2008 SHACKLEY Archeometry PDF

Archaeometry
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, 2 (2008) 194215 doi: 10.1111/j.1475-4754.2008.00390.x
*Received 10 September 2007; accepted 5 December 2007
University of Oxford, 2008

Blackwell Publishing Ltd Oxford, UK ARCH Archaeometry 0003-813X 0003-813X University of Oxford, 2008 XXX Original Articles

Archaeological petrology and the archaeometry of lithic materials M. S. Shackley

*Received 10 September 2007; accepted 5 December 2007 University of Oxford, 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

specically, 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 reection
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 technology
available to researchers in the eld.

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 rst 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 dened as the metric and
technological analysis of stone as an artefact produced by humans through time (debitage
analysis, 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.
Archaeological petrology and the archaeometry of lithic materials

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University of Oxford, 2008,

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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 eld 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 nd 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 in

Archaeometry

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 dened it above; there are very
few of these.

The Journal of Archaeological Science

(

JAS

), published rst in 1974, seems to
accept more purely technological papers on lithics than

Archaeometry

has by comparison. As
rst an associate, then the Society of Archaeological Science Managing Editor at

Archaeometry

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

JAS

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 reection of the increases in lithic material research similarly reected 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; Shackley
1998a, 2005).

THE CHEMICAL CHARACTERIZATION OF STONE:
BEYOND FISHING EXPEDITIONS

Dene the problem. A good source analysis is usually complex and expensive, and should
not be initiated merely as a shing expedition in the vague hope that you might nd some-
thing interesting. (Luedtke 1992, 117)

Since a good part of my own research is involved in the wavelength and energy-dispersive X-ray
uorescence (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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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 ne 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 assignments
are 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 macare 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
de and certied source provenance that is not probabilistic at all, but condently determined.
I am certainly not the rst 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 t to known source
Figure 1 The frequency of papers devoted to the archaeometric analysis of lithic material in Archaeometry in 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 scientic 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 their
utility 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 modied 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 rst
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 earlier
sources 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 eld, 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 technique
may not be specically 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 sufcient 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 sufcient 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 rm knowledge of potential
chert 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,
condent 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 difculties 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 aked stone raw
materials in prehistory.

Obsidian characterization and the sourcing myth

Many of the points briey 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 Heizer
1968; 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 dene 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 uorescence
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 World
and 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 uorescence 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 archaeologists
inherently 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 major
role 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 eld, 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 of
the method (Jackson 1984; Hall and Jackson 1989; Hull 2001, 2002) and those who nd 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 as
the former in her own work (Hull 2002). The recent symposium on the effects of re 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 re 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-eld studies, it has been found that there is no statistically signicant change in trace
element 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 am
glad 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 condently
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 specic (see also Maniatis
2007). This resolves some of the stable isotope difculties where source overlap problems are
not 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 condence 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 eld
and the laboratory, and while we may not always be able to fund projects based on these
precepts, 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 condent 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 ve localities, two chemical outliers were noted,
collected with signicantly higher rubidium concentration values (Shackley 1988a, 767).
These outliers have now been identied 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 eld
season, 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, gure 3.6), and signies 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 signicant 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 sufcient to
condently dene 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 (Torrence
1992; 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 eld 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 global
positioning system (GPS) coordinates, depending on the country of origin.
(4) Stratied subsamples should be derived in the laboratory by the sublocalities collected in
the eld (preferably analysing at least ve or more samples from each localitybut note that
this is not a magic number). This could mean taking thousands of samples in the eld.
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 other
stone 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 archaeological
geochemistry have similarly improved. Almost all instrumental and empirical techniques have
been used, including density, magnetism, atomic absorption, PIXEPIGME, ICP (for obsidian,
Archaeological petrology and the archaeometry of lithic materials 203
University of Oxford, 2008, Archaeometry 50, 2 (2008) 194215
see Tykot and Young 1995; Shackley 2005; Speakman and Neff 2005), megascopic criteria
and others. Today, three major instrumental methods dominate the eld: neutron activation
analysis (NAA or INAA), wavelength- and energy-dispersive X-ray uorescence (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 have
beneted 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.swxrab.net/xrnstrument.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 briey 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 cannot
analyse 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 efcient alternative. Additionally, if the sample is extremely small (< 5 mm
in largest diameter), NAA or LAICPMS may be the best analytical method. Other methods
may require a minimum sample size for optimal results (Davis et al. 1998).
For a number of years now, Michael Glascock at the University of Missouri Research Reactor
Facility, using NAA, and I at the Berkeley EDXRF Laboratory have been analysing the same
obsidian and source standards and artefacts simply as part of our routine data sharing. It is
remarkable how similar the results of the two analyses are, for the 17 or more elements measured
in common (Shackley 1998a). In his paper on the chemical variability in the Coso Volcanic
Field, Hughes (1988) also obtained similar results in the mid-Z incompatible elements
between NAA and EDXRF. Much of this is due to the extreme accuracy of EDXRF in the
mid-Z (and part of the high-Z) region, which fortunately contains some of the most sensitive
incompatible elements for discriminating volcanic rocks, including Rb, Sr, Y, Zr, Nb and Ba
(Giaque et al. 1993). Much of this paired accuracy is due to calibration to international
standards and the increasing analytical precision of todays instruments.
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
sufcient 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 region
of 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 and
prehistoric 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 akes, 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 signicance, in management decisions (see Graces
1996 review of the literature in Archaeometry).
One of the most commonly practised techniques, and one of the most empirically frustrating,
is inferring use-wear and therefore function on unmodied akes. Studies that rely on readily
available microscopic techniques are exceptions rather than the rule. Most archaeologists rely
on macroscopic examination of ake 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 identied the use-wear;
some did not. This is considerably disturbing, since the most common aked lithic tool found
in prehistoric contexts is often the utilized ake. 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 rened 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 condence, it is rarely possible to determine the
actual material that the tool was used on beyond hard or soft material. Bone and wood are
often 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.
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 that
will 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
and an 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 dened. 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 cortex
before early stages of reduction (Christensen et al. 1992, 4923). Perhaps more illuminating
was the analysis of Pre-dynastic Egyptian shtail knives and ripple-aked 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 shtail knife was used to
cut meat and the ripple-aked 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 rened 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 signicant 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 efcient, 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 sufcient to characterize any stone materialthis is a good thing.
Even obsidian, which is by denition 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
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 have
talked 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 eld (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 is
a 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 World
as far as models for archaeological science programmes are concerned.
At 50 years old, Archaeometry is 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 condent that in time all of them will be
addressed.
ACKNOWLEDGEMENTS
Reviews like this are not the work of one scholar. I beneted immensely from advice on marbles
and stone archaeometry generally from Yannis Maniatis. Obsidian, chert and marble geochemistry
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 eld 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 rst grand changes at Archaeometry, instituting Managing
Editors 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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prhistorique: actes du sminaire du Laboratoire de Recherche des Muses de France, (eds. M. Menu and P. Walter),
195200, Laboratoire de Recherche des Muses de France, Paris.
Michels, J. W., Tsong, I. S. T., and Smith, G. A., 1983, Experimentally derived hydration rates in obsidian dating,
Archaeometry, 25, 10718.
Neff, H., and Glascock, M. D., 1995, The state of nuclear archaeology in North America, Journal of Radioanalytical
and Nuclear Chemistry, 196, 27586.
Nelson, F. W., Jr, 1984, X-ray uorescence analysis of some western North American obsidians, in Obsidian studies
in the Great Basin (ed. R. E. Hughes), 2762, Contributions of the University of California Archaeological
Research Facility 45, Berkeley.
Odell, G. H., 2003, Lithic analysis, Springer Science, New York.
Odell, G., and Odell-Vereecken, F., 1980, Verifying the reliability of lithic use-wear assessments by blind tests: the
low power approach, Journal of Field Archaeology, 7, 87120.
Polikreti, K., and Maniatis, Y., 2002, A new methodology for the provenance of marble based on EPR spectroscopy,
Poupeau, G., Delerue, S., Carter, T., de B. Pereira, C. E., Miekeley, N., and Bellot-Gurlet, L., 2005, How homogeneous is
the East Gll Dag (Cappadocia Turkey) obsidian source composition? International Association for Obsidian
Studies Newsletter, 32, 38.
Ratt, J. C., 2004, A guide to the Mule Creek volcanic vent, the rhyolite of Potholes Country, and obsidian ledges,
Gila National Forest, southwestern New Mexico, New Mexico Geology, 26, 11122.
Riddings, R., 1996, Where in the world does obsidian hydration dating work? American Antiquity, 61, 13648.
Roll, T. E., Neeley, M. P., Speakman, R. J., and Glascock, M. D., 2005, Characterization of Montana cherts by
LAICP2MS, in Laser ablation ICPMS in archaeological research (eds. R. J. Speakman and H. Neff), 59
76, University of New Mexico Press, Albuquerque.
Shackley, M. S., 1988, Sources of archaeological obsidian in the southwest: an archaeological, petrological, and
geochemical study, American Antiquity, 53, 75272.
Shackley, M. S., 1995, Sources of archaeological obsidian in the greater American Southwest: an update and quanti-
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 the
American 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, in Archaeometry 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 re 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 methods
of obsidian characterization utilizing obsidian collected at prehistoric quarry sites in Oregon, Masters project,
Interdisciplinary Studies, University of Oregon.
Skinner, C. E., Thatcher, J., and Davis, K., 1996, X-ray uorescence 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 re history: implications for obsidian hydration dating, in The effects of re
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 fty 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 re effects in the Jemez Mountains, in The effects
of re 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-
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Stevenson, C. M., Freeborn, W. P., and Scheetz, B. E., 1987, Obsidian hydration dating: an improved optical tech-
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Stevenson, C. M., Mazer, J. J., and Sheetz, B. E., 1998, Laboratory obsidian hydration rates: theory, method, and
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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,
in Archaeological 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, Reguring 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:
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Nouma.
Tykot, R. H., 1992, The sources and distribution of Sardinian obsidian, in Sardinia in the Mediterranean: a footprint
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Tykot, R. H., 1998, Mediterranean islands and multiple ows: 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,
in Archaeological chemistry V (ed. M. V. Orna), 11630, American Chemical Society, Washington, DC.
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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 difculty 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,
Witthof, J., 1967, Glazed polish on int tools, American Antiquity, 32, 38388.
Young, D., and Bamforth, D. B., 1990, On the macroscopic identication of used akes, 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 rst issue in 1958 through to November 2007. The citations do not
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 uorescence 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 int: 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 int
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 uorescent 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
identication 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 uorescence, 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
int axes as an indicator of source, 25, 13564.
Croudace, I. W., and Williams-Thorpe, O., 1988, A low dilution wavelength-dispersive X-ray uorescence procedure
for the analysis of archaeological rock artefacts, 30, 22736.
DAmico, C., 2005, Neolithic greenstone axe blades from northwestern Italy across Europe: a rst 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 int artefacts, 14, 5564.
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 ints: regeneration thermoluminescence,
14, 12732.
Gordus, A. A., Fink, W. C., Hill, M. E., Purdy, J. C., and Wilcox, T. R., 1967, Identication of the geologic origins
of 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 uorescent analysis applied to archaeology, 3, 2937 [general technique].
Hall, E. T., Banks, M. S., and Stern, J. M., 1964, Uses of X-ray uorescent 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 Egyptian
sculptures, 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 scientic identication
of archaeological jet-like artefacts, 35, 6990.
Huxtable, J., and Jacobi, R. M., 1982, Thermoluminescence dating of burned ints 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, 13160 [chlorite, talc/steatite].
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 signicance, 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,
26, 2306.
Michels, J. W., Tsong, I. S. T., and Smith, G. A., 1983, Experimentally derived hydration rates in obsidian dating, 25,
10718.
Middleton, A. P., and Freestone, I. C., 1992, Archaeological stone: scientic and technical studies 1416 November
1991, the British Museum, 34, 1623.
Moffat, D., and Buttler, S. J., 1985, Rare earth element distribution patterns in Shetland steatiteconsequences for
artifact provenancing studies, 28, 10115.
Negash, Agazi, and Shackley, M. S., 2006, Geochemical provenance of obsidian artefacts from the MSA site of Porc
Epic, Ethiopia, 48, 112.
Nelson, D. E., DAuria, J. M., and Bennett, R. B., 1975, Characterization of Pacic northwest coast obsidian by X-
ray uorescence analysis, 17, 8598.
Newman, J. R., and Nielsen, R. L., 1987, Initial notes on the X-ray uorescence characterization of the rhyodacite
sources of the Taos Plateau, New Mexico, 29, 26274.
Newman, R., 1988, The materials of Hoysala temples and sculptures: a petrographic characterization, 30, 12031.
Newman, R., 1992, Applications of petrography and electron microprobe analysis to the study of Indian stone sculpture,
34, 16374.
Pecchioni, E., Cantisani, E., Pallecchi, P., Fratini, F., Buccianti, A., Pandeli, E., Rescic, S., and Conticelli, S., 2007,
Characterization of the amphorae, stone ballast and stowage materials of the ships from the archaeological site of
PisaSan Rossore, Italy: inferences on their provenance and possible trading routes, 49, 122.
Polikreti, K., 2007, Detection of ancient marble forgery: techniques and limitations, 49, 60320.
Polikreti, K., and Maniatis, Y., 2002, A new methodology for the provenance of marble based on EPR spectroscopy,
44, 121.
Pollard, A. M., Russell, G. D., and Baird, D. C., 1981, An analytical investigation of Early Bronze Age jet and
jet-like material from the Devizes Museum, 23, 13968.
Reader, C. D., 2001, A geomorphological study of the Giza Necropolis, with implications for the development of the
site, 43, 14965.
Rhodes, E. J., Stokes, S., Spooner, N. A., and Aitken, M. J., 1990, Optical dating of sediments: initial quartz results
from Oxford, 32, 1932.
Richter, D., and Krbetschek, M., 2006, A new thermoluminescence dating technique for heated int, 48, 695705.
Robins, G. V., Seeley, N. J., Symons, M. C. R., and MacNeil, D. A. C., 1981, Manganese (II) as an indicator of
ancient heat treatment of int, 23, 1038.
Rogers, M., Allen, R., Nagle, C., and Fitzhugh, W., 1983, The utilization of rare earth element concentrations for the
characterization of soapstone quarries, 25, 18695.
Rottlander, R., 1975, The formation of patina on int, 17, 1069.
Sales, K. D., Oduwole, A. D., Convert, J., and Robins, G. V., 1987, Identication of jet and related black materials
with ESR spectroscopy, 29, 1039.
Santi, P., Antonelli, F., and Renzulli, A., 2005, Provenance of medieval pietra ollare artefacts found in archaeological
sites of central-eastern Italy: insights into the Alpine soapstone trade, 47, 25364.
Sax, M., and Middleton, A. P., 1992, A system of nomenclature for quartz and its application to the material of cylinder
seals, 34, 1120.
Schwedt, A., Mommsen, H., Stephan, H.-G., and Gaimster, D., 2003, Neutron activation analyses of Falke-Group
stoneware, 45, 23350.
Scott, D. A., 1994, A useful mineral data base for the museum laboratory, 36, 1712.
Shanks, O. C., Kornfeld, M., and Ream, W., 2004, DNA and protein recovery from washed experimental stone tools,
46, 66372.
Stevenson, C. M., Carpenter, J., and Scheetz, B. E., 1989, Obsidian dating: recent advances in the experimental deter-
mination and application of hydration rates, 31, 193206.
Stevenson, C. M., Phelps Freeborn, W., and Scheetz, B. E., 1987, Obsidian hydration dating: an improved optical
technique for measuring the width of the hydration rim, 29, 1204.
Stevenson, D. P., Stross, F. H., and Heizer, R. F., 1971, An evaluation of X-ray uorescent analysis as a method for
correlating obsidian artifacts with source location, 13, 1726.
Truncer, J., Glascock, M. D., and Neff, H., 1998, Steatite source characterization in eastern North America: new
results using instrumental neutron activation analysis, 40, 2344.
Trkmenoglu, A. G., Gktrk, E. H., and Caner, E. N., 1991, The deterioration of tuffs from the Cappadocia region
of Turkey, 33, 2318.
Uchida, E., Cunin, O., Shimoda, I., Suda, C., and Nakagawa, T., 2003, The construction process of the Angkor
monuments elucidated by the magnetic susceptibility of sandstone, 45, 22132.
Unterwurzacher, M., Polleres, J., and Mirwald, P., 2005, Provenance study of marble artefacts from the Roman burial
area of Faschendorf (Carinthia, Austria), 47, 26573.
Valladas, H., 1981, Thermoluminescence de grs de foyer prhistoriques: stimation de leur temperature de chauff,
23, 2219 (burned sandstone).
Valladas, H., and Valladas, G., 1987, Thermoluminescence dating of burnt int and quartz: comparative results, 29,
21420.
Vendrell-Saz, M., Alarcn, S., Molera, J., and Garcia-Valls, M., 1996, Dating ancient lime mortars by geochemical
and mineralogical analysis, 38, 14350.
Ward, G. K., 1974, A systematic approach to the denition of sources of raw material, 16, 4154 [obsidian sources].
Weymouth, J. W., and Mandeville, M., 1975, An X-ray diffraction study of heat-treated chert and its archaeological
implications, 17, 618.
Wheeler, M. E., and Clark, D. W., 1977, Elemental characterization of obsidian from the Koyukuk River, Alaska by
atomic absorption spectrophotometry, 19, 1532.
Williams-Thorpe, O., 1995, Obsidian in the Mediterranean and the Near East: a provenancing success story, 37, 217
48.
Williams-Thorpe, O., and Thorpe, R. S., 1990, Millstone provenancing used in tracing the route of a fourth-century
bc Greek merchant ship, 32, 11538.
Williams-Thorpe, O., and Thorpe, R. S., 1993, Magnetic susceptibility used in non-destructive provenancing of
Roman granite columns, 35, 18596.
Williams-Thorpe, O., Jones, M. C., Tindle, A. B., and Thorpe, R. S., 1996, Magnetic susceptibility variations at Mons
Claudianus and in Roman columns: a method of provenancing to within a single quarry, 38, 1542.
Williams-Thorpe, O., Jones, M. C., Webb, P. C., and Rigby, I. J., 2000, Non-destructive portable gamma ray
spectrometry used in provenancing Roman granitoid columns from Leptis Magna, North Africa, 42, 77100.
Yang, M.-L., Lu, C.-W., Hsu, I.-J., and Yang, C. C., 2004, The use of optical coherence tomography for monitoring
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2008 SHACKLEY Archeometry PDF

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