&M University: characterization

of Samoan basalts, 49, 395402.

Jones, M. C., and Williams-Thorpe, O., 2001, A illustration of the use of an atypicality index in provenancing British

stone axes, 43, 118.

Kars, E. A. K., Kars, H., and McDonnell, R. D., 1992, Greenstone axes from eastern Sweden: a technologicalpetrological

approach, 34, 21322.

Kayani, P. I., and McDonnell, G., 1996, An assessment of back-scattered electron petrography as a method for dis-

tinguishing Mediterranean obsidians, 38, 4358.

Knutsson, K., and Hope, R., 1984, The application of acetate peels in lithic use wear analysis,26

, 4961.Kohl, P. L., Harbottle, G., and Sayre, E. V., 1979, Physical and chemical analyses of soft stone vessels from southwest

Asia, 21, 131 60 [chlorite, talc/steatite].


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214 M. S. Shackley

Kuzmin, Y. V., Popov, V. K., Glascock, M. D., and Shackley, M. S., 2002, Sources of archaeological volcanic glass

in the Primorye (Maritime) Province, Russian Far East, 44, 50515.

Lambert, J. B., Frye, J. S., and Jurkiewicz, A., 1992, The provenance of coal rank of jet by carbon-13 nuclear

magnetic resonance spectroscopy, 34, 1218.

Lascalea, G. E., Pifferetti, A., Fernandez de Rapp, M. E., Walse de Reca, N. E., and Northover, J. P., 2002, The

material characterization of a Santamarian ceremonial axe, 44, 8394.Latham, A. G., and Schwarcz, H. P., 1994, The Petralona hominid site: uranium-series re-analysis of layer 10 calcite

and associated palaeomagnetic analyses, 34, 13540.

Layton, T. N., 1973, Temporal ordering of surface collected artifacts by hydration measurement, 15, 12932.

Lazzarini, L., and Antonelli, F., 2003, Petrographic and isotopic characterization of the marble of the Island of Tinos

(Greece), 45, 54152.

Liritzis, I., 2006, Sims-SS, a new obsidian hydration dating method: analysis and theoretical principles, 48, 53347.

Lloyd, R. V., Smith, P. W., and Haskell, H. W., 1985, Evaluation of the manganese ESR method of marble character-

ization, 27, 10816.

Loubser, J. H. N. Sr, and Markell, A. B., 1993, Electron spin resonance thermometry applied to quartzite cobbles

from Vergelegen slave lodge, Somerset West, South Africa, 35, 110.

Luke, C., Tykot, R. H., and Scott, R. W., 2006, Petrographic and stable isotope analyses of Late Classic Ula marble

vases and potential sources, 48, 1329.Mandal, S., 1997, Striking a balance: the roles of petrography and geochemistry in stone axe studies in Ireland, 39,

289308.

Manfra, L., Masi, U., and Turi, B., 1975, Carbon and oxygen isotope ratios of marbles from some ancient quarries of

Western Anatolia and their archaeological significance, 17, 21522.

Matthews, K. J., 1997, The establishment of a data base of neutron activation analyses of white marble, 39, 32132.

Mello, E., Monna, D., and Oddone, M., 1988, Discriminating sources of Mediterranean marbles: a pattern recognition

approach, 30, 1028.

Meredith, P., Smith, J., and Edmonds, M., 1992, Rock physics and the Neolithic axe trade in Great Britain, 34, 223

34.

Merrick, H. V., and Brown, F. H., 1984, Rapid characterization of obsidian artifacts by electron microprobe analysis,

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