Identifying Migration: Strontium Isotope

Studies on an Early Bell Beaker Population

from Le Tumulus des Sables, France.

Ceridwen A Boel

Honours thesis submitted as part of the B.A. (Hons) degree completed in

the School of Archaeology and Anthropology, in conjunction with the

Research School of Earth Sciences, Australian National University,

Canberra.

24th

October 2011

Statement of Authorship

I certify that this is my own original work. No other person’s work has been used, in

part or whole, unless otherwise acknowledged in the text.

Name: Ceridwen Amy Boel

Date: 24th

October 2011

Signature:

i

Abstract

______________________________________________________

Strontium isotope ratios (87

Sr/86

Sr) can be used to trace the migration of people

and animals across geologically different regions. This study has applied

strontium isotope analysis to teeth from 16 adults and 8 juveniles from what

has been identified as an early Bell Beaker (Chalcolithic, 2500 – 2000 BC) site

at Le Tumulus des Sables in south-west France. The analysis was primarily

conducted using laser ablation ICP-MS, to determine U, Th and Sr elemental

concentrations and Sr isotope ratios. Four of the teeth were also analysed using

solution ICP-MS for comparison with the laser ablation results. Significant

offsets in the Sr isotope ratios were identified between the laser ablation and

solution methods of analysis, and the correction for this resulted in large

uncertainties (up to 0.6%). Despite this, most teeth showed a clear difference

between the enamel and the overprinted dentine, suggesting mobility. The

dental results were compared to a Sr isotope map of the Médoc region, created

using a set of soil samples collected from the major geologic units and from the

archaeological site. These were also analysed using solution ICP-MS. The

different geologic regions separated well according to Sr isotope ratios, with

the exception of the Holocene costal sediment. The Sr isotope ratio range

within the Médoc region was found to be very large, encompassing all of the

dental Sr values. The variation in the enamel signatures suggested a high

degree of mobility, but due to the large regional Sr range it was impossible to

distinguish migration from beyond the Médoc from mobility within the region.

If the individuals were from outside the Médoc, the Sr isotope ratios indicate

that they are most likely to have come from the east of the Médoc. Origins to

ii

the south in are unlikely, as are origins in mountainous areas such as the

Pyrenees and the Massif Central. The results from this study indicate that

archaeological soil cannot be considered to provide a reliable local range, and

highlights the importance of regional mapping in Sr isotope studies.

iii

Acknowledgements

______________________________________________________

This honours project would not have been possible without the support,

guidance, and assistance of a number of people. Firstly, I am indebted to my

supervisors Rainer Grün, Dougald O’Reilly, and Matthew Spriggs, for their

support and encouragement, and for helping me to negotiate the careful balance

between two related but very different disciplines, Archaeology and Earth

Sciences. Thanks also to Malte Willmes and Ian Moffatt for their assistance not

only in the lab and field, but in the office as well. Their assistance with the

practical components, as well as in refining my thoughts and ideas, has been

invaluable.

Thank you to Patrice Courtaud from the University of Bordeaux, for providing

the soil and teeth samples from Le Tumulus des Sables, as well as helping me

to understand the site itself. Thank you for allowing me to be a part of the

project, and also for giving me the opportunity to come into the field and see

the site of Le Tumulus des Sables as well as another excavation first hand.

Thanks also to Philippe Rossi from the BRGM in Orléans, for providing us

with, and helping us to understand, the geological maps of the region.

My thanks to the staff and students of the Research School of Earth Sciences,

for their assistance, support and acceptance, even though I came from the other

side of the campus. A special thanks to Les Kinsley and Linda McMorrow, for

all of their help operating and understanding the Neptune, Varian and Vista,

and to Les for helping me to make sense of the solution spreadsheet. My

sincere thanks also to Steve Eggins, for helping me to understanding the laser

iv

ablation method and to make sense of all of the raw data, even when you had a

thousand other things to do!

Last but certainly not least, thank you to my wonderful partner, Gerard

Atkinson. Thank you for your unconditional love and support, for picking me

up as late as 2am after long nights in the office/lab, and for teaching me to

drive so you wouldn’t have to do it again!

v

Contents

______________________________________________________

Abstract………………………………………………………………..……….i

Acknowledgements………………….……………………………….…..…...iii

Contents…………………………………………………………………….….v

List of Figures………………………………………………………..…...…viii

List of Tables……………………………………………………………….….x

__________________________________________________________

Chapter 1: Introduction………………………………………..………1

1.1. Significance of the research.….………………………………………….1

1.2. Aims……………………………………………….………………………2

1.3. Site description……………………………………….………………...2

1.3.1. Le Tumulus des Sables…………………………...……………...2

1.3.2. Regional geology……..…………………………….……………6

1.4. Thesis overview…………………………………………………………7

__________________________________________________________

Chapter 2: Background……………………………………………….8

2.1. The Bell Beaker Phenomenon…………………………………..……….8

2.1.1. What is the Bell Beaker phenomenon?.........................................8

2.1.2. The Bell Beaker debate……………………………….……11

2.2. Strontium as an archaeometric tool………………………………..…..12

2.2.1. Basic strontium chemistry…………………………………….12

2.2.2. Incorporation into the body…………………………………..15

2.2.3. Mapping………………………………………………………...15

vi

2.2.4. Diagenesis and the identification of migration…………………18

2.3. Previous applications…………………………………………………..21

__________________________________________________________

Chapter 3: Methodology……………………………………………...23

3.1. Sample collection………………………………………………………..23

3.2. Sample preparation……………………………………………………..27

3.2.1. Cleaning………………………………………………………..27

3.2.2. Soil……………………………………………………………...28

3.2.3. Teeth……………………………………………………………29

3.2.3.1. For laser analysis…………………………………29

3.2.3.2. For solution analysis……….…………..………..30

3.3. Sample analysis………………………………………………………….30

3.3.1. HelEx laser system……………………………………………..31

3.3.2. Varian Vista ICP-AES - Elemental concentrations (Soil)……...32

3.3.3. Varian ICP-MS – Elemental concentrations (Teeth)…………...33

3.3.4 Neptune ICP-MS – Isotopic composition………………………36

__________________________________________________________

Chapter 4 : Resul t s……………………… …………………39

4.1. Soil…………………..………………………………………………….39

4.1.1. The Médoc region………………………………………………39

4.1.2. Le Tumulus des Sables………………………………………40

4.2. Teeth…………………………………………………………………….42

4.2.1. Elemental concentrations (Varian)……………………………43

4.2.2. Isotopic composition (Neptune)………………………………46

vii

4.2.2.1. Laser………………………………………………………...46

4.2.2.2. Solution……………………………………………………49

4.2.3. Examples……………………………………………………….53

__________________________________________________________

Chapter 5: Discussion…………………………………………………62

5.1. Soil analyses………………………………………………………… .62

5.1.1. The Médoc region………………………………………………62

5.1.2. Le Tumulus des Sables…………………………………………64

5.2. Teeth analyses………………………………………………………...65

5.2.1. Laser vs. solution…………………………………………...…..65

5.2.2. Locals or non-locals?...................................................................67

5.2.2.1. Enamel vs. Dentine……………………………………...….68

5.2.2.2. Dental results in the regional context…………………..…..70

5.2.2.3. Further investigation………………………………………..74

5.2.3. Implications for the technique……………………………..….77

5.2.4. Implications for the Bell Beaker………………………………..79

5.3. Summary………………………………………………………………...82

__________________________________________________________

Chapter 6: Conclusion……………………………………………..…84

6.1. Conclusions and recommendations……………………………………84

__________________________________________________________

References……………………………………………………………...88

__________________________________________________________

Appendices………………………………………………………….…98

__________________________________________________________

viii

List of Figures

______________________________________________________

Figure 1.1.: Image of Saint-Laurent Médoc……..……………...……….……..5

Figure 1.2.: Summary plan of the excavations…………………..……………..5

Figure 1.3.: Geological map of the region, located on a larger map of

France…………….…………………………………………………….7

Figure 2.1.: The approximate distribution of the Bell Beaker Phenomenon

known from archaeological sites…………...……………..…………..10

Figure 2.2.: Periodic table of the elements………………………..…………..14

Figure 3.1.: Locations of the soil samples taken from the site of Le Tumulus

des Sables…………………………………………………………….24

Figure 3.2.: Geologic map of the Médoc and surrounding region, showing

sample locations for this study (F11-188 – F11-198) and others

taken in this region for related research……….....………...…………25

Figure 3.3.: Examples of two photographs, before any preparation and after

analysis, while still loaded in the ring……………………….………..30

Figure 3.4.: The ANU HelEx laser ablation setup…………….…….………..32

Figure 3.5.: Schematic diagram of an ICP-AES……………….……..……....33

Figure 3.6.: Schematic diagram of a laser ablation cell connected to a

quadrupole ICP-MS………………………………………….………..34

Figure 3.7.: Schematic diagram of a Finnigan MAT Neptune……...……..…36

Figure 4.1.: Graphs of the elemental concentrations and isotopic composition,

along with an image of the tooth (SLMEM1007)………………...….54

Figure 4.2.: Graphs of the elemental concentrations and isotopic composition,

along with an image of the tooth showing the spots made for

ix

Neptune analysis (SLMEM1192)……………………….….…...……57

Figure 4.3.: Graphs of the elemental concentrations and isotopic composition,

along with an image of the tooth showing the spots made for Neptune

analysis (SLMEM 491)……………………….………………..……..59

Figure 4.4.: Graphs of the elemental concentrations and isotopic composition,

along with an image of the tooth (SLMEM112)…………………..….61

Figure 5.1.: Measured 87

Sr/86

Sr ranges for each geologic unit in the Médoc

peninsula and the site of Le Tumulus des Sables………….……….…63

Figure 5.2.: Measured 87

Sr/86

Sr ratios for each geologic unit in the Médoc

peninsula and the offset adjusted enamel and dentine ranges (errors

included)…………………..……………………………………….….71

Figure 5.3.: Geological map of France around the Médoc……………………73

x

List of Tables

______________________________________________________

Table 3.1.: Sediment description for all soil samples………………………...26

Table 4.1.: 87

Sr/86

Sr ratios with voltages and errors for the samples gathered

during fieldwork. Includes standards (SRM987) measured during

the analyses……………………………………..……………………40

Table 4.2.: 87

Sr/86

Sr ratios for the first 7 soil samples including errors, and

standards (SRM987) measured intermittently during solution

analyses….……………………………………………………………41

Table 4.3.: 87

Sr/86

Sr ratios with voltages and errors for second batch of soil

samples from the site. Includes standards (SRM987) measured

during the analyses……………..…………………………………….42

Table 4.4.: U, Th and Sr concentrations in all teeth (averages across high and

low zones)………………………………………………………........45

Table 4.5.: 87

Sr/86

Sr ratios for the enamel and dentine of each tooth

(averages from appropriate locations), including errors…………..….48

Table 4.6.: Average 87

Sr/86

Sr values from standard measurements taken at

each interval (minimum of three in each group)……...………….…..49

Table 4.7.: 87

Sr/86

Sr values for the teeth analysed by solution MC-ICP-MS

including errors and standards………..…………………………...….51

Table 4.8.: 87

Sr/86

Sr values provided by solution, by laser analysis selecting

The appropriate zones, and by laser analysis using all values. The

differences between laser and solution, and laser (all values) and

solution, are provided for comparison…….………….………….......51

Table 4.9.: Laser 87

Sr/86

Sr values, with average offsets subtracted………....52

1

Chapter 1

Introduction __________________________________________________________

1.1. Significance of the research

Stable strontium isotope analysis has been used to gather information on

geological and ecological systems and processes for decades (e.g. Åberg et al.,

1999, Bain and Bacon, 1994, Karim and Veizer, 2000, Widerlund and

Andersson, 2006, Capo et al., 1998) It is only comparatively recently, however,

that researchers have begun to apply it in an archaeological context (Ericson,

1985). As such, it is hardly surprising to find that the scope of application and

depth of potential of this technique are still being realised. Of the numerous

archaeological applications of the technique, including tracing the origins and

trade patterns of pottery or determining the provenance of textiles, perhaps the

best known and best developed application is the analysis of teeth to identify

and possibly trace migration. The origin and nature of the Bell Beaker culture

in Europe has been a topic of debate for decades and, despite considerable

progress in our understanding of the phenomenon, is yet to be adequately

resolved. Through the use of strontium isotope analysis, this study provides

some insight into the mobility of what is thought to be a Bell Beaker

population from the site of Le Tumulus des Sables, and offers to continue

improvement in our understanding and utilisation of the technique.

2

1.2. Aims

The primary aim of this study is to determine whether the individuals from the

study site are of local or non-local origin. Within and relating to this primary

aim, there exist a number of secondary aims. These are:

i) To compare the juvenile and adult samples in an attempt to detect a

difference in patterns of mobility.

ii) To expand of our understanding of the Bell Beaker phenomenon as a whole.

iii) To compare the results obtained by two different extraction methods, laser

ablation and solution, to detect differences in the data sets and aid in the

evaluation of their usefulness, accuracy and viability.

1.3. Site description

1.3.1. Le Tumulus des Sables

The site of Le Tumulus des Sables is located in the town of Saint-Laurent

Médoc, in the Médoc region to the north west of Bordeaux (45°8‟44”N,

0°49‟37”W, see Figure 1.1.). The site and excavations have been fully

documented in yearly site reports and a poster (Chancerel and Courtaud, 2006,

Courtaud et al., 2008, Courtaud et al., 2007, Courtaud et al., 2010, Courtaud et

al., 2009a, Courtaud et al., 2009b). The site, located in what was a part of the

local school grounds, was discovered comparatively recently when human

remains were accidentally uncovered by the school children. The burial itself

was contained within a roughly circular raised mound 7x8m in diameter and

50cm high at the peak. The excavators believe that this mound was natural, and

3

that the burial was placed on it. The site is also distinguished by the colour of

the sediment, being mostly yellowish brown (10YR 5/4, 5/6, 6/6) to dark

yellowish brown (10YR 4/4, 4/6), while being surrounded by a sterile sand of

more gray/white hues that is at least 2m deep. So far as was visible while

conducting fieldwork in the region, the region is dominated seemingly

exclusively by sandy soils of greyish colour, ranging from almost white,

through greyish browns, to nearly black. The excavators theorise that the

brownish soil is the result of acid released by the limestone which occurs at the

site.

The burial itself is 30cm deep, and the remains are highly disarticulated and

fragmented; anatomical connections between associated bones were impossible

to establish. The archaeological deposit associated with the collective burial is

not confined to the mound itself, and is irregular in shape as pictured in Figure

1.2. Some stratigraphy is preserved, although it is not evident within the burial

context itself and is not uniform across the site. The significant fragmentation

of the remains may be in part due to bioturbation, although it is thought that

this played a minimal part in site disturbance. The presence of patches of

darker yellow and brown that have not been mixed in with the rest of the soil

are evidence for the integrity of the deposit. The skeletal fragmentation may

also be in part due to the nature of the burial, as it likely originally belonged to

a culture that predated the use of the site by Bell Beaker people. Bell Beaker

graves and tomb re-use will be discussed further in section 2.1.1. Some

artefacts and bones were able to be collected from the surface, most likely due

to a combination of some turbation and weathering.

4

The site was identified as having been used by the Bell Beaker people on the

basis of distinctive material discovered within the burial. This has been

confirmed by the dating of a bone fragment, yielding a calibrated date of 2490-

2290BC. Two dates were also obtained from coal towards the bottom and top

of the excavation, providing calibrated dates of 6072-5985BC and 1395-

1214BC respectively. The older age, corresponding to the Mesolithic, surprised

the excavators somewhat given that there was no archaeological indication of

occupation in this period. The ceramic finds also indicated occupation

extending from the Neolithic, through the Bell Beaker period, and into

protohistoric and Iron Age periods. The extent of the age range of the site and

the poor stratigraphy prevent the secure identification of a particular sample as

belonging to the Bell Beaker without individually dating it. Given our

understanding of Bell Beaker burial practices in this area, it seems likely that a

proportion of the individuals may belong to the Bell Beaker; however, the most

that can be said at this point is that Bell Beaker associated artefacts have been

identified at the site and that at least one individual was dated to this period of

time.

5

Figure 1.1.: Saint-Laurent Médoc (Google Earth 2011). Le Tumulus des

Sables is marked in red.

Figure 1.2.: Summary plan of the excavations (from Courtaud et al., 2010)

6

1.3.2. Regional geology

Saint-Laurent Médoc is situated about 40km north-west of Bordeaux on the

Médoc peninsula in southwest France. The Médoc peninsula, situated between

the Atlantic coast and the Gironde, is predominantly composed of Quaternary

sand, clay and gravel sediment, with a band of Holocene sands, clays, pebbles

and gravel along the shorelines of the Atlantic Ocean and the Gironde. Some

small patches of Eocene and Oligocene limestone, conglomerates and

sandstone occur towards the eastern edge. The region is principally used for

tree plantations and vineyards; however, some crop agriculture is also

undertaken. The whole area is quite flat and low lying, making it quite difficult

to locate rock outcrops. This has implications for mapping techniques and our

interpretation of the soil results, which will be discussed in later chapters.

Particularly towards the western edge of the peninsula, most variation in

altitude is attributable to sand dunes. Like the sediment from Le Tumulus des

Sables, the sediment in the whole region is predominantly sandy, with some silt,

clay and gravel. The majority of the soil is grey to dark grey, with some

greyish browns where the soil has a larger organic component.

7

Figure 1.3.: Geological map of the region, located on a larger map of

France (adapted from Bureau de recherches géologiques et minières, 2005,

GoogleEarth, 2011)

1.4. Thesis overview

The following chapter provides an overview of the previous work and

background information relevant to this study. This covers the fundamentals

and history of the Bell Beaker phenomenon and debate, the principals and

techniques of strontium isotope analysis for tracing migration, and the previous

applications of this technique to Bell Beaker populations. Chapter 3 details the

methods used in this study, including sample collection, preparation, and

analysis processes and techniques. The results are presented in chapter 4, and

these are subsequently discussed in depth and related back to the

archaeological problem in chapter 5. Chapter 6 provides a summary and

conclusion, as well as suggestions for further research.

8

Chapter 2

Background _______________________________________________________________

2.1. The Bell Beaker phenomenon

2.1.1. What is the Bell Beaker phenomenon?

The term “Bell Beaker” was initially used to describe a distinctive type of

ceramic ware, but has since been used to describe an artefact assemblage, a

cultural complex, a group of people, and a period in time (e.g. Benz et al., 1998,

Heyd, 1998, Price et al., 1998, Shennan, 1976, Shennan, 1977). Bell Beaker

ceramic ware is characterised by inverted-bell shaped vessels, commonly

referred to as beakers. Since the initial descriptions of the ceramics in the 19th

century, (Benz et al., 1998), a number of other artefact types have come to be

recognised as part of a Bell Beaker assemblage, including some of the first

gold and bronze objects in Europe, jet, amber and obsidian ornaments, V-

perforated buttons, tanged daggers, and archery equipment including projectile

points and stone wrist guards (Desideri, 2008, Price et al., 1998, Price et al.,

2004, Vander Linden, 2006). Some researchers have also associated specific

morphological characteristics with the Bell Beaker people. Brachycephaly, a

condition in which the head is short and broad, is one such trait, having been

observed to occur frequently among Bell Beaker populations (Benz et al., 1998,

Turek, 1998). The causes for this have not yet been thoroughly investigated,

however, and it could simply be the result of diet, socioeconomic factors, or

methods of partner selection. Dental non-metric traits have been studied on

Bell Beaker populations, with results suggesting population discontinuity

9

between the Bell Beaker and preceding cultures in most areas (Desideri, 2008,

Desideri and Besse, 2010).

The Bell Beaker phenomenon (BBP) extends across most of Europe, occurring

around the transition from the Neolithic to the Bronze Age (Figure 2.1.),

although it manifests at different times in different areas. As a whole, it is

thought to have developed around 2,900 BC and persisted until roughly 1,800

BC (Desideri, 2008). While there is still some debate on this matter, it is

considered likely that the BBP originated in the Iberian Peninsula (Lemercier,

2004, Haak, 2011, Desideri, 2008). In addition to chronological variations in

the manifestation of the phenomenon, there are also significant spatial

variations. These variations occur most prominently between the eastern and

western domains, and are evident in a number of aspects of the phenomenon. It

goes beyond the variation in material culture (e.g. Benz et al., 1998), extending

to burial traditions, physical characteristics, and possibly even isotopic data.

Most eastern Bell Beaker burials are single inhumations; however, this

tradition did not take hold in western Europe until much later. For much of the

Bell Beaker period, the western domain was characterised by the re-use of

megalithic tombs of the preceding cultures (Benz et al., 1998, Chambon, 2004,

Vaquer, 1998). These are mass inhumations of variable size, and graves

containing 20-30 individuals, as seen at Le Tumulus des Sables, are not

uncommon (e.g. Heyd, 1998). While the Bell Beaker phenomenon is often

represented in collective graves, there are only a few cases where a particular

body can be identified with certainty as a Bell Beaker individual. This is at

least in part due to the way the tombs were re-used, and this is itself is quite

10

variable. The previous occupants may have been pushed aside, the new

occupants may simply have been placed on top of or alongside them, or the

tomb may have been partially or completely emptied first (Chambon, 2004). In

terms of morphology, significant variation between the east and west was noted

in dental non-metric traits, reflecting different patterns of settlement,

population exchange and population development between the two spheres

(Desideri, 2008). While the variations are most significant between the eastern

and western spheres, there are also noticeable differences between smaller

regions. This, along with other factors, gives rise to some question as to

whether the BBP truly represents a culture in the accepted archaeological sense

(see 2.1.2.). The term „phenomenon‟ seems to be universally acceptable and

avoids the implication of alignment in the debate, hence its use in this context.

Figure 2.1.: The approximate distribution of the Bell Beaker Phenomenon

known from archaeological sites (from Vander Linden, 2006).

11

2.1.2. The Bell Beaker debate

While many explanations have been offered for the origin and nature of the

BBP, these can generally be divided into two main camps – that the

phenomenon is the result of the migration of culture bearing individuals, or that

it is instead the result of cultural diffusion, and the movement of objects and

ideas. Debate of this type is by no means restricted to the BBP, and tends to

feature quite prominently in archaeology the world over. These questions

concerning the origin and nature of the BBP became the focal point of Bell

Beaker research very early on, with debate over whether the objects were

traded or transported with mobile groups developing in 1906 (Schliz, 1906,

Benz et al., 1998). The Bell Beaker assemblage appears to be most coherent in

a funerary context, leading to the development of the “prestige goods” model

in the 1970‟s, which describes the assemblage as the material manifestation of

a Bell Beaker ethos, based upon individualistic and warlike values, and

circulated amongst the elites as a symbol of prestige and power (Benz et al.,

1998, Shennan, 1976, Shennan, 1977, Vander Linden, 2006, Bailley, 1998).

This model is one of the best known and most influential models in which

cultural diffusion and the movement of objects and ideas (rather than people) is

invoked. This model suggests that the Bell Beaker assemblage represents the

culmination or, at the very least, heightened continuation of late Neolithic

social competition. No break with the preceding cultures is recognized, just the

accumulation of non-functional items for which a prestige explanation is

necessarily invoked.

12

Despite continuity in settlement patterns and subsistence techniques, however,

there are strong arguments against a supposition of cultural continuity. Conflict

in the later neolithic does not reach a climax in the Bell Beaker period; in fact,

evidence of conflict wanes, and significant diversity in ornamentation and

weapons is replaced by homogeneity (Vander Linden, 2006). The idea that Bell

Beaker artefacts were traded amongst the elites is further undermined by

evidence for the local production of pottery, using local materials. This

indicates local know-how, which in turn indicates the mobility of people

bringing this knowledge (Benz et al., 1998, Vander Linden, 2007a, Vander

Linden, 2007b). Both artefacts and site data show the BBP to be a cultural

spread, rather than diffusion, with phases of exploration, settlement and

acculturation of local populations. Some argue that the spread of the Bell

Beaker allowed the development of lines of communication, facilitating the

exchange of objects, ideas and people (e.g. Lemercier, 2004), while others

believe that it was the establishment of this network that allowed the spread of

the BBP; the integration of individuals or groups would have led to the

emergence of Bell Beaker specific settlements, and it is then that it becomes a

true culture (e.g. Benz et al., 1998). Either way, it is agreed that during the Bell

Beaker period that exceptional lines of communication were established.

The idea of human mobility is further supported by a major strontium isotope

study on Bell Beaker people in Germany, Hungary, Austria and the Czech

Republic (Grupe et al., 1997, Grupe et al., 1999, Price et al., 1994, Price et al.,

1998, Price et al., 2002a, Price et al., 2004), which echoes the previously

mentioned study on dental morphology (Desideri, 2008, Desideri and Besse,

13

2010). This has been further demonstrated by recent work which has not yet

been published demonstrating genetic discontinuity between Bell Beaker

populations and their predecessors (Haak, 2011, pers. comm.). This genetic

work indicates a higher affinity with modern Iberian populations, supporting

the notion that the Bell Beaker people originated in this area (e.g. Desideri,

2008, Lemercier, 2004). In France, particularly, the time lag of several hundred

years between the appearance of the BBP in the south and north would seem to

support this (Salanova, 1998).

2.2. Strontium as an archaeometric tool

2.2.1. Basic strontium chemistry

Strontium (Sr) is a member of the alkaline earths, group IIA of the periodic

table (Figure 2.2.), and like all elements in this group it readily forms ions with

a charge of 2+. Almost all rocks contain strontium in detectable quantities, and

its distribution is controlled by factors such as the extent to which Sr2+

can

substitute for Ca2+

(also a group IIA element, with a similar ionic radius), and

the degree to which it can be captured in the place of K+ ions in potassium

feldspar (Faure and Powell, 1972). Strontium exists in both stable and unstable

isotopic forms; it is the stable isotopes which are used to trace mobility.

Isotopes are forms of the same element with different numbers of neutrons in

the nuclei, giving them variable atomic weights. The number of protons

remains unchanged, so they retain the same chemical properties. Strontium

occurs naturally in four stable isotopic forms, 88

Sr, 87

Sr, 86

Sr and 84

Sr, of

varying natural abundance (Faure, 1986). Of these four, only 87

Sr is radiogenic,

14

being produced by the decay of 87

Rb over a half life of roughly 4.88 x 1010

years (Bentley, 2006). As a result, the proportion of 87

Sr in a substrate is

variable with respect to the other stable strontium isotopes, which occur in

fixed proportions. It is the 87

Sr/86

Sr ratio that is generally used, being

determined both by the relative concentrations of strontium and rubidium in the

rock, as well as by the age of the formation (that is, the time over which the

87Rb in the rock has been decaying to

87Sr). As rock composition is

geographically variable, so too is the 87

Sr/86

Sr ratio. This makes it possible, in

principle, to source individuals and trace mobility (Beard and Johnson, 2000,

Bentley, 2006, Ericson, 1985, Ericson, 1989).

Figure 2.2.: Periodic table of the elements. Red is used to mark strontium

(Sr) and the alkaline earths.

(from http://www.geokem.com/images/pix/pt.gif)

15

2.2.2. Incorporation into the body

There are a number of factors which influence the incorporation of strontium

into the body. As mentioned above, the distribution of Sr in rocks is partially

determined by the extent to which Sr2+

substitutes for Ca2+

in calcium-bearing

minerals. Strontium enters the body in the same way, substituting for calcium

in a number of minerals including apatite, which is a major component of teeth

and bones (Bentley, 2006, Faure and Powell, 1972). The ratio of bodily

strontium is considered to be an average of all ingested strontium; however,

there are a number of factors to take into consideration. While strontium may

substitute for calcium, the two are absorbed by the body at different rates. On

average, 19-25% of ingested strontium is absorbed during digestion, compared

to 40-80% of calcium (Sips et al., 1996). Additionally, strontium is biopurified

where calcium is not, as it plays no role in physiological processes. This further

decreases the quantity of strontium at each trophic level. With this reduction in

quantity also comes a reduction in 87

Sr/86

Sr ratio variance; however, the ratio

itself is unchanged. Fortunately, the comparative size of strontium means that

the effects of fractionation in physiological processes, in which smaller or

larger (lighter or heavier) isotopes may be favoured, are negligible (Bentley,

2006).

2.2.3. Mapping

As mentioned previously, the 87

Sr/86

Sr ratio is geographically variable. In order

for this variability to be utilised, it is necessary to create an isotopic map of an

appropriate region around the archaeological site under investigation. While

16

bedrock regions of the same type (e.g. limestone) will generally be of similar

elemental composition and have similar isotopic signatures, variations in

composition and age of the rock make it difficult to predict the Sr isotopic

signature based on the analysis of similar rock types. To complicate matters

further, the signature of the bedrock in an area is not necessarily the same as

that of the covering soil and plants. While the weathering of bedrock is the

major contributor to plant and soil 87

Sr/86

Sr ratios (Bern et al., 2005), there are

a number of factors influencing the bioavailable 87

Sr/86

Sr ratio (i.e. the Sr

entering the food chain) in any given area. Different rock types weather

differentially and may be exposed to different weathering processes and

intensities; as such their contribution to the bioavailable strontium is uneven.

The diversity of the local geology may have large impact of the signature, as

the bioavailable strontium will reflect an aggregate of the area (Budd et al.,

2004). In addition to this effect, Sr may also be contributed to the system from

other sources. Consequently, bioavailable Sr in any given area has been more

accurately described as the result of a system of inputs and outputs (Bentley,

2006). Other sources of Sr may include sediment carried by streams from

different areas, as well as the streams themselves, and atmospheric sources

such as precipitation, and dirt and dust carried by the wind. In coastal areas,

sea spray may be a contributing factor (Bentley, 2006). In a modern context,

exotic sources of Sr such as fertiliser may also contribute to, and complicate

the system further.

As demonstrated, creating the 87

Sr/86

Sr ratio map of any given area is far more

complex than simply mapping the 87

Sr/86

Sr signatures of the bedrock in the

17

area. Perhaps the most effective way of measuring the bio-available isotopic

signature of a given area is not to measure each of these individual components

and how they interact, but to measure the 87

Sr/86

Sr ratio of the fauna and flora

in the area. Due to the impact of modern contamination of the isotopic

signatures through the introduction of fertilisers, etc, the modern fauna and

flora in the area may yield a significantly different isotopic signature to the

prehistoric samples that are more likely to be of interest in an archaeological

setting. It is most useful instead to measure archaeological remains of

herbivores. Small herbivores are suitable as they have a restricted range,

reducing the impact of exotic signatures, and they develop a consistent average

87Sr/

86Sr ratio representative of the area (Bentley et al., 2004, Price et al.,

2002b). Such measurements are best conducted on a number of individuals to

provide a local range rather than a single value, as there is demonstrated

behavioural and isotopic variation even at the herd level in many animals

(Britton et al., 2009).

The above mentioned method may be ideal for the establishment of the isotopic

signature at an archaeological site, but this is not always possible. This may be

because the site is lacking in archaeological faunal remains, or due to project

limitations. Fortunately, there are other methods involving the measurement of

local rock, soil and plant signatures. There is research to suggest that even on

highly weathered soils, bioavailable strontium still predominantly reflects local

rock sources (Bern et al., 2005). As such, soil may be used as an indicator of

the local strontium range, provided it is carefully selected to avoid major

sources of contamination, such as fertilisers on farmed land.

18

2.2.4. Diagenesis and the identification of migration

When investigating faunal material, diagenesis is a key consideration. In an

archaeological context, diagenesis refers to all chemical and mineralogical

changes that a sample experiences after deposition. Skeletal material deposited

in sediment will undergo a variety of alterations, one being the exchange of

isotopes with the surrounding sediment. While some of the original Sr isotopic

composition may be preserved, diagenetic Sr displaying the local composition

may be absorbed, altering the 87

Sr/86

Sr ratio. Different types of skeletal tissue

may be affected by diagenesis to different degrees. Previously, bone and

enamel have been compared in strontium isotope studies under the assumption

that bone, which is constantly remodelling, would reflect the location in which

the individuals resided in the final years of their lives, and that the enamel

would reflect their place of residence in the early years of their lives in which it

was formed. However, given concerns about the effects of diagenesis, doubt

has been cast upon the value of bone as a source of information. Bone is porous,

and composed of small hydroxyapatite crystals mixed with roughly 30%

organic matter. This allows significant diagenetic alteration to occur. Tooth

enamel, on the other hand, is essentially non porous, and is composed of much

larger hydroxyapatite crystals with a much smaller amount of organic matter

included. As a result, tooth enamel is much harder to penetrate, and is

correspondingly much less susceptible to diagenesis (Hoppe et al., 2003).

Dentine and enamel are formed at the same time and have the same original

isotopic composition; however, dentine, like bone, is much more susceptible to

diagenesis than enamel (Budd et al., 2000). This difference can be used to

19

ascertain the influence if diagenesis, and well as to help in the identification of

migrants. If the original isotopic signature of a tooth differs from that of the

local sediment, then diagenesis will affect the 87

Sr/86

Sr ratio in the dentine and

cause it to be different to that in the enamel. If the Sr signature in the dentine

and enamel are the same but different to the local signature, they can similarly

be identified as migrants, but it can be concluded that the effect of diagenesis

has been minimal. In this, dentine performs effectively the sample function as

bone, without the unrealistic expectations of more refined chronological

tracking from bones remodelling at different rates. It is also simpler in terms of

a sample acquisition, requiring only teeth rather than additional associated

bone fragments. This is particularly useful for sites such as Le Tumulus des

Sables where the remains are quite disarticulated and associated bones are

lacking.

While enamel is less susceptible to diagenesis, it may not necessarily be

unaffected. For the investigation of the origin of an individual, it is essential to

reconstruct the original isotopic signature. It has been proposed that diagenetic

strontium may be removed through a process involving cleaning with a series

of weak acid leaches. There are concerns, however, that these may alter the

original strontium, or even cause the diagenetic strontium to partially or even

fully replace it (Bentley, 2006). In addition to the precipitation of secondary

minerals into the bone or tooth structure, it has been shown that the biogenic

apatite is also altered by diagenesis (Kohn et al., 1999).Even working on a

relatively modern sample from Vietnam, Beard and Johnson (2000) found that

they were unable to recover much of the original strontium. Hoppe et al. (2003)

20

determined that although some contaminants could be removed using the

correct preparation process, up to 80% of the diagenetic strontium remained in

bones. On the other hand, the pre treatment appeared to remove up to 95% of

the diagenetic strontium from tooth enamel.

This study pursues a different strategy. Modern teeth contain only traces of

uranium and thorium (Tandon et al., 1998); however, due to diagenesis,

archaeological skeletal tissues contain variable amounts of U and Th. Uranium

is water soluble and highly mobile, while thorium is water insoluble. As such,

the presence of any Th is the result of mechanical contamination (for example,

clay minerals in the pores of bones) while the presence of U indicates chemical

contamination. The measurement of these can be used to identify domains in

which diagenesis has occurred mechanically or chemically, and domains in

which the original Sr isotopic signature is preserved. There is no linear

correlation between uranium uptake and the uptake of other elements, like

strontium, so where any uranium is present the extent of strontium overprint

cannot be accurately quantified (Moffatt, 2011, pers. comm.). Systematic

isotope mapping of a Neanderthal tooth has shown that there are regions in the

tooth enamel (usually close to the surface) that do not contain any uranium

(Grün et al., 2008). Domains that are free of uranium, which is much more

mobile than strontium, will preserve the original strontium isotopic signature.

21

2.3. Previous applications

While the technique is still in a phase of rapid development, it has been applied

successfully to human remains a number of times in varying locations (e.g.

Knudson et al., 2004, Giblin, 2009, Bentley et al., 2007a, Cook and Schurr,

2009, Evans et al., 2010, Hodell et al., 2004, Kusaka et al., 2011, Montgomery

et al., 2000, Bentley and Knipper, 2005, Bentley et al., 2007b, Conlee et al.,

2009, Price et al., 2000, Price et al., 2006, Smits et al., 2010), including even

fossil hominins (Copeland et al., 2011, Copeland et al., 2010). A significant

amount of work has also been conducted on animal populations (e.g. Britton et

al., 2009, Balasse et al., 2002, Balter, 2008) as well as organic materials such

as wood (English et al., 2001) and wool textiles (Frei et al., 2008).

While Bell Beaker individuals have been included in strontium isotope studies

conducted on broader populations (e.g. Chiaradia et al., 2003), these have

essentially been incidental inclusions and have produced only a minor amount

of data. Only one study, by T. Douglas Price and Gisela Grupe et al. generated

a significant amount of data and gave full consideration to the interpretations

and implications of this data. This also happens to be the first strontium isotope

study conducted on Bell Beaker people. The study was conducted over the

course of ten years, beginning with a pilot study in 1994 (Price et al., 1994).

The strontium isotope composition of compact bone and molar enamel of eight

individuals were compared, sourced from two sites in Bavaria. It is the

Bavarian Bell Beaker that later formed the core of what became a much

broader study, including samples from Germany, Hungary, Austria and the

Czech Republic, which culminated in 2004 (Price et al., 2004). By this point,

22

their sample consisted of 82 individuals from 11 sites in Bavaria, five

individuals from three sites in Austria, six individuals from three sites in the

Czech Republic, and six individuals from three sites in Hungary (Grupe et al.,

1997, Grupe et al., 1999, Price et al., 1994, Price et al., 1998, Price et al., 2002a,

Price et al., 2004).

Bone and enamel were compared under the assumption that bone, which is

constantly remodelling, would reflect the location in which the individuals

resided in the final years of their lives, and that the enamel would reflect their

place of residence in the early years of their lives during formation.

Throughout the duration of the study, the authors maintained that cleaning

procedures removed sufficient diagenetic strontium from the bone for results to

be meaningful. As previously mentioned, however, there are significant

concerns about the effectiveness of these pre-treatments. The implications of

this were not considered by the authors, but fortunately the impact is not so

great as to render the conclusions entirely invalid. Given that burial usually

occurs at the final place of residence, the overprinted signature should be

similar to the biogenic signature anyway. This ten year study provides a solid

and valuable foundation for both improvements in the technique, and further

Bell Beaker research.

23

Chapter 3

Methodology

______________________________________________________

3.1. Sample collection

The teeth were collected by Dr Patrice Courtaud of the University of Bordeaux

during the excavation of Le Tumulus des Sables, and subsequently provided to

Professor Rainer Grün of the Australian National University (ANU) for

strontium isotope analysis. Of the adult samples, the LM2 (left upper second

molar) of 21 individuals was supplied. Of the juveniles, the Ldi2

(left deciduous

upper second incisor) of 8 individuals was supplied. Selecting the same tooth

from each individual ensured that none were unintentionally represented

multiple times.

The soil samples were collected over the course of a number of years. Initially,

seven samples (SLMEM 2901-2907) from the burial itself were collected by

Dr Patrice Courtaud during the excavations and sent to the ANU, following

Australian quarantine guidelines. A further 11 samples (SLMEM 2901b-2907b,

2908-2911) from the burial itself (7) and other parts of the archaeological

deposit immediately adjacent to the burial (4) were collected in the same

manner and sent to the ANU, including doubles of the first seven samples. The

sample locations were recorded, and sediment description was conducted at the

ANU (see Figure 3.1. for locations, and Table 3.1. for descriptions).

24

Figure 3.1.: Locations of the soil samples taken from the site of Le

Tumulus des Sables, adapted from Patrice Courtaud (2011 pers. comm.).

Eleven further soil samples (F11-188 – F11-198) were collected during

fieldwork in late June 2011 from carefully selected locations around the Médoc

peninsula. This was conducted with Mr Malte Willmes as part of the creation

of a broader isotopic map of France. The samples were predominantly taken

from steep roadside cuts or beneath large fallen trees to access deeper,

uncontaminated soil, and they were taken far enough from farmed or

residential land to avoid the impact of fertilisers and other modern

contaminants. They were placed so that all geologic units in the study area

were appropriately represented (Figure 3.2.). The descriptions can be found in

Table 3.1. The sampling procedure involved thorough documentation of the

location and description of the samples, which included not only soil, but

bedrock and associated plant samples. This was done according to the Research

25

School of Earth Sciences (RSES, ANU) lab and field guide for strontium

isotope analysis (Moffatt and Willmes, 2011). As mentioned previously, the

Médoc is quite flat and lacking in accessible rock outcrops, meaning that a rock

sample was only able to be collected at one of the 11 locations. Plant samples

were also collected, but neither the rock nor the plants were included in this

study due to limitations in the available time and scope of the project.

Figure 3.2.: Geologic map of the Médoc and surrounding region, showing

sample locations for this study (F11-188 – F11-198) and others taken in

this region for related research (adapted from Bureau de recherches

géologiques et minières, 2005, GoogleEarth, 2011).

26

27

3.2. Sample preparation

Samples were prepared at the Research School of Earth Sciences, ANU, with

the guidance, assistance and supervision of Professor Rainer Grün, Mr Ian

Moffatt and Miss Tegan Kelly, and the aid of Mr Malte Willmes. Preparation

was conducted according to the RSES lab and field guide for strontium isotope

analysis (Moffatt and Willmes, 2011).

3.2.1. Cleaning

All laboratory containers and equipment were chemically cleaned before use.

Pipette tips, columns, and generic glassware were cleaned with a series of

rinses in tap water and Milli-Q purified water, followed by immersion in 10-

50% HNO3 for several days. After this time, the equipment was again cleaned

with a series of Milli-Q rinses and dried in an oven at 60°C. The columns were

additionally rinsed and soaked in acetone throughout the cleaning process.

Teflon beakers and Neptune, AES and centrifuge tubes were initially immersed

in Acetone for 1-2 hours, before being soaked sequentially in 2-5% Decon

(laboratory detergent) and Milli-Q, 10-50% HNO3, 10-50% HCl and then

Milli-Q H2O, all heated to 60°C and left over night, with a series of Milli-Q

rinses between each step. To the Teflon beakers alone, a small amount of 2M

HNO3 was added to each bottle and capped beakers were heated for two days

at 60°C, followed by a number of Milli-Q rinses. All equipment was dried in

an oven and stored in a sealed container or bag.

28

3.2.2. Soil

The soil samples were baked in an oven at 60 °C for 24 hours prior to use, and

1 gram subsamples of each soil sample were carefully sieved (2mm sieve)and

measured out on equipment cleaned according to lab procedures and standards.

To leach bio-available strontium, 2.5mls of 1M ammonium nitrate (NH4NO3)

was added to each sample and they were loaded into a retsch shaking for 24

hours along with blanks containing just 0.5ml of 1M NH4NO3. They were put

into the centrifuge at 3000 RPM for no less than five minutes to separate the

liquid component, and the maximum amount of clear liquid (1-2ml) was

extracted and evaporated overnight on a hotplate at 60°C. Once the leaching

process was complete and the liquid evaporated, the samples were dissolved

again in 15 drops of distilled concentrated HNO3 to break down residual

organic matter, and left on the hotplate with the cap on for one hour to allow

full dissolution. The cap was then removed and the samples were fully

evaporated once again. Once evaporated, 2mls of 2M nitric acid was added to

each beaker, which was then placed on the hotplate for one hour with the caps

on to allow full dissolution. At this stage, 0.1 ml of each sample was removed

and added to 9.9ml 2% HNO3 for Sr concentration measurement via ICP-AES

(see section 3.3.1.1.).

Using the Sr concentration results provided by the ICP-AES, the volume of

each sample required to obtain sufficient Sr levels in the end sample was

calculated with the aid of an excel spreadsheet. The samples were then put

through iron exchange chromatography to separate the Sr from matrix elements

in the sample, particularly 87

Rb which interferes with the 87

Sr signal in the ICP-

29

MS. The samples were passed through prepared columns loaded with pre-filter,

and columns loaded with Sr specific resin. Throughout the process, the pre-

filter and Sr specific resin columns change places above one another, and a

series of acids (0.02M HNO3, 8M HCl, 2M HNO) were run through the

columns in varying order a number of times in order to preferentially retain the

Sr in the resin until a breakthrough point was reached and the Sr is released and

collected. One drop of H3PO4 was added to each sample to keep them moist

during the subsequent evaporation, as the H3PO4 will not evaporate. The day

before Neptune ICP-MS analysis, 2ml 2% concentrated HNO3 was added to

each sample, and they were transferred to 4ml Neptune vials for analysis.

3.2.3. Teeth

3.2.3.1. For laser analysis

For laser ablation sampling, teeth were cut using a fine diamond saw along the

axis which would provide the best enamel and dentine surfaces for analysis.

This varied slightly between teeth, but generally followed the buccal-lingual

(cheek to tongue) axis. A segment comprising approximately half the dentine

and enamel was removed from each tooth, leaving the remainder of the tooth

intact and minimising the damage. The teeth were then sanded lightly using

fine grained sandpaper to ensure the smooth surface required for analysis, and

loaded into standardised metal rings. Yellow-tack was used as a base to support

the teeth and hold them in place, as seen in Figure 3.3. The teeth were recorded

(length, width, thickness and weight) and photographed in high resolution

30

before preparation, after being cut, after being mounted and after analysis was

completed.

Figure 3.3.: Examples of two photographs, before any preparation (left)

and after analysis, while still loaded in the ring (right).

3.2.3.2. For solution analysis

Four of the adult teeth were additionally analysed in solution. Using a fine drill,

a small amount of the dentine and enamel were removed (approx 0.02g each)

and crushed with a mortar and pestle, and dissolved in 0.5ml of concentrated

baseline HNO3. These were left, lidded, on the hotplate over night at 60°C. The

lids were subsequently removed to allow the evaporation. Once complete, 2ml

of 2M HNO3 was added to each sample before sub-sampling for ICP-AES

along with the soil samples, followed by ion exchange chromatography and

analysis.

3.3. Sample analysis

Samples were analysed at the RSES, ANU, with the guidance, assistance, and

supervision of Professor Rainer Grün, Mr Ian Moffatt, Mr Les Kinsley, Ms

31

Linda McMorrow and Dr Steve Eggins, and the aid of Mr Malte Willmes.

Concentrations and isotope compositions were calculated from the raw data

provided by each of the analysis methods using Microsoft Excel spreadsheets

specifically formulated for the task.

3.3.1. HelEx laser system

Laser ablation analysis was conducted using the custom built ANU HelEx laser

sampling system, coupling an ArF excimer laser system (193nm; Lambda

Physik Compex 110) with one of two inductively coupled plasma mass

spectrometers (ICP-MS), a Varian-820 quadrupole ICP-MS and a Finnigan

MAT Neptune multi-collector ICP-MS (MC-ICP-MS). The ANU system and

its capabilities have previously been described in detail by Eggins et al. (1998).

In brief, a single lens is employed to project and demagnify the image of a laser

illuminated apparatus onto the sample, producing relatively sharp edged

ablation pits of controllable dimensions. The atmosphere under which ablation

is carried out is carefully controlled to be compatible with the argon ICP, an

atmospheric pressure ion source. This ensures uncontaminated transport of the

ablation products to the ICP, and the use of helium as a carrier gas maximises

the transmission. To reduce the pulsations in sample delivery resulting from the

pulsed laser ablation, a signal smoothing device is employed during

transportation of the ablation products to the ICP.

32

Figure 3.4.: The ANU HelEx laser ablation setup (courtesy of Steve Eggins)

3.3.2. Varan Vista ICP-AES - Elemental concentrations (Soil)

A Varian Vista Pro Axial ICP-AES was used to calculate the Sr concentrations

during the solution preparation process, as required during the ion exchange

chromatography. The sample is nebulised and passed through inductively

coupled plasma (a partially ionised gas to which energy is supplied by

electromagnetic induction), which atomises the sample. These atoms are

excited, and individual elements emit a characteristic wavelength when the

atoms return to their original energy level. A grating can be used to disperse

the light and separate elements, and the intensity of target wavelengths is

measured to determine quantities.

33

Figure 3.5.: Schematic diagram of an ICP-AES

(from http://www.balticuniv.uu.se/environmentalscience/ch12/chapter12_

g.htm)

3.3.3. Varian ICP-MS - Elemental concentrations (Teeth)

In ICP-MS, an inductively coupled plasma is used to atomise and ionize the

sample – in this case, the ablation product. The vaporised sample particles are

passed through the ICP using argon as a carrier gas. Ions then pass through a

small sample orifice, and are accelerated by a pumped vacuum system into an

expansion chamber. Ions are extracted from the chamber using a skimmer cone,

and are shaped and focused with ion lenses. The Varian-820 ICP-MS uses a

quadrupole mass filter composed of four parallel metal rods, through which the

ion stream is directed. The voltages of the rods are selected and varied so that

only ions of specific mass to charge ratios may pass through to the detector.

The Varian was used to gather data on elemental concentrations in the teeth,

largely for the purpose of detecting diagenesis.

34

Figure 3.6.: Schematic diagram of a laser ablation cell connected to a

quadrupole ICP-MS (adapted from D. J. Sinclair).

The samples were analysed using two methods; ablating a series of spots across

the teeth, and ablating a single track across the tooth. All of the preliminary

work on the teeth (using the Neptune MC-ICP-MS for isotopic ratios rather

than elemental concentrations) was conducted using laser tracks; however,

there is some concern that the values may be affected by the tracking laser.

Four of the teeth were re-analysed using spots, which provide a more solid,

reliable signature, as well as allowing easier interpretation. These four teeth

were analysed on the Varian using spots in corresponding locations to the spots

made in the previous Neptune analysis. This approach is much more time

consuming, and laser tracks were sufficient for the Varian elemental

concentrations for our purposes. As such, the remaining 20 teeth, 12 adult and

8 juvenile, were analysed using tracks.

35

To remove any surface contamination received during the preparation process,

such as dust and fine particles deposited during the light sanding, the samples

were first subjected to a cleaning run using the laser, following the path set for

the analysis but for a shorter time and using a slightly larger spot size. For the

four teeth on which spots were used, the ablation time was 2 seconds using a

spot size of 63μm with no pre and post-ablation time. Pre- and post-ablation

times were set during the runs to measure background levels for comparison,

and to allow time for the lines to clear between analyses. This ensures that

there is no contamination between samples. This is unnecessary during the

cleaning run, as no data are recorded. For the teeth analysed using tracks, the

cleaning run used a spot size of 233μm, moved at a speed of 100μm per second,

and had no pre - and post-ablation times.

For the spot analyses, a spot size of 47μm was used, with an ablation time of

30 seconds and 50 seconds pre-ablation and 10 seconds post-ablation. For the

track analyses, the laser moved at a speed of 20μm per second, the pre-ablation

time was 50 seconds, the post-ablation time was 10 seconds, and a spot size of

47μm was used. All analyses began in the enamel and proceeded into the

dentine. Two standard glasses of known composition, NIST 610 and NISE 612,

were used, each being measured twice with spots before and after each tooth.

All analyses were conducted with the laser pulse rate set to 5Hz, and the

elements measured were 24

Mg, 25

Mg, 31

P, 43

Ca, 86

Sr, 88

Sr, 137

Ba, 138

Ba, 232

Th

and 238

U.

36

3.3.4. Neptune MC-ICP-MS - Isotopic composition

Finnigan MAT Neptune MC-ICP-MS operates on similar principals to the

Varian ICP-MS described above, although they use different methods to

separate and count the ions. The Neptune is a magnetic sector mass

spectrometer, which separates the ions by dispersing them in a magnetic field.

These are then doubly focussed and counted in a number of Faraday cups

(hence the title „multi-collector‟), each adjusted to collect a different ionic mass.

The Neptune was used to determine the strontium isotopic compositions of

both the soil and the teeth.

Figure 3.7.: Schematic diagram of a Finnigan MAT Neptune (from

http://www.dur.ac.uk/geochem.www/group/pimms.htm)

Analysis proceeded differently depending upon sample type. The teeth were

analysed using laser ablation, using the Neptune interfaced with the ANU

37

HelEx laser sampling system described previously (section 3.3.2.). Sixteen

adult teeth and eight juvenile teeth were analysed using a series of spots

proceeding from the enamel to the dentine in each tooth. The location for these

spots was determined by reviewing the Varian elemental concentration data in

an effort to choose the part of the tooth least affected by diagenesis. The four

adult teeth that were selected for bulk analysis in solution were analysed in the

same manner as the soil samples, with the solution being nebulised for

introduction to the plasma through an Apex desolvator.

For solution analysis, the Faraday cups were set to collect ions with masses of

82.4652, 83(Kr), 83.466, 84(Sr+Kr), 85(Rb), 86(Sr+Kr), 86.469, 87(Sr+Rb)

and 88(Sr). The half mass positions are set to monitor for the contribution of

doubly charged rare earth elements (REE‟s), and along with Kr and Rb these

are monitored and measured so that interference corrections can be applied.

During the analysis, a strontium isotope standard (SRM987) was measured

periodically to monitor the accuracy and precision of the measurements. To

facilitate further corrections, a blank (2% HNO3) was measured before each

sample, including the blanks created during the preparation process. A

sequence of acid and detergent rinses was used between each measurement to

ensure there was no contamination between samples during measurement.

As in analysis with the Varian, the samples for analysis using the laser were

subjected to a cleaning run to remove any surface contamination received

during the preparation process. To simplify interpretation of the isotopic

composition results when compared to the elemental concentrations, the spots

were set to overlay the large shallow tracks created during analysis using the

38

Varian. As mentioned previously, four of the teeth had already been subjected

to Neptune analysis using spots prior to elemental concentration analysis using

the Varian, and the results from this were evaluated alongside the newer data.

A spot size of 233μm was used for the cleaning run, and a spot size of 178μm

was used for the analysis. The step size between each spot (centre to centre)

was as close to 400μm could be achieved on each tooth, varying with the

length of the track from enamel to dentine and the number of spots that could

be accommodated fully within that track. For cleaning, each spot was ablated

for 2 seconds with no pre- and post-ablation times, and for analysis each spot

was analysed for 60 seconds with 50 seconds pre-ablation and 10 seconds post-

ablation. The laser pulse rate was set to 5Hz, and the Faraday cups were set to

collect 83

Kr, 167

Er++, 84

Sr, 85

Rb, 86

Sr, 173

Yb++, 87

Sr, 88

Sr, and 177

Hf++. A

tridacna shell was used as a standard for the Sr isotope ratios and measured 3

times before and after each set of samples.

39

Chapter 4

Results

______________________________________________________

4.1. Soil

4.1.1. The Médoc region

Results from the 11 soil samples collected from the region are presented in

Table 4.1 below, including voltages, 87

Sr/86

Sr ratios and errors for the samples

and standards (SRM987). The standards show good reproducibility and low

errors. Errors in the soil measurements, while higher, are still quite low. The

strontium isotope values have quite a large range, from 0.7092±0.0001 to

0.7231±0.00002, and there is clear separation in the values between the

different geologic units (see Figure 5.1.). This is true for all units other than the

Holocene sands, whose signatures presumably reflect the diverse sources from

which they originated before being washed into the peninsula.

40

Table 4.1.: 87

Sr/86

Sr ratios with voltages and errors for the samples

gathered during fieldwork. Includes standards (SRM987) measured

during the analyses.

Sample 88Sr

Volts

87Sr/

86Sr ±

87Sr/

86Sr

F11-188 3.669982 0.713918 0.000025

F11-189 6.814904 0.709784 0.000018

F11-190 3.774493 0.715560 0.000026

F11-191 5.308487 0.721426 0.000022

F11-192 3.250591 0.717748 0.000031

F11-193 4.229294 0.711634 0.000023

F11-194 1.632383 0.709178 0.000050

F11-195 5.014138 0.709420 0.000021

F11-196 5.084050 0.723147 0.000022

F11-197 13.684909 0.722062 0.000010

F11-198 4.588683 0.715563 0.000025

SRM987 #1 39.522276 0.710216 0.000006

SRM987 #2 39.185098 0.710217 0.000006

SRM987 #3 39.551973 0.710216 0.000006

4.1.2. Les Tumulus des Sables

The first seven soil samples that were analysed from the site showed

unexpected variability in the 87

Sr/86

Sr ratios, and there was some doubt as to

the validity of these initial results. The 88

Sr voltages, 87

Sr/86

Sr ratios and errors

for these samples and standards (SRM987) have been presented below in Table

4.2. Some concerns were raised about contamination during the preparation

process, and the Neptune analyses had to be conducted a number of times due

to errors and very low voltages in the earlier attempts. Some of better data

obtained still have reasonably low voltages (below 3.0), increasing the errors

and giving some reason for doubt as to their validity. Given the good

reproducibility and low errors of the SRM987 standards, there is little reason to

suspect analytical error. Note that no value was obtained for SLMEM 2901.

41

Table 4.2.: 87

Sr/86

Sr ratios for the first 7 soil samples including errors, and

standards (SRM987) measured intermittently during solution analyses.

Sample 88Sr

Volts

87Sr/

86Sr ±

87Sr/

86Sr

SLMEM 2901 0.000000 - -

SLMEM 2902 2.134248 0.712825 0.000046

SLMEM 2903 18.33808 0.710010 0.000010

SLMEM 2904 2.813816 0.720237 0.000034

SLMEM 2905 5.129897 0.717742 0.000022

SLMEM 2906 13.049800 0.713557 0.000012

SLMEM 2907 3.841983 0.710340 0.000031

SRM987 #1 28.694181 0.710239 0.000008

SRM987 #2 28.506605 0.710236 0.000007

SRM987 #3 27.793754 0.710237 0.000007

SRM987 #4 28.284651 0.710231 0.000008

The 11 newer samples, including samples taken from the same location as the

first seven, were subjected to column chemistry in a clean lab, while the first

samples were not. They yielded generally higher voltages and lower errors than

the first seven, and consistently uniform standard values with very low errors.

The voltages, 87Sr/86Sr ratios, errors of these samples and standards are

presented in Table 4.3. The standards also show good reproducibility and very

low errors. SLMEM 2902b, 2906b and 2907b agree reasonably well with the

results from the first set of samples and sample 2903b is outside error range but

still reasonably close, whereas samples 2904b and 2905b are significantly

different. Given the lower voltages, higher errors and concerns about

contamination in the first set of samples, the second set of results can be

considered more reliable and will be used preferentially. The isotope ratios of

the samples from the archaeological site range from 0.7097±0.00001 to

0.7188±0.00001. The lowest values occur within the burial and the highest

42

come from the external architecture, but there are no clear boundaries between

the two – the intermediate values come from a mixture of the locations. The

strontium isotope ratios from the site have quite a large range, but fit within the

range established for the Médoc region

Table 4.3.: 87

Sr/86

Sr ratios with voltages and errors for second batch of soil

samples from the site. Includes standards (SRM987) measured during the

analyses.

Sample 88Sr

Volts

87Sr/

86Sr ±

87Sr/

86Sr

SLMEM 2901b 8.733223 0.711492 0.000015

SLMEM 2902b 9.209545 0.712334 0.000014

SLMEM 2903b 10.329395 0.709676 0.000017

SLMEM 2904b 10.840188 0.716264 0.000013

SLMEM 2905b 9.113053 0.718785 0.000013

SLMEM 2906b 10.371188 0.713436 0.000014

SLMEM 2907b 17.671749 0.710145 0.000011

SLMEM 2908 13.812316 0.710084 0.000010

SLMEM 2909 6.902643 0.712592 0.000011

SLMEM 2910 9.147795 0.710763 0.000015

SLMEM 2911 12.308025 0.713385 0.000018

SRM987 #1 39.522276 0.710216 0.000006

SRM987 #2 39.185098 0.710217 0.000006

SRM987 #3 39.551973 0.710216 0.000006

4.2. Teeth

Due to the amount of data, only a few examples will be presented and

explained in detail. These have been selected to be as representative as possible;

however, it is important to note that each sample requires individual attention

in the interpretation of the results. These examples will be presented further in

section 4.2.3., after a brief overview of the results obtained using each

analytical method. The full data set is available in the appendices (Appendix 2).

43

4.2.1. Elemental concentrations (Varian)

There is significant variation both within and between the teeth, making

sweeping statements regarding diagenesis of the sample set unfeasible. The

concentrations of the elements of interest in detecting diagenesis, 238

U, 232

Th

and 88

Sr, have been graphed for each tooth and supplied in Appendix 2. Within

most teeth, the dentine and enamel can be divided into a number of zones, in

which diagenesis has been absent or present to varying degrees. Table 4.3

shows the average concentrations of U, Th and Sr in high and low zones in the

enamel and dentine of each tooth. Red indicates zones in which contamination

is likely, and blue indicates zones in which it is possible. Note that there are no

set cut off values, individual judgements must be made on the basis on

comparative concentrations within and between elements and samples. Note

also that the 88

Sr concentrations are typically not coloured, given the difficulty

in distinguishing diagenetic from biogenic strontium. Where significantly

heightened strontium concentrations correspond with high uranium and/or

thorium concentrations, these are coloured blue. Only one very extreme case

has been coloured red, indicating that it is likely the result of contamination

(J1). Where thorium is concerned, any occurrence that has been labelled blue is

possibly the result of background interference. Where the reading can be

confidently identified as genuine, no matter the magnitude of the value, red is

used.

Despite the variation between samples, there are a few overall trends that can

be noted.

44

In the majority of cases, the U and Sr are higher in the dentine than in

the enamel. In the case of the uranium, this is attributable to diagenesis.

The same cannot be assumed for strontium. While it is possible that the

raised concentrations may be in part due to the entry of diagenetic

strontium, there is no way to quantify how much (if any) of this is

diagenetic. Strontium concentrations tend to be higher in the dentine

than the enamel in modern teeth, and concentrations vary between

individuals.

A number of samples display a small spike in U and/or Th at the

beginning or the end of the track. This is likely due to the track

beginning or ending slightly over the edge of the cut surface, and the

reading is being affected by sediment residues at the occlusal surface or

pulp cavity.

In almost all cases, U and Th do not remain constant within the dentine

or the enamel. This is likely due to the presence of microscopic cracks

allowing easier passage for diagenetic material into the tooth (see also

Grün et al., 2008).

Very few of the teeth have entirely uncontaminated enamel, but pristine

zones are identified in most. The dentine is almost entirely

contaminated, although there are zones in some samples in which

diagenesis may have been minimal.

As a group, the juvenile teeth appear to be generally more contaminated

than the adult teeth, and tend to contain particularly large amounts of

Th.

45

46

4.2.2. Isotopic composition (Neptune)

4.2.2.1. Laser

The results provided by laser analysis showed a reasonably high degree of

variation. Table 4.5 gives the values for the enamel and dentine of each tooth.

These values were obtained by comparing the isotopic data to the elemental

concentrations data and locating the zones in which diagenesis appeared to be

absent. Averages were taken where there was more than one suitable zone, and

these usually had very similar values. No such pristine zones could be

identified in the dentine of any of the samples, and the values tend to be

reasonably homogenous. As such, averages are taken from the majority, if not

all, of the data from the dentine in most samples.

The dentine 87

Sr/86

Sr values range between 0.7106±0.0003 and 0.7134±0.0002,

which is largely within the expected range given the site location. The values in

the enamel range between 0.7133±0.0004 and 0.7244±0.0005, although the

lowest of these are taken from teeth in which no pristine zones could be

identified, and contain elevated U and/or Th concentrations. As such, some of

these values may be heavily influenced by diagenetic input. The juvenile teeth

(0.7146±0.0006 – 0.7230±0.0008) cannot be distinguished from the adult teeth

on the basis of the values, being dispersed throughout the adult range. They do

appear to have been more heavily influenced by diagenesis, but the effect that

this had on the Sr results is difficult to gauge.

The teeth show similar errors, which are somewhat higher than those obtained

during the standard measurements. A total of 154 standard measurements were

47

made throughout the analysis, with a minimum of three being performed at

each interval. As such, Table 4.6 (below) only shows averages taken from each

of these groups. The full list of standard measurements including 87

Sr/86

Sr

ratios and errors can be found in the appendices (Appendix 1). The standards

measured during the analysis of the four teeth also analysed using solution

have lower errors than the others, as do the laser analyses on these teeth. As

these laser analyses were performed at different times, this difference in errors

is attributable to differences in the setup, calibration and possibly condition of

the equipment. The difference in error magnitude is not so much as to cause

problems with the comparison and interpretation of the data.

48

Table 4.5.: 87

Sr/86

Sr ratios for the enamel and dentine of each tooth

(averages from appropriate locations), including errors. Red indicates a

signature that is likely heavily influenced by diagenesis, as indicated by U

and Th, and orange indicates a signature taken from zones with very high

Th content, but low U.

Tooth Enamel 87

Sr/86

Sr

2se Dentine 87

Sr/86

Sr

2se

A1 (SLMEM1007) 0.724369 0.000471 0.711349 0.000225

A2 (SLMEM466) 0.718634 0.000313 0.713176 0.000196

A3 (SLMEM308) 0.715640 0.000289 0.712493 0.000296

A4 (SLMEM263) 0.720533 0.000294 0.712481 0.000130

A5 (SLMEM861) 0.722658 0.000543 0.711701 0.000156

A6 (SLMEM112) 0.715797 0.000147 0.713439 0.000182

A7 (SLMEM491) 0.713302 0.000418 0.711423 0.000313

A8 (SLMEM1094) 0.715698 0.000384 0.710956 0.000255

A9 (SLMEM454) 0.722278 0.000677 0.713131 0.000309

A10 (SLMEM900) 0.717876 0.000442 0.712092 0.000305

A11 (SLMEM432) 0.715841 0.000535 0.710831 0.000314

A12 (SLMEM509) 0.719563 0.000749 0.711380 0.000321

A13 (SLMEM282) 0.716824 0.000586 0.712492 0.000335

A14 (SLMEM298) 0.716146 0.000426 0.711886 0.000315

A15 (SLMEM1157) 0.721258 0.000884 0.711865 0.000318

A16 (SLMEM5) 0.720057 0.000561 0.711821 0.000297

J1 (SLMEM1192) 0.719712 0.000666 0.711505 0.000351

J2 (SLMEM1251) 0.715088 0.000387 0.710640 0.000309

J3 (SLMEM276) 0.723010 0.000777 0.711027 0.000277

J4 (SLMEM66) 0.719776 0.000753 0.711141 0.000309

J5 (SLMEM102) 0.714607 0.000593 0.711664 0.000301

J6 (SLMEM119) 0.719197 0.000555 0.711825 0.000301

J7 (SLMEM86) 0.719931 0.000486 0.711542 0.000281

J8 (SLMEM 291) 0.718307 0.000488 0.711095 0.000289

49

Table 4.6.: Average 87

Sr/86

Sr values from standard measurements taken at

each interval (minimum of three in each group).

Number 87

Sr/86

Sr

Value

2se

Run 1 (1007 & 308) Before 0.709161 0.000169

Run 1 (1007 & 308) After 0.709175 0.000151

Run 2 (491 & 1094) Before 0.709196 0.000114

Run 2 (491 & 1094) After 0.709198 0.000124

Run 3 (454 & 900) Before 0.709164 0.000161

Run 3 (454 &900) After 0.709170 0.000175

Run 4 (432 – 5) Before 0.709166 0.000145

Between 509 & 282 0.709176 0.000147

Between 298 & 1157 0.709194 0.000157

Run 4 (432 – 5) After 0.709170 0.000192

Run 5 (Juvenile) Before 0.709146 0.000126

Between 1192 & 119 0.709188 0.000226

Between 66 & 276 0.709152 0.000210

Run 5 (Juvenile) After 0.709154 0.000141

Run 1b (112) Before 0.709213 0.000027

Run 1b (112) After 0.709209 0.000027

Run 2b (263) Before 0.709207 0.000025

Run 2b (263) After 0.709212 0.000028

Run 3b (466) Before 0.709210 0.000025

Run 4b (466) After 0.709203 0.000027

Run 5b (861) Before 0.709217 0.000027

Run 5b (861) After 0.709214 0.000029

Averages 0.709186 0.000112

4.2.2.2 Solution

Simonetti et al. (2008) observed a systematic offset between laser ablation and

solution results, in which laser ablations uniformly provided higher 87

Sr/86

Sr

values (on average by 0.0013±0.0006). This systematic offset was attributed to

the interference of 40

Ca-31

P-16

O molecules with 87

Sr. For this reason, four of

the teeth from our sample set were analysed using both laser ablation and

solution ICP-MS. The analyses by solution returned significantly different

50

results to the analyses by laser ablation. The solution results are presented in

Table 4.7. The offsets between the laser and solution results were not uniform,

ranging from 0.0012±0.0002 to 0.0089±0.0003, though most of the variation

occurred in the enamel. Three of the four dentine samples had quite similar

offsets, on the lower end of the range (0.0026±0.0002, 0.0026±0.0003 and

0.0028±0.0002) and the fourth provided the lowest offset of all

(0.0012±0.0002). It is worth noting that the voltages obtained in the enamel

were significantly lower than those in the dentine, casting some doubt upon

their accuracy and indicating that this may potentially be partially responsible

for the variation in the enamel offsets.

The solution samples had lower errors than the laser analyses, and uniformly

lower values. To determine whether the difference in values was due to the

method, which cannot avoid zones of diagenesis like laser ablation can, the

average of all values obtained using laser ablation was calculated for each

sample (see Table 4.8.). In most cases, the difference was minor. Note that no

value was obtained for SLMEM 861EN. No consistent offset was able to be

identified, so averages were taken from the enamel and the dentine offsets

between the solution and all laser values. These average offsets were subtracted

from the dental results provided by the laser (Table 4.9.). Despite the

difference in signatures, the solution samples also demonstrate a significant

difference between the dentine and the enamel suggesting that the phenomenon

is real regardless of the exact values (see Example 4 in section 4.2.3. below).

51

Table 4.7.: 87

Sr/86

Sr values for the teeth analysed by solution MC-ICP-MS

including errors and standards measured intermittently during solution

analysis.

Sample 88

Sr Volts 87

Sr/86

Sr ± 87

Sr/86

Sr

SLMEM 112DE 5.284534 0.710860 0.000019

SLMEM 112EN 1.723297 0.714010 0.000054

SLMEM 263DE 7.756951 0.709697 0.000026

SLMEM 263EN 3.571105 0.711647 0.000028

SLMEM 466DE 5.217999 0.710585 0.000019

SLMEM 466EN 1.714757 0.711915 0.000051

SLMEM 861DE 6.294880 0.710466 0.000020

SRM987 #1 3.710665 0.710187 0.000022

SRM987 #2 3.864663 0.710268 0.000024

SRM987 #3 3.945157 0.710280 0.000031

SRM987 #4 4.282606 0.710234 0.000023

SRM987 #5 3.638225 0.710202 0.000024

SRM987 #6 3.821130 0.710173 0.000025

Table 4.8.: 87

Sr/86

Sr values provided by solution, by laser analysis selecting

the appropriate zones, and by laser analysis using all values. The

differences between laser and solution, and laser (all values) and solution,

are provided for comparison

Sample Solution 87

Sr/86

Sr

Laser 87

Sr/86

Sr Laser (all)

Laser

- Solution

Laser

(all)

- Solution

112EN 0.71401 ±

0.00002

0.71580 ±

0.00015

0.71592 ±

0.00015 0.001787 0.001906

112DE 0.71086 ±

0.00005

0.71344 ±

0.00018

0.71344 ±

0.00018 0.002579 0.002579

263EN 0.71165 ±

0.00003

0.72053 ±

0.00029

0.72005 ±

0.00028 0.008886 0.008399

263DE 0.70970 ±

0.00003

0.71248 ±

0.00014

0.71248 ±

0.00014 0.002784 0.002784

466EN 0.71192 ±

0.00002

0.71863 ±

0.00031

0.71624 ±

0.00026 0.006719 0.004323

466DE 0.71059 ±

0.00005

0.71318 ±

0.00020

0.71318 ±

0.00020 0.002591 0.002590

861EN - 0.72266 ±

0.00054

0.72220 ±

0.00054 - -

861DE 0.71047 ±

0.00002

0.71170 ±

0.00016

0.71170 ±

0.00016 0.001235 0.001235

EN average & St.dev. 0.004867±0.00329

DE average & St.dev. 0.002275±0.00072

52

Table 4.9.: Laser 87

Sr/86

Sr values, with average offsets subtracted

Tooth Enamel Dentine

A1 (SLMEM1007) 0.719502 ± 0.003758 0.709074 ± 0.000943

A2 (SLMEM466) 0.713767 ± 0.0036 0.710901 ± 0.000914

A3 (SLMEM308) 0.710773 ± 0.003576 0.710218 ± 0.001014

A4 (SLMEM263) 0.715666 ± 0.003581 0.710206 ± 0.000848

A5 (SLMEM861) 0.717791 ± 0.00383 0.709426 ± 0.000874

A6 (SLMEM112) 0.710930 ± 0.003434 0.711164 ± 0.0009

A7 (SLMEM491) 0.708435 ± 0.003705 0.709148 ± 0.001031

A8 (SLMEM1094) 0.710831 ± 0.003671 0.708681 ± 0.000973

A9 (SLMEM454) 0.717411 ± 0.003964 0.710856 ± 0.001027

A10 (SLMEM900) 0.713009 ± 0.003729 0.709817 ± 0.001023

A11 (SLMEM432) 0.710974 ± 0.003822 0.708556 ± 0.001032

A12 (SLMEM509) 0.714696 ± 0.004036 0.709105 ± 0.001039

A13 (SLMEM282) 0.711957 ± 0.003873 0.710217 ± 0.001053

A14 (SLMEM298) 0.711279 ± 0.003713 0.709611 ± 0.001033

A15 (SLMEM1157) 0.716391 ± 0.004171 0.709590 ± 0.001036

A16 (SLMEM5) 0.715190 ± 0.003848 0.709546 ± 0.001015

J1 (SLMEM1192) 0.714845 ± 0.003953 0.709230 ± 0.001069

J2 (SLMEM1251) 0.710221 ± 0.003674 0.708365 ± 0.001027

J3 (SLMEM276) 0.718143 ± 0.004064 0.708752 ± 0.000995

J4 (SLMEM66) 0.714909 ± 0.00404 0.708866 ± 0.001027

J5 (SLMEM102) 0.709740 ± 0.00388 0.709389 ± 0.001019

J6 (SLMEM119) 0.714330 ± 0.003842 0.709550 ± 0.001019

J7 (SLMEM86) 0.715064 ± 0.003773 0.709267 ± 0.000999

J8 (SLMEM 291) 0.713440 ± 0.003775 0.708820 ± 0.001007

53

4.2.3. Examples

Example 1 – Adult 1 (SLMEM 1007)

Two tracks were made across the tooth, beginning at each of the cusps. The

first appeared to have been less affected by diagenesis and had a larger enamel

surface for analysis, so was chosen for the Neptune isotopic analysis. The

uranium content in the enamel is quite low, although zones of lower (0.04ppm)

and higher (0.123ppm) content are able to be distinguished. The content in the

higher zone is still quite low and in other circumstances it may be interpreted

differently; however, in this tooth there is a noticeable peak in the strontium

concentration where the uranium peaks, suggesting that this added strontium is

diagenetic. To be certain that the isotopic signature is pristine, it was safest to

take the value from the lower zone. The uranium content rises sharply at the

dentine-enamel junction (DEJ), jumping to an average of 12.373 within a short

distance. The uranium remains quite high for about 3mm through the dentine,

before gradually dropping back down to sub-ppm concentrations. A number of

other samples demonstrate this sharp rise at the DEJ, with the highest uranium

values in the dentine domain closest to the DEJ. In conjunction with the greater

susceptibility of dentine to diagenesis, the slight cracks at the DEJ between the

enamel and dentine likely allow diagenetic material to penetrate the tooth. The

strontium also rises sharply at the DEJ, but it doesn‟t mimic the uranium and

does not drop down further into the dentine. It was theorised that the part of the

dentine in which the uranium is lowest may preserve an unaltered strontium

signature, but comparison of the concentration data with the isotopic data

revealed this not to be the case. Across all samples, isotope ratios in the dentine

54

show clear overprint and generally remain relatively constant regardless of

large fluctuations in uranium and thorium content.

A1 - SLMEM 1007

Figure 4.1.: Graphs of the elemental concentrations and isotopic

composition, along with an image of the tooth. (Note that the laser track

made during the Varian analysis underlies the spots made for the Neptune

analysis. A track from previous analysis is also visible)

0.01

0.1

1

10

100

1000

567 617 667 717 767

pp

m

Time (sec)

Sr

Th

U

0.708

0.712

0.716

0.72

0.724

0.728

1 2 3 4 5 6 7 8 9 10 11 12 13

87 S

r/8

6 Sr

Spot Number

55

Example 2 – Juvenile 1 (SLMEM1192)

While this tooth is quite an extreme example, a number of the other teeth

exhibit similar traits to varying degrees. The concentrations of all three

elements display very dramatic spatial variation in this tooth. The uranium

concentrations never drop below 1.5ppm, higher than some other teeth ever

reach, and climb as high as 38ppm. Thorium is constantly present, the likes of

which is only seen in one other tooth, A7. Concentrations exceed 35ppm in

places, and average in the dentine is slightly under 10ppm – concentrations one

might expect to find in soil. The strontium concentrations are at their lowest at

95 ppm, consistent with what might be found in unaltered human enamel.

These low points only occur briefly, however, and concentrations reach as high

as 500ppm, far beyond anything seen in any other samples. Given that a

cleaning run was conducted with the laser prior to analysis, this is unlikely to

be surface contamination. The chemical and physical contamination in this

tooth are extensive, and there don‟t appear to be any zones in which the

original strontium might have been preserved.

Many of the samples display a clear rise in concentration at the DEJ in at least

one element, demonstrating the increased susceptibility of dentine to diagenesis.

This is not the case in this tooth, and on the basis of the elemental

concentrations alone one might expect that the entire tooth has undergone

significant diagenetic overprint. Interestingly, when the isotopic compositions

are considered, this does not appear to be the case. As was seen in the last

example, the isotopic ratio remained relatively constant in the dentine despite

the fluctuation in elemental concentrations. The same is true for this tooth,

56

displaying no apparent correlation between isotopic ratios and elemental

concentrations in the dentine. This suggests that the dentine has been

completely overprinted, which is supported by the isotopic signature which

matches what we expect for area in which the burial is located. Surprisingly,

despite the very high concentrations of all elements in the enamel, with a very

large amount of spatial variation, the enamel signature has not been overprinted.

This is evidenced by the very high values obtained for the enamel, which far

exceed the local range. Unfortunately, while it is apparent that the signature has

not been entirely overprinted, we cannot be sure that a smaller degree of

diagenetic alteration has not taken place, and so cannot ascertain the biogenic

strontium signature.

57

J1 – SLMEM 1192

Figure 4.2.: Graphs of the elemental concentrations and isotopic

composition, along with an image of the tooth showing the spots made for

Neptune analysis (overlaying the Varian laser track)

0.01

0.1

1

10

100

1000

1882 1912 1942 1972 2002

pp

m

Time (sec)

Sr

Th

U

0.71

0.712

0.714

0.716

0.718

0.72

0.722

1 2 3 4 5 6 7

87 S

r/8

6 Sr

Spot Number

58

Example 3 – Adult 7 (SLMEM 491)

This tooth is unusual in that it is the only tooth with an enamel value that falls

within the range of the dentine values for the teeth. This could have a number

of explanations. The tooth may have been so affected by diagenesis that the

enamel was also overprinted with the dentine, however, even with the

enormous levels of contamination apparent in the previous example, the

enamel retained a significantly higher signature. It is also possible that the

original enamel value was quite low and was only affected to the same extent

as other teeth, or not at all. The dentine is still lower, at the lower end of the

dentine range, but this is likely overprint and the original signature may well

have matched the enamel.

Thorium is present across the entirety of the tooth, although uranium levels are

still reasonably low in most places. The DEJ is not able to be seen in any of the

elements, and there is no clear difference between the dentine and the enamel

in the strontium concentrations. This may suggest that significant diagenetic

strontium has indeed entered the tooth, as most teeth do show a noticeable

jump in Sr concentration after the DEJ. This supports the proposition that the

enamel signature may have been altered quite significantly from its original

value.

59

A7 – SLMEM 491

Figure 4.3.: Graphs of the elemental concentrations and isotopic

composition, along with an image of the tooth showing the spots made for

Neptune analysis (overlaying the Varian laser track)

0.01

0.1

1

10

100

1000

2739 2789 2839 2889 2939 2989 3039

pp

m

Time (sec)

Sr

Th

U

0.711

0.7115

0.712

0.7125

0.713

0.7135

0.714

1 6 11 16

87 S

r/8

6Sr

Spot Number

60

Example 4 – Adult 6 (SLMEM112)

This tooth is one of the four analysed previously using spots, and so was

analysed on the Varian using spots in corresponding locations. These four teeth

were also the ones analysed using solution. Like many other samples, there is a

clear rise in uranium at the DEJ. Like the previous sample, though, there is no

clear difference in strontium concentrations between the dentine and the

enamel. There are slight thorium spikes throughout the sample, but these are

generally small and isolated and it is likely that many of them are erroneous. It

is quite interesting in this sample to note the apparent correlation between the

quantity of uranium in the sample and the strontium isotopic signature. Where

the uranium is higher, the signature is lower (see figure 4.4.). This suggests that

in this tooth at least, the amount of diagenetic strontium entering the tooth was

proportional to the amount of uranium. This is not generally the case, however,

and there is no linear relationship between uranium content and diagenetic

strontium content - the extent of strontium signature modification cannot be

assessed on the basis of uranium content.

The solution analyses returned quite different values to the laser analyses, as

was seen in all teeth on which solution analysis was conducted. The difference

between the dentine signatures was twice that of the enamel, although this is

not standard for all teeth. The variation is quite considerable between samples,

and no standard offset is able to be observed between the laser and solution

analysis methods. While no standard offset is able to be identified, all solution

samples demonstrate a significant difference in values between the enamel and

the dentine. This tooth shows a difference of approximately 0.003 between the

61

enamel and dentine using both sampling methods. This confirms that the

difference is certainly real, even if the values themselves are inaccurate.

A6 – SLMEM 112

Figure 4.4.: Graphs of the elemental concentrations and isotopic

composition, along with an image of the tooth. (Note that the laser track

made during the Varian analysis is not visible, but it underlies the spots

made for the Neptune analysis. A track from previous analysis is also

visible)

0.01

0.1

1

10

100

1000

558 758 958 1158 1358 1558 1758

pp

m

Time (sec)

Sr

Th

0.71

0.711

0.712

0.713

0.714

0.715

0.716

0.717

1 3 5 7 9 11 13 15

laser

62

Chapter 5

Discussion

5.1. Soil analyses

As mentioned in the previous chapter, the first seven soil samples were

reproduced with a second set of samples taken from the same location. Only

six of the original seven returned results, and these had higher errors and lower

voltages than their newer counterparts. This is mostly likely due to errors in the

preparation and analysis, and along with the concerns about contamination

rising from the fact that the first seven samples were not subjected to the

column chemistry in a clean lab like the others, results from the original seven

samples are not considered to be as reliable. As such, the 11 newer results have

been used preferentially and they, along with 11 samples taken from the Médoc

region during fieldwork, form the basis for the discussions below.

5.1.1. The Médoc region

The geologic mapping of the region (Bureau de recherches géologiques et

minières, 2005) was based upon formation age rather than lithology, so each

unit may be composed of a number of rock types. For example, the Eocene unit

(orange in figures 1.3., 3.2., and 5.1.) is composed of marl, clay, limestone,

sandstone, and conglomerates. Thus, it is impractical to attempt to estimate the

expected Sr signature of each region based upon typical isotope ratios for the

rock types. Fortunately, as mentioned in the results section, the samples from

different units group together quite well and show clear separation in their

ranges. The exceptions to this are the lower Pleistocene and Holocene units

63

(light and dark green) that follow the coasts, which are likely formed by the

transportation and deposition of sediment by the Atlantic Ocean and the

Gironde rather than the weathering of local bedrock. The lower Pleistocene

unit (light green) fits within the range of the Pliocene and lower Pleistocene

pink unit which covers the majority of the peninsula. The Holocene (dark

green) unit has variable signatures, presumably reflecting the locations from

which the sediment originated. The Pliocene and lower Pleistocene sediment

(pink unit) that covers most of the inland area in the Médoc has a much higher

isotope ratio than the Eocene and Oligocene (orange and yellow) bedrock units,

reflecting the signatures of the source material from higher altitudes (Pyrenees).

Figure 5.1.: Measured 87

Sr/86

Sr ranges for each geologic unit in the Médoc

peninsula and the site of Le Tumulus des Sables. Note that the green units

have patchier distributions.

64

5.1.2. Le Tumulus des Sables

The soil samples from Le Tumulus des Sables display significantly more

variation than one may expect from sediment taken from the same location. In

addition to the difference in sediment colour at the site when compared to the

rest of the region, as noted in Chapter 1 (1.3.1.), this suggests the presence of

factors influencing the composition of the sediment other than those usually

involved (as in Section 2.2.3.). The site is situated within the Oligocene unit

(yellow), although, given the comparatively small size of the Médoc region, it

is not far from each of the others - particularly the Pliocene and lower

Pleistocene unit which covers much of the region (pink). Given the clear

separation in values from the different geologic units (other than the coastal

Holocene sands), one may expect the site of Le Tumulus des Sables to have a

signature similar to the Oligocene (yellow) unit. In part it does; however, its

range is much broader (while still fitting within the total range for the region).

This unexpectedly high degree of variation is difficult to explain. The

depositional setting is certainly quite complex, involving the input of sediment

washed down from higher areas (such as the Massif Central and the Pyrenees)

as well as tidal deposition. The samples taken from other locations, however,

grouped according to their geologic unit quite well. It is unlikely that this

complex deposition could have resulted in such an array of values in such a

confined location. It is more likely to have been caused by factors specific to

the burial itself. As mentioned in Section 1.3.1, the excavators theorised that

the brownish soil was the result of acid released by the limestone occurring at

the site (Courtaud et al., 2010). Similarly, it is possible that the degree of

65

variation within the site is the result of decomposition of buried archaeological

material. Whatever the source of this variation, it makes the local signature

quite difficult to define. Given that the overprinted values in the dentine

generally reflect the local value for the Oligocene unit in which the site is

located (see below), this may indicate that the site originally displayed a typical

signature for this area. This cannot be conclusively proven, but it is worth

consideration when interpreting the results from the teeth.

5.2. Teeth analyses

5.2.1. Laser vs. solution

The average offset between laser ablation and solution results identified by

Simonetti et al. (2008) was 0.0013±0.0006. While two of our solution samples,

112EN and 861DE, had offsets within this range, all others were significantly

higher. The offsets also displayed more variation than one might expect,

ranging from 0.0012±0.0002 to 0.0089±0.0003. While neither the enamel nor

the dentine was consistently higher than the other, patterns were able to be

identified in the offsets – the dentine offsets were much more consistent,

whereas most of the variation in values occurred in the enamel. The

significantly lower voltages in the enamel may be partially responsible for the

degree of variation in the offsets; however, there are a number of other

potential contributing factors.

The laser ablation was conducted using a series of spots, and the sample for

solution was taken from a different part of the dentine/enamel. As

demonstrated in both the elemental concentrations and strontium isotopic

66

analyses, both the enamel and dentine are heterogeneous in their composition.

Variation in the quantities of 87

Sr and 40

Ca-31

P-16

O molecules throughout the

tooth may affect the isotopic ratio (Simonetti et al., 2008). It is possible that the

differences in the offsets are at least partly an artefact of this heterogeneity.

Similarly, variation in the extent of diagenesis throughout the tooth, as

identified in the Varian elemental analysis, may be partially responsible for the

variation in the offsets. The laser spots can avoid zones of increased diagenesis,

whether intentionally or unintentionally, where the bulk sampling used for

solution analysis does not. The spots are also much less likely to be

representative of the entire tooth composition than the bulk sampling. In order

to assess whether the difference in the offsets is due to variation in the

elemental composition and diagenetic alteration within the tooth, micro-drilling

for the solution sample in the exact location of the laser analysis may be useful.

Despite the problem that the offset between laser ablation and solution presents,

and the difficulties in identifying and confirming these offsets in this study, this

does not necessarily cause significant problems for the interpretation of the

results. In fact, uncertainty over the exact signature is probably of less

importance in this study than in most others. Because the regional isotope

mapping revealed such a large range in Sr signatures, the capacity for the

identification of migration in the sample set is diminished to the point where

the exact Sr signatures are of little importance. The most important

observations in this case are the difference between the enamel and dentine in

the samples, and the fact that the dentine isotopic signatures all fall within a

comparatively small range. From this we have been able to determine that the

67

dentine has been subjected to significant diagenetic overprint and that the

original signature in many of the teeth was quite different, suggesting non-

locality. Due to the large regional range, it is impossible to tell whether this

„non-locality‟ represents true migration or small scale mobility. Only the

existence of a significant difference between the enamel and dentine is

important in this case, and the solution results support this. For example, in

tooth A6 (SLMEM112) (as in section 4.2.3.), the difference between the

enamel and dentine is roughly 0.003 in both sampling methods. After the

subtraction of the average laser offset from each sample (see table 4.8.), the

average difference between the enamel and dentine in all samples is 0.0043,

though it ranges from 0.0002 to 0.0104. This is significantly lower than the

unadjusted laser values, providing an average difference between enamel and

dentine of 0.0068, and ranging from 0.0019 to 0.0130.

5.2.2. Locals or non-locals?

The primary aim of this study has been to determine whether the individuals

from the study site are of local or non-local origin. In the preliminary work

conducted on this site, the local signature could not be determined and so the

only recourse was to compare the Sr results of the enamel to the dentine.

Given the significant difference that was observed between the dentine and the

enamel in all teeth, indicating diagenetic overprint in the dentine, it was

theorised that the whole population may have been non-local in origin. This

study attempted to create more reliable results, in conjunction with the creation

of a regional isotope map. As such, both the difference between the enamel and

dentine and the comparison of the dental values to the regional isotopic map

68

are available as methods of origin determination. The 87

Sr/86

Sr values were

adjusted using the average solution/laser offsets. While these are the more

realistic results, the errors are very large and the interpretation of the data

becomes complicated.

5.2.2.1. Enamel vs. Dentine

In interpreting the enamel and dentine results, careful attention must be paid to

the individual circumstances of each. While there is no linear correlation

between uranium concentration and diagenetic strontium uptake, 87

Sr/86

Sr

values appear largely to reflect the changes in uranium concentration. Where

the uranium concentrations are higher, the strontium isotope ratios are

generally lower, indicating the diagenetic impact of the local soil. While the

87Sr/

86Sr values have only been taken from the most appropriate domains in the

enamel, it is not necessarily the case that this represents a pristine zone in each

of the teeth. The enamel values tend to be lowest where either there is no clear

DEJ in the strontium concentrations, or where the concentrations fluctuate

significantly within the enamel. The correlation between these raised or

abnormal strontium concentrations in the enamel as compared to the dentine

and the lower enamel values seems to indicate that diagenetic strontium uptake

has occurred in these domains.

In the dentine, overprint appears to be universal. Fluctuations in uranium

within the tooth do not, other than in one or two samples, appear to be reflected

in the isotopic values. It is interesting to note, however, that while these

fluctuations within the tooth seem to have little impact on the signature, the

69

overall concentration of uranium compared to the other teeth does seem to bear

some relation to the Sr signature. Generally, where the uranium concentrations

are lower overall, the dentine Sr signature is higher. This supports the notion

that the low dentine values reflect extensive overprint, indicating that some

teeth have been less affected than others. Despite this variation in the extent of

overprint, there can be little doubt that all dentine has been affected quite

significantly, and it is unlikely that any of the dentine values reflect the

biogenic strontium signature. The fact that all of these samples in such a

comparatively young site show such extensive overprint, even where uranium

concentrations in the dentine are low, only serves to reinforce the notion that

dentine (and presumably bone) are poor materials for Sr isotope analysis.

The unadjusted laser data shows the dentine range falling entirely below all but

one enamel sample. The offset-adjusted data are significantly different, and

show no separation in the ranges. The dentine signatures range from 0.7084 ±

0.00103 – 0.7112 ± 0.0009. Nine of the offset-adjusted enamel signatures fall

immediately within this range, and when errors are considered this number

increases to 20. While there is little significant distinction between the overall

dentine and enamel ranges, most individual samples show a significant

distinction between the enamel and the dentine (with the exception of

SLMEM308, 491, and 102). With the consideration of the large errors,

however, the number of teeth in which there is actually a clear distinction

between the enamel and dentine falls to 11, and those in which the minimum

difference is larger than 0.0010 falls to 7. At this stage of the examination, it

appears likely that at least nine of the individuals are non-local. Within errors

70

ranges, is possible that all individuals are non-locals; however, the errors are so

large that it is impossible to make any firm conclusions.

5.2.2.2. Dental results in the regional context

As mentioned previously, the soil samples taken from the site itself display a

much higher range that expected, and may have been affected by factors

specific to the depositional circumstances. In this case, these cannot be used for

the determination of the local Sr isotope range. For this, we must turn to the

soil mapping conducted in the Médoc region. The offset-adjusted dentine Sr

signatures range from 0.7084 ± 0.0010 – 0.7112 ± 0.0009. With errors

considered, these values fall within and below the low end of the range for the

region, largely within the range identified for the Eocene (orange) unit. Given

the location of the site, situated with the Oligocene unit and in close proximity

to the Eocene unit, this is not unexpected. It is likely that the low local

signature is due to the input of marl, which forms a component of both of the

Oligocene and Eocene units. The higher values of the Pliocene/lower

Pleistocene (pink) sedimentary unit, located within very close proximity of Le

Tumulus des Sables, appear not to have had any impact on the local signature.

71

Figure 5.2.: Measured 87

Sr/86

Sr ratios for each geologic unit in the Médoc

peninsula and the offset adjusted enamel and dentine ranges (errors

included)

As well as the local range, the regional range must also be considered in order

to determine whether the individuals are truly foreign to the area. As discussed

in section 5.1, the different geologic units in the region have distinct ranges,

with the exclusion of the recent Holocene coastal deposition (see Figure 5.1.).

Unfortunately, the range in the Médoc is quite large, with lower values

exhibited in the older bedrock regions and much higher values being displayed

in the Pliocene/lower Pleistocene sediment (pink) which covers much of the

Médoc region. A number of the offset-adjusted enamel signatures (errors

included) possibly fall within the range of the Pliocene/lower Pleistocene unit;

however, none, except Adult 1 (SLMEM1007) with a signature of

0.7195±0.0038, could possibly reach above it. This means that despite the

differences between the enamel and dentine, and in many cases the enamel and

72

range at the site, no conclusion can be reached on the origin of these individual

using strontium isotopes. Under these circumstances, there is no way to

differentiate a migrant from hundreds of kilometres away from someone who

grew up two kilometres from Le Tumulus des Sables. Presuming the

individuals are migrants, a number of potential areas of origin can be ruled out

on the basis of general knowledge of the geology and previous mapping work

in France (Grün, pers. comm., Kelly, 2007). The enamel Sr values are

generally lower than the Pliocene/lower Pleistocene sedimentary unit, which

comprises much of the area within and immediately to the south of the Médoc,

including the Aquitaine basin. This sediment has its origins in the Pyrenees,

which has similarly has high Sr signatures, as do other highland areas in France

(such as the Massif Central). If these areas can be excluded, and the individuals

were indeed migrants, the most likely area of origin is directly to the east of the

Médoc.

While the Sr values may not be able to tell us whether the individuals are

migrants or not, they do indicate a certain degree of mobility within the Médoc

region at the very least. The geologic unit in which the site is located is quite

small (no more than 2x5km) and the site itself is right on the border of this unit

with the next, meaning that individuals need only travel a few kilometres to

obtain a non-local signature. The fact that there is so much variation in the

enamel signature, however, indicates that the population movement is far more

complex. All signatures could have come from the Médoc region, but they

reflect locations all over the region. Some of the difference in signatures may

be attributable to mixing of food sources from various regions, but one would

73

expect that within the same family or small community that people would

largely be eating similar foods from similar sources, and would thus obtain

similar signatures. The significant variation in signatures between the

individuals indicates considerable regional mobility at the very least.

Figure 5.3.: Geological map of France around the Médoc. The most likely

origin for any migrants would be to the east of the Médoc, before reaching

the Massif Central. The Pyrenees and Aquitaine basin to the south are

unlikely points of origin (from Bureau de recherches géologiques et

minières, 2005, GoogleEarth, 2011)

Given the impossibility of sex determination of the individuals due to the

disarticulated state of the remains, it is difficult to tell from this work whether

74

the variation in signatures was due to the movements of small groups and

individuals, or the result of marriage partner exchange. Presuming that the

values obtained from the juvenile enamel can be trusted to some extent, despite

the higher degree of contamination, these may provide more of a clue as to the

nature of population movement. If the variation was due to the exchange of

marriage partners, one would expect that the juveniles, all growing up in the

same community, would display similar signatures. The process of adjusting

for the offset increased the errors massively, meaning that all juvenile teeth are

now within range of one another; however, four of the teeth are particularly

similar in Sr values (averaging around 0.7148 ± 0.004.). In unadjusted laser

values, these four are also very similar. One tooth came close, although not

within error range of the first four, and the other three provided much higher

and lower values. This indicates that these juveniles spent the initial periods of

their lives in different locations to the others, and migrated later on. This

certainly does not rule out some of the variation in signatures coming from

marriage exchange partners, but it does indicate that this is not the sole source

of the variation. The presence of these children with different signatures

indicates the movement of family groups.

5.2.2.3. Further investigation

There is a large amount of variation in the both the enamel and dentine

strontium values within the group, and this was examined in terms of the

placement of each sample in the burial. This was done in an attempt to

determine whether there were any patterns in enamel signature and burial

location, and whether there was any correlation between burial location and the

75

diagenetic overprint. The site was excavated in grid squares using spits (R

values) rather than by context, although a number of different contexts were

able to be indentified (C values). The soil and dental samples were examined

by each of these unit types, where such information was provided by the site

excavators. Unfortunately, none of these groupings (grid squares, depths (R) or

context (C)) allowed the identification of any correlation between location and

strontium values in the soil, enamel or dentine.

The enamel Sr values were also considered in light of dental morphology.

During sample preparation, it was noted that a number of the teeth appear to be

taurodont, a dental condition characterised by an enlarged pulp chamber, an

elongated body relative to the roots, and a lack of or reduced constriction at the

cementoenamel junction (Ackerman et al., 1973, Jafarzadeh et al., 2008,

Jaspers and Witkop Jr, 1980, Keeler, 1973, Manjunatha and Kovvuru, 2010,

Shaw, 1928). While a number of the teeth appear to display the characteristic

to varying degrees, only five of them can be identified comfortably.

Taurodonty is caused by the failure of Hertwig‟s epithelial sheath diaphragm to

invaginate at the proper level (Ackerman et al., 1973, Jafarzadeh et al., 2008,

Manjunatha and Kovvuru, 2010). While it has been associated with a number

of syndromes and abnormalities, largely genetic and developmental, it occurs

most frequently in the absence of disease and appears to be a heritable trait

(Jafarzadeh et al., 2008, Jaspers and Witkop Jr, 1980, Manjunatha and Kovvuru,

2010). It is generally considered to be quite a rare trait, although prevalence

differs between populations from as little as 0.3% of the population to as much

as 48% (Jafarzadeh et al., 2008, and sources therein). It should be noted that

76

some of this variation may be attributed to different diagnostic criteria, but the

variation between study populations is certainly significant.

Taurodontism is only occasionally observed in the incisors and has a very low

incidence in deciduous dentition (Jafarzadeh et al., 2008), so the juvenile

samples have not been included as part of the sample for the investigation of

the trait in this population. Of the 15 teeth in which at least half of the roots and

pulp chamber remains attached to the crown, five of these are identified as

taurodont (SLMEM 1157, 454, 432, 112 and 900). A population frequency of

1/3rd

is very high, and given the heritability of the trait it was presumed that

these individuals represented a family group. Upon consideration of the

strontium isotope results in these teeth, this was found not to be the case; two

individuals have reasonably high signatures, two have reasonably low

signatures within, and one is in between. The unadjusted laser values, with

much lower errors, indicated that the three signature groups were statistically

different. With the offset correction, however, all of the values fall within error

range of one another. Unfortunately, with the current data, there is no way to

tell whether the differences in the values are real or not. If the individuals do

represent a family, this would lend support to the idea of migratory family

groups as is possibly indicated by the juvenile teeth. If the signatures are

different, it may still be possible that the individuals comprised a migratory

family group of different ages, having spent their childhoods in different

locations. The other interpretation is that these individuals do not represent a

family group at all. It may be that this population displays the trait in high

frequency. It may also be the case that this high percentage is simply an

77

artefact of the small sample size. In order to confirm that the reliability of this

result, morphological analysis on a much larger sample would be necessary.

Of course, any observations about trait frequency and mobility within this

population rest upon the assumption that the individuals from the burial do in

fact represent a single population. As noted in the first chapter, the site was

identified as Bell Beaker based upon the presence of distinctive bell Beaker

artefacts. Dating of one bone fragment provided a date which confirmed

occupation of the site during the Bell Beaker era, but charcoal dates from the

upper and lower layers of the excavation provided much older and younger

dates, suggesting site occupation over a much broader period of time. The age

range and poor stratigraphy of the site prevent the secure identification of a

sample as belonging to the correct time period without individual dating. Given

the propensity for Bell Beaker people in this region to re-use tombs of the

preceding cultures, and the variable ways in which these tombs were used (as

discussed in section 2.1.1), the most that can be said at this point is that Bell

Beaker associated artefacts have been identified at the site and that at least one

individual has been dated to this period of time.

5.2.3. Implications for the technique

As observed by Simonetti et al. (2008), significant offsets were identified

between the laser ablation and solution methods of analysis. The offsets were

reasonably large and quite variable, particularly in the enamel. The correction

of the laser results by averaging these offsets created very large errors, and

rendered the results almost unusable. Much more investigation into the cause

78

of the magnitude and variability of the offset needs to be conducted if the laser

ablation technique is to be applied in further Sr isotope studies.

Another existing concern that was addressed was the effect of diagenesis on

dentine and enamel. Even in such comparatively young samples, the overprint

in the dentine was found to be extensive. While concentrations of Sr, U and Th

may be used to indicate the presence of diagenesis, no consistent correlation

was able to be found between elevated levels of these contaminants and Sr

isotopic signature in the dentine. Even where levels of contaminants might

have been considered to indicate minimal contamination in the enamel, the

dentine was found to be entirely overprinted (for example, A1 – SLMEM1007).

In the enamel, the level of diagenetic alteration was considerably lower, and

pristine zones were identified in most. Some relation between elevated levels

of U, Th and the isotopic signature was able to be identified, with the isotopic

values usually dropping noticeably in zones where these were elevated,

although there is no constant or linear correlation. Where raised Sr levels

occurred at the same time as high U levels, isotopic ratios dropped significantly,

and this was found to be a good indicator of contamination. These results

suggest that even where concentrations of the elemental contaminants are low,

dentine is highly unlikely to preserve any pristine zones.

While the investigation of the concerns discussed above may have their place

in the continuing improvement of our understanding and utilisation of the

technique, perhaps the most significant contributions made by this study arise

from the local and regional mapping. As discussed previously, the soil samples

from the archaeological site display much more variation in values than might

79

have been expected, and this is likely at least partially attributable to factors

specific to archaeological contexts such as the decomposition of buried

material. This, in conjunction with the agreement between the dentine values

and the expected local range based upon regional mapping, suggests that the

sediment from an archaeological site should not be considered to be

representative of the local range. The regional mapping itself turned out to

have more of an impact on the interpretation of the results than was foreseen.

The preliminary results, based upon the difference between the enamel and

dentine, seemed to suggest that the population was largely composed of

migrants. Upon consideration of the map, this conclusion was invalidated

completely. The value of regional mapping, which is largely underused in

strontium isotope studies, could not have been better demonstrated.

5.2.4. Implications for the Bell Beaker

Before any discussion of potential implications for our understanding of the

Bell Beaker phenomenon, it is necessary to emphasise that we do not know

with certainty that the individuals from the site truly represent a single, Bell

Beaker, population. Given that no groups or trends are able to be identified in

the enamel strontium values within the group, it seems possible at least that this

is a single, highly mobile population. Whether this mobility is simply within

the local region or over a larger area is impossible to tell at this point. The

variation in enamel signatures suggests a number of source locations for the

individuals, possibly also indicating that the group is not in fact part of a single

population. For the time being, the results are being treated as if representative

of a single Bell Beaker population; however, all discussion about the potential

80

implications for the Bell Beaker phenomenon should be read with this

uncertainty about the sample composition in mind.

Due to impossibility of distinguishing small scale local mobility from large

scale migration in this study, no grand conclusions can be drawn regarding the

origins of this population or the role of migration in the spread of the Bell

Beaker culture. However, this does not mean that the results have no use. The

difference between enamel and dentine strontium values along with the

significant variation between the enamel values suggests a high degree of

mobility within the population with individuals coming from a number of

source locations. We may not be able to identify how far away these source

locations may have been, but there is little doubt that the people were highly

mobile within the region at the very least. As mentioned previously, the

inability to determine the sex of each individual makes it difficult to determine

the degree to which the variation in the signatures is attributable to the

exchange of marriage partners. The variation in juvenile signatures may,

however, be indicative of the movement of family groups. The movement of

family groups rather than individual marriage exchange partners is certainly

what one might expect to see if migration were the driving factor behind the

spread of the Bell Beaker culture. One should also consider that even if the

enamel signatures were only obtained from the local region, this does not rule

out migratory origins for the Bell Beaker culture. There is no reason to assume

that a burial of Bell beaker individuals must necessarily represent the first

generation of migrants into the area. It is possible, even, that the large amount

of variation in the enamel signatures is partially attributable to the varying

81

origins of different generations. Again, the broad range of signatures obtainable

from the local region alone make this impossible to ascertain.

Presuming that the individuals at Le Tumulus des Sables were of migrant

origin, the most likely origin (as established in Section 5.2.2.2) for these people

would be the area directly to the east of the Médoc. It is unlikely that they

came from the south, anywhere between the Pyrenees and the Médoc, although

extremely distant origins on the other side of the Pyrenees cannot be excluded.

It seems unlikely, however, that any of these individuals had direct origins in

the Iberian Peninsula. This does not necessarily pose a problem for the

hypothesis that the Bell Beaker Phenomenon had its origins in the Iberian

Peninsula; it simply indicates that this population certainly is not a first

generation wave of settlers originating in the Pyrenees.

While results do not firmly indicate whether the Bell Beaker phenomenon was

the result of migration or cultural diffusion, the answer need not necessarily be

just one or the other. One theory proposed by Vander Linden (2007b) suggests

that the Bell Beaker phenomenon neither represented the simple diffusion of

objects and ideas, nor a single group of people with territorial unity. Instead, he

proposed that the Bell Beaker culture was composed of a series of discrete

groups, in which the constant flow of people, ideas and technologies produced

a chain of networks which led to the witnessed global effect. This was

suggested to have been the result of generalised exchange in marriage partners,

rather than reciprocity. Again, the inability to determine the sex of the

individuals means that investigation of marriage partner exchange is not

possible; however, the indication from the juvenile remains of the movement of

82

family groups would seem to suggest that more was going on than the

exchange of marriage partners. The mechanism may not be strongly supported

by our data, but the concept may well be. There is good evidence for high

regional mobility at the very least. Based upon our data, diffusion as the

mechanism for the spread of the Bell Beaker culture is least supported, but is

not directly contraindicated.

The possible identification of a high frequency of taurodontism in the sample

set may also have implications for our understanding of the Bell Beaker, but

morphological analysis of a much larger Bell Beaker sample set would be

required to verify its existence. If the individuals displaying taurodonty

represent a family group, the variation in strontium isotope ratios may

represent migration across generations. If these individuals are not a family

group, the high prevalence of taurodonty within the population that this would

indicate may be used to indicate the origins of the individual - the trait is

usually quite rare, although the frequency has been seen to vary between „racial‟

groups (Jafarzadeh et al., 2008, and sources therein). Detailed consideration of

this is beyond the scope of this study, but may be worth future investigation.

5.3. Summary

The different geologic units in the Médoc region separate well

according to Sr values, with the exception of the Holocene sediment.

The soil samples from Le Tumulus des Sables display unexpected

variation, likely due to the complex depositional geology and

83

decomposition of buried material. This archaeological soil does not

provide a reliable local range.

Significant offsets between laser ablation and solution are identified.

The dentine offsets are more constant than the enamel offsets, with vary

considerably. There are a number of potential factors contributing to

this variation.

The offset corrections applied to the original laser ablation results

lower them, reduce the difference between the enamel and dentine, and

create massive error ranges. Despite this, most teeth still show a clear

difference between enamel and dentine.

All dentine shows extensive overprint, despite the comparatively young

age of the samples. Sr values were only taken from appropriate domains

in the enamel, and not all samples preserved pristine zones.

In the context of the mapping of the Médoc region, and due to the

massive errors introduced by the offset corrections, it is impossible to

tell from the dental Sr results whether the individuals are migrants or

local

Despite our inability to determine geographic origins, the variability in

enamel values suggests that the population is highly mobile.

Examination of the juvenile teeth may suggest the movement of small

family groups. If they were migrants, they are most likely to have come

from the East of the Médoc. Origins in the South seem highly unlikely.

84

Chapter 6

Conclusions

______________________________________________________

6.1. Conclusions and recommendations

Significant difficulties were encountered in answering the main aim of the

study, but all aims were addressed to the fullest extent allowed by the data and

this led to a number of conclusions. The results from this study ultimately

turned out to be inconclusive due to a number of factors, but this does not mean

that migration cannot be distinguished at the site. The biggest source of error

was the laser ablation/solution offset and this has to be resolved before any

further work can be conducted at this site or elsewhere using laser ablation. It

is suggested that until the cause of the offset has been fully investigated and a

solution identified, that laser only be used to determine elemental

concentrations and identify pristine domains within the tooth. It is

recommended that micro drilling is used to extract samples for solution

analyses from these pristine zones, given that the current bulk sampling method

does not avoid diagenetic material.

With more accurate and precise results, more could be said about the mobility

of the individuals. Whether they were true migrants, however, or simply

mobile within the Médoc would still be impossible to distinguish due to the

large range of Sr signatures within the Médoc. Other isotopic proxies, such as

oxygen and lead, may be used to trace migration. These work in slightly

different ways, meaning that they may not be affected by the same obstacles as

the strontium work in this region. Together, these isotopic proxies may not

85

only distinguish locals from non-locals, but with extensive mapping it may be

possible even to determine the origins of any migrants.

While it was not possible to distinguish migrants from locals, it is possible to

identify mobility within the Médoc region at the very least. Whether this is true

group mobility or the exchange of marriage partners is difficult to tell. Sex

determination on the basis of physical anthropology is impossible given the

fragmentation of the human remains, but there are other options. DNA could be

used, depending on the preservation of the material. Detailed studies would not

be required; a look at the karyotype is all that is necessary to determine the

presence or absence of a „y‟ chromosome. Given that taurodonty is sometimes

associated with genetic abnormalities, such as Kleinfelter‟s syndrome, in which

the male has an extra „x‟ chromosome (xxy), it may also be interesting to

investigate whether this is the case in any of the taurodont individuals.

The results of this study have a number of implications not only for the site

itself, but for the technique in general. The state of diagenesis in the dentition

in even a comparatively young site such as this suggests that dentine, and

perhaps bone by association, should only be used for comparison with the

enamel and possibly for confirmation of the local signature. Future studies in

the area, and perhaps in general, should focus on tooth enamel to gather the

most reliable results. It is recommended that elemental concentrations are

examined and compared to the isotopic data in order to determine the most

pristine zones. One or the other is insufficient for the firm identification of

contaminated Sr signatures.

86

In this case, the level of contamination in the dentine made it quite useful in

determining and confirming the local signature. The overprint was lower than

might have been expected for the Oligocene unit, in which the site was located;

however, the geologic maps reflect chronology rather than lithology. The low

Sr signature likely came from rock types which were a component in both the

Oligocene and Eocene units. Interestingly, the local signature, as determined

by this mapping and by the overprinted dentine, was nothing like the soil

samples taken from the site itself. The unexpected variation in the soil samples

from the site is likely to have been caused by the complex depositional setting,

as well as the effect of decomposing material within the burial. This

phenomenon is likely not restricted to this site, and may be applicable

elsewhere. The implication of this is that archaeological soil should not be

considered to reflect the local range. This should be taken into account in

future studies, and the local signature should be determined through other

means, such as more extensive mapping or through the analysis of teeth from

small mammals with confined ranges.

The importance of mapping could not have been better demonstrated than in

this study. Without the mapping of the Médoc, many of the individuals would

have been identified as migrants on the basis of the clear difference in Sr

signatures between the enamel and the dentine. Had the local signature been

determined on the basis of the enamel of small mammalian remains, many of

the individuals would still likely have been outside this range and would have

been firmly identified as non-local. It is only with mapping of the Médoc

region that the magnitude of the regional Sr range was discovered, it was

87

realised that the individuals were not necessarily migrants. It is recommended

that all future studies incorporate mapping of the region around the site at the

very least. More detailed mapping across larger areas may provide further

valuable insights, but basic mapping of the surrounding area in consultation

with a geologic map is the minimum required to ensure that migration is not

falsely identified.

The inability to distinguish true migration from outside the Médoc from

mobility within the region has hampered attempts at expanding our

understanding of the Bell Beaker, but this is just one site of many across

Europe. Particularly in light of the observed differences between the eastern

and western domains of the Bell Beaker people, it is recommended that

mobility studies using Sr isotopes, and other isotopic proxies where necessary,

are extended to many other sites. With the inclusion of isotope mapping,

perhaps then it may be possible to determine the origin and nature of the Bell

Beaker phenomenon once and for all.

88

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composition of modern and Holocene mollusc shells as a palaeosalinity

indicator. Chemical Geology, 232, 54-66.

98

Appendix 1

Full list of the standard (Tridacna shell) measurements taken throughout

the Neptune laser analyses

Batch Number 87

Sr/86

Sr 2se

1.1 1007 & 308 Before 0.709155 0.000138

1.1 1007 & 308 Before 0.709166 0.000190

1.1 1007 & 308 Before 0.709161 0.000179

1.1 1007 & 308 After 0.709180 0.000139

1.1 1007 & 308 After 0.709164 0.000144

1.1 1007 & 308 After 0.709182 0.000169

1.1 Average 0.709168 0.000159

1.2 491 & 1094 Before 0.709192 0.000114

1.2 491 & 1094 Before 0.709189 0.000124

1.2 491 & 1094 Before 0.709206 0.000104

1.2 491 & 1094 After 0.709205 0.000122

1.2 491 & 1094 After 0.709188 0.000121

1.2 491 & 1094 After 0.709201 0.000130

1.2 Average 0.709197 0.000119

1.3 454 & 900 Before 0.709154 0.000150

1.3 454 & 900 Before 0.709181 0.000178

1.3 454 & 900 Before 0.709157 0.000156

1.3 454 &900 After 0.709175 0.000225

1.3 454 &900 After 0.709177 0.000148

1.3 454 &900 After 0.709159 0.000152

1.3 Average 0.709167 0.000168

1.4 432 - 5 Before 0.709184 0.000155

1.4 432 - 5 Before 0.709154 0.000153

1.4 432 - 5 Before 0.709161 0.000128

1.4 Between 509 & 282 0.709178 0.000149

1.4 Between 509 & 282 0.709171 0.000130

1.4 Between 509 & 282 0.709178 0.000163

1.4 Between 298 & 1157 0.709202 0.000157

1.4 Between 298 & 1157 0.709199 0.000162

1.4 Between 298 & 1157 0.709181 0.000152

1.4 432 - 5 After 0.709172 0.000197

1.4 432 - 5 After 0.709172 0.000180

1.4 432 - 5 After 0.709167 0.000200

1.4 Average 0.709176 0.000160

1.5 Juvenile Before 0.709136 0.000159

1.5 Juvenile Before 0.709158 0.000113

1.5 Juvenile Before 0.709144 0.000106

1.5 Between 1192 & 119 0.709203 0.000235

99

1.5 Between 1192 & 119 0.709193 0.000226

1.5 Between 1192 & 119 0.709167 0.000218

1.5 Between 66 & 276 0.709190 0.000147

1.5 Between 66 & 276 0.709153 0.000160

1.5 Between 66 & 276 0.709113 0.000323

1.5 Juvenile After 0.709158 0.000122

1.5 Juvenile After 0.709175 0.000143

1.5 Juvenile After 0.709129 0.000158

1.5 Average 0.709159 0.0001758

2.1 112 Before 0.709211 0.000025

2.1 112 Before 0.709221 0.000031

2.1 112 Before 0.709229 0.000025

2.1 112 Before 0.709216 0.000026

2.1 112 Before 0.709219 0.000027

2.1 112 Before 0.70922 0.000028

2.1 112 Before 0.70923 0.000032

2.1 112 Before 0.709201 0.000023

2.1 112 Before 0.709194 0.000028

2.1 112 Before 0.709203 0.000030

2.1 112 Before 0.709195 0.000022

2.1 112 Before 0.709213 0.000023

2.1 112 Before 0.709222 0.000031

2.1 112 After 0.709211 0.000028

2.1 112 After 0.70922 0.000029

2.1 112 After 0.709217 0.000027

2.1 112 After 0.70922 0.000028

2.1 112 After 0.709214 0.000024

2.1 112 After 0.709215 0.000026

2.1 112 After 0.709202 0.000028

2.1 112 After 0.709179 0.000027

2.1 112 After 0.709218 0.000020

2.1 112 After 0.709196 0.000026

2.1 112 After 0.709215 0.000023

2.1 112 After 0.709211 0.000030

2.1 112 After 0.709199 0.000029

2.1 Average 0.709211 0.000026

2.2 263 Before 0.709201 0.000024

2.2 263 Before 0.709215 0.000025

2.2 263 Before 0.709230 0.000025

2.2 263 Before 0.709199 0.000030

2.2 263 Before 0.709207 0.000027

2.2 263 Before 0.709194 0.00004

2.2 263 Before 0.709192 0.000026

2.2 263 Before 0.709213 0.000023

2.2 263 Before 0.709209 0.000024

2.2 263 After 0.709190 0.000026

100

2.2 263 After 0.709224 0.000028

2.2 263 After 0.709226 0.000033

2.2 263 After 0.709214 0.000029

2.2 263 After 0.709198 0.000030

2.2 263 After 0.709219 0.000025

2.2 263 After 0.709208 0.000029

2.2 263 After 0.709219 0.000026

2.2 Average 0.709209 0.000027

2.3 466 Before 0.709203 0.000020

2.3 466 Before 0.709219 0.000028

2.3 466 Before 0.709218 0.000029

2.3 466 Before 0.709201 0.000025

2.3 466 Before 0.709196 0.000026

2.3 466 Before 0.709205 0.000025

2.3 466 Before 0.709212 0.000027

2.3 466 Before 0.709217 0.000026

2.3 466 Before 0.709215 0.000025

2.3 466 Before 0.709185 0.000026

2.3 466 Before 0.709219 0.000023

2.3 466 Before 0.709209 0.000025

2.3 466 Before 0.709225 0.000024

2.3 466 After 0.709199 0.000027

2.3 466 After 0.709214 0.000029

2.3 466 After 0.709205 0.000027

2.3 466 After 0.709193 0.000026

2.3 466 After 0.709192 0.000025

2.3 466 After 0.709221 0.000030

2.3 466 After 0.709204 0.000026

2.3 466 After 0.709211 0.000026

2.3 466 After 0.709211 0.000031

2.3 466 After 0.709202 0.000026

2.3 466 After 0.709177 0.000023

2.3 466 After 0.709205 0.000027

2.3 Average 0.709206 0.000026

2.4 861 Before 0.709216 0.000034

2.4 861 Before 0.709203 0.000025

2.4 861 Before 0.709215 0.000032

2.4 861 Before 0.709246 0.000023

2.4 861 Before 0.70922 0.000026

2.4 861 Before 0.709217 0.000024

2.4 861 Before 0.709229 0.000026

2.4 861 Before 0.70921 0.000028

2.4 861 Before 0.709219 0.000024

2.4 861 Before 0.709229 0.000023

2.4 861 Before 0.709216 0.000031

2.4 861 Before 0.709196 0.000026

101

2.4 861 Before 0.70922 0.000027

2.4 861 Before 0.709211 0.000030

2.4 861 Before 0.709216 0.000028

2.4 861 Before 0.709199 0.000026

2.4 861 Before 0.709227 0.000030

2.4 861 Before 0.709217 0.000024

2.4 861 Before 0.70922 0.000007

2.4 861 Before 0.709214 0.000026

2.4 861 After 0.70922 0.000033

2.4 861 After 0.709232 0.000028

2.4 861 After 0.709235 0.000029

2.4 861 After 0.7092 0.000029

2.4 861 After 0.709223 0.000028

2.4 861 After 0.709216 0.000029

2.4 861 After 0.709224 0.000027

2.4 861 After 0.709221 0.000026

2.4 861 After 0.70923 0.000030

2.4 861 After 0.709222 0.000027

2.4 861 After 0.709209 0.000027

2.4 861 After 0.7092 0.000030

2.4 861 After 0.709207 0.000030

2.4 861 After 0.709205 0.000021

2.4 861 After 0.709202 0.000029

2.4 861 After 0.70919 0.000030

2.4 861 After 0.709206 0.000030

2.4 861 After 0.709226 0.000030

2.4 861 After 0.709209 0.000027

2.4 861 After 0.709216 0.000030

2.4 861 After 0.709199 0.000026

2.4 861 After 0.709228 0.000033

2.4 861 After 0.709209 0.000030

2.4 Average 0.709215 0.000027

102

Appendix 2

Complete illustrated data sheets for each tooth

______________________________________________________

103

Adult 1 - SLMEM 1007

Elemental Concentrations

Isotopic Composition

0.01

0.1

1

10

100

1000

567 617 667 717 767

pp

m

Time (sec)

Sr

Th

U

0.708

0.712

0.716

0.72

0.724

0.728

1 2 3 4 5 6 7 8 9 10 11 12 13

87 S

r/8

6 Sr

Spot Number

Average 87

Sr/86

Sr ratios *

Enamel Dentine 87

Sr/86

Sr 2se 87

Sr/86

Sr 2se

0.724369 0.000471 0.711349 0.000225

*From selected zones, avoiding areas affected

by diagenesis areas where possible

Elemental Concentrations – High and low zones 238

U Concentration (ppm) 232

Th Concentration (ppm) 88

Sr Concentration (ppm)

EN

High

EN

Low

DE

High

DE

Low

EN

High

EN

Low

DE

High

DE

Low

EN High EN Low DE

High

DE

Low

0.123 0.040 10.081 0.293 0.000 0.000 0.000 0.000 48.544 39.727 156.636 142.933

104

Adult 2 – SLMEM 466

Elemental Concentrations

Isotopic Composition

0.01

0.1

1

10

100

1000

1 101 201 301 401 501 601 701

pp

m

cycle

Sr

Th

U

0.71

0.712

0.714

0.716

0.718

0.72

1 3 5 7 9 11 13

87

Sr/8

6Sr

Spot number

Average 87

Sr/86

Sr ratios

Enamel Dentine 87

Sr/86

Sr 2se 87

Sr/86

Sr 2se

Laser* 0.718634 0.000313 0.713176 0.000196

Solution 0.711915 0.000051 0.710585 0.000019

*From selected zones, avoiding areas

affected by diagenesis areas where

possible

Elemental Concentrations – High and low zones 238

U Concentration (ppm) 232

Th Concentration (ppm) 88

Sr Concentration (ppm)

EN

High

EN

Low

DE

High

DE

Low

EN

High

EN

Low

DE

High

DE

Low

EN High EN

Low

DE

High

DE Low

0.052 0.000 0.267 0.144 0.001 0.000 0.000 0.000 79.456 56.928 111.648 101.8566

105

Adult 3 - SLMEM 308

Elemental Concentrations

Isotopic Composition

0.01

0.1

1

10

100

1000

1617 1667 1717 1767 1817

pp

m

Time (sec)

Sr

Th

U

0.711

0.712

0.713

0.714

0.715

0.716

0.717

1 3 5 7 9 11 13

87 S

r/8

6Sr

Spot Number

Average 87

Sr/86

Sr ratios *

Enamel Dentine 87

Sr/86

Sr 2se 87

Sr/86

Sr 2se

0.715640 0.000289 0.712493 0.000296

*From selected zones, avoiding areas

affected by diagenesis areas where possible

Elemental Concentrations – High and low zones

238U Concentration (ppm)

232Th Concentration (ppm)

88Sr Concentration (ppm)

EN

High

EN

Low

DE

High

DE

Low

EN

High

EN

Low

DE

High

DE

Low

EN High EN Low DE

High

DE

Low

0.464 0.000 4.593 0.071 0.043 0.000 0.000 0.000 93.601 76.647 105.460 100.169

106

Adult 4 – SLMEM 263

Elemental Concentrations

Isotopic Composition

0.708

0.71

0.712

0.714

0.716

0.718

0.72

0.722

1 3 5 7 9 11 13 15

87

Sr/8

6Sr

Spot Number

Average 87

Sr/86

Sr ratios

Enamel Dentine 87

Sr/86

Sr 2se 87

Sr/86

Sr 2se

Laser* 0.720533 0.000294 0.712481 0.00013

Solution 0.711647 0.000028 0.709697 0.000026

*From selected zones, avoiding areas

affected by diagenesis areas where

possible

Elemental Concentrations – High and low zones 238

U Concentration (ppm) 232

Th Concentration (ppm) 88

Sr Concentration (ppm)

EN

High

EN

Low

DE

High

DE

Low

EN

High

EN

Low

DE

High

DE

Low

EN High EN Low DE

High

DE

Low

0.177 0.046 0.242 0.209 0.000 0.000 0.000 0.000 48.445 45.582 129.241 129.734

107

Adult 5 – SLMEM 861

Elemental Concentrations

Isotopic Composition

0.01

0.1

1

10

100

1000

525 725 925 1125 1325 1525 1725

pp

m

Time (sec)

Sr

Th

U

0.708

0.71

0.712

0.714

0.716

0.718

0.72

0.722

0.724

1 3 5 7 9 11 13 15

87

Sr/8

6Sr

Spot number

Average 87

Sr/86

Sr ratios

Enamel Dentine 87

Sr/86

Sr 2se 87

Sr/86

Sr 2se

Laser* 0.722658 0.000543 0.711701 0.000156

Solution - - 0.710466 0.000020

*From selected zones, avoiding areas

affected by diagenesis areas where

possible

Elemental Concentrations – High and low zones 238

U Concentration (ppm) 232

Th Concentration (ppm) 88

Sr Concentration (ppm)

EN

High

EN

Low

DE

High

DE

Low

EN

High

EN

Low

DE

High

DE

Low

EN High EN Low DE

High

DE

Low

0.017 0.000 3.044 2.347 0.000 0.000 0.020 0.000 51.145 41.541 176.905 164.910

108

Adult 6 – SLMEM 112

Elemental Concentrations

Isotopic Composition

0.01

0.1

1

10

100

1000

558 758 958 1158 1358 1558 1758

pp

m

Time (sec)

Sr

Th

U

0.71

0.711

0.712

0.713

0.714

0.715

0.716

0.717

1 3 5 7 9 11 13 15

87

Sr/8

6Sr

Spot number

Average 87

Sr/86

Sr ratios

Enamel Dentine 87

Sr/86

Sr 2se 87

Sr/86

Sr 2se

Laser* 0.715797 0.000147 0.713439 0.000182

Solution 0.714101 0.000054 0.710860 0.000019

*From selected zones, avoiding areas

affected by diagenesis areas where

possible

Elemental Concentrations – High and low zones 238

U Concentration (ppm) 232

Th Concentration (ppm) 88

Sr Concentration (ppm)

EN

High

EN

Low

DE

High

DE

Low

EN

High

EN

Low

DE

High

DE

Low

EN High EN Low DE

High

DE

Low

0.002 0.000 1.222 0.313 0.000 0.000 0.000 0.001 140.742 115.855 126.531 113.048

109

Adult 7 – SLMEM 491

Elemental Concentrations

Isotopic Composition

0.01

0.1

1

10

100

1000

2739 2789 2839 2889 2939 2989 3039

pp

m

Time (sec)

Sr

Th

U

0.711

0.7115

0.712

0.7125

0.713

0.7135

0.714

1 3 5 7 9 11 13 15 17

87 S

r/8

6 Sr

Spot Number

Average 87

Sr/86

Sr ratios *

Enamel Dentine 87

Sr/86

Sr 2se 87

Sr/86

Sr 2se

0.713302 0.000418 0.711423 0.000313

*From selected zones, avoiding areas

affected by diagenesis areas where possible

Elemental Concentrations – High and low zones 238

U Concentration (ppm) 232

Th Concentration (ppm) 88

Sr Concentration (ppm)

EN

High

EN

Low

DE

High

DE

Low

EN

High

EN

Low

DE

High

DE

Low

EN High EN Low DE

High

DE

Low

0.109 0.027 2.178 0.373 0.053 0.000 0.048 0.045 158.058 124.530 146.815 138.116

110

Adult 8 – SLMEM 1094

Elemental Concentrations

Isotopic Composition

0.01

0.1

1

10

100

1000

539 589 639 689 739 789

pp

m

Time (sec)

Sr

Th

U

0.71

0.711

0.712

0.713

0.714

0.715

0.716

0.717

1 3 5 7 9 11 13

87 S

r/8

6 Sr

Spot Number

Average 87

Sr/86

Sr ratios *

Enamel Dentine 87

Sr/86

Sr 2se 87

Sr/86

Sr 2se

0.715698 0.000384 0.710956 0.000255

*From selected zones, avoiding areas

affected by diagenesis areas where possible

Elemental Concentrations – High and low zones

238U Concentration (ppm)

232Th Concentration (ppm)

88Sr Concentration (ppm)

EN

High

EN

Low

DE

High

DE

Low

EN

High

EN

Low

DE

High

DE

Low

EN High EN Low DE

High

DE

Low

0.072 0.000 9.870 7.962 0.000 0.000 0.013 0.010 152.039 89.234 234.123 214.377

111

Adult 9 – SLMEM 454

Elemental Concentrations

Isotopic Composition

0.01

0.1

1

10

100

1000

1367 1417 1467 1517

pp

m

Time (sec)

Sr

Th

U

0.712

0.714

0.716

0.718

0.72

0.722

0.724

1 3 5 7 9 11

87 S

r/8

6 Sr

Spot Number

Average 87

Sr/86

Sr ratios *

Enamel Dentine 87

Sr/86

Sr 2se 87

Sr/86

Sr 2se

0.722278 0.000677 0.713131 0.000309

*From selected zones, avoiding areas

affected by diagenesis areas where possible

Elemental Concentrations – High and low zones 238

U Concentration (ppm) 232

Th Concentration (ppm) 88

Sr Concentration (ppm)

EN

High

EN

Low

DE

High

DE

Low

EN

High

EN

Low

DE

High

DE

Low

EN High EN Low DE

High

DE

Low

0.002 0.000 1.644 0.610 0.002 0.000 0.000 0.000 48.153 37.060 96.490 96.189

112

Adult 10 – SLMEM 900

Elemental Concentrations

Isotopic Composition

0.01

0.1

1

10

100

1000

2499 2549 2599 2649 2699 2749

pp

m

Time (sec)

Sr

Th

U

0.711

0.712

0.713

0.714

0.715

0.716

0.717

0.718

0.719

1 3 5 7 9 11

87Sr

/86 S

r

Spot Number

Average 87

Sr/86

Sr ratios *

Enamel Dentine 87

Sr/86

Sr 2se 87

Sr/86

Sr 2se

0.717876 0.000442 0.712092 0.000305

*From selected zones, avoiding areas

affected by diagenesis areas where possible

Elemental Concentrations – High and low zones 238

U Concentration (ppm) 232

Th Concentration (ppm) 88

Sr Concentration (ppm)

EN

High

EN

Low

DE

High

DE

Low

EN

High

EN

Low

DE

High

DE

Low

EN High EN Low DE

High

DE

Low

0.324 0.003 0.858 0.242 0.001 0.000 0.000 0.000 61.407 50.445 108.170 96.817

113

Adult 11 – SLMEM 432

Elemental Concentrations

Isotopic Composition

0.01

0.1

1

10

100

1000

486 536 586 636 686

pp

m

Time (sec)

Sr

Th

U

0.71

0.711

0.712

0.713

0.714

0.715

0.716

0.717

1 3 5 7 9 11

87 S

r/8

6 Sr

Spot Number

Average 87

Sr/86

Sr ratios *

Enamel Dentine 87

Sr/86

Sr 2se 87

Sr/86

Sr 2se

0.715841 0.000535 0.710831 0.000314

*From selected zones, avoiding areas

affected by diagenesis areas where possible

Elemental Concentrations – High and low zones 238

U Concentration (ppm) 232

Th Concentration (ppm) 88

Sr Concentration (ppm)

EN

High

EN

Low

DE

High

DE

Low

EN

High

EN

Low

DE

High

DE

Low

EN High EN Low DE

High

DE

Low

0.317 0.027 3.245 - 0.004 0.002 0.000 - 51.732 49.830 123.165 -

114

Adult 12 – SLMEM 509

Elemental Concentrations

Isotopic Composition

0.01

0.1

1

10

100

1000

1239 1289 1339 1389 1439 1489 1539

pp

m

Time (sec)

Sr

Th

U

0.71

0.712

0.714

0.716

0.718

0.72

1 3 5 7 9 11 13 15 17

87 S

r/8

6 Sr

Spot Number

Average 87

Sr/86

Sr ratios *

Enamel Dentine 87

Sr/86

Sr 2se 87

Sr/86

Sr 2se

0.719563 0.000749 0.711380 0.000321

*From selected zones, avoiding areas

affected by diagenesis areas where possible

Elemental Concentrations – High and low zones 238

U Concentration (ppm) 232

Th Concentration (ppm) 88

Sr Concentration (ppm)

EN

High

EN

Low

DE

High

DE

Low

EN

High

EN

Low

DE

High

DE

Low

EN High EN Low DE

High

DE

Low

0.053 0.008 2.277 1.121 0.000 0.000 0.001 0.000 62.118 44.797 121.283 109.944

115

Adult 13 – SLMEM 282

Elemental Concentrations

Isotopic Composition

0.01

0.1

1

10

100

1000

2499 2549 2599 2649 2699 2749

pp

m

Time (sec)

Sr

Th

U

0.711

0.712

0.713

0.714

0.715

0.716

0.717

0.718

1 3 5 7 9 11 13 15

87 S

r/8

6 Sr

Spot Number

Average 87

Sr/86

Sr ratios *

Enamel Dentine 87

Sr/86

Sr 2se 87

Sr/86

Sr 2se

0.716824 0.000586 0.712492 0.000335

*From selected zones, avoiding areas

affected by diagenesis areas where possible

Elemental Concentrations – High and low zones 238

U Concentration (ppm) 232

Th Concentration (ppm) 88

Sr Concentration (ppm)

EN

High

EN

Low

DE

High

DE

Low

EN

High

EN

Low

DE

High

DE

Low

EN High EN Low DE

High

DE

Low

0.104 0.012 9.681 0.362 0.000 0.000 0.000 0.000 83.294 68.825 92.923 85.472

116

Adult 14 – SLMEM 298

Elemental Concentrations

Isotopic Composition

0.01

0.1

1

10

100

1000

974 1074 1174 1274 1374

pp

m

Time (sec)

Sr

Th

U

0.71

0.711

0.712

0.713

0.714

0.715

0.716

0.717

1 6 11 16 21

87Sr

/86 S

r

Spot Number

Average 87

Sr/86

Sr ratios *

Enamel Dentine 87

Sr/86

Sr 2se 87

Sr/86

Sr 2se

0.716146 0.000426 0.711886 0.000315

*From selected zones, avoiding areas

affected by diagenesis areas where possible

Elemental Concentrations – High and low zones 238

U Concentration (ppm) 232

Th Concentration (ppm) 88

Sr Concentration (ppm)

EN

High

EN

Low

DE

High

DE

Low

EN

High

EN

Low

DE

High

DE

Low

EN High EN Low DE

High

DE

Low

0.011 0.001 1.453 0.272 0.004 0.001 0.006 0.002 59.970 58.974 112.829 105.660

117

Adult 15 – SLMEM 1157

Elemental Concentrations

Isotopic Composition

0.01

0.1

1

10

100

1000

1974 2024 2074 2124 2174

pp

m

Time (sec)

Sr

Th

U

0.71

0.712

0.714

0.716

0.718

0.72

0.722

0.724

1 2 3 4 5 6 7 8 9 10

87 S

r/8

6 Sr

Spot Number

Average 87

Sr/86

Sr ratios *

Enamel Dentine 87

Sr/86

Sr 2se 87

Sr/86

Sr 2se

0.721258 0.000884 0.711865 0.000318

*From selected zones, avoiding areas

affected by diagenesis areas where possible

Elemental Concentrations – High and low zones 238

U Concentration (ppm) 232

Th Concentration (ppm) 88

Sr Concentration (ppm)

EN

High

EN

Low

DE

High

DE

Low

EN

High

EN

Low

DE

High

DE

Low

EN High EN Low DE

High

DE

Low

0.064 0.001 1.646 0.124 0.005 0.000 0.004 0.001 46.007 29.045 110.112 95.969

118

Adult 16 – SLMEM 5

Elemental Concentrations

Isotopic Composition

0.01

0.1

1

10

100

1000

2729 2779 2829 2879 2929

pp

m

Time (sec)

Sr

Th

U

0.71

0.712

0.714

0.716

0.718

0.72

0.722

1 3 5 7 9 11

87 S

r/8

6 Sr

Spot Number

Average 87

Sr/86

Sr ratios *

Enamel Dentine 87

Sr/86

Sr 2se 87

Sr/86

Sr 2se

0.720057 0.000561 0.711821 0.000297

*From selected zones, avoiding areas

affected by diagenesis areas where possible

Elemental Concentrations – High and low zones 238

U Concentration (ppm) 232

Th Concentration (ppm) 88

Sr Concentration (ppm)

EN

High

EN

Low

DE

High

DE

Low

EN

High

EN

Low

DE

High

DE

Low

EN High EN Low DE

High

DE

Low

- 0.001 2.500 0.127 - 0.001 0.002 0.002 - 53.523 126.699 108.654

119

Juvenile 1 – SLMEM 1192

Elemental Concentrations

Isotopic Composition

0.01

0.1

1

10

100

1000

1882 1902 1922 1942 1962 1982 2002

pp

m

Time (sec)

Sr

Th

U

0.71

0.712

0.714

0.716

0.718

0.72

0.722

1 2 3 4 5 6 7

87 S

r/8

6 Sr

Spot Number

Average 87

Sr/86

Sr ratios *

Enamel Dentine 87

Sr/86

Sr 2se 87

Sr/86

Sr 2se

0.719712 0.000666 0.711505 0.000351

*From selected zones, avoiding areas

affected by diagenesis areas where possible

Elemental Concentrations – High and low zones 238

U Concentration (ppm) 232

Th Concentration (ppm) 88

Sr Concentration (ppm)

EN

High

EN

Low

DE

High

DE

Low

EN

High

EN

Low

DE

High

DE

Low

EN High EN Low DE

High

DE

Low

18.543 4.386 7.159 5.625 1.192 0.032 8.011 0.030 179.852 136.615 391.951 125.713

120

Juvenile 2 – SLMEM 1251

Elemental Concentrations

Isotopic Composition

0.01

0.1

1

10

100

1000

2568 2588 2608 2628 2648

pp

m

Time (sec)

Sr

Th

U

0.71

0.711

0.712

0.713

0.714

0.715

0.716

1 2 3 4 5 6

87 S

r/8

6 Sr

Spot Number

Average 87

Sr/86

Sr ratios *

Enamel Dentine 87

Sr/86

Sr 2se 87

Sr/86

Sr 2se

0.715088 0.000387 0.710640 0.000309

*From selected zones, avoiding areas

affected by diagenesis areas where possible

Elemental Concentrations – High and low zones 238

U Concentration (ppm) 232

Th Concentration (ppm) 88

Sr Concentration (ppm)

EN

High

EN

Low

DE

High

DE

Low

EN

High

EN

Low

DE

High

DE

Low

EN High EN Low DE

High

DE

Low

0.496 0.163 2.366 0.406 0.097 0.003 0.000 0.001 106.695 97.210 185.827 144.722

121

Juvenile 3 – SLMEM 276

Elemental Concentrations

Isotopic Composition

0.01

0.1

1

10

100

1000

1946 1956 1966 1976 1986 1996 2006

pp

m

Time (sec)

Sr

Th

U

0.71

0.712

0.714

0.716

0.718

0.72

0.722

0.724

1 2 3 4 5 6

87 S

r/8

6 Sr

Spot Number

Average 87

Sr/86

Sr ratios *

Enamel Dentine 87

Sr/86

Sr 2se 87

Sr/86

Sr 2se

0.723010 0.000777 0.711027 0.000277

*From selected zones, avoiding areas

affected by diagenesis areas where possible

Elemental Concentrations – High and low zones 238

U Concentration (ppm) 232

Th Concentration (ppm) 88

Sr Concentration (ppm)

EN

High

EN

Low

DE

High

DE

Low

EN

High

EN

Low

DE

High

DE

Low

EN High EN Low DE

High

DE

Low

0.461 0.294 43.138 28.465 0.125 0.003 0.002 0.019 56.091 50.915 190.385 142.930

122

Juvenile 4 – SLMEM 66

Elemental Concentrations

Isotopic Composition

0.01

0.1

1

10

100

1000

1220 1270 1320 1370

pp

m

Time (sec)

Sr

Th

U

0.71

0.712

0.714

0.716

0.718

0.72

0.722

1 2 3 4 5 6 7 8 9

87 S

r/8

6 Sr

Spot Number

Average 87

Sr/86

Sr ratios *

Enamel Dentine 87

Sr/86

Sr 2se 87

Sr/86

Sr 2se

0.719776 0.000753 0.711141 0.000309

*From selected zones, avoiding areas

affected by diagenesis areas where possible

Elemental Concentrations – High and low zones 238

U Concentration (ppm) 232

Th Concentration (ppm) 88

Sr Concentration (ppm)

EN

High

EN

Low

DE

High

DE

Low

EN

High

EN

Low

DE

High

DE

Low

EN High EN Low DE

High

DE

Low

0.097 0.011 5.164 0.296 0.041 0.001 0.001 0.015 55.134 51.638 146.413 106.258

123

Juvenile 5 – SLMEM 102

Elemental Concentrations

Isotopic Composition

0.01

0.1

1

10

100

1000

562 582 602 622 642 662

pp

m

Time (sec)

Sr

Th

U

0.711

0.7115

0.712

0.7125

0.713

0.7135

0.714

0.7145

0.715

1 2 3 4 5 6 7 8

87 S

r/8

6 Sr

Spot Number

Average 87

Sr/86

Sr ratios *

Enamel Dentine 87

Sr/86

Sr 2se 87

Sr/86

Sr 2se

0.714607 0.000593 0.711664 0.000301

*From selected zones, avoiding areas

affected by diagenesis areas where possible

Elemental Concentrations – High and low zones 238

U Concentration (ppm) 232

Th Concentration (ppm) 88

Sr Concentration (ppm)

EN

High

EN

Low

DE

High

DE

Low

EN

High

EN

Low

DE

High

DE

Low

EN High EN Low DE

High

DE

Low

0.545 0.354 23.722 17.714 0.025 0.004 0.020 0.008 68.776 66.929 147.171 144.415

124

Juvenile 6 – SLMEM 119

Elemental Concentrations

Isotopic Composition

0.01

0.1

1

10

100

1000

2562 2582 2602 2622 2642 2662

pp

m

Time (sec)

Sr

Th

U

0.71

0.712

0.714

0.716

0.718

0.72

1 2 3 4 5 6 7

87 S

r/8

6 Sr

Spot Number

Average 87

Sr/86

Sr ratios *

Enamel Dentine 87

Sr/86

Sr 2se 87

Sr/86

Sr 2se

0.719197 0.000555 0.711825 0.000301

*From selected zones, avoiding areas

affected by diagenesis areas where possible

Elemental Concentrations – High and low zones 238

U Concentration (ppm) 232

Th Concentration (ppm) 88

Sr Concentration (ppm)

EN

High

EN

Low

DE

High

DE

Low

EN

High

EN

Low

DE

High

DE

Low

EN High EN Low DE

High

DE

Low

- 0.717 20.225 17.848 - 0.005 0.019 0.008 - 64.810 140.582 134.989

125

Juvenile 7 – SLMEM 86

Elemental Concentrations

Isotopic Composition

0.01

0.1

1

10

100

1000

1225 1245 1265 1285 1305 1325

pp

m

Time (sec)

Sr

Th

U

0.71

0.712

0.714

0.716

0.718

0.72

0.722

1 2 3 4 5 6 7

87Sr

/86 S

r

Spot Number

Average 87

Sr/86

Sr ratios *

Enamel Dentine 87

Sr/86

Sr 2se 87

Sr/86

Sr 2se

0.719931 0.000486 0.711542 0.000281

*From selected zones, avoiding areas

affected by diagenesis areas where possible

Elemental Concentrations – High and low zones 238

U Concentration (ppm) 232

Th Concentration (ppm) 88

Sr Concentration (ppm)

EN

High

EN

Low

DE

High

DE

Low

EN

High

EN

Low

DE

High

DE

Low

EN High EN Low DE

High

DE

Low

5.251 0.221 12.593 7.602 0.019 0.002 0.038 0.011 132.823 64.493 139.181 134.664

126

Juvenile 8 – SLMEM 291

Elemental Concentrations

Isotopic Composition

0.01

0.1

1

10

100

1000

558 578 598 618 638 658

pp

m

Time (sec)

Sr

Th

U

0.71

0.711

0.712

0.713

0.714

0.715

0.716

0.717

0.718

0.719

1 2 3 4 5 6 7

87 S

r/8

6 Sr

Spot Number

Average 87

Sr/86

Sr ratios *

Enamel Dentine 87

Sr/86

Sr 2se 87

Sr/86

Sr 2se

0.718307 0.000488 0.711095 0.000289

*From selected zones, avoiding areas

affected by diagenesis areas where possible

Elemental Concentrations – High and low zones 238

U Concentration (ppm) 232

Th Concentration (ppm) 88

Sr Concentration (ppm)

EN

High

EN

Low

DE

High

DE

Low

EN

High

EN

Low

DE

High

DE

Low

EN High EN Low DE

High

DE

Low

2.815 1.628 28.328 - 0.013 0.002 0.021 - 78.798 64.271 147.678 -